Compound 4a

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InChIKey BVPSIWPFRSVRGI-UHFFFAOYSA-N

Compound data: CIF

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

To a solution of a bisligated complex 2a (0.125 mmoles) AgBF₄ (48 mg, 0.25 mmoles, 1 equiv) was added and the cloudy mixture was left vigorously stirring for 1 hour. In situ³¹P/³¹P{¹H} and other NMR techniques were used to confirm quantitative abstractions. 2awas purified as follows: the solutions were filtered through a layer of Celite™, filtrate was evaporated in vacuo and the resulting oily residues were 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 7.76-6.98 (bm, 20H, ArH), 3.58-1.26 (bm, 30H, cage-BH, cage-CH, Alkyl-CH); ¹¹B (128.4 MHz, CD₂Cl₂, 30 ^oC, BF₃-Et₂O): - 2.2 (s, 2B, BF₄), δ - 4.3 (s, 2B, B-S), - 5.5 to - 24.8 (bm, 18BH); ³¹P{¹H} NMR (100.6 MHz, CD₂Cl₂, 30 °C): δ 48.2 (s, ¹J_P-Pt=3135). HRMS (ESI): m/z calcd for C₃₂B₂₀H₅₀P₂PtS₂ [M-2BF₄]²⁺: 485.7242, found: 485.7267. Calculated for C₃₂B₂₂H₅₀F₈P₂PtS₂: C, 33.55; H, 4.40; found: C, 35.78; H, 4.37. Single crystals suitable for X-Ray studies were grown by slow diffusion of diethyl ether, layered on top of a dichloromethane solution of 4a in a NMR tube. Complexes 4b, 4c, 4d, 4e, 4f,4g, 4h and 4i were synthesised by an analogous method from a corresponding bisligated complex. For complexes characterized by NMR in situ CD₂Cl₂ was used instead of CH₂Cl₂.