The interaction of H2S gas with aqueous ammonium heptamolybdate solution in the presence of diethylenetriamine (dien) led to the formation of diethylenetriammonium tetrathiomolybdate crystals. The elemental analyses, UV-Visible, IR, and 1H NMR spectra suggested the presence of organic cation and (MoS4)2- moiety. The 1H NMR revealed the presence of two sets of symmetrical A2X2 multiple patterns. The compound crystallizes in the monoclinic system with space group Pn, a = 7.196(6), b = 7.532(3), c = 11.525(10) Å, α = 90°, β = 90.17(3)°, γ = 90°, V = 624.78(8) Å3, and Z = 2, wR1 = 0.0261 and wR2 = 0.0698. The structure consists of tetrahedral tetrathiomolybdate anions, which form an extended three-dimensional network in the solid state with Mo-S⋯H-N hydrogen bonding with the organic cation.

Babu Varghese

Ammonia

anion

cation

DIETHYLENETRIAMMONIUM TETRATHIOMOLYBDATE

ethylene derivative

Hydrogen

molybdic acid

nitrogen

Sulfur

Thiophene

unclassified drug

aqueous solution

article

complex formation

Crystal Structure

Crystallization

hydrogen bond

infrared spectroscopy

molecular dynamics

molecular interaction

Molecular mechanics

proton nuclear magnetic resonance

reaction analysis

solid state

structure analysis

synthesis

Ultraviolet spectroscopy

X ray analysis

IIT Madras is a public technical and research university located in Chennai, Tamil Nadu. Founded in 1959, it is recognised as an Institute of National Importance.

IIT Madras has been ranked as the top engineering institute in India for four years in a row by the National Institutional Ranking Framework of the MHRD

It currently offers undergraduate, postgraduate and research degrees across 16 disciplines in Engineering, Sciences, Humanities and Management. About 596 faculty belonging to science and engineering departments and centres of the Institute are engaged in teaching, research and industrial consultancy.

IIT Madras

Preparation, characterization, and X-ray structure analysis of diethylenetriammonium tetrathiomolybdate

Journal of Chemical Crystallography

The reaction of H2S gas with an aqueous solution of ammonium heptamolybdate in the presence of 1,4-diazabicyclo-2,2,2-octane (DABCO) led to the formation of a red colored complex. The complex was recrystallized in hot water and characterized by elemental analysis and UV-Visible, FT-IR, and 1H NMR spectroscopy. The single sharp peak in the 1H NMR spectrum has revealed that all the methylene protons are equivalent due to the hydrogen resonating between the two nitrogens in the DABCO cation. The complex crystallizes in a cubic system with space group P213, a = 10.9482(9) Å, α = 90°, V = 1325.3(7) Å3, R 1 = 0.0154, wR 2 = 0.038, Z = 4. The structure consists of the tetrahedral tetrathiomolybdate anions, which form an extended three-dimensional network in the solid state involving Mo-S...H-N hydrogen bonding interactions with DABCO and the ammonium cation. © 2004 Springer Science+Business Media, Inc.

Journal of Structural Chemistry

Preparation, characterization, and x-ray structure analysis of 1,4-diazabicyclo-2,2,2-octane (DABCO) and ammonium cation with tetrathiomolybdate anion

The interaction of hard base chelating agents (LH) such as 8-quinolinol (oxH), salicylaldehyde (salH) and N-nitrosophenylhydroxylamine (NphaH) with ammonium tetrathiomolybdate(VI), (1), in aqueous solution yields disulphidomolybdenum(VI) complexes, [MoS2L2]. The i.r. absorptions at 540 and 510 cm-1 are assigned to v(Mo-S), which indicate that the two sulphido-groups are cis to each other, The interaction of (1) with soft base chelating agents (SS), such as dithiocarbamates (dtc), dithiophosphate (dtp) and xanthates (xan) yields dimeric sulphido-bridged sulphidomolybdenum(V) complexes, [Mo2S4(SS)2] and with potassium ethylthioxanthate (KEttxan) yields a molybdenum(IV) complex, [Mo(Ettxan)4]. The [Mo2S4(R2dtc)2] complexes were also obtained by the interaction of [MoO2(R2dtc)2] with phosphorus pentasulphide in xylene. It was concluded that tetrathiomolybdate(VI) undergoes facile reduction when compared with tetraoxomolybdate(VI). © 1986 VCH Verlagsgesellschaft mbH.

Transition Metal Chemistry

Reactivity of the tetrathiomolybdate(VI) anion towards hard and soft base chelating agents

Isothiocyanatooxomolybdenum(V) complexes, [MoO-(NCS)(R2dtc)2] (R=ethyl or dibenzyl; R2=piperidinyl or 4-morpholinyl) have been prepared and characterized. The i.r. spectral bands at 2020 cm-1 are assigned to v(CN) which suggest that thiocyanate coordinates through nitrogen. The bands at 930, 1500 and 960 cm-1 are attributed to v(MoO), v(CN) and v(CS), respectively, and indicate the presence of the MoO3+ moiety and a bidentate dithiocarbamate group. The e.p.r. and electronic spectral data together with magnetic moment values (1.69 B.M.) suggest the presence of one unpaired electron. The complexes are monomeric. The thermal decomposition behaviour of the complexes is reported. © 1984 Verlag Chemie GmbH.

Isothiocyanatooxomolybdenum(V) dithiocarbamates

Electron Crystallography

Crystal Structure Refinement Incorporating Chemical Information

Journal of Materials Science

10.1023/a:1018538424373

Advances in Catalysis

Fundamental Studies of Transition-Metal Sulfide Catalytic Materials

Journal	Journal of Chemical Crystallography
ISSN	10741542
Open Access	No