Bis(isopropylammonium) tetrasulfidomolybdate(VI)

Srinivasan, Bikshandarkoil R.; Näther, Christian; Bensch, Wolfgang

doi:10.1107/s1600536807063337

Cited by 6 publications

(6 citation statements)

References 9 publications

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“…The anionic chains of the coordination polymer 1 exhibit a {[CuL 2 ] 2– } n layered structure, which acts as an inorganic layer to hold the [Hipa] + cations. This provides an example of isopropyl ammonium cations held between the layers of complex anions through –NH 3 + –COO – hydrogen bonds (Figure 1, b); isopropyl ammonium cations are generally held in the layers of complex anions such as tetrachlorocuprate15a or molybdate15b by other weak interactions.…”

Section: Resultsmentioning

confidence: 99%

Cation Exchange in Layered Copper(II) Coordination Polymers

2013

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The covalently linked anionic layers of a series of CuII 2,3‐pyridinecarboxylate anions containing organic cations are characterized. Depending on the cations, mononuclear, dinuclear or polynuclear complexes are formed. The complex with adeninium cations is mononuclear, whereas the complexes bearing cations of 4‐aminobenzylamine, 1,5‐diaminopentane, and 5‐aminoquinoline are dinuclear, and complexes bearing cations of isopropylamine, ethylenediamine, 1,8‐diaminooctane, N,N,N′,N′‐tetramethylethylenediamine, tris(2‐aminoethyl)amine, 1,4‐diazabicyclo[2.2.2]octane, imidazole, pyridine, 8‐hydroxyquinoline, and cytidine are coordination polymers. All of the complexes other than the one bearing tris(2‐aminoethyl)amine cations have lamellar structures. The polynuclear complex anion with tris(2‐aminoethyl)amine trications exhibits an unusual –3 charge for the polynuclear anionic nodes. The 1H,9H‐adeninium cationic dimers are stabilized in the interstices of mononuclear CuII quinolinate complex anions. The interlayer separations in the layered polymers varied from 8.5 to 15.9 Å and are guided by the cations. Biologically relevant cytidinium cations are trapped in the layers of polymeric anions. The complexes bearing organocations undergo exchange of the organic cations with alkali, alkaline earth, or transition metal ions or with smaller cations without disturbance of the polymeric inorganic layer. The exchange of the cytidinium cations by metal ions resulted in polymeric complexes in which the cationic organic layer is replaced by a layer of aquated metal cations. The thermochemical properties, electron paramagnetic resonance (EPR) spectroscopy, and solid‐state conductance of the complexes are described.

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Section: Resultsmentioning

confidence: 99%

Cation Exchange in Layered Copper(II) Coordination Polymers

2013

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“…In compound 3 two C atoms are disordered in two orientations and were refined using a split model and restraints. For compound 4 the absolute structure was determined and is in agreement with the selected setting (Flack X parameter: À 0.039 (43) by classical fit to all intensities and À 0.031(24) from 1376 selected quotients (Parsons' method). The technical details of data acquisition and some selected refinement results are summarized in Table 1.…”

Section: X-ray Crystal Structure Determinationmentioning

confidence: 99%

“…A survey of the Cambridge Structural Database (CSD) [36] reveals more than thirty tetrasulfidomolybdates have been structurally characterized (Table 4). [21,25,26,30,33,35,[37][38][39][40][41][42][43][44][45][46][47][48][49][50][51][52][53][54][55] The availability of structural information of several compounds permits a comparative study, the details of which are described here. The isolation of [MoS 4 ] 2 À anions charge balanced by a variety of cations namely alkali metal cations like K + , Rb + , Cs + , (entry nos.…”

Section: Structural Chemistry Of Tetrasulfidomolybdatesmentioning

confidence: 99%

Synthesis, Spectral Characterization and Crystal Structures of Five Organic Ammonium Tetrasulfidomolybdates

et al. 2021

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The syntheses, spectral characterization and crystal structures of five organic ammonium tetrasulfidomolybdates namely (C 4 H 12 N) 2 [MoS 4 ] 1 (C 4 H 12 N is 2-methyl-propan-2-aminium), (C 5 The charge balancing cations in 1-3 are protonated methyl substituted propanamines, while the dications of 4 and 5 are derived from a tetraamine and a cyclic diamine respectively. The crystal structures of 1 to 5 consist of an unique tetrahedral [MoS 4 ] 2À dianion charge balanced by a crystallographically independent organic dication for all compounds excepting 1 which contains a pair of unique (2-methylpropan-2-aminium) monocations. Although all the compounds are crystallized from aqueous solutions, 1 to 4 are anhydrous while 5 is a hemihydrate. In the crystal structures, the organic cations and the tetrasulfidomolybdate dianions are interlinked with the aid of several NÀ H⋅⋅⋅S and CÀ H⋅⋅⋅S hydrogen bonding interactions. In addition to NÀ H⋅⋅⋅S and CÀ H⋅⋅⋅S hydrogen bonds, compound 5 exhibits NÀ H⋅⋅⋅O and OÀ H⋅⋅⋅O hydrogen bonding interactions involving the H 2 O molecule, which interlinks pairs of anions with pairs of cations. Hirshfeld surface analyses were performed which reveal distortion of the [MoS 4 ] 2À tetrahedra, extensive S⋅⋅⋅H interactions between the anions and cations and also H⋅⋅⋅H contacts between the cations. A comparative study of the structural chemistry of thirty-eight tetrasulfidomolybdates is described.

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“…[11][12][13][14][15][16][17] A number of salts consisting of discrete tetrathiomolybdate and organic ammonium ions, associated with one another through NH 3 3 3 S hydrogen bonding, have been prepared. [18][19][20][21][22][23][24][25][26][27] The ability of MoS 4 2-to coordinate transition metal centers, particularly Cu þ , has also led to its use as a component in clusters and networks. [28][29][30][31][32][33] Polymorphism has so far been observed in a very limited number of tetrathiomolybdate-based compounds.…”

Section: Introductionmentioning

confidence: 99%

“…The tetrathiomolybdate anion, MoS 4 2− , is a versatile building block that can act as a ligand or counteranion in mixed inorganic−organic structures. Because of the decomposition of MoS 4 2− to MoS 2 at elevated temperatures, (NH 4 ) 2 MoS 4 and other compounds containing the anion are frequently used as precursors to hydrodesulfurization (HDS) catalysts. − A number of salts consisting of discrete tetrathiomolybdate and organic ammonium ions, associated with one another through NH···S hydrogen bonding, have been prepared. − The ability of MoS 4 2− to coordinate transition metal centers, particularly Cu + , has also led to its use as a component in clusters and networks. − Polymorphism has so far been observed in a very limited number of tetrathiomolybdate-based compounds. Two tetragonal forms have been reported for a tetra- n -butylammonium salt of the MoS 4 (CuCl) 4 2− cluster .…”

Section: Introductionmentioning

confidence: 99%

Structure and Polymorphism in M(ethylenediamine)₃MoS₄ (M = Mn, Co, Ni)

Tian

Iliff

Moore

et al. 2009

Crystal Growth & Design

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Polymorphism in hybrid inorganic-organic materials has not been explored as extensively as that in organic compounds, yet differences in solid-state structure can significantly affect the physical properties central to application of these materials. A new polymorph of Ni(en) 3 MoS 4 (en = ethylenediamine), a hydrodesulfurization catalyst precursor, has been synthesized solvothermally and structurally characterized by single-crystal X-ray diffraction. The new structure (2) assumes the orthorhombic Pcab space group with a=14.020(5) A ˚, b=14.821(7) A ˚, and c=16.230(6) A ˚. The structure of a polymorph that had been found previously (1) was redetermined at 100 K, confirming the orthorhombic Pna2 1 structure with a=15.916(13) A ˚, b=7.610(3) A ˚, and c=14.093(6) A ˚. Solvothermal reaction conditions including temperature, solvent water content, and nickel source were important in controlling polymorph formation. Differential scanning calorimetry and solvent-mediated conversion studies were used to compare the stabilities of the two nickel-containing polymorphs. The system was characterized as enantiotropic, with 2 favored at ambient temperature and 1 favored at 120 °C. However, kinetic factors are influential in the intermediate temperature range, and conversion is kinetically hindered under certain conditions. The new structures Co-(en) 3 MoS 4 (3) and Mn(en) 3 MoS 4 (4) were determined through single-crystal methods to be isostructural to 2. Compounds 1-4 were also characterized by elemental analysis, infrared spectroscopy, variable-temperature magnetic susceptibility measurements, and thermogravimetric analysis.

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Bis(isopropylammonium) tetrasulfidomolybdate(VI)

Abstract: Acta Cryst. (2008). E64, m66-m67 Srinivasan et al. (C 3 H 10 N) 2 [MoS 4 ] m67

Cited by 6 publications

References 9 publications

Cation Exchange in Layered Copper(II) Coordination Polymers

Cation Exchange in Layered Copper(II) Coordination Polymers

Synthesis, Spectral Characterization and Crystal Structures of Five Organic Ammonium Tetrasulfidomolybdates

Structure and Polymorphism in M(ethylenediamine)₃MoS₄ (M = Mn, Co, Ni)

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Bis(isopropylammonium) tetrasulfidomolybdate(VI)

Abstract: Acta Cryst. (2008). E64, m66-m67 Srinivasan et al. (C 3 H 10 N) 2 [MoS 4 ] m67

Cited by 6 publications

References 9 publications

Cation Exchange in Layered Copper(II) Coordination Polymers

Cation Exchange in Layered Copper(II) Coordination Polymers

Synthesis, Spectral Characterization and Crystal Structures of Five Organic Ammonium Tetrasulfidomolybdates

Structure and Polymorphism in M(ethylenediamine)3MoS4 (M = Mn, Co, Ni)

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Structure and Polymorphism in M(ethylenediamine)₃MoS₄ (M = Mn, Co, Ni)