19-Tungstodiarsenate(III) Functionalized by Organoantimony(III) Groups: Tuning the Structure–Bioactivity Relationship

A family of three discrete organoantimony­(III)-functionalized heteropolyanions[Na­{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­As^III₂W₁₉O₆₇(H₂O)]^10– (<b>1</b>), [{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}₂As^III₂W₁₉O₆₇(H₂O)]^8– (<b>2</b>), and [{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­{WO₂(H₂O)}­{WO­(H₂O)}₂(<i>B</i>-β-As^IIIW₈O₃₀)­(<i>B</i>-α-As^IIIW₉O₃₃)₂]^14– (<b>3</b>)have been prepared by one-pot reactions of the 19-tungstodiarsenate­(III) precursor [As^III₂W₁₉O₆₇(H₂O)]^14– with 2-(Me₂NCH₂)­C₆H₄SbCl₂. The three novel polyanions crystallized as the hydrated mixed-alkali salts Cs₃KNa₆[Na­{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­As^III₂W₁₉O₆₇(H₂O)]·43H₂O (<b>CsKNa-1</b>), Rb_2.5K_5.5[{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}₂As^III₂W₁₉O₆₇(H₂O)]·18H₂O·Me₂NCH₂C₆H₅ (<b>RbK-2</b>), and Rb_2.5K_11.5[{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­{WO₂(H₂O)}­{WO­(H₂O)}₂(<i>B</i>-β-As^IIIW₈O₃₀)­(<i>B</i>-α-As^IIIW₉O₃₃)₂]·52H₂O (<b>RbK-3</b>), respectively. The number of incorporated {2-(Me₂HN⁺CH₂)­C₆H₄Sb^III} units could be tuned by careful control of the experimental parameters. Polyanions <b>1</b> and <b>2</b> possess a dimeric sandwich-type topology, whereas <b>3</b> features a trimeric, wheel-shaped structure, representing the largest organoantimony-containing polyanion. All three compounds were fully characterized in the solid state via single-crystal X-ray diffraction (XRD), infrared (IR) spectroscopy, and thermogravimetric analysis, and their aqueous solution stability was validated by ultraviolet–visible light (UV-vis) and multinuclear (¹H, ¹³C, and ¹⁸³W) nuclear magnetic resonance (NMR) spectroscopy. Effective inhibition against six different types of bacteria was observed for <b>1</b> and <b>2</b>, and we could extract a structure–bioactivity relationship for these polyanions

19-Tungstodiarsenate(III) Functionalized by Organoantimony(III) Groups: Tuning the Structure–Bioactivity Relationship

A family of three discrete organoantimony­(III)-functionalized heteropolyanions[Na­{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­As^III₂W₁₉O₆₇(H₂O)]^10– (<b>1</b>), [{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}₂As^III₂W₁₉O₆₇(H₂O)]^8– (<b>2</b>), and [{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­{WO₂(H₂O)}­{WO­(H₂O)}₂(<i>B</i>-β-As^IIIW₈O₃₀)­(<i>B</i>-α-As^IIIW₉O₃₃)₂]^14– (<b>3</b>)have been prepared by one-pot reactions of the 19-tungstodiarsenate­(III) precursor [As^III₂W₁₉O₆₇(H₂O)]^14– with 2-(Me₂NCH₂)­C₆H₄SbCl₂. The three novel polyanions crystallized as the hydrated mixed-alkali salts Cs₃KNa₆[Na­{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­As^III₂W₁₉O₆₇(H₂O)]·43H₂O (<b>CsKNa-1</b>), Rb_2.5K_5.5[{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}₂As^III₂W₁₉O₆₇(H₂O)]·18H₂O·Me₂NCH₂C₆H₅ (<b>RbK-2</b>), and Rb_2.5K_11.5[{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­{WO₂(H₂O)}­{WO­(H₂O)}₂(<i>B</i>-β-As^IIIW₈O₃₀)­(<i>B</i>-α-As^IIIW₉O₃₃)₂]·52H₂O (<b>RbK-3</b>), respectively. The number of incorporated {2-(Me₂HN⁺CH₂)­C₆H₄Sb^III} units could be tuned by careful control of the experimental parameters. Polyanions <b>1</b> and <b>2</b> possess a dimeric sandwich-type topology, whereas <b>3</b> features a trimeric, wheel-shaped structure, representing the largest organoantimony-containing polyanion. All three compounds were fully characterized in the solid state via single-crystal X-ray diffraction (XRD), infrared (IR) spectroscopy, and thermogravimetric analysis, and their aqueous solution stability was validated by ultraviolet–visible light (UV-vis) and multinuclear (¹H, ¹³C, and ¹⁸³W) nuclear magnetic resonance (NMR) spectroscopy. Effective inhibition against six different types of bacteria was observed for <b>1</b> and <b>2</b>, and we could extract a structure–bioactivity relationship for these polyanions

19-Tungstodiarsenate(III) Functionalized by Organoantimony(III) Groups: Tuning the Structure–Bioactivity Relationship

A family of three discrete organoantimony­(III)-functionalized heteropolyanions[Na­{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­As^III₂W₁₉O₆₇(H₂O)]^10– (<b>1</b>), [{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}₂As^III₂W₁₉O₆₇(H₂O)]^8– (<b>2</b>), and [{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­{WO₂(H₂O)}­{WO­(H₂O)}₂(<i>B</i>-β-As^IIIW₈O₃₀)­(<i>B</i>-α-As^IIIW₉O₃₃)₂]^14– (<b>3</b>)have been prepared by one-pot reactions of the 19-tungstodiarsenate­(III) precursor [As^III₂W₁₉O₆₇(H₂O)]^14– with 2-(Me₂NCH₂)­C₆H₄SbCl₂. The three novel polyanions crystallized as the hydrated mixed-alkali salts Cs₃KNa₆[Na­{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­As^III₂W₁₉O₆₇(H₂O)]·43H₂O (<b>CsKNa-1</b>), Rb_2.5K_5.5[{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}₂As^III₂W₁₉O₆₇(H₂O)]·18H₂O·Me₂NCH₂C₆H₅ (<b>RbK-2</b>), and Rb_2.5K_11.5[{2-(Me₂HN⁺CH₂)­C₆H₄Sb^III}­{WO₂(H₂O)}­{WO­(H₂O)}₂(<i>B</i>-β-As^IIIW₈O₃₀)­(<i>B</i>-α-As^IIIW₉O₃₃)₂]·52H₂O (<b>RbK-3</b>), respectively. The number of incorporated {2-(Me₂HN⁺CH₂)­C₆H₄Sb^III} units could be tuned by careful control of the experimental parameters. Polyanions <b>1</b> and <b>2</b> possess a dimeric sandwich-type topology, whereas <b>3</b> features a trimeric, wheel-shaped structure, representing the largest organoantimony-containing polyanion. All three compounds were fully characterized in the solid state via single-crystal X-ray diffraction (XRD), infrared (IR) spectroscopy, and thermogravimetric analysis, and their aqueous solution stability was validated by ultraviolet–visible light (UV-vis) and multinuclear (¹H, ¹³C, and ¹⁸³W) nuclear magnetic resonance (NMR) spectroscopy. Effective inhibition against six different types of bacteria was observed for <b>1</b> and <b>2</b>, and we could extract a structure–bioactivity relationship for these polyanions

Tetra-Antimony(III)-Bridged 18-Tungsto-2-Arsenates(V), [(LSb^III)₄(<i>A</i>‑α-As^VW₉O₃₄)₂]^10– (L = Ph, OH): Turning Bioactivity On and Off by Ligand Substitution

Two tetra-antimony­(III)-bridged, sandwich-type 18-tungsto-2-arsenates­(V), [(LSbIII)4(A-α-AsVW9O34)2]10– (L = Ph (1), OH (2)), were prepared and fully characterized in the solid state and in solution. Both polyanions are stable in aqueous physiological medium for at least 24 h (at concentrations ≥2.5 × 10–6 M). Despite the presence of an isostructural tetra-antimony­(III) motif in 1 and 2, distinctly different antibacterial activity was observed for both polyanions. The minimum inhibitory concentrations (MIC) of 1 (7.8–62.5 μg/mL) is lower than for any other organoantimony­(III)-containing polyoxometalate reported to date

Tetra-Antimony(III)-Bridged 18-Tungsto-2-Arsenates(V), [(LSb^III)₄(<i>A</i>‑α-As^VW₉O₃₄)₂]^10– (L = Ph, OH): Turning Bioactivity On and Off by Ligand Substitution

Two tetra-antimony­(III)-bridged, sandwich-type 18-tungsto-2-arsenates­(V), [(LSb^III)₄(<i>A</i>-α-As^VW₉O₃₄)₂]^10– (L = Ph (<b>1</b>), OH (<b>2</b>)), were prepared and fully characterized in the solid state and in solution. Both polyanions are stable in aqueous physiological medium for at least 24 h (at concentrations ≥2.5 × 10^–6 M). Despite the presence of an isostructural tetra-antimony­(III) motif in <b>1</b> and <b>2</b>, distinctly different antibacterial activity was observed for both polyanions. The minimum inhibitory concentrations (MIC) of <b>1</b> (7.8–62.5 μg/mL) is lower than for any other organoantimony­(III)-containing polyoxometalate reported to date

Tetra-Antimony(III)-Bridged 18-Tungsto-2-Arsenates(V), [(LSb^III)₄(<i>A</i>‑α-As^VW₉O₃₄)₂]^10– (L = Ph, OH): Turning Bioactivity On and Off by Ligand Substitution

Two tetra-antimony­(III)-bridged, sandwich-type 18-tungsto-2-arsenates­(V), [(LSb^III)₄(<i>A</i>-α-As^VW₉O₃₄)₂]^10– (L = Ph (<b>1</b>), OH (<b>2</b>)), were prepared and fully characterized in the solid state and in solution. Both polyanions are stable in aqueous physiological medium for at least 24 h (at concentrations ≥2.5 × 10^–6 M). Despite the presence of an isostructural tetra-antimony­(III) motif in <b>1</b> and <b>2</b>, distinctly different antibacterial activity was observed for both polyanions. The minimum inhibitory concentrations (MIC) of <b>1</b> (7.8–62.5 μg/mL) is lower than for any other organoantimony­(III)-containing polyoxometalate reported to date

Synthesis and Biological Activity of Organoantimony(III)-Containing Heteropolytungstates

Three discrete organoantimony­(III)-containing heteropolytungstates [(PhSbIII)4(A-α-GeIVW9O34)2]12– (1), [(PhSbIII)4(A-α-PVW9O34)2]10– (2), and [{2-(Me2NCH2C6H4)­SbIII}3(B-α-AsIIIW9O33)]3– (3) have been synthesized in one-pot reactions in aqueous medium using the appropriate lacunary heteropolyanion precursor and organoantimony­(III) source. Polyanions 1–3 were isolated as hydrated salts, (NH4)12[(PhSbIII)4(A-α-GeIVW9O34)2]·20H2O (1a), Rb9Na­[(PhSbIII)4(A-α-PVW9O34)2]·20H2O (2a), and Rb3[{2-(Me2NCH2C6H4)­SbIII}3(B-α-AsIIIW9O33)]·7H2O (3a). The compounds 1a–3a were fully characterized in the solid state using infrared (IR) spectroscopy, single-crystal XRD, and thermogravimetric and elemental analyses. The stability of 1–3 in aqueous solution was confirmed by multinuclear NMR (1H, 13C, 31P, and 183W) spectroscopy. Preliminary studies on the biological activity of 1–3 showed that all three compounds might act as potent antimicrobial agents

Synthesis and Biological Activity of Organoantimony(III)-Containing Heteropolytungstates

Three discrete organoantimony­(III)-containing heteropolytungstates [(PhSb^III)₄(<i>A</i>-α-Ge^IVW₉O₃₄)₂]^12– (<b>1</b>), [(PhSb^III)₄(<i>A</i>-<i>α</i>-P^VW₉O₃₄)₂]^10– (<b>2</b>), and [{2-(Me₂NCH₂C₆H₄)­Sb^III}₃(<i>B</i>-α-As^IIIW₉O₃₃)]^3– (<b>3</b>) have been synthesized in one-pot reactions in aqueous medium using the appropriate lacunary heteropolyanion precursor and organoantimony­(III) source. Polyanions <b>1</b>–<b>3</b> were isolated as hydrated salts, (NH₄)₁₂[(PhSb^III)₄(<i>A</i>-α-Ge^IVW₉O₃₄)₂]·20H₂O (<b>1a</b>), Rb₉Na­[(PhSb^III)₄(<i>A</i>-α-P^VW₉O₃₄)₂]·20H₂O (<b>2a</b>), and Rb₃[{2-(Me₂NCH₂C₆H₄)­Sb^III}₃(<i>B</i>-α-As^IIIW₉O₃₃)]·7H₂O (<b>3a</b>). The compounds <b>1a</b>–<b>3a</b> were fully characterized in the solid state using infrared (IR) spectroscopy, single-crystal XRD, and thermogravimetric and elemental analyses. The stability of <b>1</b>–<b>3</b> in aqueous solution was confirmed by multinuclear NMR (¹H, ¹³C, ³¹P, and ¹⁸³W) spectroscopy. Preliminary studies on the biological activity of <b>1</b>–<b>3</b> showed that all three compounds might act as potent antimicrobial agents