A High-Yield Synthesis of Chalcopyrite CuIn S

We report high-yield and efficient size-controlled syntheses of Chalcopyrite CuInS2 nanoparticles by decomposing molecular single source precursors (SSPs) via microwave irradiation in the presence of 1,2-ethanedithiol at reaction temperatures as low as 100°C and times as short as 30 minutes. The nanoparticles sizes were 1.8 nm to 10.8 nm as reaction temperatures were varied from 100°C to 200°C with the bandgaps from 2.71 eV to 1.28 eV with good size control and high yields (64%–95%). The resulting nanoparticles were analyzed by XRD, UV-Vis, ICP-OES, XPS, SEM, EDS, and HRTEM. Titration studies by 1H NMR using SSP 1 with 1,2-ethanedithiol and benzyl mercaptan were conducted to elucidate the formation of Chalcopyrite CuInS2 nanoparticles

3-(4-Bromophenyl)cyclopent-2-en-1-one

In the title compound, C11H9BrO, the cyclopentenone ring is almost planar with an r.m.s. deviation of 0.0097 Å. The largest inter-ring torsion angles [2.4 (3), 1.3 (3) and 3.53 (2)°] reveal only a very small twist between the rings, and suggest that the two rings are conjugated. The molecule is slightly bowed, as shown by the small dihedral angle between the rings [5.3 (1)°]. The crystal packing pattern consists of parallel sheets that stack parallel to the ac plane. Each sheet consists of molecules that pack side-to-side with the same relative orientation of phenyl and cyclopentenone rings along the a- and c-axis directions. Slipped side-to-side, face-to-face and edge-to-face interactions exist between pairs of sheets with edge-to-edge and edge-to-face O...H—C(sp2) weak hydrogen-bond contacts. A relatively short edge-to-face contact (2.77 Å) also exists between pairs of sheets

CCDC 1479096: Experimental Crystal Structure Determination

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.,Related Article: N. P. Godman, D. B. Barbee, F. B. Carty, C. D. McMillen, C. A. Corley, E. Shurdha, S. T. Iacono|2016|Polym.Chem.|7|5799|doi:10.1039/C6PY00966

Extended Network Thiocyanate- and Tetracyanoethanide-Based First-Row Transition Metal Complexes

Linear chain thiocyanate complexes of M­(NCS)₂(OCMe₂)₂ (M = Fe, Mn, Cr) composition have been prepared and structurally, chemically, and magnetically characterized. Fe­(NCS)₂(OCMe₂)₂ exhibits metamagnetic-like behavior, and orders as an antiferromagnet at 6 K. The Mn and Cr compounds are antiferromagnets with <i>T</i>_c of 30 and 50 K, respectively, with <i>J</i>/<i>k</i>_B = −3.5 (−2.4 cm^–1) and −9.9 K (−6.9 cm^–1), respectively, when fit to one-dimensional (1-D) Fisher chain model (<i>H</i> = −2<i>J</i>S_<i>i</i>·S_<i>j</i>). Co­(NCS)₂ was prepared by a new synthetic route, and powder diffraction was used to determine its structure to be a two-dimensional (2-D) layer with μ_N,S,S-NCS motif, and it is an antiferromagnet (<i>T</i>_c = 22 K; θ = −33 K for <i>T</i> > 25 K). M­(NCS)₂(OCMe₂)₂ (M = Fe, Mn) and Co­(NCS)₂ react with (NBu₄)­(TCNE) in dichloromethane to form M­(TCNE)­[C₄(CN)₈]_1/2, and in acetone to form M­[C₄(CN)₈]­(OCMe₂)₂ (M = Fe, Mn, Co). These materials possess μ₄-[C₄(CN)₈]^2– that form 2-D layered structural motifs, which exhibit weak antiferromagnetic coupling. Co­(TCNE)­[C₄(CN)₈]_1/2 behaves as a paramagnet with strong antiferromagnetic coupling (θ = −50 K)

Extended Network Thiocyanate- and Tetracyanoethanide-Based First-Row Transition Metal Complexes

Linear chain thiocyanate complexes of M­(NCS)₂(OCMe₂)₂ (M = Fe, Mn, Cr) composition have been prepared and structurally, chemically, and magnetically characterized. Fe­(NCS)₂(OCMe₂)₂ exhibits metamagnetic-like behavior, and orders as an antiferromagnet at 6 K. The Mn and Cr compounds are antiferromagnets with <i>T</i>_c of 30 and 50 K, respectively, with <i>J</i>/<i>k</i>_B = −3.5 (−2.4 cm^–1) and −9.9 K (−6.9 cm^–1), respectively, when fit to one-dimensional (1-D) Fisher chain model (<i>H</i> = −2<i>J</i>S_<i>i</i>·S_<i>j</i>). Co­(NCS)₂ was prepared by a new synthetic route, and powder diffraction was used to determine its structure to be a two-dimensional (2-D) layer with μ_N,S,S-NCS motif, and it is an antiferromagnet (<i>T</i>_c = 22 K; θ = −33 K for <i>T</i> > 25 K). M­(NCS)₂(OCMe₂)₂ (M = Fe, Mn) and Co­(NCS)₂ react with (NBu₄)­(TCNE) in dichloromethane to form M­(TCNE)­[C₄(CN)₈]_1/2, and in acetone to form M­[C₄(CN)₈]­(OCMe₂)₂ (M = Fe, Mn, Co). These materials possess μ₄-[C₄(CN)₈]^2– that form 2-D layered structural motifs, which exhibit weak antiferromagnetic coupling. Co­(TCNE)­[C₄(CN)₈]_1/2 behaves as a paramagnet with strong antiferromagnetic coupling (θ = −50 K)

First Row Transition Metal(II) Thiocyanate Complexes, and Formation of 1‑, 2‑, and 3‑Dimensional Extended Network Structures of M(NCS)₂(Solvent)₂ (M = Cr, Mn, Co) Composition

The reaction of first row transition M^II ions with KSCN in various solvents form tetrahedral (NMe₄)₂[M^II(NCS)₄] (M = Fe, Co), octahedral <i>trans</i>-M^II(NCS)₂(Sol)₄ (M = Fe, V, Ni; Sol = MeCN, THF), and K₄[M^II(NCS)₆] (M = V, Ni). The reaction of M­(NCS)₂(OCMe₂)₂ (M = Cr, Mn) in MeCN and [Co­(NCMe)₆]­(BF₄)₂ and KSCN in acetone and after diffusion of diethyl ether form M­(NCS)₂(Sol)₂ that structurally differ as they form one-dimensional (1-D) (M = Co; Sol = THF), two-dimensional (2-D) (M = Mn; Sol = MeCN), and three-dimensional (3-D) (M = Cr; Sol = MeCN) extended structures. 1-D Co­(NCS)₂(THF)₂ has <i>trans</i>-THFs, while the acetonitriles have a <i>cis</i> geometry for 2- and 3-D M­(NCS)₂(NCMe)₂ (M = Cr, Mn). 2-D Mn­(NCS)₂(NCMe)₂ is best described as Mn^II(μ_N,N-NCS)­(μ_N,S-NCS)­(NCMe)₂ [= Mn₂(μ_N,N-NCS)₂(μ_N,S-NCS)₂(NCMe)₄] with the latter μ_N,S-NCS providing the 2-D connectivity. In addition, the reaction of Fe­(NCS)₂(OCMe₂)₂ and 7,7,8,8-tetracyanoquino-<i>p</i>-dimethane (TCNQ) forms 2-D structured Fe^II(NCS)₂TCNQ. The magnetic behavior of 1-D Co­(NCS)₂(THF)₂ can be modeled by a 1-D Fisher expression (<i>H</i> = −2<i>J</i>S_<i>i</i>·S_<i>j</i>) with <i>g</i> = 2.4 and <i>J</i>/<i>k</i>_B = 0.68 K (0.47 cm^–1) and exhibit weak ferromagnetic coupling. Cr­(NCS)₂(NCMe)₂ and Fe^II(NCS)₂TCNQ magnetically order as antiferromagnets with <i>T</i>_c’s of 37 and 29 K, respectively, while Mn­(NCS)₂(NCMe)₂ exhibits strong antiferromagnetic coupling. M­(NCS)₂(THF)₄ and K₄[M­(NCS)₆] (M = V, Ni) are paramagnets with weak coupling between the octahedral metal centers