23 J. R. Dilworth, S. A. Harrison, D. R. M. Walton and E. Schweda,
Inorg. Chem., 1985, 24, 2594.
24 H. Mohd and G. J. Leigh, J. Chem. Soc., Dalton Trans., 1986, 213.
25 T. Nicholson, P. Lombardi and J. Zubieta, Polyhedron, 1987, 6, 1577.
26 J. R. Dilworth, P. Jobanputra, S. J. Parrott, R. M. Thompson, D. C.
Povey and J. A. Zubieta, Polyhedron, 1992, 11, 147.
arrangement of the ligands. In an attempt to form mixed POx/
hydrazine complexes, 1 and 2 were reacted with a variety of
hydrazines under a wide range of conditions. The POx ligands
are clearly not suitable for this type of reaction since no prod-
ucts were isolated from these reactions.
The reaction of [Re(Hhypy)(hypyH)Cl3] with the PO ligand
in the presence of base afforded 3 and 4 as a mixture. The major
product of the reaction was the cationic 3. The neutral minor
product 4 was easily separated from the cationic 3 on silica gel.
Crystal structures were obtained for both complexes. Com-
pound 3 was found to have an N3OP2 coordination sphere
about a cationic Re() centre, 4 had an N3OPCl donor set
about a neutral Re() centre. The (ϩ)LSIMS, IR and NMR
data are consistent with the crystal structures of each. The same
reaction was extended to the H2PO2 and H2(Me2PO2) ligands to
27 J. R. Dilworth, P. Jobanputra, J. R. Miller, S. J. Parrott, Q. Chen and
J. Zubieta, Polyhedron, 1993, 12, 513.
28 M. T. A. Ribeiro, A. J. L. Pombeiro, J. R. Dilworth, Y. Zheng and
J. R. Miller, Inorg. Chim. Acta, 1993, 211, 131.
29 B. Coutinho, J. R. Dilworth, P. Jobanputra, R. M. Thompson,
S. Schmid, J. Strähle and C. M. Archer, J. Chem. Soc., Dalton Trans.,
1995, 1663.
30 M. Hirsch-Kuchma, T. Nicholson, A. Davison, W. M. Davis and
A. G. Jones, J. Chem. Soc., Dalton Trans., 1997, 3185.
31 M. Hirsch-Kuchma, T. Nicholson, A. Davison and A. G. Jones,
J. Chem. Soc., Dalton Trans., 1997, 3189.
32 M. T. A. R. S. da Costa, J. R. Dilworth, M. T. Duarte, J. J. R.
Fraústo da Silva, A. M. Galvão and A. J. L. Pombeiro, J. Chem.
Soc., Dalton Trans., 1998, 2405.
33 I. Chakraborty, S. Bhattacharyya, S. Banerjee, B. K. Dirghangi and
A. Chakravorty, J. Chem. Soc., Dalton Trans., 1999, 3747.
34 G. Albertin, S. Antoniutti, A. Bacchi, G. B. Ballico, E. Bordignon,
G. Pelizzi, M. Ranieri and P. Ugo, Inorg. Chem., 2000, 39, 3265.
35 G. Albertin, S. Antoniutti, A. Bacchi, E. Bordignon, F. Miani and
G. Pelizzi, Inorg. Chem., 2000, 39, 3283.
1
obtain 5 and 6 respectively as the major products. H and 31P
NMR spectral evidence shows these products to have the same
structure in solution as the structurally characterised 3. Three
of the four phenolic arms remain protonated and uncoordin-
ated in 6. Clearly, the mismatched donor sets of PO2 and
Me2PO2 would be unfavourable from a clinical standpoint.
36 S. Banerjee, S. Bhattacharyya, B. K. Dirghangi, M. Menon and
A. Chakravorty, Inorg. Chem., 2000, 39, 6.
Acknowledgements
37 F. J. Femia, X. Chen, K. P. Maresca, J. W. Babich and J. Zubieta,
Inorg. Chim. Acta, 2000, 307, 160.
38 S. Liu, D. S. Edwards, A. R. Harris and P. R. Singh, Appl. Radiat.
Isot., 1997, 48, 1103.
We thank the Natural Sciences and Engineering Research
Council (NSERC) of Canada and DuPont Pharmaceuticals,
Inc. for financial support.
39 P. Pérez-Lourido, J. Romero, J. A. García-Vázquez, A. Sousa, K. P.
Maresca and J. Zubieta, Inorg. Chem., 1999, 38, 1511.
40 D. J. Rose, K. P. Maresca, T. Nicholson, A. Davison, A. G. Jones,
J. Babich, A. Fischman, W. Graham, J. R. D. DeBord and J. Zubieta,
Inorg. Chem., 1998, 37, 2701.
41 T. Nicholson, J. Cook, A. Davison, D. J. Rose, K. P. Maresca, J. A.
Zubieta and A. G. Jones, Inorg. Chim. Acta, 1996, 252, 421.
42 H. Luo, I. Setyawati, S. J. Rettig and C. Orvig, Inorg. Chem., 1995,
34, 2287.
43 C. Bolzati, F. Tisato, F. Refosco, G. Bandoli and A. Dolmella, Inorg.
Chem., 1996, 35, 6221.
44 F. Loiseau, F. Connac, Y. Lucchese, M. Dartiguenave, S. Fortin,
A. L. Beauchamp and Y. Coulais, Inorg. Chim. Acta, 2000, 306, 94.
45 F. Loiseau, Y. Lucchese, M. Dartiguenave and Y. Coulais,
Polyhedron, 2000, 19, 1111.
References
1 E. Deutsch, K. Libson, S. Jurisson and L. F. Lindoy, Prog. Inorg.
Chem., 1983, 30, 75.
2 M. Clarke and L. Podbielski, Coord. Chem. Rev., 1987, 78, 253.
3 S. Jurisson, C. P. Desilets, W. Jia and D. Ma, Chem. Rev., 1993, 93,
1137.
4 F. Tisato, F. Refosco and G. Bandoli, Coord. Chem. Rev., 1994, 135,
235.
5 J. R. Dilworth and S. J. Parrott, Chem. Soc. Rev., 1998, 27, 43.
6 W. A. Volkert and T. J. Hoffman, Chem. Rev., 1999, 99, 2269.
7 S. S. Jurisson and J. D. Lydon, Chem. Rev., 1999, 99, 2205.
8 M. J. Abrams, M. Juweid, C. I. tenKate, D. A. Schwartz, M. M.
Hauser, F. E. Gaul, A. J. Fuccello, R. H. Rubin, H. W. Strauss and
A. J. Fischman, J. Nucl. Med., 1990, 31, 2022.
9 D. S. Edwards and S. Liu, Transition Met. Chem., 1997, 22, 425.
10 D. S. Edwards, S. Liu, J. A. Barrett, A. R. Harris, R. J. Looby,
M. C. Ziegler, S. J. Heminway and T. R. Carroll, Bioconjugate Chem.,
1997, 8, 146.
46 F. Connac, Y. Lucchese, M. Gressier, M. Dartiguenave and A. L.
Beauchamp, Inorg. Chim. Acta, 2000, 304, 52.
47 T. B. Rauchfuss, Inorg. Chem., 1977, 16, 2966.
48 J. Chatt and G. A. Rowe, J. Chem. Soc., 1962, 4019.
49 D. D. Perrin, W. L. F. Armarego and D. R. Perrin, Purification of
Laboratory Chemicals, Pergamon Press, Oxford, 1980.
50 J. P. Yardley and H. Fletcher, Synthesis, 1975, 244.
51 P. T. Beurskens, G. Admiraal, W. P. Beurskens, S. Garcia-Granda,
R. O. Gould, J. M. M. Smits and C. Smykalla, The DIRDIF
program system, University of Nijmegen, The Netherlands, 1992.
52 A. Altomare, M. C. Burla, G. Camalli, M. Cascarano,
C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori and
A. Spagna, J. Appl. Crystallogr., 1999, 32, 115.
11 S. Liu, D. S. Edwards and J. A. Barrett, Bioconjugate Chem., 1997, 8,
621.
12 J. A. Barrett, A. C. Crocker, D. J. Damphousse, S. J. Heminway,
S. Liu, D. S. Edwards, J. L. Lazewatsky, M. Kagan, T. J. Mazaika
and T. R. Carroll, Bioconjugate Chem., 1997, 8, 155.
13 S. Liu, D. S. Edwards, R. J. Looby, A. R. Harris, M. J. Poirier, J. A.
Barrett, S. J. Heminway and T. R. Carroll, Bioconjugate Chem.,
1996, 7, 63.
14 D. A. Schwartz, M. J. Abrams, M. M. Hauser, F. E. Gaul, S. K.
Larsen, D. Rauh and J. A. Zubieta, Bioconjugate Chem., 1991, 2,
333.
15 S. K. Larsen, H. F. Solomon, G. Caldwell and M. J. Abrams,
Bioconjugate Chem., 1995, 6, 635.
16 M. Rajopadhye, T. D. Harris, K. Yu, D. Glowacka, P. R.
Damphousse, J. A. Barret, S. J. Heminway, D. S. Edwards and T. R.
Carroll, Bioorg. Med. Chem. Lett., 1997, 7, 955.
53 P. T. Beurskens, G. Admiraal, G. Beurskens, W. P. Bosman,
R. de Gelder, R. Israel and J. M. M. Smits, The DIRDIF-94
program system, University of Nijmegen, The Netherlands, 1994.
54 G. M. Sheldrick, in SHELXL-97, Program for Crystal Structure
Refinement, University of Göttingen, Germany, 1997.
55 A. L. Spek, Acta Crystallogr., Sect. A, 1990, 46, 34.
56 G. M. Sheldrick, in SHELX-76, Program for Crystal Structure
Determination, University of Cambridge, UK, 1976.
17 T. Nicholson, A. Mahmood, G. Morgan, A. G. Jones and
A. Davison, Inorg. Chim. Acta, 1991, 179, 53.
18 T. Nicholson and J. Zubieta, Polyhedron, 1988, 7, 171.
19 J. Chatt, J. R. Dilworth, G. L. Leigh and V. D. Gupta, J. Chem. Soc.
A, 1971, 2631.
20 V. F. Duckworth, P. G. Douglas, R. Mason and B. L. Shaw, Chem.
Commun., 1970, 1083.
21 R. Mason, K. M. Thomas, J. A. Zubieta, P. G. Douglas, A. R.
Galbraith and B. L. Shaw, J. Am. Chem. Soc., 1974, 96, 260.
22 P. G. Douglas, A. R. Galbraith and B. L. Shaw, Transition Met.
Chem., 1975/76, 1, 17.
57 G. M. Sheldrick, in SHELXS-86, Program for the Solution of
Crystal Structures, University of Göttingen, Germany, 1986.
58 F. H. Allen and O. Kennard, Chem. Des. Automat. News, 1993, 8, 31.
59 B. Nock, T. Maina, F. Tisato, M. Papadopoulos, C. P. Raptopoulou,
A. Terzis and E. Chiotellis, Inorg. Chem., 1999, 38, 4197.
60 B. Nock, T. Maina, F. Tisato, M. Papadopoulos, C. P. Raptopoulou,
A. Terzis and E. Chiotellis, Inorg. Chem., 2000, 39, 2178.
61 B. Nock, T. Maina, F. Tisato, C. P. Raptopoulou, A. Terzis and
E. Chiotellis, Inorg. Chem., 2000, 39, 5197.
62 C. K. Johnson, ORTEP, Report ORNL-5138, Oak Ridge National
Laboratory, Oak Ridge, TN, 1976.
3024
J. Chem. Soc., Dalton Trans., 2001, 3015–3024