592-87-0Relevant articles and documents
A preparation of lead thiocyanate
Lambou,Dollear
, p. 97 - 101 (1946)
A new and improved method for the preparation of a pure and stable lead thiocyanate in practically theoretical yield has been described. A comprehensive investigation of other published methods has been reported and preparations of lead thiocyanate made by these methods have been compared with the improved compound and various commercial products. All of the products were assayed for purity on the basis of their chemical analyses and tests were made of their capacity for saturating double bonds in cottonseed, peanut, and soybean oils. The lead thiocyanate prepared according to the recommended procedure was found superior to all the other products in stability, purity, and ability to produce dependable and reproducible thiocyanogen values. It has been demonstrated that the ratio of lead ions to thiocyanogen ions and the order of addition of these ions to each other are of major importance in the preparation of pure lead thiocyanate.
Two-dimensional holo- and hemidirected lead(II) coordination polymers: Synthetic, spectroscopic, thermal, and structural studies of [Pb(μ-SCN) 2(μ-ebp)1.5]n and {[Pb(μ-OAc)(μ-ebp)] (ClO4)}n (ebp = 4,4′-[(1E)-ethane-1,2-diyl] bis[pyridine]; OAc = Acetato)
Morsali, Ali,Yilmaz, Veysel T.,Kazak, Canan,Zhu, Long-Guan
, p. 2513 - 2522 (2005)
Two new coordination polymers of Pb11 complexes with bridging 4,4′-[(1E)-ethane-1,2-diyl]bis[pyridine] (ebp), thiocyanato, and acetato ligands, [Pb(μ-SCN)2(μ-ebp)1.5]n (1) and {[Pb(μ-OAc)(μ-ebp)](ClO4)}n (2), were synthesized and characterized by elemental analysis, FT-IR, 1H- and 13C-NMR, thermal analysis, and single-crystal X-ray diffraction. In 1, the Pb2+ ions are doubly bridged by both the ebp and the SCN - ligands into a two-dimensional polymeric network. The seven-coordinate geometry around the Pb2+ ion in 1 is a distorted monocapped trigonal prism, in which the Pb2+ ions have a less-common holodirected geometry. In 2, the Pb2+ ions are bridged by AcO - ligands forming linear chains, which are also further bridged by the neutral ebp ligands into a two-dimensional polymeric framework. The Pb 2+ ions have a five-coordinate geometry with two N-atoms from two ebp ligands and three O-atoms of AcO-. Although ClO4 acts as a counter-ion, it also makes weak interactions with the Pb2+ center. The arrangement of the ligands in 2 exhibits hemidirected geometry, and the coordination gap around the Pb2+ ion is possibly occupied by a configurationally active lone pair of electrons.
Synthesis of anisotropic PbS nanoparticles using heterocyclic dithiocarbamate complexes
Nyamen, Linda D.,Rajasekhar Pullabhotla,Nejo, Adeola A.,Ndifon, Peter T.,Warner, Jamie H.,Revaprasadu, Neerish
, p. 8297 - 8302 (2012)
We report the synthesis of lead piperidine and lead tetrahydroquinoline dithiocarbamate (DTC) complexes and their use as single source precursors for the preparation of anisotropic PbS nanoparticles. The complexes were thermolysed in coordinating solvents such hexadecylamime (HDA), tri-n-octylphosphine oxide (TOPO), oleylamine (OA) and decylamine (DA) at various reaction temperatures. The variation of the reaction conditions and precursors produced PbS particles with shapes ranging from spheres to cubes and rods. The size of the particles is generally larger than those synthesized by conventional precursor routes. The electron microscopy and X-ray diffraction data confirm the particles to be very crystalline with the dominant cubic rock salt phase present in all samples. The Royal Society of Chemistry 2012.
Binucleating N624- and 26-Membered Macrocyclic Ligands. Part 2. Transitionmetal Homo- and Hetero-binuclear Complexes: X-Ray Crystallographic Structure Determination of a Lead-Manganese Heterobinuclear Complex
Nelson, Jane,Murphy, Brian P.,Drew, Michael G. B.,Yates, Paul C.,Nelson, S. Martin
, p. 1001 - 1010 (1988)
Template condensation products of 1,5-diaminopentane and 1,6-diaminohexane with 2,6-diacetylpyridine on Pb(NCS)2 have been transmetallated with CoII and CuII to yield homobinuclear complexes of the 24- and 26-membered macrocycles, L1 and L2 respectively.In the dicobalt(II) complex of the smaller macrocycle, L1, a thermally populated spin equilibrium exists lying well to the low-spin side at 93 K.E.s.r. spectra indicate the complex has an equatorially compressed tetragonal geometry.The dicobalt(II) complex of the larger macrocycle, L2, is effectively high-spin, down to 93 K.Dicopper(II) complexes of L1 display a weak antiferromagnetic interaction, absent in analogous complexes of L2.Heterobinuclear complexes 1(NCS)2(MeCN)2>2 of the 24-membered macrocycle heve been prepared for M = NiII and FeII, as confirmed by fast-atom bombardment (f.a.b.) mass spectra.An X-ray crystallographic structure determination on the heterobinuclear complex PbMnL1(NCS)4 reveals a Pb-Mn distance of 4.857(2) Angstroem and confirms that the metal centres are bridged by two 1,3-μ-NCS-bridges, as inferred from i.r. spectroscopy for the other thiocyanato complexes studied.However, the X-ray structure shows that in this case the thiocyanate bridges present both S-donors to Pb and both N-donors to Mn.
Structure and Optical Properties of Layered Perovskite (MA)2PbI2-xBrx(SCN)2(0 ≤ x < 1.6)
Yamamoto, Takafumi,Oswald, Iain W. H.,Savory, Christopher N.,Ohmi, Takuya,Koegel, Alexandra A.,Scanlon, David O.,Kageyama, Hiroshi,Neilson, James R.
, p. 17379 - 17384 (2020/12/22)
The layered perovskite (MA)2PbI2(SCN)2 (MA = CH3NH3+) is a member of an emerging series of compounds derived from hybrid organic-inorganic perovskites. Here, we successfully synthesized (MA)2PbI2-xBrx(SCN)2 (0 ≤ x a solid-state reaction. Despite smaller bromide substitution for iodine, 1% linear expansion along the a axis was observed at x ～0.4 due to a change of the orientation of the SCN- anions. Diffuse reflectance spectra reveal that the optical band gap increases by the bromide substitution, which is supported by the DFT calculations. Curiously, bromine-rich compounds where x ≥ 0.8 are light sensitive, leading to partial decomposition after ～24 h. This study demonstrates that the layered perovskite (MA)2PbI2(SCN)2 tolerates a wide range of bromide substitution toward tuning the band gap energy.
Synthesis and schematic mechanism of 3-phenylamino-4-phenyl-5-tetra-O-acetyl-β-D-glucopyranosylimino-1,2,4-dithiazolidines and Its De-acetylated Nucleoside
Hardas, Aruna,Tayade, Priti
, p. 2310 - 2316 (2018/09/10)
A systematic synthesis of 3-phenylimino-4-phenyl-5-tetra-O-acetyl-β-D-glucopyranosylimino-1,2,4-dithiazolidine (acetylated glucopyranosylimino nucleoside) from glucose as starting material. The steps included acetylating glucose to glucose penta-acetate (II). Step 2 involves the bromination of glucose penta-acetate (II) to 2,3,4,6 tetra-O-acetyl-α-D-glucopyranosyl bromide (III). In step 3 compound (III) reacted with lead thiocyanate to give 2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl isothiocyanate (IV). In the step 4 N-phenyl-3-tetra-O-acetyl-β-D-glucopyranosyl isothiocyanate (V) was prepared. In the last step on refluxing compound (V) with N-phenyl S-chloro isothiocarbamoyl chloride to yield acetylated glucopyranosyl nucleoside. Furthermore de-acetylating of acetylated glucopyranosyl nucleoside was carried out to obtain 3-phenylimino-4-phenyl-5-β-D-gluopyranosyl imino 1,2,4-dithiazolidine (de-acetylated glucopyranosylimino nucleoside). The synthesized acetylated glucopyranosylimino nucleoside and deacetylated glucopyranosylimono nucleoside were structurally confirmed by elemental analysis, ultraviolet spectral analysis, infrared spectroscopy, nuclear magnetic resonance spectroscopy and mass spectroscopy.
Pseudohalide-Induced Moisture Tolerance in Perovskite CH3NH3Pb(SCN)2I Thin Films
Jiang, Qinglong,Rebollar, Dominic,Gong, Jue,Piacentino, Elettra L.,Zheng, Chong,Xu, Tao
, p. 7617 - 7620 (2015/06/25)
Two pseudohalide thiocyanate ions (SCN-) have been used to replace two iodides in CH3NH3PbI3, and the resulting perovskite material was used as the active material in solar cells. In accelerated stability tests, the CH3NH3Pb(SCN)2I perovskite films were shown to be superior to the conventional CH3NH3PbI3 films as no significant degradation was observed after the film had been exposed to air with a relative humidity of 95% for over four hours, whereas CH3NH3PbI3 films degraded in less than 1.5 hours. Solar cells based on CH3NH3Pb(SCN)2I thin films exhibited an efficiency of 8.3%, which is comparable to that of CH3NH3PbI3 based cells fabricated in the same way.
13C NMR and FT-IR spectra of thiocyanogen, S2(CN)2, selenocyanogen, Se2(CN)2, and related compounds
Cataldo
, p. 681 - 688 (2008/10/08)
The pseudohalogens thiocyanogen [(SCN)2], sulfur dicyanide [S(CN)2], selenocyanogen [(SeCN)2], selenium dicyanide [Se(CN)2] and selenium diselenocyanate [Se(SeCN)2] have been prepared and studied by 13C NMR spectroscopy for the first time. The 13C NMR results confirm the structure previously assigned to these compounds on the basis of vibrational spectroscopy. Thiocyanogen, sulfur dicyanide, selenocyanogen and selenium dicyanide have been also studied as liquid film on KBr plate in the solid state (KBr pellet) by FT-IR spectroscopy and the data collected have been compared and discussed with previous results recorded on solutions in organic solvents. Good agreement with early results has been obtained. It has been confirmed by solid state 13C NMR-MAS that under mild conditions selenocyanogen disproportionates into selenium dicyanide and selenium diselenocyanate. By heating selenocyanogen above 180°C it polymerizes irreversibly into a brown polymer known as paraselenocyanogen whose FT-IR spectrum is surprisingly very similar to that of parathiocyanogen or polythiocyanogen, the product of self-polymerization of thiocyanogen. (C) 2000 Elsevier Science Ltd.
Lewis-Base Adducts of Lead(II) Compounds. Part 4. Novel Isomeric Dimers of Lead(II) Thiocyanate-1,10-Phenanthroline(1/2). Crystal Structure Determinations
Engelhardt, Lutz M.,Furphy, Brenda M.,Harrowfield, Jack McB.,Patrick, Jennifer M.,Skelton, Brian W.,White, Allan H.
, p. 595 - 600 (2007/10/02)
The 1:2 adduct of lead(II)thiocyanate-1,10-phenanthroline has been shown to crystallise as two distinc polymorphs, monoclinic and triclinic.Single-crystal X-ray structure determination show that in both forms the complexes exist as discrete dimers, all lead environments being seven-co-ordinate.The lead environment in all cases comprises a pair of bidentate phenanthroline ligands, unidentate N-thiocyanate, and a pair of bridging thiocyanate ligands, one with bridging sulphur and one bridging through the terminal atoms.In the monclinic form, C2/c, the dimer has crystallographically imposed two-fold symmetry with the N,S-bridging thiocyanate disordered about that axis; this ligand in the triclinic form is fully ordered, with ligand rearrangement about one of the lead atoms so that the dimer symmetry is more nearly inversion rather than two-fold.
