[HTeV9O28]4−: A new vanadotellurate with decavanadate structure

Discovery of Heteroatom‐“Embedded” Te⊂{W18O54} Nanofunctional Polyoxometalates by Use of Cryospray Mass Spectrometry

“…Although the crystallization-based approach to cluster discovery has transformed the field, the direct unambiguous discovery of new clusters in a given reaction system is difficult. Compounds 1-3 were fully characterized by use of elemental analysis and single-crystal structure determination, and compounds 1 and 2 were detected by use of CSI-MS.The participation of tellurate and tellurite as heteroanions in POM chemistry is reasonably well known: tellurate is employed in the formation of the Anderson-type cluster {Te VI M 6 }(M=Mo or W) [16,17] and tellurite in the {Te IV W 9 } Scheme 1. However, by probing the reaction mixture with CSI-MS, we were able to screen different cation systems.…”

“…However, by probing the reaction mixture with CSI-MS, we were able to screen different cation systems. Cluster 2 a has also been isolated in the solid state as (TBA) 5 The participation of tellurate and tellurite as heteroanions in POM chemistry is reasonably well known: tellurate is employed in the formation of the Anderson-type cluster {Te VI M 6 }(M=Mo or W) [16,17] and tellurite in the {Te IV W 9 } Scheme 1. Cluster 2 a has also been isolated in the solid state as (TBA) 5 The participation of tellurate and tellurite as heteroanions in POM chemistry is reasonably well known: tellurate is employed in the formation of the Anderson-type cluster {Te VI M 6 }(M=Mo or W) [16,17] and tellurite in the {Te IV W 9 } Scheme 1.…”

“…This redox reaction, which transforms 1 a into 2 a, can be monitored in situ by use of CSI-MS. Finally, the inclusion of the Te-based heteroanion activates the surface of the {W 18 O 54 } cluster cage, facilitating the assembly of the cluster to nanoscale structures without the introduction of other transition metal electrophiles, with two {W 18 Te VI } units linked together by two {W 11 } units to give [H 10 Te VI 2 W 58 O 198 ] 26À 3 a, which was isolated as Na 8 -(DMAH) 18 [H 10 Te VI 2 W 58 O 198 ]·35 H 2 O 3 in the solid state.Compounds 1-3 were fully characterized by use of elemental analysis and single-crystal structure determination, and compounds 1 and 2 were detected by use of CSI-MS.The participation of tellurate and tellurite as heteroanions in POM chemistry is reasonably well known: tellurate is employed in the formation of the Anderson-type cluster {Te VI M 6 }(M=Mo or W) [16,17] and tellurite in the {Te IV W 9 } Scheme 1. The three steps for conventional cluster discovery compared to the one-step approach using cryospray mass spectrometry.…”

“…The participation of tellurate and tellurite as heteroanions in POM chemistry is reasonably well known: tellurate is employed in the formation of the Anderson-type cluster {Te VI M 6 }(M=Mo or W) [16,17] and tellurite in the {Te IV W 9 } Scheme 1. The three steps for conventional cluster discovery compared to the one-step approach using cryospray mass spectrometry.…”

“…However, by probing the reaction mixture with CSI-MS, we were able to screen different cation systems. Of the cations screened, dimethylammonium (DMAH + ) and tetrabutylammonium (TBA + ) were successful, yielding [H 3 W 18 O 56 (TeO 6 )] 7À (1 a; Figure 1) as Na-(DMAH) 6 The participation of tellurate and tellurite as heteroanions in POM chemistry is reasonably well known: tellurate is employed in the formation of the Anderson-type cluster {Te VI M 6 }(M=Mo or W) [16,17] and tellurite in the {Te IV W 9 } Scheme 1. The three steps for conventional cluster discovery compared to the one-step approach using cryospray mass spectrometry.…”