“…4,5 New developments in the latter respect came from the utilization of small clusters as building blocks for the formation of nanoparticles with controllable size and shape through photolytic decomposition and solvothermal synthesis. [6][7][8][9][10] For some time metal chalcogenolato complexes have also been investigated due to oligomeric (e.g. ring-like) or polymeric structures.…”
Reactions of [Co(N(SiMe))thf] with 2.1 equiv. of MesSH (Mes = CH-2,4,6-(CH)) yield dark brown crystals of the one dimensional chain compound [Co(SMes)]. In contrast reactions of [Co(N(SiMe))thf] with 2.1 equiv. of PhSH result in the formation of a dark brown almost X-ray amorphous powder of 'Co(SPh)'. Addition of aliquots of CHOH to the latter reaction resulted in the almost quantitative formation of crystalline ammonia thiolato complexes either [Co(SPh)(NH)] or [Co(SPh)NH]. Single crystal XRD reveals that [Co(SPh)NH] forms one-dimensional chains in the crystal via μ-SPh bridges whereas [Co(SPh)(NH)] consists at a first glance of isolated distorted tetrahedral units. Magnetic measurements suggest strong antiferromagnetic coupling for the two chain compounds [Co(SMes)] (J = -38.6 cm) and [Co(SPh)NH] (J = -27.1 cm). Interestingly, also the temperature dependence of the susceptibility of tetrahedral [Co(SPh)(NH)] shows an antiferromagnetic transition at around 6 K. UV-Vis-NIR spectra display d-d bands in the NIR region between 500 and 2250 nm. Thermal gravimetric analysis of [Co(SPh)(NH)] and [Co(SPh)NH] reveals two well separated cleavage processes for NH and SPh upon heating accompanied by the stepwise formation of 'Co(SPh)' and cobalt sulfide.
“…4,5 New developments in the latter respect came from the utilization of small clusters as building blocks for the formation of nanoparticles with controllable size and shape through photolytic decomposition and solvothermal synthesis. [6][7][8][9][10] For some time metal chalcogenolato complexes have also been investigated due to oligomeric (e.g. ring-like) or polymeric structures.…”
Reactions of [Co(N(SiMe))thf] with 2.1 equiv. of MesSH (Mes = CH-2,4,6-(CH)) yield dark brown crystals of the one dimensional chain compound [Co(SMes)]. In contrast reactions of [Co(N(SiMe))thf] with 2.1 equiv. of PhSH result in the formation of a dark brown almost X-ray amorphous powder of 'Co(SPh)'. Addition of aliquots of CHOH to the latter reaction resulted in the almost quantitative formation of crystalline ammonia thiolato complexes either [Co(SPh)(NH)] or [Co(SPh)NH]. Single crystal XRD reveals that [Co(SPh)NH] forms one-dimensional chains in the crystal via μ-SPh bridges whereas [Co(SPh)(NH)] consists at a first glance of isolated distorted tetrahedral units. Magnetic measurements suggest strong antiferromagnetic coupling for the two chain compounds [Co(SMes)] (J = -38.6 cm) and [Co(SPh)NH] (J = -27.1 cm). Interestingly, also the temperature dependence of the susceptibility of tetrahedral [Co(SPh)(NH)] shows an antiferromagnetic transition at around 6 K. UV-Vis-NIR spectra display d-d bands in the NIR region between 500 and 2250 nm. Thermal gravimetric analysis of [Co(SPh)(NH)] and [Co(SPh)NH] reveals two well separated cleavage processes for NH and SPh upon heating accompanied by the stepwise formation of 'Co(SPh)' and cobalt sulfide.
“…The inner angle Se1-In-Se1 i (98.0 ) of the "CuSe 2 In" ring and outer angle Se2-In-Se2 i (111.1 ) formed by the terminal selenolate groups are less deviated from the ideal tetrahedral angle in comparison to the corresponding angles (96.1 and 116.6) in the reported complex [(Ph 3 P) 2 Cu(m-SePh) 2 In(SePh) 2 ]. 15 The spacer CH 2 group of the benzylselenolate ligand in the present complex helps to minimise the steric repulsion between the bulkier groups which is manifested in the reduced non-bonded Cu/In distance of about 3.35Å, compared to analogous phenyl selenolate complex (3.50Å). 15 The benzyl groups adopt anti conformation and a two-fold symmetry axis exist along the Cu-In bond in the molecular structure.…”
Section: Crystallographymentioning
confidence: 87%
“…15 The spacer CH 2 group of the benzylselenolate ligand in the present complex helps to minimise the steric repulsion between the bulkier groups which is manifested in the reduced non-bonded Cu/In distance of about 3.35Å, compared to analogous phenyl selenolate complex (3.50Å). 15 The benzyl groups adopt anti conformation and a two-fold symmetry axis exist along the Cu-In bond in the molecular structure. As expected the tetrahedral Cu center is more distorted due to the two bulkier phosphines as revealed by the P1-Cu-P1 i angle measuring 122.2 .…”
Section: Crystallographymentioning
confidence: 87%
“…In contrast to the complexes of Cu and In using ethyl selenolate/phenyl selenolate, 5,13,15 the pyridylselenolates of Cu and In do not react with each other to form heterometallic chalcogenolates. 16 This non reactivity can be attributed to the presence of the pyridine donors, which compete effectively with bridging selenolate ligands for access to the metal coordination sphere to form molecular indium compounds and to the stabilizing inuence of the Cu-Cu bonds in the copper compounds.…”
Section: Syntheses and Nmr Spectroscopymentioning
confidence: 95%
“…10 The solvothermal route under mild reaction conditions using single-source precursors (SSPs) has emerged as highly efficient tool for the controlled preparation of nanostructures. Since the rst report of [(PPh 3 ) 2 CuIn(SEt) 4 ] in 1993 by Hirpo et al, 13 the complexes of the general formula [(PR 3 ) n CuM(ER 0 ) 4 ] (R, R 0 ¼ alkyl, aryl) 5, [13][14][15][16] have been extensively investigated as SSPs for the preparation of thin lm of CuME 2 using CVD technique. A few such SSPs have also been used to prepare the nanoparticles of CuME 2 at reduced temperature.…”
The complex [(Ph3P)2Cu(μ-SeCH2Ph)2In(SeCH2Ph)2] has been synthesized and structurally characterized, which on solvolysis yielded single phasic CuInSe2 nanoparticles. The particles were characterized by pXRD, SEM, HRTEM, EDX and DRS analysis.
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