Synthesis and Characterisation of the First Cyanodiselenoimidocarbonate [C2N2Se2]2− Complexes

Burchell, Colin J.; Aucott, Stephen M.; Slawin, Alexandra M. Z.; Woollins, J. Derek

doi:10.1002/ejic.200400292

Cited by 7 publications

(5 citation statements)

References 32 publications

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“…In the same work it was reported that polyselenocyanogen could alternatively be prepared from selenocyanogen by heating in high boiling solvents such as xylenes and decalin. We have examined a number of selenium-containing systems [39][40][41][42][43][44] and it is reasonable to anticipate that CSe-N analogues of the C-S-N described here could exist and thus we conducted some preliminary experiments on (SeCN) x and it is appropriate to include our preliminary observations here.…”

mentioning

confidence: 92%

Investigations on Organo–Sulfur–Nitrogen Rings and the Thiocyanogen Polymer, (SCN)_x

Bowman

Burchell

Kilián

et al. 2006

Chemistry A European J

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The synthesis and full characterisation of a series of 1,2,4-thiadiazoles is reported. (SCN)(x) has been studied by a variety of techniques and the data compared with 1,2,4-thiadiazole and 1,2,4-dithiazoles. The observed data suggest that the polymer consists of 1,2,4-dithiazole rings linked by nitrogen atoms. For (SCN)(x), the MALDI-TOF mass spectroscopy showed a parent ion at 1149 and a series of peaks with (SCN)(2) repeat units (116 m/z); this result implies that (SCN)(2) may be the monomer unit of the polymer. Its IR spectrum shows a very broad peak with maximum at 1134 cm(-1) consisting of several overlapping peaks in the same region as ring vibrations for 1,2,4-thiadiazole and 1,2,4-dithiazole compounds. Peaks in the Raman spectrum in the range 400-480 cm(-1) support the presence of disulfide units within the polymer. The solid-state (13)C NMR (99 % (13)C-labelled) spectrum is dominated by two singlets of equal intensity at approximately 187 and 184 ppm with low intensity peaks in the range 152-172 ppm, in approximately the same range as both 1,2,4-thiadiazoles and 1,2,4-dithiazoles. The solid-state (15)N NMR (99 % (15)N labelled) spectrum displays two major peaks of similar intensity at 236.9 and 197.2 ppm, which are clearly very different environments to those observed in bis(3-bromo-1,2,4-thiadiazol-5-yl) disulfide, but similar to 1,2,4-dithiazoles. The X-ray structures of seven C-S-N systems are reported. Preliminary studies on (SeCN)(x) suggest that literature references to this polymer may be in error with the red solid actually being red selenium.

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confidence: 92%

Investigations on Organo–Sulfur–Nitrogen Rings and the Thiocyanogen Polymer, (SCN)_x

Bowman

Burchell

Kilián

et al. 2006

Chemistry A European J

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“…There are quite a few reports of platinum complexes containing selenium and phosphorus ligands, cis-P 2 PtSe 2 , and their NMR properties. 40,44,[50][51][52][53][54][55][56][57][58][59] For reasons of symmetry, most isotopomers of such complexes will constitute a higher-order spin system of type ABX 60,61 or of its limiting, non-existent, AA′X case. 62,63 Exceptions are the 31 P 2 and 31 P 2 , 195 Pt isotopomers and one 31 P 2 , 13 C isotopomer containing 13 C at the central CH 2 carbon of the dppp ligand.…”

Section: Nmr Spectroscopymentioning

confidence: 99%

“…The magnitude of the 2 J( 77 Se, 31 P) coupling constants obtained here is in agreement with values found in the literature. 40,44,[50][51][52][53][54][55][56][57][58][59]66 For the compound that comes closest to 1 and 2, [Pt(PPh 3 ) 2 (1,2-Se 2 -1,2-C 2 B 10 H 10 ], Wrackmeyer et al reported that the values of the 2 J( 77 Se, 31 P) coupling constants for the cis and trans pathways are very similar, around 51 Hz. 50 This could actually indicate a dynamic process, converting the AA′X spin system into A 2 X, not observed for 1, 2.…”

Section: Nmr Spectroscopymentioning

confidence: 99%

Selenium adducts of germa- and stanna-closo-dodecaborate: coordination at platinum, structural studies and NMR spectroscopy

et al. 2012

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The selenium adducts of germa- and stanna-closo-dodecaborate can coordinate at platinum via the selenium atom and result in the products [Pt(dppp)(Se-TB(11)H(11))(2)](2-) (T = Ge, Sn) (dppp = 1,3-bis(diphenylphosphino)propane). The monomeric tin compound [Pt(dppp)(Se-SnB(11)H(11))(2)](2-) is converted to a dimeric complex [Pt(2)(dppp)(2)(μ(2),μ'(2)-η(2)-Se(2)SnB(11)H(11))]. The new compounds were characterized by NMR spectroscopy in solution ((1)H, (11)B, (13)C, (31)P, (77)Se, (119)Sn, (195)Pt), elemental analysis and single crystal X-ray diffraction.

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“…3 ) 2 ] (R 0 ¼ H or Me; M ¼ Pd or Pt) has demonstrated that activation barriers are higher for platinum than palladium for all R, R 0 and E combinations studied. 63 Mono-, bi-and tetranuclear platinum group metal complexes of cyanodiselenoimidocarbonate, [C 2 N 2 Se 2 ] 2-, and triselenocarbonate, [CSe 3 ] 2were prepared by Woollins and co-workers, 64,65 , which was formulated on the basis of UV-Vis, RR and crystallography to possess a bis(m-S 2 dÀ ) dicopper(II) core, 68 the tetranuclear niobium complex [Nb 4 SO 5 (NCS) 10 ] 6is capped by a m 4 -sulfido ligand. 69 The counterion and crystallisation solvent are the dominant factors in determining the solid-state structures of [9]aneS 3 and [18]aneS 6 complexes of platinum(II), 70 while the first mononuclear selenoaroyl complexes were prepared from molybdenum alkylidyne precursors using mesityl isoselenocyanate.…”

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confidence: 99%

Oxygen, sulfur, selenium and tellurium

Bhattacharyya¹

2006

Annu. Rep. Prog. Chem., Sect. A: Inorg. Chem.

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As in previous years, this review will emphasise synthetic, structural and spectroscopic aspects of discrete molecular species containing Group 16 elements. Notable advances include the increasing prominence of organochalcogen-nitrogen heterocycles for materials applications and the wealth of structural motifs and forms of reactivity afforded by simple chemical transformations. Sulfur, selenium and telluriumWe begin by reviewing carbon-free rings, cages and clusters. [As 3 S 5 ][AlCl 4 ] and [As 3 Se 4 ][AlCl 4 ] are obtained by reaction of S 8 or selenium respectively with As-AsCl 3 -AlCl 3 melts at 80 1C, followed by slow cooling to 50 1C. 1 The cation structures are derived from As 3 E tetrahedra (E ¼ S or Se) with three edge-bridging selenium atoms in [As 3 Se 4 ] 1 and four edge-bridging sulfurs in [As 3 S 5 ] 1 . The geometry, phase stability and electronic properties of isolated selenium chains incorporated into nanoporous AlPO 4 -5 crystals were investigated, 2 [2,2,2-crypt-Na] 1 salts of [Tl 4 Se 8 ] 4and [Tl 2 Se 4 ] 2are generated by extracting NaTl 0.5 Se into ethylenediamine in the presence of 2,2,2-crypt and 18-crown-6, 3 and [cyclo-Te 4 ] [Ga 2 Br 7 ] 2 is available from the reaction between Te and GaBr 3 in benzene. 4 Potential energy hypersurfaces of S 7 and of [LiS 7 ] 1 were investigated by Steudel and coworkers using ab initio MO calculations at the G3X(MP2) level of theory. 5 The boatlike cyclo-S 7 conformer is less stable (by E12 kJ mol À1 ) than the chairlike form, for the fifteen [LiS 7 ] 1 complexes modelled, the calculated binding energies were À93.8 to À165.7 kJ mol À1 . The same workers have also investigated Li 1 complex formation with H 2 S, Me 2 S n (n ¼ 1-5) and isomers of S 6 . 6 The first telluradistibirane and telluradibismirane (Bbt) 2 E 2 Te (E ¼ Sb or Bi), containing E 2 Te rings, were obtained by treating (Bbt)EQE(Bbt) with n Bu 3 PTe at room temperature. 7 The telluradistibirane is stable in solution up to 140 1C, whereas the bismuth analogue eliminates (Bbt)BiQBi(Bbt) and (Bbt) 2 Te 2 at 100 1C. The S-S bond order in [S 2 I 4 ] 21 , judged by crystallography, vibrational spectroscopy and normal co-ordinate analysis to be 2.2-2.4, is among the highest values determined for heavier maingroup elements in an isolated compound. 8 Passmore and Laitinen have applied MP2, B3PW91 and PBE0 methods to predict structural and spectroscopic parameters for [SeX 3 ] 1 and SeX 2 (X ¼ Cl, Br or I), 9 finding close agreement with experimental data, while the mixed-valence bromoselenate [Et 4 N] 2 [Se 3 Br 8 (Se 2 Br 2 )] is accessible from the reaction between selenium and Br 2 in acetonitrile, in the presence GDC,

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Synthesis and Characterisation of the First Cyanodiselenoimidocarbonate [C₂N₂Se₂]²⁻ Complexes

Cited by 7 publications

References 32 publications

Investigations on Organo–Sulfur–Nitrogen Rings and the Thiocyanogen Polymer, (SCN)_x

Investigations on Organo–Sulfur–Nitrogen Rings and the Thiocyanogen Polymer, (SCN)_x

Selenium adducts of germa- and stanna-closo-dodecaborate: coordination at platinum, structural studies and NMR spectroscopy

Oxygen, sulfur, selenium and tellurium

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Synthesis and Characterisation of the First Cyanodiselenoimidocarbonate [C2N2Se2]2− Complexes

Cited by 7 publications

References 32 publications

Investigations on Organo–Sulfur–Nitrogen Rings and the Thiocyanogen Polymer, (SCN)x

Investigations on Organo–Sulfur–Nitrogen Rings and the Thiocyanogen Polymer, (SCN)x

Selenium adducts of germa- and stanna-closo-dodecaborate: coordination at platinum, structural studies and NMR spectroscopy

Oxygen, sulfur, selenium and tellurium

Contact Info

Product

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Synthesis and Characterisation of the First Cyanodiselenoimidocarbonate [C₂N₂Se₂]²⁻ Complexes

Investigations on Organo–Sulfur–Nitrogen Rings and the Thiocyanogen Polymer, (SCN)_x

Investigations on Organo–Sulfur–Nitrogen Rings and the Thiocyanogen Polymer, (SCN)_x