X-ray diffraction investigation of the crystals of the octamolybdate (NH4)4Mo8O26� 4H2O

Atovmyan, L. O.; Krasochka, O. N.

doi:10.1007/bf00744514

Cited by 14 publications

(8 citation statements)

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“…Both anions 1 and 2 contain the [β-Mo 8 O 26 ] 4- unit as their main building block (see Figures and ). The atoms in those units are labeled in a manner that reflects the fact that the β-octamolybdate structure is composed of two Mo 4 O 13 subunits stacked together by relatively long Mo−O bonds. , The Mo−O bonds within those subunits are depicted by filled thick lines in both Figures and . There are four such subunits in the structure of 1 , and they are named A, B, C, and D, respectively.…”

Section: Discussionmentioning

confidence: 99%

β-Octamolybdate as a Building Block. Synthesis and Structural Characterization of Rare Earth−Molybdate Adducts

Kitamura

Yagasaki

1997

Inorg. Chem.

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Reaction of [(n-C4H9)4N]4[Mo8O26] with nitrate salts of rare earth metals yields two different series of new compounds [Ln(Mo8O26)2]5- and [{Ln(NO3)3}2(Mo8O26)]4- (Ln = Y, La, Ce, Pr, Nd, Gd, Yb) as tetra-n-butylammonium salts. X-ray structural analyses of [(n-C4H9)4N]5[La(Mo8O26)2]·CH3CN [monoclinic, space group P21/c, a = 25.8332(6) Å, b = 17.5054(7) Å, c = 32.6565(12) Å, β = 91.699(2)°, Z = 4] and [(n-C4H9)4N]4[{La(NO3)3}2(Mo8O26)]·2CH3CN [monoclinic, space group P21/n, a = 17.702(2) Å, b = 17.2646(12) Å, c = 18.965(2) Å, β = 102.132(3)°, Z = 2] revealed that these compounds contain the Mo8O26 unit as their building block.

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Section: Discussionmentioning

confidence: 99%

β-Octamolybdate as a Building Block. Synthesis and Structural Characterization of Rare Earth−Molybdate Adducts

Kitamura

Yagasaki

1997

Inorg. Chem.

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“…Before entering into a description of the anions observed in the crystal structures of 1-3, it is prudent to note some of their available features. Octamolybdates show the most extensive structural diversity among isopolyoxomolybdates in the solid state, where at least nine structural disparate isomers (, , , , , , , and ) have already been crystallographically studied (: Day et al, 1977;: Atovmyan & Krasochka, 1972;: Niven et al, 1991;: Xi et al, 1994;, : Hagrman et al, 1997;: Xiao et al, 2004;: Allis et al, 2004;: Yue et al, 2013). Other structural variants have also been found in different crystal structures containing a ligand attached to the cluster (Gili et al, 1992) or as a building block in molybdate one-dimensional (1D) polymers (Hagrman et al, 1999;Atencio et al, 2007).…”

Section: General Features Of Octamolybdatesmentioning

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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“…Von den aus angesS.uerten wfissrigen L6sungen kristallisierenden Alkaliisopolymolybdaten sind bisher die Strukturen der Heptamolybdate M6MOTOz4.4H20 (M=NH+,K+,Rb+,Na +) (Lindqvist, 1950b,c;Shimao, 1967;Evans, 1968;Gatehouse & Leverett, 1968;Sj6bom & Hedmann, 1973;Evans, Gatehouse & Leverett, 1975), des Oktamolybdat-Ions im (NH4)4MosO26.4HzO und (NH4)4MosOa6 • 5H20 (Lindqvist, 1950d;Atovmyan & Krasochka, 1972), des Polyoktamolybdats (NH4)6MosOzT.4H20 (B6schen, Buss, Krebs & Glemser, 1973;B6schen, Buss & Krebs, 1974), des Hexamolybdats [HN3P3(NMe2)6]2Mo6Oa9 (Allcock, Bissell & Shawl, 1973) und des sogenannten Dimolybdats (NH4)2Mo207 (Kn6pnadel, Hartl, Hunnius & Fuchs, 1974) bekannt. Das erste echte strukturell charakterisierte Dekamolybdat mit isolierten MoloO~4-Ionen ist das kilrzlich beschriebene (NH4)sMo10034 (Fuchs, Hartl, Hunnius & Mahjour, 1975).…”

Section: Introductionunclassified

“…Fig. 2 (Lindqvist, 1950b,c;Shimao, 1967;Evans, 1968;Gatehouse & Leverett, 1968;Sj6bom & Hedmann, 1973;Evans, Gatehouse & Leverett, 1975), des Hexamolybdat-Ions MO6029 (Allcock, Bissell & Shawl, 1973), des Oktamolybdat-Ions MosO46 (Lindqvist, 1950d;Atovmyan & Krasochka, 1972), des PolyoktamolybdatIons (Mo8067),, (B6schen, Buss, Krebs & Glemser, 1973;B6schen, Buss & Krebs, 1974;B6schen, 1974) und des echten Dekamolybdat-Ions Mo10084 (Fuchs, Hartl, Hunnius & Mahjour, 1975) (Sotani, 1975), eine gewisse Berechtigung. Die 'Dekamolybdate' weisen keine isolierten Polyanionen mehr auf, sondern bilden /~hnlich den bei weiterem AnsS.uern der L6sungen auskristallisierenden Oxidhydraten polymere Strukturen.…”

Section: Introductionunclassified

Kristallstruktur des sogenannten Kaliumdekamolybdats KMo₅O₁₅OH.2H₂O

Krebs¹,

Paulat‐Böschen²

1976

Acta Crystallogr Sect B

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The crystal structure of the so-called potassium decamolybdate, the formula of which has to be written as KMosOlsOH. 2H20, was determined from single-crystal diffractometer data. The compound crystallizes with hexagonal symmetry in the space group P63/m, the cell parameters being a= 10.550 (8), c--3-727 (3) ,~ and Z= 1. The structure has been solved from the Patterson function and chemical considerations and refined by full-matrix least squares to a conventional R of 0.042 based on 335 independent reflexions. The structure consists of double chains made of edge-sharing, strongly distorted MoO6 octahedra. The double chains are linked by common corners of octahedra to form a threedimensional network. The double chains are not perfect due to statistical non-occupation of one of the six equivalent Mo positions in the unit cell. Along the short c axis the polymeric structure forms tunnels in which the potassium ions are located. Mo-O bond lengths in the MoO6 octahedra are: 1.698, 1.701, 1.955 (2 x ), 2.190 and 2.373/~. The chemical composition and the observed interatomic distances lead to a plausible model of the structural disorder: In the neighbourhood of a vacant Mo position the O atoms are partially replaced by coordinated H20 molecules, isolated H20 molecules (crystal water), and OH groups. The statistical distribution of the Mo vacancies can be interpreted as resulting in smaller sub-units of edge-sharing octahedra linked in the direction of the double chains only by common corners. The structure is only weakly related to the structures of the other typical polymolybdates crystallizing from aqueous solutions. Closer relations are found to the structures of ~-MoO3.H20 and of MOO3.

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X-ray diffraction investigation of the crystals of the octamolybdate (NH4)4Mo8O26� 4H2O

Cited by 14 publications

References 2 publications

β-Octamolybdate as a Building Block. Synthesis and Structural Characterization of Rare Earth−Molybdate Adducts

β-Octamolybdate as a Building Block. Synthesis and Structural Characterization of Rare Earth−Molybdate Adducts

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

Kristallstruktur des sogenannten Kaliumdekamolybdats KMo₅O₁₅OH.2H₂O

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X-ray diffraction investigation of the crystals of the octamolybdate (NH4)4Mo8O26� 4H2O

Cited by 14 publications

References 2 publications

β-Octamolybdate as a Building Block. Synthesis and Structural Characterization of Rare Earth−Molybdate Adducts

β-Octamolybdate as a Building Block. Synthesis and Structural Characterization of Rare Earth−Molybdate Adducts

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

Kristallstruktur des sogenannten Kaliumdekamolybdats KMo5O15OH.2H2O

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

Kristallstruktur des sogenannten Kaliumdekamolybdats KMo₅O₁₅OH.2H₂O