An unprecedented ι-type octamolybdate: [TbI1]2[(β-Mo8O26)0.5(ι-Mo8O26)] directed by a new tricationic template

Yue, Zhong-Cheng; Du, Haijuan; Niu, Yun‐Yin; Jin, Guo‐Xin

doi:10.1039/c3ce41418c

Cited by 31 publications

(14 citation statements)

References 29 publications

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“…More recently, Niu et al (2011) reported the solid-state concomitance ofand -isomers in a crystal structure, in which the asymmetric unit is composed of two organic 1,9-bis(pyridiniumyl)nonane cations and two independent (+)-[Mo 8 O 26 ] 4À anions. Third, XRD analyses revealed that the asymmetric unit of the crystal structure of [TbI1] 2 [(-Mo 8 O 26 ) 0.5 (-Mo 8 O 26 )] {where the cation TbI1 is 1,3,5-tris [(3-methylimidazol-3-iumyl)methyl]benzene tribromide} consisted of half an independent [-Mo 8 O 26 ] 4À anion, two TbI1 3+ cations and one unprecedented [-Mo 8 O 26 ] 4À cluster (Yue et al, 2013).…”

Section: Introductionmentioning

confidence: 99%

Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic Co^II/Co^III complexes as structure-directing templates

Atencio¹,

Briceño²,

Bruno-Colmenárez³

et al. 2021

Acta Crystallogr Sect B

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Exploiting the kinetic domain provided by hydrothermal conditions, it was possible to isolate three transient metastable crystal structures, each bearing concomitant pairs of octamolybdate isomers, namely, α–β, γ–β or βcs–βgp stabilized by distinctive homoleptic [Co(bpy)3] n+ (bpy = 2,2′-bipyridine; n = 2 or 3) cations generated in situ: [Co(bpy)3]4[(α-Mo8O26)(β-Mo8O26)]·5H2O (1), [NH4][Co(bpy)3][(γ-Mo8O26)0.5(β-Mo8O26)0.5]·4H2O (2) and [Co(bpy)3]2[(βcs-Mo8O26)0.5(βgp-Mo8O26)]·12H2O (3). Solid 1 with the space group P21/n and unit-cell parameters a = 22.160 (6), b = 14.209 (3), c = 24.641 (4) Å, β = 99.10 (2)° and V = 7661 (3) Å3 resulted in the same crystal structure as that synthesized previously under different conditions by Sun et al. [J. Mol. Struct. (2005), 741, 149–153]. Factors directing the reaction, such as product composition and phase stability, were monitored by analysis of the PXRD patterns of the bulk solids obtained under different experimental conditions. The relative proportions of the mixed phases 1–3 or their stabilization are highly dependent on the initial Co:Mo molar ratio and the reaction temperature. In particular, an increase in temperature induces the transformation of 1–3 into more thermodynamically stable phases formed by one-dimensional coordination polymers [Co(bpy)2(β-Mo8O26)0.5] n (4) and [(MoO3)(bpy)] n (5). The crystal structures of 1–3 correspond to molecular salts self-assembled by C—H...O—Mo, C...H and H...H intermolecular contacts. A Hirshfeld surface analysis for 1 showed that the C...H and H...H interactions represent an average of 51.8% of the total cation–cation intermolecular contacts. In contrast, these interactions are vastly reduced in 2 (23.0%) and 3 (average 28.5% for both isomers). EPR experiments indicated that the crystal structures of 1 and 3 are paramagnetic, and that for 2 is diamagnetic. The paramagnetism of 3 stems from the in situ formation of [Co(bpy)3]3+ in a high-spin configuration. The structure-directing properties of the [Co(bpy)3] n+ cations in the isolation and self-assembly of concomitant octamolybdate isomers are also described from the viewpoint of crystal engineering.

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Section: Introductionmentioning

confidence: 99%

Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic Co^II/Co^III complexes as structure-directing templates

Atencio¹,

Briceño²,

Bruno-Colmenárez³

et al. 2021

Acta Crystallogr Sect B

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“…We concentrated on the use of the imidazolium cation as the template because it has a positive charge on its own. 16−18…”

Section: Introductionmentioning

confidence: 99%

Assembly and Adsorption Properties of Seven Supramolecular Compounds with Heteromacrocycle Imidazolium

Wang

et al. 2019

ACS Omega

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Seven supramolecular compounds comprising multivalent imidazolium macrocycles and metal halides, {[MC-IM][Ag 2 I 4 ]} n ( 1 ), {[PC-IM] 2 [Ag 7 I 11 ]} n ( 2 ), {[ODC-IM][Ag 3 I 7 ]} ( 3 ), {[ODC-IM][Bi 2 I 10 ]} ( 4 ), {[MDC-IM][Bi 2 I 10 ]} ( 5 ), {[PDC-IM][Bi 2 I 10 ]} ( 6 ), and {[MDC-IM][HgI 4 ]} ( 7 ), have been synthesized by solvothermal reactions and structurally characterized by IR spectroscopy, thermogravimetric analysis, and single-crystal X-ray diffraction. Notably, the three tetravalent imidazolium macrocycles were introduced for the first time and the extended anion structures are featured with three-dimensional coordination networks, one-dimensional chains, or zero-dimensional oligomers. This new study attempts to not only fill the gap in this supramolecular hybrid area that has been neglected but also enrich the type of imidazolium cyclophane. It is important that good efforts were devoted to study the adsorption properties of supramolecular compounds. Compound 5 exhibited great adsorption performance for organic dyes methylene blue, methyl orange, and rhodamine B (RhB) and can be evaluated as a potential candidate for industrial wastewater treatment.

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“…The {Mo 8 O 26 } 4− species belonged to a polymeric structure formed by γ-octamolybdate subunits. It is worth highlighting the large variety of octamolybdate-type clusters that can be found in the literature since crystal structures of as much as nine isomeric forms namely α, β, γ, δ, ε, ζ, η, θ, ι and the partially reduced χ have been reported to date [46][47][48][49][50]. The [γ-Mo 8 O 26 ] 4-anion consists of six octahedral {MoO 6 } and two five-coordinated {MoO 5 }, resulting in two {Mo 4 O 15 } rhomb-like tetramers linked to each other through edge sharing.…”

Section: Crystal Structures Of 1 and 1amentioning

confidence: 99%

A Robust Framework Based on Polymeric Octamolybdate Anions and Copper(II) Complexes of Tetradentate N-donor Ligands

et al. 2018

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An unprecedented ι-type octamolybdate: [TbI1]2[(β-Mo8O26)0.5(ι-Mo8O26)] directed by a new tricationic template

Cited by 31 publications

References 29 publications

Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic Co^II/Co^III complexes as structure-directing templates

Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic Co^II/Co^III complexes as structure-directing templates

Assembly and Adsorption Properties of Seven Supramolecular Compounds with Heteromacrocycle Imidazolium

A Robust Framework Based on Polymeric Octamolybdate Anions and Copper(II) Complexes of Tetradentate N-donor Ligands

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An unprecedented ι-type octamolybdate: [TbI1]2[(β-Mo8O26)0.5(ι-Mo8O26)] directed by a new tricationic template

Cited by 31 publications

References 29 publications

Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic CoII/CoIII complexes as structure-directing templates

Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic CoII/CoIII complexes as structure-directing templates

Assembly and Adsorption Properties of Seven Supramolecular Compounds with Heteromacrocycle Imidazolium

A Robust Framework Based on Polymeric Octamolybdate Anions and Copper(II) Complexes of Tetradentate N-donor Ligands

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Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic Co^II/Co^III complexes as structure-directing templates

Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic Co^II/Co^III complexes as structure-directing templates