High‐Yield Synthesis and Crystal Structure Determination of Sodium Triphenylphosphane Monosulfonate (TPPMS^Na)

Abstract

A simple, high-yield synthesis is described that leads to the sodium salt of monosulfonated triphenylphosphane (TPPMS Na ) as a pure product in large quantities without complicated workup techniques. The single-crystal X-ray structure of TPPMS Na ·2.5H 2 O is reported. The structure is built up by alternating layers of aquated sodium sulfonate units and hydrophobic triphenyl units. Thermogravimetric

Gold Nanoclusters as Nanoantibiotic Auranofin Analogues

“…[53] Water-soluble analogues 4a-4d were synthesized by first replacing PPh 3 in cluster 1 with TPPMS, prepared by sulfonation of PPh 3 using oleum (Figure 2B). [62] A 50-molar excess of TPPMS in a biphasic water/DCM solution resulted in the complete transfer of cluster 1 to the aqueous layer after 12 h at room temperature. Purification by size exclusion chromatography gave cluster 3 as a black powder.…”

Two in one: Charged tertiary phosphines held together by ionic or covalent interactions as bidentate phosphorus ligands for synthesis of half-sandwich Ru(II)-complexes

“…Selected bond lengths (Å), angles ( o ) and torsion angles ( o ) with estimated standard deviations: P1 -C1: 1.761 (7); P1 -C2: 1.807 (7); P1 -C3: 1.807(9); P2 -C11: 1.827(6); P2 -C21: 1.819(6); P2 -C31: 1.830 (7); P1 -C1 -N1: 115.2(4); C1 -N1 -C41: 113.0(5); C1 -N1 -C41 -C42: -68.4(1). Sodium salt of mtppms was prepared already in 1958 [36], however, due to its poor crystallization properties its X-ray structure was not determined until 2010 [37]. In addition, structure of mtppms was determined with benzyltriethylammonium [38], guanidinium [39] and imidazolium [40] cations, however, (2)(1), (4)(1) and (5)(1) are the first structurally characterized mtppms salts containing water-soluble phosphines both as cation and anion.…”

Synthesis of Na2{trans‐[PdCl2(mTPPMS‐κP)2]}: Interaction with DNA and Reactivity with 8‐Thiotheophylline

“…As indicated previously, the distorted square‐pyramidal coordination geometry of Na + is formed of two O atoms from two different sulfonate groups that are trans to each other, an O6 purine located in the vertex of the pyramid and two water molecules. The Na–O sulfonate [Na1–O1T 2.583(10) Å, Na1–O2T 2.672(13) Å] and Na–OH 2 bond lengths [Na1–O2W 2.444(13) Å, Na1–O1W 2.536(2) Å] are longer than those found in mTPPMS Na [O sulfonate –Na 2.323(3)–2.442(4) Å, O water –Na 2.317(3)–2.359(6) Å] 10. The only reported11 crystal structure of a metal complex containing a purine coordinated to a Na, trans ‐[Pt(NH 3 )(Hmgua‐ N 7 ) 2 (myct‐ N 3 )Na(H 2 O) 2 ][ClO 4 ] 3 · 0.5H 2 O,12 is characterized by Na–O water [Na(1)–O(1w) 2.308(9) Å, Na(1)–O(2w) 2.40(2) Å] and Na–O6 purine [Na(1)–O(6a) 2.261(9) Å, Na(1)–O(6b) 2.379(8) Å] distances shorter than those found in 3 [Na1–O6 2.551(10) Å].…”