Novel tridentate chiral-NHC ligand precursor 167
13C NMR: δ 23.4 (CH2), 27.9 (CH2), 49.8 (CH2), 51.0 (CH2), 54.5
(CH2), 59.7 (CH), 61.2 (CH2), 127.2 (CH), 128.5 (CH), 128.9 (CH),
139.2 (C), 158.0 (CH). Anal. calcd for C27H37F6N4P: C, 57.64; H, 6.63;
N, 9.96. Found: C, 57.28; H, 6.32; N, 10.19%.
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X-Ray crystallographic analysis of 5
The crystal for the solid state structure of compound 5 was obtained
by slow diffusion of ether into THF solution. Preliminary examina-
tion and data collection were carried out on a Rigaku Mercury CCD
device at the window of a sealed X-ray tube with graphite-mono-
chromated Mo Kα radiation (λ=0.71073 Å). Absorption correction
was performed by the SADABS program. The structure was solved
by directed methods using the SHELXS-97 program and refined by
full-matrix least squares techniques on F2. The single-crystal of 5 is
monoclinic, space group P2(1) with a=6.0816(12) Å, b=32.899(7)
Å, c=14.360(3) Å, α=90°, β=90.56(3)°, γ=90°, Mr=2250.30,
V=2873.0(10) Å3. The formula is C108H148F24N16P4, Z=1, µ (Mo
Kα)=0.157 mm-1, -7≤h≤7, -39≤k≤39, -17≤l≤17, total number of re-
flection=9845, number of independent reflections=5254, R=0.0538,
the largest difference peak and hole of electron density are 0.178 and
-0.145 Å-3, respectively. Selected bond lengths (Å) and angles (°):
N(1)-C(1) 1.275(5), N(1)-C(2) 1.453(5), N(1)-C(4) 1.448(5), N(2)-
C(1) 1.316(5), N(2)-C(3) 1.464(5), N(2)-C(16) 1.446(6), C(2)-C(3)
1.534(6), C(4)-C(5) 1.519(5), C(16)-C(17) 1.505(6), N(1)-C(1)-
N(2) 115.6(4), C(1)-N(1)-C(4) 125.1(4), C(1)-N(1)-C(2) 109.5(3),
C(2)-N(1)-C(4) 125.4(3), C(1)-N(2)-C(16) 125.8(4), C(1)-N(2)-
C(3) 108.7(3), C(3)-N(2)-C(16) 124.9(4), N(1)-C(2)-C(3) 103.7(3),
N(2)-C(3)-C(2) 102.4(3), C(4)-C(5)-C(6) 114.1(4), C(4)-C(5)-N(3)
109.0(3), C(16)-C(17)-C(18) 115.1(4), C(16)-C(17)-N(4) 112.3(4).
CCDC-825945 contains the supplementary crystallographic data
for this paper. These data can be obtained free of charge from the
data_request/cif.
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Acknowledgments
Weskamp, T.; Schattenmann, W. C.; Spiegler, M.; Herrmann, W.
A. A. Novel class of ruthenium catalysts for olefin metathesis.
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We are grateful to the foundation of the Qing Lan Project (08QLT001
and 08QLD006) of the Jiangsu Education Committee, SRF for
ROCS, SEM, NSFC (21071121, 21172188 and 21104064), PAPD
and the State Key Laboratory of Inorganic Synthesis and Preparative
Chemistry at Jilin University (2009-06) for financial support.
References
Alcon, M. J.; Gutierrez-Puebla, E.; Iglesias, M.; Monge, M. A.;
Sanchez, F. Copper complexes with multidentate ligands derived
Received August 20, 2011; accepted October 23, 2011; previously
published online November 29, 2011
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