Crystal structures of bis(cyanido)bis(N,N′-diethylthiourea-κS) mercury(II) and bis(cyanido)bis(N,N′-dipropylthiourea-κS) mercury(II)

Two mercury(II) complexes containing cyanide and, N,N′-diethylthiourea (detu) and N,N′-dipropylthiourea (dprtu) ligands, [(detu)₂Hg(CN)₂] (1) and [(dprtu)₂Hg(CN)₂] (2), respectively, have been prepared and characterized by X-ray crystallography. In the both complexes Hg atom lies on a 2-fold rotation axis, and is coordinated to the sulfur atoms of two thiourea ligands and to two cyanide carbon atoms. Both have a distorted tetrahedral environment with bond angles about the Hg atoms in the range of 93.41(4)°–146.75(19)°. In the crystal structures symmetry related molecules are linked via N-H-N hydrogen bonds resulting in the formation of a two-dimensional network in 1, while in 2 a double stranded one-dimensional chain is formed.     

A quasi-layer structure of trinuclear molybdenum(IV) cluster, [Mo3S7(S2CNEt2)3]I·S8

The title compound, [Mo₃(₃-S)(-S₂)₃(S₂CNEt₂)₃]I·S₈, was obtained by solid state reaction of (NH₄)₂MoS₄, Et₂NCS₂Na, and Et₄NI at low heating temperature and crystallizes in space group P with a = 13.572(3), b = 13.813(4), c = 13.239(3) Å, = 92.63(3), = 100.15(3), = 117.89(2)°, V = 2136(2) ų, and D _calc. = 2.08 g/cm³ for Z = 2. The structure reveals that it consists of a trinuclear Mo cluster molecule, [Mo₃S₇(S₂CNEt₂)₃]I, and one S₈, which are connected to form a quasi-layer structure by the interaction between S₈ and the S atoms of the cluster molecule.     

Structure and spectral properties of (O-Cyclohexyldithiocarbonatio-S,S′) bis(triphesnylphosphine) copper(I) complex

The complex [(C₆H₁₁OCS₂)(PPh₃)₂Cu], was synthesized and characterized using IR, UV, and ¹H NMR. The crystal and molecular structure has been determined by X-ray diffraction. The yellow crystal of the complex is triclinic of space group , with parameters a=10.370(2)Å, b=13.530(3)Å, c=14.640(3)Å, =92.60(3)°, =108.00(3)°, =97.70(3)°, and Z=2. In the complex, the central Cu atom is in a distorted tetrahedral environment and chelated by two phosphorus atoms of the TRIPHOS and two sulfur atoms from the O-cyclohexyldithiocarbonate. The cyclohexane ring adopts a chair conformation. The thermal analytical data indicate that the complex begins to decompose at 101°C and stop at 360°C , leaving CuS. IR, UV, and NMR results supported the crystal structure.     

Structure of bis(O,O′-diisopropyldithiophosphato-S,S′) (1,10-phenanthroline-N1,N10)zinc(II) complex, [Zn(phen)(S2P(OiPr)2)2]

The crystal and molecular structure of [Zn(phen)(S₂P(OiPr)₂)₂] (Phen = 1,10-phenanthroline) has been determined by X-ray crystallography. It crystallizes in the Monoclinic system, space group C2/c, with lattice parameters a = 19.315(4), b = 10.438(2), c = 16.567(3)Å, = 102.89 (3)°, and Z = 4. The complex has C₂ symmetry. The coordination geometry of each Zn atom, by two S atoms from two (O,O-diisopropyldithiophosphato) anions and by two N atoms from phenanthroline ligand, is that of a slightly distorted tetrahedron [Zn—S 2.2914(8)Å Zn—N 2.111(2)Å]. The Zn···S distances to the noncoordinated S atoms are long: 3.5276 Å, which are indicated that there are much weaker interactions between them.     

Si(100)表面S钝化效果与稳定性研究

基于Valence-Mending概念对Si(100)表面进行S钝化研究.对于Ni/n-Si肖特基接触,S钝化使其肖特基势垒高度向其理想势垒高度靠近了0.09 eV;对于Al/p-Si肖特基接触,S钝化使其肖特基势垒高度向其理想势垒高度靠近了0.08 eV.少子寿命测试结果表明S钝化使Si(100)表面少子寿命提高大约1个数量级;热稳定性实验结果表明560℃时S钝化效果退化;XPS测试结果表明S离子化学吸附在Si表面并形成Si-S键,样品在空气中放置一段时间后表面Si-S键被氧化,表明S钝化抗氧化性不强.     

The crystal and molecular structure of spiro[1-(S)-Br-3-(S)-H-4-(R)-l-(1′ R,2′ S,5′R)-menthyloxy-5-oxo-6-oxa-bicyclo[3.1.0]hexane-2,3′-(R)-(4′-(R)-diphenylmethoxy-5′-l-(1′ R,2′ S,5′ R)-menthyloxy-butyrolactone)]

Crystal structure of C₄₁H₅₃O₇Br has been determined by single-crystal X-ray diffraction. The compound crystalline in the orthorhombic space group P2₁2₁2₁, with a = 11.264(2), b = 12.058(2), c = 29.337(6) Å, Z = 4. The bond angles of cyclopropane moiety in the molecule are approximate to 60° and agree with theoretic values of the internal angles in a cyclopropane, and two chiral menthyloxy groups are located above and under the whole chiral molecule, respectively. The configuration of the pentacyclic lactone is shown as envelope form.     

以1,4-DAB为溶剂(1,4-DABH2)2Sn2S6·(1,4-DAB)和(1,4-DABH2)Sb4S7的合成与表征

以1,4-丁二胺为溶剂合成两种硫属化合物(1,4-DABH2)2Sn2S6·(1,4-DAB)(1)和(1,4-DABH2) Sb4S7(2)(1,4-DAB =1,4-丁二胺),单晶X-射线衍射分析表明化合物1为单斜晶系,空间群为P21/c,a=1.0862(5) nm,b=1.3053(6) nm,c=1.0283(5) nm,β=101.20(2)°,V=1.4302(12) nm3,Z=2;化合物2为三斜晶系,空间群为P-1,a=0.6009(4) nm,b =0.8989(7) nm,c=1.6548(12) nm,α =89.774(12)°,β=86.481 (12)°,γ=84.495(12)°,V=0.8880(11)nm3,Z=2.化合物1由离散的[Sn2S6]2+、质子化的有机胺和未质子化有机胺组成.化合物2是由质子化的有机胺和双链的[Sb4S7]2-离子组成的二维层状化合物.紫外-可见漫反射光谱研究结果表明,化合物1和2的禁带宽度分别为1.80 eV和1.54 eV,均为半导体.     

Cyclic dithiophosphate salts [Et3NH+[(OCH2CMe2CH2O)P(S)S]− and [Et3NH]+[CH2{6-t-Bu-4-Me-C6H4O}2P(S)S]−

X-ray structures of the cyclic dithiophosphate salts [Et₃NH]⁺[(OCH₂CMe₂CH₂O)P(S)(S)]^– (1) and [Et₃NH]⁺[CH₂{6-t-Bu-4-Me-C₆H₄O}₂P(S)S]^– (2) have been determined. Crystal data for 1: Tetragonal, P4₂/m, a = 13.416(7), b = 13.416(2), c = 9.153(2) Å, and Z = 4. Crystal data for 2 = Monoclinic, P2₁/c, a = 19.1112(17), b = 14.649(9), c = 22.7166(19) Å, = 102.883(7)°, and Z = 8. The six- and eight-membered rings in 1 and 2 have chair and boat-chair conformations respectively. Both of these compounds show weak N—H······S hydrogen bonds; interestingly, in 2 both two-center and three-center hydrogen bonds are observed in the solid state.     

Crystal and molecular structure of tetraiodo (1,8-di-2-pyridyl-3,6-dithiaoctane-N,S,S′,N′)dimercury(II)

Summary The X-ray crystal structure of the title compound, [Hg₂(C₁₆H₂₀N₂S₂)I₄], has been determined. The crystals are monoclinic (space groupP2₁/c), with cell dimensionsa=15.016(2),b=6.201(3),c=15.273(2) Å,=115.18(1)°;V _o =1287.0(7) ų,M _r =1213.266,Z=4,D _x =6.26mg m^–3, MoK radiation (graphite crystal monochromator, ),(MoK)=336 cm^–1,F(000)=4272, andT=290°K. The final conventionalR factor=0.054, andR _w =0.062 for 2799 observed reflections. The structure was solved by Patterson and Fourier methods and refined by block-diagonal least-squares methods. The coordination around the mercury atoms is approximately tetrahedral, although with considerable distortion, with two iodine atoms and the N and S atoms of one-half of the ligand molecule.     

Sb2(S1-x Sex)3(0≤x≤1)薄膜太阳能电池的研究进展

Sb2(S1-xSex)3(0≤x≤1)化合物是重要的半导体材料,主要包括Sb2Se3、Sb2Se3及Sb2(S,Se)3三种材料,元素储量丰富且环境友好、组分简单、价格低廉,同时其禁带宽度合适(1.1～1.8 eV),吸光系数大(＞105 cm-1),非常适合用作新型低成本低毒的薄膜太阳能电池的吸收层,有可能成为下一个研究热点.本文综述了近几年来Sb2Se3、Sb2Se3及Sb2(S,Se)3薄膜太阳能电池的研究进展,并对其发展趋势进行了展望.     

Synthesis and structural characterization of a (N,N′-bis[2(S)-pyrrolidylmethyl]-propane-1,3-diamine) nickel (II) complex

The nickel(II) complex [Ni(C₄H₃NCH=N–(CH₂)₃–N=CHC₄H₃N)], (1) containing the symmetrical N₄ tetradentate Schiff base ligand, which is the 2:1 condensation product of pyrrole-2-carboxaldehyde and 1,3-diaminopropane respectively, was prepared. Structural investigation shows that it is monomeric, having space group P2₁/c, a = 7.989(7), b = 17.406(14), c = 9.193(5) Å, = 90, = 100.39(6), = 90, and Z = 4. The coordination geometry around the nickel atom is slightly distorted square planar and the conformation of the six-membered ring containing the metal,azomethine nitrogens and three carbon atoms of the connecting 1,3-diaminopropane is a symmetric boat.     

Synthesis and crystal structures of [Na{Ph2P(S)NP(S)Ph2}(L)] (where L=triglyme or tetraglyme); two air stable complexes containing six-membered S—P—N—P—S—Na rings

The title complexes [Na{Ph₂P(S)NP(S)Ph₂}(L)] (where L=triglyme 1, or tetraglyme 2) were prepared in an aqueous/methanolic mixture by reaction of the sodium salt of Ph₂P(S)NHP(S)Ph₂ with the respective glyme ligand. Compound 1 crystallizes in the orthorhombic space group Pbca with a = 19.526(5), b = 16.102(4), c = 21.168(5) Å, and Z = 8. The complex is monomeric with all four oxygen atoms of the glyme moiety coordinated to the Na⁺ cation. The S atoms of the Ph₂P(S)NP(S)Ph₂ anion are bound in a symmetrical fashion to the sodium cation. Compound 2 crystallizes in the triclinic space group P with a = 10.747 (3), b = 11.541(3), c = 14.932(4) Å, = 81.28(3), = 81.96(4), = 74.41(3)° and Z = 2. This structure was also found to be monomeric, with the additional oxygen of tetraglyme giving a seven coordinate rather than six coordinate Na⁺ cation.     

Synthesis and characterization of the dodecanuclear heterobimetallic Mo—Cu—S cage cluster: (Ph4P)2[{Mo2Cu2O2S2(S2)2}3(μ6-S)]

The complex (Ph₄P)₂[Mo₂S₂O₂(S₂)(S₄)] reacts with CuBr to give the dodecanuclear heterobimetallic Mo—Cu—S cage cluster: (Ph₄P)₂[{Mo₂Cu₂O₂S₂(S₂)₂}₃(₆-S)] (1), which crystallizes in the triclinic space group P1¯, a = 14.445(5), b = 15.396(5), c = 18.858(5) Å, = 103.12(3), = 101.93(2), = 113.92(3)°, and V = 3517(2) ų for Z = 2. The anion 1 can be described as a cage with S^2– at the center binding to six Cu atoms; the cage has two big windows each composed of a puckered Cu₃S₆ 9-membered ring.     

Bias-induced changes in carrier type of Pb(1−x)Fe(x)S nanocrystalline solution grown thin films

Change of majority carrier type was achieved in nanocrystalline Pb_(1−x)Fe_(x)S thin films by applying a DC-bias on the substrate during their growth by solution growth technique. Critical control of biasing and pH of the solution bath are observed to be necessary to achieve this change. The DC-bias results in slight change in relative concentrations of the constituents in the films, which lead to change in majority carriers without any measurable change in lattice parameter. This modification to the conventional solution growth technique provides the possibility to grow abrupt homojunctions in the nanocrystalline films by sudden change in DC-biasing during film growth.     

A crystallographic study of (2-acetylpyridine-κN 4-phenylthyosemicarbazonate-κ2N1,S) methyl-trans-dichlorotin(IV)

The preparation and characterization of [Sn(C₁₄H₁₃N₄S)(CH₃)Cl₂], an organotin(IV) complex containing 2-acetylpyridine(4)-phenylthiosemicarbazone, is described. The molecular structure was studied by single crystal X-ray diffraction, and IR and Mössbauer spectroscopies. The title compound crystallizes in the centric triclinic space group, P , as discrete neutral complexes, with the Sn(IV) ion in a distorted octahedral coordination geometry, with the thiosemicarbazone derivative in a meridional configuration and the chlorides in trans positions.     

Structure and characterization of tris(4-morpholinedithiocarbamato-S,S′)cobalt(·)acetonitrile solvate complex: [Co(S2CNC4H8O)3]·CH3CN

The crystal and molecular structure of the complex [Co(S₂CNC₄H₈O)₃]·CH₃CN has been determined by X-ray crystallography. The compound crystallizes in the triclinic system, space group P\overline 1 , with lattice parameters a = 10.561(2), b = 11.114(2), c = 13.011(3) Å, = 103.88(3), = 101.58(3), = 114.91(1)°, and Z = 2. X-ray analysis reveals that the cobalt(III) atom is located at the apparent intersection of D ₃ symmetry. Despite the apparent presence of the rotational axes, all of the atoms in the structure were found to be unique; there are no symmetry-related atoms. The central cobalt atom is octahedrally coordinated by an arrangement of six S atoms. The octahedron is distorted as a result of the forced configuration of the four-membered chelate ring. The average Co–S distance is 2.273 Å. The FT-IR spectra clearly show there are acetonitrile molecules in the crystal lattice.     

n(Sm3+)/n(S2O2-3)对液相自组装法制备Sm2S3薄膜的影响

采用液相自组装法,以氯化钐( SmCl3·6H2O)和硫代硫酸钠(Na2S2O3·5H2O)为原料,在不同n(Sm3 )/n(S2O2-3)(物质的量比)条件下,于硅基板上制备了α-Sm2S3光学薄膜.利用X射线衍射仪(XRD)、光电子能谱分析(XPS)、原子力显微镜(AFM)和紫外-可见吸收光谱仪(UV-Vis)对SmS3薄膜的物相组成、表面形貌和光学性能进行了表征.结果表明:所制备的Sm2S3薄膜为α-Sm2S3,在一定范围内,随着n(Sm3+)/n(S2O2-3)的增加,α-Sm2S3薄膜的结晶性先增强后降低,并表现出(105)晶面取向生长的特征.紫外透射光谱分析表明,当n(Sm3+)/n(S2O2-3)=1∶2时,Sm2S3薄膜在可见光范围内透过率高达85;,禁带宽度为4.12 eV.     

溅射制备Zn(O,S)薄膜及其在CIGS电池中的应用

通过射频磁控溅射(MS)工艺,在不同溅射功率下制备Zn(O,S)薄膜,并将其应用于CIGS异质结器件结构中.采用XRD、XRF、台阶仪、透反射光谱仪、SEM以及wxAMPS仿真软件对Zn(O,S)薄膜以及MS-Zn(O,S)/CIGS异质结器件进行研究.结果表明,低功率条件下(<80 W),Zn(O,S)薄膜内S/Zn明显降低,带隙减小,所制备的微晶或非晶结构Zn(O,S)薄膜材料中生成闪锌矿结构ZnS (α-ZnS);高溅射功率下(>100 W),薄膜内S/Zn增加并趋于稳定,Zn(O,S)材料结晶性能改善,α-ZnS消失,带隙增加.器件仿真结果表明,低功率条件下,缓冲层与吸收层(AB)界面导带失调值(CBO)增大,空间电荷区(SCR)复合加剧;高功率条件下,器件品质因子升高明显,主要是由于高功率引起的异质结界面类受主缺陷浓度增加.     

Crystal structure of (3-aminopropionato)bis(ethylenediamine)cobalt(III) catena-di(μ-chloro)dichloroplumbate(II) monohydrate

Crystals of [Co(C₂H₈N₂)₂(C₃H₆NO₂)]PbCl₄ · H₂O [a = 7.627(1) Å, b = 11.238(1) Å, c = 11.444(1) Å, α = 99.125(1)°, β = 103.80(1)°, γ = 94.739(1)°, V = 933.09(1) ų, Z = 2, and space group $P\bar 1$ ] contain the octahedral PbCl₆ groups that share edges to form infinite [Cl₂Pb(μ-Cl)₂] _n ²ⁿ chains, in which the terminal Cl atoms occupy the cis positions. The Pb-Cl bond lengths are 2.763(1)–3.180(3) Å. In the discrete cationic complexes, the Co atom is coordinated by two ethylenediamine molecules and the 3-aminopropionate anion. In the enantiomeric complex with the Δ absolute configuration, the ethylenediamine rings have the λ and δ configurations and the aminopropionate ring has the λ configuration.     

Study of the Phase Situation in 4-n-pentylphenyl-4′-n-heptyloxythiobenzoate (7S5)

Results of measurements of the specific heat of 4-n-pentylphenyl-4′-n-heptyloxythiobenzoate in the temperature range from about 90 K to about 370 K are presented. They were carried out with an adiabatic calorimeter, a differential scanning calorimeter and a polarizing microscope. Adiabatic calorimetry revealed four anomalies in the specific heat vs. temperature curve viz., two associated with transitions in the solid phase, one with melting and one with the liquid-crystalline nematic-to-isotropic phase transition. Also, two modifications of the solid, stable and metastable, were found to exist. In addition, the DSC method applied in the 285 K to 370 K range revealed a smectic C phase, but only when the sample is being cooled. The polarizing microscope showed the structural polymorphism of the solid phase in the 297 K to 327 K range to be more complex than would stem from adiabatic calorimetry and DSC measurements alone. It also confirmed the occurence of the S_c phase on cooling as ascertained by the DSC method.