<div><p></p><p>The reaction of Ph<sub>3</sub>Bi with a sterically hindered phosphinic acid, 1,1,2,3,3- pentamethyltrimethylene phosphinic acid, {<i>cyc</i>P(O)OH路2H<sub>2</sub>O} at two different temperatures, one at refluxing conditions and another at room temperature in THF have been investigated. At refluxing conditions, cleavage of two Bi-C bonds (of BiPh<sub>3</sub>) leads to the formation of a 16-membered macrocycle [(PhBi)<sub>4</sub>(<i>cyc</i>PO<sub>2</sub>)<sub>8</sub>] (<b>1</b>). On the other hand, the reaction at room temperature leads to only cleavage of one Bi-C bond affording a 1D polymer [(Ph<sub>2</sub>Bi)(<i>cyc</i>PO<sub>2</sub>)]<sub>n</sub>, (1,1,2,3,3-pentamethyltrimethylene phosphinate is denoted as <i>cyc</i>PO<sub>2</sub>) (<b>2</b>). Both the complexes were characterized by single crystal X-ray diffraction. In both of these complexes the phosphinate ligands are present in anisobidentate (bridging) coordination mode.
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