R. Neumann et al.
FULL PAPER
obtained by a least-squares fit of 24 centered reflections in the range of
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Tateishi, M. Iwamoto, Chem. Lett. 1993, 1839; b) N. Mizuno, M.
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1
0 ꢁ q ꢁ 15. Intensity data were collected by the w À 2q method to a
maximum of 2q of 508. The scan width, Dw, for each reflection was
1
À1
.000.035tanq with a scan speed of 3.08 min . Background measure-
ments were made for a total of 10 s at both limits of each scan. Three
standard reflections were measured every 60 min and no systematic
variations were observed. Intensities were corrected for Lorentz, polar-
ization and absorption effects. All non-hydrogen atoms were found from
the results of the SHELXS-86 direct method analysis. The tungsten atoms
were refined on the assumption of a random substitution of one substituted
metal atom, and the electron densities were adjusted accordingly. Refine-
2
ment proceeded to convergence after Sw j F
0
jÀj F
c
j
was minimized. A
final difference Fourier synthesis map showed several peaks less than
.3 e scattered about the unit cell without significant feature. The
À3
2
discrepency indices are R S j jF
0
j À jF
c
j j/S j F
0
j and R
w
[Sw j F
0
j À jF
c
2
2 1/2
j /S j F
0
j ] . Further details of the crystal structure investigation may be
obtained from the Fachinformationszenstrum Karlsruhe, 76344 Eggen-
stein-Leopoldshafen, Germany (fax: (49)7247-808-666; e-mail: crysdata
[14] M. V. George in Organic Syntheses by Oxidation with Metal Com-
pounds (Eds.: W. J. Mijs, C. R. H. I. de Jonge), Plenum, New York,
@
fiz-karlsruhe.de) on quoting the depository number CSD-410811.
1
986, pp.373 ± 422.
Catalytic epoxidation reactions: Typically, epoxidation reactions were
carried out in 5-mL vials: the vial was loaded with catalyst (10 mmol)
dissolved in 1,2-dichloroethane (1 mL) and substrate (1 mmol). Hydrogen
peroxide (35% aqueous, 3 mmol) was added after the reaction temperature
was equilibrated. The reaction mixture was stirred magnetically and
aliquots were removed at the appropriate time intervals for analysis by gas
chromatography.
[
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Acknowledgements
This research was supported by the Basic Research Foundation adminis-
tered by the Israeli Academy of Science and Humanities.
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[
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6
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[
[
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[
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Received: February 7, 2000 [F2285]
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