A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni-3(II) complexes

Feldscher B, Theil H, Stammler A, Bögge H, Glaser T (2014)
Dalton Transactions 43(10): 4102-4114.

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Abstract
A protocol for the synthesis of trinucleating C3-symmetric ligands based on a central meta-phenylene bridging 1,3,5-trimercaptobenzene (thiophloroglucinol) backbone has been established. The key compound turned out to be the trialdehyde obtained from the triple nucleophilic attack of dimethyldithiocarbamate at 1,3,5-tribromo-2,4,6-triformylbenzene. Reacting this trialdehyde with six equivalents of a primary amine results in the simultaneous dithiocarbamate cleavage and Schiff-base formation providing the extended thiophloroglucinol ligands H(3)bertdien, H(6)bert(Me), H(6)bert(t-Bu2), and H(6)habbi. Reaction with NiII leads to the formation of the trinuclear Ni-3(II) complexes [(bertdien) Ni-3(II)](X)(3) (X = BPh4-, BF4-), [(bert(Me))Ni-3(II)], [(bert(t-Bu2))Ni-3(II)], and [(habbi) Ni-3(II)], which are characterized spectroscopically, electrochemically, and crystallographically.
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Feldscher B, Theil H, Stammler A, Bögge H, Glaser T. A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni-3(II) complexes. Dalton Transactions. 2014;43(10):4102-4114.
Feldscher, B., Theil, H., Stammler, A., Bögge, H., & Glaser, T. (2014). A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni-3(II) complexes. Dalton Transactions, 43(10), 4102-4114.
Feldscher, B., Theil, H., Stammler, A., Bögge, H., and Glaser, T. (2014). A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni-3(II) complexes. Dalton Transactions 43, 4102-4114.
Feldscher, B., et al., 2014. A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni-3(II) complexes. Dalton Transactions, 43(10), p 4102-4114.
B. Feldscher, et al., “A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni-3(II) complexes”, Dalton Transactions, vol. 43, 2014, pp. 4102-4114.
Feldscher, B., Theil, H., Stammler, A., Bögge, H., Glaser, T.: A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni-3(II) complexes. Dalton Transactions. 43, 4102-4114 (2014).
Feldscher, Bastian, Theil, Hubert, Stammler, Anja, Bögge, Hartmut, and Glaser, Thorsten. “A streamlined synthesis of extended thiophloroglucinol ligands and their trinuclear Ni-3(II) complexes”. Dalton Transactions 43.10 (2014): 4102-4114.
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