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1.
The Reaction of Bunsen's Cacodyl Disulfide,Me2As(S)‐S‐AsMe2, with Iodine: Preparation and Properties of Dimethylarsinosulfenyl Iodide,Me2As‐S‐I 下载免费PDF全文
Panayiotis V. Ioannou Dimitris G. Vachliotis Athanassios Chrissanthopoulos 《无机化学与普通化学杂志》2015,641(7):1340-1346
Bunsen's cacodyl disulfide, Me2As(S)‐S‐AsMe2 ( 1 ), reacted with iodine giving the novel dimethylarsinosulfenyl iodide, Me2As‐S‐I ( 3 ) although theoretical calculations indicated that the AsV compound Me2As(S)‐I ( 4 ) was more stable in the gas phase. The oily product was stable neat and as a solution in CDCl3 at +4 °C and –20 °C for at least 15 d. Light, H2O, H2O2, and Zn dust, but not NaI or Ag, decomposed it. Compound 3 did not interact with Ph3N, with Ph2NH and PhNH2 it interacted but not reacted. 3 was decomposed by piperidine, with pyridine and 4‐dimethylaminopyridine it interacted and produced Me2As‐SS‐AsMe2 ( 2 ) and I2 that formed charge transfer complexes Base · I2, whereas Et3N decomposed 3 , and 3Et3N · 2I2 was isolated. 3 was desulfurized by Ph3P and (Me2N)3P completely, and by (PhO)3P and (PhS)3P partially. The reactions of 3 with (Me2N)3P, (PhS)3P, and (EtO)3P were complicated. From the AsIII nucleophiles, only Ph3As was bound, while (PhS)3As reacted slowly in a complicated manner with 3 . No interaction of 3 with MeOH or PhOH was observed but NaOH, Ag2O, and PhONa decomposed it. Thiophenol produced traces of Me2As‐SPh ( 10 ) and sodium thiophenolate attacked mainly at AsIII of 3 . Thus, externally stabilized sulfenium ions of the type Me2As‐S‐Nu+I– were not obtained. 相似文献
2.
Iliana E. Medina‐Ramírez Mark J. Fink James P. Donahue 《Acta Crystallographica. Section C, Structural Chemistry》2009,65(12):m475-m477
The title compound, [Zn3(C9H21SiS)6] or [(iPr3SiS)Zn(μ‐SSiiPr3)2Zn(μ‐SSiiPr3)2Zn(SSiiPr3)], is the first structurally characterized homoleptic silanethiolate complex of zinc. A near‐linear arrangement of three ZnII ions is observed, the metals at the ends being three‐coordinate with one terminally bound silanethiolate ligand. The central ZnII ion is four‐coordinate and tetrahedral, with two bridging silanethiolate ligands joining it to each of the two peripheral ZnII ions. The nonbonding intermetallic distances are 3.1344 (11) and 3.2288 (12) Å, while the Zn...Zn...Zn angle is 172.34 (2)°. A trimetallic silanethiolate species of this type has not been previously identified by X‐ray crystallography for any element. 相似文献
3.
Tomoyuki Mochida Kousuke Takazawa Michio M. Matsushita Tadashi Sugawara 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(8):m431-m433
In the title compound, (C16H36N)2[Co(C4N2S2)2]2, pairs of [Co(C4N2S2)2]? anions combine to form discrete crystallographically centrosymmetric dimers, which stack along the c axis, surrounded by the counter‐cations. The metal atom in the anion has a five‐coordinate distorted square‐pyramidal geometry. 相似文献
4.
Ali M. S. Hebishy Galal H. Elgemeie Ahmed H. M. Elwahy 《Journal of heterocyclic chemistry》2019,56(5):1581-1587
A synthesis of novel bis(aminopyrazoles) by the reaction of hydrazine hydrate with the appropriate bis(2‐cyanoketene‐S,N‐acetals) was reported. The latter compounds were prepared by treatment of bis(cyanoacetamides) with phenyl isothiocyanate in KOH/EtOH and subsequent alkylation with methyl iodide. The utility of bis(2‐cyanoketene‐S,S‐acetals) as building blocks for novel bis(aminopyrazoles) was also investigated. 相似文献
5.
Takayoshi Suzuki Hideo D. Takagi Kazuo Kashiwabara 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(2):m95-m97
Purple prismatic crystals of the title compound, [Co2(C3H6NS2)4(C8H11O2P)2](PF6)2, were obtained by repeated recrystallization of trans‐[Co(C3H6NS2)2‐(C8H11O2P)2]PF6 from CH3CN/Et2O and then from MeOH/CH2Cl2; during recrystallization one of the P(OMe)2Ph ligands was dissociated from the CoIII center and the resulting CoIII complex fragment underwent dimerization. The complex cation has a dinuclear structure bridged by one S atom of each of two of the N,N‐dimethyldithiocarbamate ligands, and has crystallographically imposed C2 symmetry. Two P(OMe)2Ph ligands are coordinated at the transoid positions of the Co2(μ‐C3H6NS2)2(C3H6NS2)2 moiety, with Co—P bond lengths of 2.1921 (11) Å. 相似文献
6.
CuYS2: A Ternary Copper(I) Yttrium(III) Sulfide with Chains {[Cu(S1)3/3(S2)1/1]3–} of cis ‐Edge Connected [CuS4]7– Tetrahedra Pale yellow, lath‐shaped single crystals of the ternary copper(I) yttrium(III) sulfide CuYS2 are obtained by the oxidation of equimolar mixtures of the metals (copper and yttrium) with sulfur in the molar ratio 1 : 1 : 2 within fourteen days at 900 °C in evacuated silica ampoules, while the presence of CsCl as fluxing agent promotes their growth. The crystal structure of CuYS2 (orthorhombic, Pnma; a = 1345.3(1), b = 398.12(4), c = 629.08(6) pm, Z = 4) exhibits chains of cis‐edge linked [CuS4]7– tetrahedra with the composition {[Cu(S1)3/3(S2)1/1]3–} running along [010] which are hexagonally bundled as closest rod packing. Charge equalization and three‐dimensional interconnection of these anionic chains occur via octahedrally coordinated Y3+ cations. These are forming together with the S2– anions a network [Y(S1)3/3(S2)3/3]– of vertex‐ and edge‐shared [YS6]9– octahedra with ramsdellite topology. The metall‐sulfur distances of the [CuS4]7– tetrahedra (230 (Cu–S2), 232 (Cu–S1), and 253 pm (Cu–S1′, 2 × )) cover a very broad interval, whilst these (Y–S: 267–280 pm) within the [YS6]9– octahedra range rather closely together. 相似文献
7.
The centrosymmetric [Zn2{CH3OC6H4P(OC5H9)S2}4], features an eight‐membered Zn2S4P2 ring as a result of two bidentate bridging thiolate ligands; the remaining ligands are chelating. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
8.
Jos S. Casas Eduardo E. Castellano M. S. García Tasende Agustín Snchez Jos Sordo Ezequiel M. Vzquez‐Lpez Julio Zukerman‐Schpector 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(2):182-183
The crystal structure of the title compound, [Hg(C11H8N)(C12H22PS2)], consists of molecules in which the Hg atom is coordinated strongly to the C atom in position 2 of the phenyl group and to one of the dithiophosphinate S atoms, and at longer distances to the pyridine N atom and the other S atom. The C—Hg—S fragment involving the S atom more strongly bound to Hg is almost linear [C—Hg—S = 178.9 (3)°]. 相似文献
9.
Stphane A. Baudron Patrick Batail 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(12):m575-m577
The crystal structures of the title compounds, (C24H20P)2[Ni(C6H6O4S2)2], (I), and (C24H20P)2[Ni(C6H6O4S2)2]I, (II), in the diamagnetic reduced (2–) and paramagnetic oxidized (1–) states, are reported at 200 and 293 K, respectively. In both compounds, the Ni atom lies on an inversion centre and the NiS4 coordination is thus required to be exactly planar. In the diamagnetic complex, (I), the Ni—S distances are 2.1818 (7) and 2.1805 (6) Å, while they are 2.1481 (6) and 2.1392 (5) Å in the paramagnetic complex, (II). This results from both the different complex core oxidation states and the different conformations of the methoxycarbonyl groups. 相似文献
10.
Hiroshi Katagiri Masao Morimoto Kenichi Sakai 《Acta Crystallographica. Section C, Structural Chemistry》2010,66(1):o20-o24
The crystal structures of a pair of diastereomeric 1:2 salts of (R)‐ and (S)‐2‐methylpiperazine with (2S,3S)‐tartaric acid, namely (R)‐2‐methylpiperazinediium bis[hydrogen (2S,3S)‐tartrate] monohydrate, (I), and (S)‐2‐methylpiperazinediium bis[hydrogen (2S,3S)‐tartrate] monohydrate, (II), both C5H14N22+·2C4H5O6−·H2O, each reveal the formation of well‐defined head‐to‐tail‐connected hydrogen tartrate chains; these chains are linked into a two‐dimensional sheet via intermolecular hydrogen bonds involving hydroxy groups and water molecules, resulting in a layer structure. The (R)‐2‐methylpiperazinediium ions lie between the hydrogen tartrate layers in the most stable equatorial conformation in (I), whereas in (II), these ions are in an unstable axial position inside the more interconnected layers and form a larger number of intermolecular hydrogen bonds than are observed in (I). 相似文献
11.
Raymundo Cea-Olivares Klaus H. Ebert Luminita Silaghi-Dumitrescu Ionel Haiduc 《Heteroatom Chemistry》1997,8(4):317-321
The crystal and molecular structures of bismuth(III) dimethyldithioarsinate, Bi(S2AsMe2)2, were investigated by X-ray diffraction. The compound is a centrosymmetric dimer in which pentagonal-bipyramidal monomeric units are associated through secondary Bi–S interactions. The structure is compared with that of the analogous dithiophosphinate, Bi(S2PMe2)2. © 1997 John Wiley & Sons, Inc. 相似文献
12.
《Journal of mass spectrometry : JMS》2017,52(10):681-688
The ability of positively charged aggregates of the surfactant (1R ,2S )‐dodecyl(2‐hydroxy‐1‐methyl‐2‐phenylethyl)dimethylammonium bromide (DMEB) to incorporate D‐tryptophan or L‐tryptophan in the gas phase has been investigated by electrospray ion mobility mass spectrometry (ESI‐IM‐MS). Strongly impacted by the pH of the electrosprayed solutions, both protonated (T+) and deprotonated (T−) tryptophan are effectively included into the aggregates, whereas, tryptophan in zwitterionic (T0) form is practically absent in singly charged DMEB aggregates but can be found in multiply charged ones. The ability to incorporate tryptophan increases with the aggregation number and charge state of aggregates. More than 1 tryptophan species can be entrapped (aggregates including up to 5 tryptophan are observed). Collision induced dissociation experiments performed on the positively singly charged DMEB hexamer containing 1 T− show that at low collision energies the loss of a DMEB molecule is preferred with respect to the loss of the DMEB cation plus T− species which, in turn, is preferred with respect to the loss of mere tryptophan, suggesting that the deprotonated amino acid is preferentially located in proximity of a DMEB head group and with the ionic moiety pointing towards the core of the aggregate. The analysis of the collision cross sections (CCS) of bare and tryptophan containing aggregates allowed evaluating the contributions of tryptophan and bromide ions to the total aggregate CCS. No significant discrimination between D‐tryptophan and L‐tryptophan by the chiral DMEB aggregates has been evidenced by mass spectra data, CID experiments, and CCS values. 相似文献
13.
The centrosymmetric title compound, [Cd2{CH3OC6H4P(OC5H9)S2}4], features an eight‐membered [? Cd? S? P? S? ]2 ring owing to the presence of bridging dithiolate ligands. Tetrahedral coordination geometries for cadmium are completed by chelating ligands. Copyright © 2004 John Wiley & Sons, Ltd. 相似文献
14.
The preparation of three new N‐Fmoc‐protected (Fmoc=[(9H‐fluoren‐9‐yl)methoxy]carbonyl) β2‐homoamino acids with proteinogenic side chains (from Ile, Tyr, and Met) is described, the key step being a diastereoselective amidomethylation of the corresponding Ti‐enolates of 3‐acyl‐4‐isopropyl‐5,5‐diphenyloxazolidin‐2‐ones with CbzNHCH2OMe/TiCl4 (Cbz=(benzyloxy)carbonyl) in yields of 60–70% and with diastereoselectivities of >90%. Removal of the chiral auxiliary with LiOH or NaOH gives the N‐Cbz‐protected β‐amino acids, which were subjected to an N‐Cbz/N‐Fmoc (Fmoc=[(9H‐fluoren‐9‐yl)methoxy]carbonyl) protective‐group exchange. The method is suitable for large‐scale preparation of Fmoc‐β2hXaa‐OH for solid‐phase syntheses of β‐peptides. The Fmoc‐amino acids and all compounds leading to them have been fully characterized by melting points, optical rotations, IR, 1H‐ and 13C‐NMR, and mass spectra, as well as by elemental analyses. 相似文献
15.
Yuki Matsunaga Kiyoshi Fujisawa Nagina Amir Yoshitaro Miyashita Ken‐ichi Okamoto 《应用有机金属化学》2005,19(1):208-208
The Zn center in [ZnCl2(L‐S‐S‐L)], where L‐S‐S‐L = bis(1‐methylimidazole‐2)disulfide, adopts a tetrahedral configuration defined by two Cl atoms and two N atoms from L‐S‐S‐L, which was obtained by in situ oxidation of 1‐methylimidazole‐2‐thione. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
16.
Reactions of SmI2 in THF with ArSSAr produced two binuclear samarium thiolate complexes [(THF)3I2- Sm(μ-SAr)]2 [Ar=Ph (1), 4-Me2NC6H4 (2)] in high yields. The structure of 2 was characterized by single crystal X-ray crystallography. The crystal of 2 belongs to the triclinic system with space group P 1 and a=0.95705(13) nm, b= 1.22287(14) nm, c= 1.26450(14) nm, a=64.194(11)°, B=78.491(13)°, y=76.176(12)°, V= 1.2860(3) nm^3, Z= 1,μ=4.783 mm^-1, Dc= 1.964 Mg/m^3, M= 1521.19, S= 1.046, R1=0.0358, wR2=0.0910. X-ray analysis revealed that 2 is a thiolate-bridged dimer in which each Sm atom adopts a distorted pentagonal bipyramidal coordi- nation geometry. 相似文献
17.
[Et2Sn(O2AsMe2)2] ( 1 ) and [Ph2Sn(O2AsMe2)(μ‐OMe)]2 ( 2 ) were synthesized by treatment of Et2SnO and Ph2SnS with HO2AsMe2 in Methanol, respectively. The compounds were characterized by elemental analyses, vibrational spectroscopy and mass spectrometry. According to X‐ray diffraction measurements compound 1 crystallizes monoclinic in space group P21/n with cell parameters a = 804.89(3), b = 987.11(5), c = 966.42(4) pm, β = 113.354(3)°. The unit cell parameters of 2 , which crystallizes in the same space group, are a = 974.4(1), b = 1463.3(1), c = 1228.9(1) pm, β = 111.324(3)°. The (SnOAsO)4 rings of 1 are linked and form a two‐dimensional network with the SnEt groups pointing into the holes of the next layer. Compound 2 occurs as a dimer with internal Sn(OMe)2Sn bridges in the (SnOAsO)2 rings. The vibrational and mass spectra are given and discussed. 相似文献
18.
Li‐Ming Wu Ling Chen Jingcao Dai Ping Lin Wen‐Xin Du Xin‐Tao Wu 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(9):e382-e382
The title compound, [Sn(C5H5NS)2(C2H4S2)2], was obtained from a 1:2 mixture of bis(ethane‐1,2‐dithiolato)tin(IV) and 2‐mercaptopyridine. The molecules are discrete monomeric trans‐octahedral units, with the SnIV atom at the centre of symmetry, planar 2‐mercaptopyridine zwitterions and SnS2C2 groups in twist–envelope conformations. The 2‐mercaptopyridine ligands are monodentate and are bonded through the S atoms. The S—Sn distances between the S atom of edt (edt is ethane‐1,2‐dithiolate) and the Sn atom are 2.473 (1) and 2.505 (1) Å, which are slightly longer than the S—Sn distance in Sn(edt)2 of 2.390 (1) Å. The bond between the 2‐mercaptopyridine S atom and the Sn atom are, remarkably, weaker than the S—Sn bond involving edt. 相似文献
19.
Trinuclear [CoIII2–LnIII] (Ln=Tb,Dy) Single‐Ion Magnets with Mixed 6‐Chloro‐2‐Hydroxypyridine and Schiff Base Ligands 下载免费PDF全文
Prof. Dr. Cai‐Ming Liu Prof. Dr. De‐Qing Zhang Prof. Dr. Xiang Hao Prof. Dao‐Ben Zhu 《化学:亚洲杂志》2014,9(7):1847-1853
The Schiff base ligand N1,N3‐bis(3‐methoxysalicylidene)diethylenetriamine (H2valdien) and the co‐ligand 6‐chloro‐2‐hydroxypyridine (Hchp) were used to construct two 3d–4f heterometallic single‐ion magnets [Co2Dy(valdien)2(OCH3)2(chp)2] ? ClO4 ? 5 H2O ( 1 ) and [Co2Tb(valdien)2(OCH3)2(chp)2] ? ClO4 ? 2 H2O ? CH3OH ( 2 ). The two trinuclear [CoIII2LnIII] complexes behave as a mononuclear LnIII magnetic system because of the presence of two diamagnetic cobalt(III) ions. Complex 1 has a molecular symmetry center, and it crystallizes in the C2/c space group, whereas complex 2 shows a lower molecular symmetry and crystallizes in the P21/c space group. Magnetic investigations indicated that both complexes are field‐induced single‐ion magnets, and the CoIII2–DyIII complex possesses a larger energy barrier [74.1(4.2) K] than the CoIII2–TbIII complex [32.3(2.6) K]. 相似文献
20.
Three new triruthenium clusters, Ru3(CO)9(μ‐arphos)AsPh3 ( 1 ), Ru3(CO)9(μ‐arphos)As(m‐C6H4Me)3 ( 2 ), and Ru3(CO)9(μ‐arphos)As(p‐C6H4Me)3 ( 3 ) were synthesized via thermal reactions of Ru3(CO)10(μ‐arphos) with different tertiary arsine ligands [AsPh3, As(m‐C6H4Me)3, As(p‐C6H4Me)3]. All these complexes were fully characterized by elemental analysis, FT‐IR, NMR spectroscopy, and single‐crystal X‐ray diffraction. 相似文献