| Summary: | Two new phases derived from the layered ternary chalcogenide Ta<sub>2</sub>PdS<sub>6</sub> have been successfully synthesised via the intercalation of sodium or potassium. <i>M</i>Ta<sub>2</sub>PdS<sub>6</sub> (<i>M</i> = Na, K) crystallise in monoclinic space group <i>I</i>2/<i>m</i> (No. 12), <i>Z</i> = 2, with lattice parameters <i>a</i> = 8.1366(7) Å, <i>b</i> = 3.2876(1) Å, <i>c</i> = 15.3279(3) Å, β = 97.407(2)° for NaTa<sub>2</sub>PdS<sub>6</sub>, and <i>a</i> = 8.3845(3) Å, <i>b</i> = 3.2955(1) Å, <i>c</i> = 16.7416(8) Å, β = 86.339(3)° in the case of KTa<sub>2</sub>PdS<sub>6</sub>. The general structure of the parent phase is retained upon intercalation, with increased unit cell volumes of 17.3% and 33.2% for the Na and K intercalates respectively. SQUID magnetometry shows that both intercalates are net diamagnets, but shows a significant reduction of magnetic susceptibility from Ta<sub>2</sub>PdS<sub>6</sub> due to the increase in a Pauli paramagnetic component due to partial band filling.
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