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To study pnictogen bonding involving bismuth, flexible accordion‐like molecular complexes of the composition [P(C 6 H 4 ‐ o ‐CH 2 SCH 3 ) 3 BiX 3 ], (X=Cl, Br, I) have been synthesised and characterised. The strength of the weak and mainly electrostatic interaction between the Bi and P centres strongly depends on the character of the halogen substituent on bismuth, which is confirmed by single‐crystal X‐ray diffraction analyses, DFT and ab initio computations. Significantly,  209 Bi– 31 P through‐space coupling ( J =2560 Hz) is observed in solid‐state  31 P NMR spectra, which is so far unprecedented in the literature, delivering direct information on the magnitude of this pnictogen interaction.

Weak Pnictogen Bond with Bismuth: Experimental Evidence Based on Bi−P Through‐Space Coupling