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tained as a dark solid. Yield: 87%. Mp 238–240 °C. C29H22NiOP2S4:
calcd. C 54.82; H 3.49%; found: C 54.67; H 3.60%. IR (KBr): ν(C=O)
1
1623 (m) cm–1. H NMR (400 MHz, DMSO): δ = 7.56–8.04 (m, 22
H, 4C6H5, CH=CH) ppm. 13C NMR (100.6 MHz, DMSO): δ = 123.53,
123.62, 129.65, 129.88, 130.07, 130.27, 132.25, 133.33 (C6H5,
S2C=CS2), 147.41 (PCH=CHP), 198.98 (C=O) ppm. 31P NMR
(162 MHz, DMSO, 85% H3PO4): δ = 69.44 (s) ppm.
(dppb)Ni(dmio) (4): The same procedure as that for 2 was followed,
but (PhCO)2(dmio) (0.195 g, 0.5 mmol) was used in place of
(PhCO)2(dmit). From the main band, complex 4 (0.285 g) was ob-
tained as a dark solid. Yield: 83%. Mp 281–283 °C. C33H24NiOP2S4:
calcd. C 57.82; H 3.53%; found: C 57.65; H 3.80%. IR (KBr): ν(C=O)
1615 (m) cm–1. 1H NMR (400 MHz, CDCl3): δ = 7.36–7.64 (m, 24
H, 4C6H5, C6H4) ppm. 13C NMR (100.6 MHz, CDCl3): δ = 124.37,
124.45, 128.70, 128.79, 131.40, 132.57, 133.08, 133.71, 142.18 (C6H5,
C6H4, S2C=CS2), 201.07 (C=O) ppm. 31P NMR (162 MHz, CDCl3,
85% H3PO4): δ = 58.73 (s) ppm.
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X-ray Crystallographic Analysis: The single crystals of 1, 3, and 4
suitable for X-ray diffraction analyses were grown by slow evaporation
of the CH2Cl2/n-hexane solutions at about –20 °C. The single crystals
were mounted on a Rigaku MM-007 (rotating anode) diffractometer
equipped with Saturn 70CCD. Data were collected at 293 K by using
a graphite monochromator with Mo-Kα radiation (λ = 0.71073) in the
ω-φ scanning mode. Absorption correction was performed by the
CRYSTALCLEAR program.[25] The structure was solved by direct
methods using the SHELXS-97 program[26] and refined by full-matrix
least-squares techniques (SHELXL-97)[27] on F2. Hydrogen atoms
were located by using the geometric method. Details of crystal data,
data collections, and structure refinements are summarized in Table 2.
Crystallographic data (excluding structure factors) for the structures in
this paper have been deposited with the Cambridge Crystallographic
Data Centre, CCDC, 12 Union Road, Cambridge CB21EZ, UK. Copies
of the data can be obtained free of charge on quoting the depository
numbers CCDC-914956, CCDC-907972, and CCDC-918231 (for 1,
3, and 4) (Fax: +44-1223-336-033; E-Mail: deposit@ccdc.cam.ac.uk,
http://www.ccdc.cam.ac.uk)
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Acknowledgements
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Dalton Trans. 1984, 459–467.
We are grateful to Sichuan Science and Technology Department
(2012JY0115, 2011JY0052, 2010GZ0130) and Sichuan University of
Science & Engineering (2011RC06, 2012PY04, 2012PY14) for finan-
cial support.
[25] Crystalclear and Crystalstructure, Rigaku and Rigaku Americas.
9009 New Trails Dr. The Woodlands TX 77381 USA.
[26] G. M. Sheldrick, SHELXS97, A Program for Crystal Structure
Solution; University of Göttingen: Germany, 1997.
[27] G. M. Sheldrick, SHELXL97, A Program for Crystal Structure Re-
finement; University of Göttingen: Germany, 1997.
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Received: March 31, 2013
Published Online: May 27, 2013
1790
© 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Z. Anorg. Allg. Chem. 2013, 1787–1790