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Abstract. [PdI{(C6H5) Introduction. In the course of research into the cross-coupling reaction (Negishi, 1978) catalyzed by Pd(PPh3)4, we isolated an intermediate Pd(C6H4CH 2-SCHa)(PPh3)2I by reacting the organic halide [o-C6H4(CH2SCH3)I] with excess of Pd(PPh3) 4. We undertook this X-ray analysis to find out whether the coordination geometry about the Pd atom is squareplanar or square-based pyramidal with an intramolecularly coordinated S atom in apical position.