Compound 2a

View in PubChem | MDL Molfile | ChemDraw

InChIKey CYGMTXODCJLSKO-UHFFFAOYSA-L

Compound data: CIF

Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.

A solution of ligand 1a (0.125 mmol) in CH₂Cl₂ (5 mL) was added slowly dropwise to a solution of [Pt(cod)Cl₂] (47 mg, 0.125 mmol, 1 eq.) in CH₂Cl₂ (5 mL) at room temperature. The solution was allowed to stir for 5 min and a specific complexation motif of the P,S ligand was confirmed via in situ³¹P/³¹P{¹H} and other NMR techniques. 2a was purified as follows: solvent was evaporated in vacuo and the oily residue was triturated three times with hexanes (ca. 5 mL each time). The resulting oily substance was dried in vacuo to afford solid product, which was subjected to analytical characterization.¹H NMR (400.1 MHz, CD₂Cl₂, 30 °C): δ 7.84-7.65 (m, 3H, ArH), 7.55-7.09 (m, 7H, ArH), 3.19 (s, 2H, cage-CH), 3.34-1.46 (m, 13H, cage-BH, alkyl-CH); ¹¹B NMR (128.4 MHz, CD₂Cl₂, 30 °C, BF₃-Et₂O): δ -4.7 (s, 1B, SB), -7.4 (d, ¹J_B-H= 82 Hz, 2BH), -9.3 to -20.91 (m, 7BH); ³¹P {¹H} NMR (162.0 MHz, CD₂Cl₂, 30 °C): δ 40.8 (s, J_P-Pt = 3625 Hz). HRMS (ESI): m/z calcd for C₁₆H₂₅B₁₀ClPPtS [M-Cl]⁺: 618.1754, found: 618.1760. Calculated for C₁₆B₁₀H₂₅Cl₂PPtS·¼C₆H₁₄: C, 31.09; H, 4.25; found: C, 31.10; H, 4.30. Single crystals suitable for X-ray diffraction studies were grown by slow evaporation from CH₂Cl₂ in a NMR tube. Complexes 2c, 2d, 2e, 2f and 2gwere synthesised by an analogous method, with the corresponding ligand.