A Convenient Synthesis of Triarylbismuth Diacetates

The hybrid dibismuthines O(CH2CH2BiPh2)2 and MeN(CH2-2-C6H4BiPh2)2 react with [M(CO)5(thf)] (M = Cr or W) to form [{M(CO)5}2{O(CH2CH2BiPh2)2}] and [{Cr(CO)5}2{MeN(CH2-2-C6H4BiPh2)2}] containing bridging bidentate (Bi2) coordination. The unsymmetrical tertiary bismuthine complexes [M(CO)5{BiPh2(o-C6H4OMe)}] are also described. Depending upon the molar ratio, the hybrid distibines O(CH2CH2SbMe2)2 and MeN(CH2-2-C6H4SbMe2)2 react with [M(CO)5(thf)] to give the pentacarbonyl complexes [{M(CO)5}2{O(CH2CH2SbMe2)2}] and [{Cr(CO)5}2{MeN(CH2-2-C6H4SbMe2)2}] or tetracarbonyls cis-[M(CO)4{O(CH2CH2SbMe2)2}] and cis-[M(CO)4{MeN(CH2-2-C6H4SbMe2)2}]. The latter can also be obtained from [Cr(CO)4(nbd)] or [W(CO)4(pip)2], and contain chelating bidentates (Sb2-coordinated) as determined crystallographically. S(CH2-2-C6H4SbMe2)2 coordinates as a tridentate (SSb2) in fac-[M(CO)3{S(CH2-2-C6H4SbMe2)2}] (M = Cr or Mo) and fac-[Mn(CO)3{S(CH2-2-C6H4SbMe2)2}][CF3SO3]. Fac-[Mn(CO)3{MeN(CH2-2-C6H4SbMe2)2}][CF3SO3] contains NSb2-coordinated ligand in the solid state, but in solution a second species, Sb2-coordinated and with a κ1-CF3SO3 replacing the coordinated amine is also evident. X-ray crystal structures were also determined for fac-[Cr(CO)3{S(CH2-2-C6H4SbMe2)2}], fac-[Mn(CO)3{S(CH2-2-C6H4SbMe2)2}][CF3SO3] and fac-[Mn(CO)3{MeN(CH2-2-C6H4SbMe2)2}] [CF3SO3]. Hypervalent N⋯Sb interactions are present in cis-[M(CO)4{MeN(CH2-2-C6H4SbMe2)2}] (M = Mo or W), but absent for M = Cr.

Hybrid dibismuthines and distibines as ligands towards transition metal carbonyls.

The interaction between water protons and suitable quadrupolar nuclei (QN) can lead to quadrupole relaxation enhancement (QRE) of proton spins, provided the resonance condition between both spin tr ...

/pdf/tuning-nuclear-quadrupole-resonance-a-novel-approach-for-the-1y1jfy3lje.pdf

Tuning Nuclear Quadrupole Resonance: A Novel Approach for the Design of Frequency-Selective MRI Contrast Agents

To study and evaluate the structure-activity relationships in di-aryl bismuth phosphinates on antibacterial activity and cytotoxicity a series of complexes containing ortho-methoxyphenyl, meta-methoxyphenyl, meta-tolyl and para-tolyl aryl groups; [Bi(o-MeOPh)2(O(O)P(H)Ph)]n1, [Bi(o-MeOPh)2(O(O)PPh2)]n2, [Bi(o-MeOPh)2(O(O)P(p-MeOPh)2)]n3, [Bi(m-MeOPh)2(O(O)P(H)Ph)]n4, [Bi(m-MeOPh)2(O(O)PPh2)]n5, [Bi(m-MeOPh)2(O(O)P(p-MeOPh)2)]n6, [Bi(m-tol)2(O(O)P(H)Ph)]n7, [Bi(m-tol)2(O(O)PPh2)]n8, [Bi(m-tol)2(O(O)P(p-MeOPh)2)]n9, [Bi(p-tol)2(O(O)P(H)Ph)]n10, [Bi(p-tol)2(O(O)PPh2)]n11 and [Bi(p-tol)2(O(O)P(p-MeOPh)2)]n12, were synthesised and characterised. Complexes 4, 7, 8, 10 and 11 were structurally authenticated by X-ray crystallography. Evaluation of their antibacterial activity towards methicillin-resistant Staphylococcus aureus (MRSA), vancomycin-resistant Enterococcus (VRE), Escherichia coli (E. coli) and Pseudomonas aeruginosa (P. aeruginosa) showed that the bismuth bound aryl group has a profound influence on activity, with the o-MeOPh complexes 1-3 showing very little activity while the m-MeOPh complexes have the greatest activity towards MRSA and VRE in the range of 0.63 to 1.25 μM. Viability studies with Cos-7 cells showed that the di-aryl bismuth complexes 1-12 are less cytotoxic than their di-phenyl bismuth analogues, with a general trend of toxicity observed as p-tolyl > m-tolyl > m-methoxyphenyl > o-methoxyphenyl. The large difference in Cos-7 viability for complexes 1 (IC50 > 80 μM) and 4 (IC50 14.0 μM) was further investigated through bismuth uptake studies, where there was no obvious difference in Cos-7 bismuth uptake at 5 μM. This suggests that the bismuth-bound aryl group has a significant impact on biological activity, which is then further mediated by other ligands. 

Aryl bismuth phosphinates [BiAr2(O(O)PRR’)]: structure-activity relationships for antibacterial activity and cytotoxicity

The key features of arsines, stibines and bismuthines as ligands towards transition metal and main group metal/metalloids are described. Following a brief review of the development of the chemistry, the main synthetic routes to the ligands are described and the advantages and limitations of the various approaches outlined. Current views of the nature of the metal-ligand bonding are evaluated, and the main coordination modes of the ligands described with illustrative examples.

Acyclic Arsine, Stibine, and Bismuthine Ligands

The synthesis of functionally substituted (OMe, -NMe2, -SMe) organobismuthine ligands -specifically (o-MeOC6H4)3Bi, (o-MeSC6H4)3Bi, (o-Me2NC6H4)3Bi, (o-MeOC6H4)Ph2Bi, (o-MeSC6H4)Ph2Bi, (o-Me2NC6H4)Ph2Bi, is described. (o-Chlorophenyl)diphenylbismuthine reacts with sodium diphenylstibide (NaSbPh2) to give (o-diphenylstibinophenyl)diphenylbismuthine o-C6H4(SbPh2)(BiPh2). The 1H nmr and mass spectra of these ligands, and of (o-MeC6H4)3Bi and (p-MeC6H4)3Bi are reported and discussed.

The synthesis and properties of substituted tertiary bismuthine ligands

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The synthesis and properties of substituted tertiary bismuthine ligands