Synthesis and structure of the cluster μ₃‐sulfido‐μ‐–(diethylphosphorodithioato‐S, S'‐)‐allylthioureocyclo‐tris‐[ (μ‐sulfido)‐χ‐(diethylphosphorodithioato‐S, S')‐molybdenum(IV)], Mo₃S₄(C₄H₁₀O₂S₂P)₄(C₄H₈N₂S)

Abstract

Title compound, Mr =1273.16, was synthesized by a substitution reaction and its crystal is triclinic belonging to space group P1 with cell parameters: a =13.944(2), b =14.143(7), c =14.233(3) Å, α =77.35(3)°, β =69.94(2)°, γ =63.50(3)°, V=2351(1) Å3, Z=2, Dc =1.799g cm−2. Room temperature, graphite‐filtered Mo Kα radiation (λ =0.71073Å) was used for data collection. μ =14.988 cm−1, F(000) =1280, R=0.051 for 7025 observed reflections. The crystal consists of decrete cluster molecules containing a cluster core [Mo2(μ3‐S)]10+ with three μ‐S, one μ‐dtp(dtp =[S2P(OC2H5)]2‐), three χ‐dtp and one allylthioureo to form a local six‐coordinated sphere around each Mo atom. The bonds of cluster skeleton [Mo3(μ3‐S)(μ‐S)3]4+, MoMo 2.744∼2.766, Mo—(μ2‐S) 2.340∼2.342 and Mo—(μ‐S)2.272∼2.296 Å, are comparable with those found in the related analogues.

Surface Analysis and Photoelectrochemical Studies of Mixed Polycrystals of p ‐ WSe2 / WS 2

“…This tendency has been previously observed in RuS2 xSe~ single crystals. 25 We have noticed from the SEM that the distribution of the crystal size of compound IIIr was not as homogeneous as in compounds Ir and IIr. In addition, in the XRF and in AES depth profile semiquantitative analysis, compound IIIs had shown an unexpectedly huge Se/S intensity ratio.…”

Preparation and Crystal Growth of Transition Metal Dichalcogenides

“…[238] RuSe 2 : (a) [251,257,258] , (b) [251,255,256] On (a): RuSe 2 can be crystallized by chemical transport with Cl 2 or ICl 3 . [251,257,258] On (b): The synthesis of large single crystals of RuSe 2 from a tellurium melt was described. [255,256] Se and Bi melts are also suitable for crystallization.…”

“…RuCh 2 mixed phases (Ch = S, Se, Te): (a) [257,258] , (c) [255] On (a): The synthesis of mixed phases, in which the substitution takes place in the anion sub-lattice, succeeds in the same way as that of the binary Ru chalcogenides.…”

“…[251,[254][255][256] It was also possible to grow RuS 2 crystals from a PbCl 2 melt. [238] RuSe 2 : (a) [251,257,258] , (b) [251,255,256] On (a): RuSe 2 can be crystallized by chemical transport with Cl 2 or ICl 3 . [251,257,258] On (b): The synthesis of large single crystals of RuSe 2 from a tellurium melt was described.…”