COMMUNICATIONS
S. S. M. Ling, M. A. Thomson, R. J. Puddephatt, Organometallics
1984, 3, 1637.
Experimental Section
[7] T. E. Muller, J. C. Green, D. M. P. Mingos, C. M. McPartlin, C.
Whittingham, D. J. Williams, T. M. Woodroffe, J. Organomet. Chem.
1998, 551, 313.
All syntheses were carried out using standard Schlenck techniques.
Solvents used for spectroscopic measurements were purified according to
the literature methods.
[8] Crystallographic data of 1 ´ 0.5Et2O: C116H89Au3Cl3O12.5P6, fw
2565.94, monoclinic space group P21, a 16.5060(3), b 22.1432(3)
c 16.6942(2) , a g 908, b 100.907(1)8, V 5991.4(2) 3,
Synthesis of 9,10-bis(diphenylphosphino)anthracene (PAnP): nBuLi
(12 mmol) was added to a suspension of 9,10-dibromoanthracene (2.0 g,
6 mmol) in Et2O (100 mL). The solution was stirred for 10 min before
addition of PPh2Cl (3.2 mL, 12 mmol). The suspension was stirred for 12 h,
collected by filtration, and the yellow solid thus obtained washed with
diethyl ether. Crystals were obtained from CH2Cl2/Et2O by slow diffusion,
yield 75%; elemental analysis calcd (%) for C38H28P2: C 83.5, H 5.0; found:
1calcd 1.422 gcm 3, Z 2, m(MoKa) 0.71073 , T 223 K, 2q
w
scan, absorption coefficient 3.865 mm 1, a total of 30295 unique
data with 19001 reflections having I > 2s(I) were collected. Index
range: 17 ꢁ h ꢁ 19, 23 ꢁ k ꢁ 26, 19 ꢁ l ꢁ 14. Refinement of F 2
converged with R1 0.0591 and wR2 0.1048. The diffraction experi-
ments were carried out on a Bruker AXS SMART CCD 3-circle
diffractometer with a MoKa sealed tube. The software used was:
SMART for collecting frames of data, indexing reflection, and
determination of lattice parameters; SAINT for integration of
intensity of reflections and scaling; SADABS for empirical absorption
correction; and SHELXTL for space group determination, structure
1
C 83.4, H 5.1, H NMR (CD2Cl2, 300 MHz): d 7.23 (m, 4H, H2,3,6,7, An),
7.25 ± 7.43 (m, 20H, Ph), 8.85 (m, 4H, H1,4,5,8, An). 31P{1H} NMR (CDCl3,
300 MHz): d 21.9; m.p. 2608C (decomp).
1:
A methanol suspension (50 mL) of PAnP (1.0 g, 1.8 mmol) and
Me2SAuCl (0.53 g, 1.8 mmol) was heated at reflux for 4 days, insoluble
material was then removed by filtration. Excess LiClO4 was added to the
yellow filtrate and the resulting yellow solid was crystallized from CH3CN/
Et2O at 208C, yield 40%, elemental analysis calcd (%) for C114H84Au3-
Cl3O12P6: C 54.1, H 3.4, P 7.4; found: C 54.3, H 3.5, P 7.3; m.p. 1248C
(decomp); for NMR data, see text.
2
solution, and least-squares refinements on jF j . The residual electron
density is 1.000 and 0.612 e 3. Crystallographic data (excluding
structure factors) for the structures reported in this paper have been
deposited with the Cambridge Crystallographic Data Centre as
supplementary publication no. CCDC-158656 (1) and CCDC-158657
(PAnP). Copies of the data can be obtained free of charge on
application to CCDC, 12 Union Road, Cambridge CB21EZ, UK (fax:
(44)1223-336-033; e-mail: deposit@ccdc.cam.ac.uk).
Physical measurements: The UV/Vis absorption and emission spectra of
the complexes were recorded on a Hewlett-Packard HP8452A diode array
spectrophotometer and a Perkin-Elmer LS-50D fluorescence spectropho-
tometer, respectively. Anthracene was used as a standard in measuring the
quantum yield of emission. 1H and 31P{1H} NMR spectra were recorded at
258C on either a Bruker ACF 300 spectrometer or a Bruker AMX500
spectrometer. All chemical shifts are quoted relative to SiMe4 (1H) or
H3PO4 (31P). Variable temperature spectra were obtained by using a Bruker
variable temperature unit B-VT2000 to control the probe temperature. The
sample temperature is considered to be accurate to Æ18C. 1H 2D-EXSY
and COSY spectra were obtained using standard NOESYPH.AU (mixing
time of 0.5 s) and COSY-AU programs, respectively. Elemental analyses of
the complexes were carried out in the microanalysis laboratory in the
department of chemistry, the National University of Singapore.
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Received: January 12, 2001 [Z16413]
1
1
1
1
[14] The coupling constants are: J1,2 10, J2,3 18, J3,4 10, JA,B 18,
2JA,C 7, 1JB,C 10, JD,E 14 Hz.
1
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