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Crystal Structure of bis(O,O′-neopentylene dithiophosphato)nickel(II) Ni[S2 \(\kern2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise14pt\hbox{\vrule height.5pt width145pt depth0pt}\hspace*{-147pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 and bis(O,O′-hexylene dithiophosphato)nickel(II) Ni[S2 \(\kern2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise14pt\hbox{\vrule height.5pt width164pt depth0pt}\hspace*{-166pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2

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Purple crystals of bis(O,O′-neopentylene dithiophosphato)nickel(II), Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width74pt depth0pt}\hspace*{-76pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 and bis(O,O′-hexylene dithiophosphato)nickel(II), Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width83.5pt depth0pt}\hspace*{-85pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 were obtained by layering benzene solutions of the complexes with ether and maintaining the samples at room temperature. The molecular structures of Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width74pt depth0pt}\hspace*{-76pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 and Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width84pt depth0pt}\hspace*{-85pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 were determined by single-crystal X-ray diffraction. Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width74pt depth0pt}\hspace*{-76pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 crystallizes as monoclinic in the space group P21/c with cell parameters a = 7.051(2) Å, b = 6.453(2) Å, c = 19.686(6) Å, β = 99.45(3)°, V = 883.6(5) Å−3, Z = 2, R = 0.0251, R w = 0.0599. Ni[S2 \(\kern2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise10pt\hbox{\vrule height.5pt width84pt depth0pt}\hspace*{-85pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise7pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 crystallizes as triclinic in the space group P-1 with cell parameters a = 8.394(5) Å, b = 11.070(5) Å, c = 12.124(5) Å, α = 71.287(5)°, β = 76.227(5)°, γ = 88.319(5)°, V = 1035.0(9) Å−3, Z = 2, R = 0.0655, R w = 0.1545. In both complexes the environment around nickel is distorted square planar.

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Acknowledgments

One of us (M.N.) is grateful to CSIR, New Delhi for financial support. M.B.H. Thanks to the UK Engineering and Physical Sciences Council for support of the X-ray facilities at Southampton University. J.E.D. thanks the University of Windsor for financial support.

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Authors and Affiliations

  1. Department of Chemistry, University of Southampton, Highfield, Southampton, Hampshire, United Kingdom

    A. L. Bingham, M. B. Hursthouse & M. E. Light

  2. Department of Chemistry and Biochemistry, University of Windsor, Windsor, Ontario, Canada

    J. E. Drake

  3. Department of Pure and Applied Chemistry, M.D.S. University, Ajmer, India

    K. Saraswat, M. Nirwan & R. Ratnani

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  1. A. L. Bingham
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Correspondence to R. Ratnani.

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Supplementary material

Additional material available from the Cambridge Crystallographic Data Centre (CCDC nos. 265694-265695) comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email:deposit@ccdc.cam.ac.uk or www: http://www.ccdc.cam.ac.uk).

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Bingham, A.L., Drake, J.E., Saraswat, K. et al. Crystal Structure of bis(O,O′-neopentylene dithiophosphato)nickel(II) Ni[S2 \(\kern2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise14pt\hbox{\vrule height.5pt width145pt depth0pt}\hspace*{-147pt}{\rm POCH}_2{\rm CMe}_2{\rm CH}_2{\rm O}\kern-4.2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 and bis(O,O′-hexylene dithiophosphato)nickel(II) Ni[S2 \(\kern2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt}\kern-.5pt\raise14pt\hbox{\vrule height.5pt width164pt depth0pt}\hspace*{-166pt}{\rm POCMe}_2{\rm CH}_2{\rm CHMeO}\kern-4.2pt\raise12pt\hbox{\vrule height3pt width.5pt depth0pt\kern3pt}]\) 2 . J Chem Crystallogr 36, 249–254 (2006). https://doi.org/10.1007/s10870-005-9007-y

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