1388
K. C. Potgieter, P. Mayer, and T. I. A. Gerber
was filtered off, washed with diethyl ether and dried under vac-
uum. Recrystallization from 1:2 (v/v) ethanol:dichloromethane
and the addition of NH4PF6 afforded dark brown crystals, suit-
able for X-ray analysis. Yield = 80%, mp >300◦C. νmax/cm−1
ν(C=N) 1610; ν(Re=O) 983; ν(P-F) 805; ν(Re-N) 495, 468.
λmax (MeOH)/nm (ε/M−1 cm−1) 364 (1150), 425 (1280). δH
(295 K) 13.12 (s, 2H, H(7), H(10)), 7.95 (s, 2H, 2NH), 7.71 (d,
2H, H(2), H(15)), 7.59 (t, 2H, H(4), H(13)), 7.18 (d, 2H, H(5),
H(12)), 6.83 (t, 4H, H(3), H(14)), 4.35 (t, 4H, 2CH2). Conduc-
tivity (CH3CN, 10−3 M) 133 −1 cm2 mol−1. Anal. Calc. for
C16H16N4ORePF6: C 32.27, H 2.71, N 9.41. Found: C 32.29,
H 2.69, N 9.50%.
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Synthesis of [ReO(dne)] (2) from [ReO4]− and Na2S2O4
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A mass of 100 mg of NH4[ReO4] (373 μmol) and 250 mg
of H2ane (939 μmol) were dissolved in 20 mL of a 1:1
water/ethanol mixture. Sodium dithionite (600 mg) and 2 mL of
a 1.0 M NaOH solution were added, and the mixture was heated
under reflux for 2 h, and then filtered while hot. The solvent
was reduced in volume under vacuum, and a brown precipi-
tate was collected by filtration. It was recrystallized from 1:2
(v/v) ethanol:dichloromethane. Yield = 38%, mp 148–151◦C.
Anal. Calc. for C16H17N4ORe: C 41.10, H 3.66, N 11.98.
Found: C 40.86, H 3.41, N 12.31%. This product has identi-
cal spectroscopic properties to the sample prepared above from
trans-[ReO2(py)4]Cl.
X-ray Diffraction
X-ray diffraction studies on crystals of 1, 2, and
3
were performed at 200(2) K using a Nonius Kappa CCD
diffractometer with graphite monochromated Mo Kα radiation
(λ = 0.71072 Å). The structures were solved by direct methods
and refined by least-squares procedures using SHELXL-97.[36]
All non-hydrogen atoms were refined anisotropically, and the
hydrogen atoms were calculated in idealized geometrical posi-
tions. Crystal and structure refinement data are given in Table 5.
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