Dissertation

|6.2 Synthesis of the Metal Complexes|
1H (CH3 ”-bpy)), 1.36 (s, 1H (CH3 ”’-bpy)) ppm.
Crystals suitable for X-ray diffraction were
obtained from diethyl ether/chloroform.
Crystal
data for Ru(Br 2 bip): [C 56 H 60 N 8 Br 2 Ru]Cl 2
× 3.5 CHCl 3 × C 2 H 5 OC 2 H 5 ,
M r = 1668.82 g /mol, red-brown cuboid, size
0.46 × 0.30 × 0.24 mm 3 , monoclinic, space
group C2/c (No. 15), a = 28.494(2),
b = 16.7022(14), c = 30.867(3) Å, α =
90.000, β = 96.8970(10), γ = 90.000°, V
= 14583(2) Å 3 , T = 100K, Z = 8, ρ calcd. =
1.520 g /cm 3 , µ (Mo-Kα) = 1.815 cm -1 , F(000) =
6760, 65649 reflections in h(-34/32), k(-20/19), l(-37/37) measured in the range 2.07° ≤ Θ ≤ 25.35°,
completeness Φ max = 99.4%, 13274 independent reflections, R int = 0.0420, 13274 reflections with
F o > 4σ(F o ), 1014 parameters, 393 restraints, R obs. = 0.0711, wR 2 obs.
= 0.1853, R all = 0.1019, wR 2 all =
0.2087 , GOOF = 1.087 , largest difference peak and hole: 2.106 / -1.586 e /Å 3 . The data file dp1004
includes the full crystallographic data and can be obtained from Dr. Frank Heinemann (IAC,
FAU-Erlangen-Nürnberg).
6.2.23 [Ru(tbbpy) 2 (eip)][PF 6 ] 2 - Ru(eip)
The title compound was obtained, following method C1. 104 mg (146 µmol) of [Ru(tbbpy) 2 Cl 2 ]
and 36.4 mg (146 µmol) of eip were reacted in the microwave for 90 minutes in 50 ml of
ethanol/water. After cooling and removal of ethanol and a dark precipitate 142 mg (870 µmol) of
NH 4 PF 6 were added. The formed precipitate was collected and washed with water several times.
Purification was achieved by recrystallization from acetone/ethanol/water by slow evaporation.
After removal of water the pure Ru(eip) was obtained as red powder. The yield was 155 mg
(132 µmol, 90%).
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