单斜RbInS_2、CsInS_2的红外光谱及拉曼光谱

我们采用传统的助熔剂合成方法制备单斜RbInS2 、CsInS2 晶体并对它们的红外光谱和拉曼光谱进行研究。与RbInS2 相比 ,CsInS2 的红外吸收峰和拉曼吸收峰向长波方向移动。红外光谱和拉曼光谱均表明单斜RbInS2 、CsInS2 具有很好的红外透过性能。

Z状顺磁性化合物[{Cu(bipy)[C_6H_4(COO)_2]}_2·H_2O]_n和[Cu(phen)[C_6H_4(COO)_2]]_n的分子振动光谱研究

用分子振动光谱对已合成的具有顺磁性的化合物 [{Cu(bipy) [C6H4(COO) 2 ]} 2 ·H2 O]n(Ⅰ )和 [Cu( phen) [C6H4(COO) 2 ]]n(Ⅱ )进行深入研究 ,推测它们的结构 ,并将得到的结果与X射线晶体衍射测定的结构进行比较。文章对化合物的红外、拉曼光谱进行归属 。

混配配合物[Cu(1,10-phen)(CH_2(COO)_2)(H_2O)]_2·3H_2O的合成和晶体结构(英文)

在碱式碳酸铜与丙二酸水溶液反应后的滤液中加入 1 ,1 0—口菲口罗啉的乙醇溶液 ,放置获得一种蓝色块状的晶体 X—ray衍射显示为三斜P1群 ,a =1 1 .5 60 ( 2 ) ,b =1 1 .75 0 ( 2 ) ,c=1 2 .5 1 0 ( 3) A ,α =92 .1 3( 3) 。,β =1 0 5 .5 0 ( 3) 。,γ =1 0 9.30 ( 3)°,v=1 5 30 6( 5 ) A3,z=2 ,Mr=781 66,F( 0 0 0 ) =80 0 ,Dc=1 .696g/cm3,μ(MoKα) =1 .467mm- 1 ,R =0 .0 392 二聚体 [Cu( 1 ,1 0 -phen) (CH2 (COO) 2 ) (H2 O) ]2

Synthesis and Single Crystal Structure of RbEr_2Cu_3Se_5

Single crystals of a new quaternary rare-earth selenide RbEr2Cu3Se5 have been isolated through the RbCl flux reaction in the RE-Cu-Se system. The title compound crystallizes in an orthorhombic system, space group Cmcm with a = 4.089(2), b = 14.498(6), c = 16.977(2) ? V = 1006.5(7) ?, Z = 4, Dc = 6.63 g/cm3, F(000) = 1720 and m(MoKa) = 45.51 mm-1. The final R = 0.0498 and wR = 0.0734 for 1401 observed reflections with I > 3s(I). The structure of RbEr2Cu3Se5 is a three-dimensional tunnel structure composed of ErSe6 and CuSe4 polyhedra with the charge-balanced Rb+ cations stuffing into the one-dimensional channels along the a direction. In the Er2RbCu3Se5 structure, the 1[Er2Se(1)4/2Se(2)2Se(3)4/2] double-octahedral chains are linked into a 2[Er2Cu2Se6] layer in the a-b plane via sharing Se(1)Se(3) edges with the 1[Cu(2)2Se(1)2Se(3)4/2] double tetrahedral chains, and 2[Er2Cu2Se6] layers are further interconnected along the c direction by sharing Se(1)Se(2) edges with the 1[Cu(1)Se(1)2Se(2)2/2] tetrahedral chains, forming a three-dimensional framework with the channels along the a axis accommodated by Rb+ ions.

Synthesis and Crystal Structure of Ho_4S_3Si_2O_7

In an attempt to synthesize the homologous sulfide of KHo2CuSe4 by using KBr as flux in a sealed evacuated quartz tube, transparent crystals of Ho4S3Si2O7 (Mr = 924.08) were isolated. The crystal structure of Ho4S3Si2O7 was determined by single-crystal X-ray diffraction method. Ho4S3Si2O7 crystallizes in a tetragonal system, space group I41/amd (No. 141) with a = 11.666(4), c = 13.593(5) ? V = 1850(2) ?, Z = 8, Dc = 6.64g/cm3, F(000)= 3200, m(MoKa) = 34.79mm-1, final R = 0.0355 and Rw = 0.0378 for 851 reflections with I > 3s(I). The structure of Ho4S3Si2O7 contains two crystallographically independent Ho3+ cations that are interconnected by S2 anions and the isolated [Si2O7]6 units. Ho(1) is coordinated by three O atoms and three S atoms to form a trigonal prismatic geometry, while Ho(2) is coordinated by six O atoms and three S atoms to form a tricapped trigonal prismatic geometry. The Si2O7 double tetrahedra are in the eclipsed configuration with non-linear SiOSi bridges (angle : 129.2(9)).

Syntheses and Single-crystal Structures of Er_3Ge_xGeS_7 (1/4≤x≤1/2)

As part of our systematic research on the acentric rare earth chalcogenides, the ErAlGeS5/KBr, Er3AgGeS7/KBr and Er6Ge3S14/KBr systems were investigated and three compounds belonging to the R6B2C2Q14 (R = rare earth, B = 6-coordinated element, C = 4-coordinated element, Q = S and Se) family were identified. These compounds crystallize in the P63 space group, and the crystal data are as follows: Er3Ge1/4GeS7, a = 9.6480(14), c = 5.7920(12), Z = 2; Er3Ge0.382(8)GeS7, a = 9.6360(14), c = 5.8460(12), Z = 2; Er3Ge1/2GeS7, a = 9.6061(13), c = 5.8346(18), Z = 2. Single-crystal analysis indicated that the Er3GexGeS7 (x = 1/4, 0.382(8), 1/2) structures consist of three types of building blocks: ErS7, GeS4 and GeS6 units. Er3MxGeS7 are deficient compounds with the B sites occupied partly by Ge(IV) and /or Ge(II).

Syntheses,Structures and Band Gaps of KLnSiS_4(Ln=Sm,Yb)

Two new quaternary sulfides,KSmSiS4(1) and KYbSiS4(2),have been synthesized by high-temperature solid-state reaction.Single-crystal X-ray diffraction analyses indicate that both compounds crystallize in the space group P21/m,and the crystal data are as follows:a = 6.426(11),b = 6.582(11),c = 8.602(15) ,β = 107.90(13)°,Z = 2,V = 346.2(10) 3,Dc = 3.317 g/cm3,F(000) = 318,μ(MoKα) = 10.334 mm-1,the final R = 0.0559 and wR = 0.1370 for 1;and a = 6.3244(10),b = 6.5552(10),c = 8.5701(15) ,β = 108.001(13)°,Z = 2,V = 337.91(9) 3,Dc = 3.621 g/cm3,F(000) = 334,μ(MoKα) = 15.737 mm-1,the final R = 0.0422 and wR = 0.0960 for 2.The KLnSiS4(Ln = Sm,Yb) structure consists of corrugated ∞2 [LnSiS4]-layers which are formed by edge-sharing LnS8 bicapped trigonal prisms and SiS4 tetrahedra.The K+ cations are located in the cavities defined by S2-anions between the ∞2 [LnSiS4]-layers.Band-gap analyses show that compounds 1 and 2 are semiconductors with optical band-gaps of 2.40 and 2.34 eV,respectively.

Crystal Structure and Magnetic Property of a Quaternary Sulfide, Al_(0.36)Sm_3Ge_(0.98)S_7

A new quaternary sulfide, Al0.36Sm3Ge0.98S7 1, has been prepared by a facile solid- state reaction, and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the hexagonal space group P63 with a = 9.964(1), c = 5.768(2) , V = 495.9(1) 3 and Z = 2. In the crystal structure of 1, Al3+ and Ge4+ occupy the octahedral and tetrahedral interspaces of the 3-D main-framework constructed by SmS8 bicapped trigonal prisms, respectively. The investigation of optical and magnetic properties of 1 indicates that its optical band gap is 2.18 eV and it shows antiferromagnetic-like interaction.

Syntheses and Single-crystal Structures of New Deficient Compounds in the R_6B_2C_2Q_(14)Family

Four new deficient compounds in the R_6B_2C_2Q_(14)family,La_5CaSn_(2.75)S_(14)1,Y_6Al_(0.67)Ge_2S_(14_2,Er_(5.33)Si_4S_(14)3 and Er_4Ge_4S_(14)4,have been obtained via a precursor/flux method.Single-crystal analysis indicated that their crystal structures consist of three types of building blocks:RS_7(R=La/Ca for 1,R=Y for 2,R=Er for 3 and 4)mono-triangonal prism,CS_6(C=Al for 1,C=Sn(2)for 2,C=Si(2)for 3,C=Ge(2)for 4)octahedron,and BS_4(B=Si for 1,B=Sn(1)for 2,B=Si(1)for 3,B=Ge(1)for 4)tetrahedron,as any other compounds belong to the R_6B_2C_2Q_(14)family.

Syntheses and Single-crystal Structures of Ln_3Sn_(0.25)GeS_7 (Ln=La,Sm)

Two new quaternary sulfides,La3Sn0.25GeS71 and Sm3 Sn0.25GeS72,have been synthesized by a facile solid-state reaction,and their crystal structures were determined by singlecrystal X-ray diffraction analysis.The two compounds crystallize in the P6 3 space group,and the crystal data are as follows-La3Sn0.25GeS7:a=10.3335(7),c=5.8455(7),Z=2;Sm3Sn0.25GeS7:a=9.999(3),c=5.787(2),Z=2.Single-crystal analysis indicated that the two compounds consist of three types of building blocks:LnS 8 anti-tetragonal prism,SnS 6 octahedron,and GeS 4 tetrahedron.

Synthesis and Structure of Paramagnetic β-OctamolybdateComplex, [Fe(2,2'bipy)_3]_2[Mo_8O_26]·6H_2O

A novel octamolybdate complex, [Fe(2,2?bipy)3]2[Mo8O26]6H2O has been synthesized via the hydrothermal technique, and it crystallizes in monoclinic, space group P21/c with two molecules in a unit cell: a = 1.21512(5), b = 1.36840(5), c = 2.18823(9) nm, b = 90.515(1), Mr = 2340.42, Z = 2, V = 3.6384(2) nm3, Dc = 2.136 g/cm3, F(000) = 2296, l(MoKa) = 0.071073 nm, = 1.813 mm-1, R = 0.0719 and wR = 0.1093 for 4058 observed reflections with I≥2s(I). The structure is characterized by the co-existence of octahedral [Fe(2,2?bipy)3]2+ cations and b-octamolybdate [Mo8O26]4- anions. The magnetic susceptibility data show a Curie-Weiss paramagnetic behavior (q = -5.201 K) in accordance with the spin-only ground state of FeⅡ ions. IR, UV-Vis, and EPR spectra are also briefly noted in this paper.

Syntheses and Crystal Structure of [Cu(pyr)_3]·Hg_2I_6

A new compound containing discrete cationic and anionic complexes, [Cu(pyr)3]Hg2I6 (C30H24CuHg2I6N6), where pyr = 2,2-bipyridine, was prepared by the reaction of CuBr with pyr and HgI2 in a mixed solvent of acetone, methanol and acetonitrile. Single-crystal X-ray diffraction analysis indicates that it crystallizes in an orthorhombic system, Pna21 (No. 33), a = 33.1595(7), b = 9.4605(1), c = 13.0899(2) ? V = 4106.4(1) 3, Mr = 1694.67, Dc = 2.741 g/cm3, Z = 4, F(000) = 3012, m(MoKa) = 12.511 mm-1, R = 0.0736, wR = 0.1360 (I > 2(I)) and S = 1.218. The structure consists of discrete [Hg2I6]2- anions and [Cu(bipyridine)3]2+ cations. The double tetrahedral [Hg2I6]2- unit is formed by sharing one tetrahedral edge and possesses approximate D2h symmetry. The mononuclear Cu2+ ion is coordinated by six N atoms from three pyr molecules to form a slightly disordered octahedral geometry.

Solvothermal Synthesis and Structure Studies of a Mixed-valence Oxochloromolybdenum Complex

Emerald green crystals of a new mixed-valence oxochloromolybdenum complex, Mo(OH)2(2,2-bipy)Cl2[MoO(2,2-bipy)Cl3]2, were obtained in an attempt to synthesize the MoS cluster compounds under solvothermal conditions. The title compound was characterized by EPR and X-ray single-crystal diffraction techniques. Crystallographic data: orthorhombic, space group Fdd2, a = 12.684(1), b = 21.518(2), c = 29.096(3) , Mr = 1103.97, V = 7941(1) 3, Z = 8, Dc = 1.843 g/cm3, = 1.514 mm-1, F(000) = 4304, R = 0.0654 and wR = 0.1544 for 1944 observed reflections with I ≥ 2(I). The compound consists of two different neutral molecules, MoⅣ- (OH)2(2,2-bipy)Cl2 and MoⅤO(2,2-bipy)Cl3. Both MoⅣ and MoⅤ ions are in a distorted octahedral environment. The Mo(1)Ⅳ atom is surrounded by two Cl- ions and two O atoms from OH- and two N atoms from a 2,2-bipy ligand. The Mo(2) atom is surrounded by three Cl- ions, one O2- anion and two N atoms from another 2,2-bipy ligand. The bipyridine occupies two cis-equatorial sites, while the Cl- ions are located at the axial and equatorial positions.

Synthesis and Structure of Zinc 3-Hydroxy-2-mercaptopyridine Complex, Zn(C_5H_4NOS)_2

The zinc 3-hydroxy-2-mercaptopyridine complex was prepared by self-assemby reaction of Zn(NO3)2 and 3-hydroxy-2-mercaptopyridine (hmp). Single-crystal X-ray diffraction analysis indicates that it crystallizes in a tetragonal system, space group (No. 122) with a = 13.4562(6), c = 13.6860(8) , V = 2478.1(2) 3, Z = 8, Mr = 317.67, Dc = 1.703 g/cm3, m(Mo-Ka) = 2.308 mm-1 and F(000) = 1280. R = 0.0289 and wR = 0.0676 for 1040 observed reflections (I > 2s(I)). The crystal structure consists of a neutral molecule with a distorted tetrahedral cis-ZnS2O2 core, in which the mononuclear Zn2+ ion is coordinated by two O and two S atoms from two hmp ligands with the average bond distances of 2.301(1) ?for ZnS and 1.986(3) ?for ZnO. The 1H . NMR and IR spectra of the compound are discussed.

Synthesis,Crystal Structure and Magnetic Properties of the New Quaternary Thiophosphate Rb_2FeP_2S_6

A new quaternary thiophosphate Rb_2FeP_2S_6 was synthesized by the alkali metal halide flux method.The compound crystallizes in the monoclinic space group P2_1/c(No.14) with a = 6.042(3),b = 12.338(6),c = 9.045(4) ?,b = 124.25(2)°,V = 557.3(5) ?~3 and Z = 2.Its structure features 1-D infinite _∞~1[FeP_2S_6]^(2-) chains and counter cations Rb^+.It shows a band gap of 2.03 eV.The nearest intra-chain Fe^(2+) cations are antiferromagnetically coupled with each other,and there are weak ferromagnetic-like interactions between neighboring _∞~1[FeP_2S_6]^(2-) chains,resulting in two successive magnetic phase transitions.

两个含镧硫化物的结构及红外非线性光学性质

通过高温固相反应得到了两个新的四元稀土硫化物,La_3MgGaS_7(1)和La_6MgSn_2S_(14)(2)。化合物1和2都结晶于六方晶系手性空间群P63且异质同构,其三维晶体结构可描述为:化合物中的MgS_6八面体通过共面形成一条以沿63轴对称的一维链,其周围被三重轴对称的MS4(M=Ga,Sn)四面体包围,MgS_6一维链和MS4四面体通过S-La键连接而形成三维结构。化合物2的二阶非线性信号在入射光波长为1910nm时为AgGaS_2(AGS)的0.2倍。第一性计算表明,化合物1和2的光吸收主要是由电子从S-3p轨道跃迁至La-6s轨道引起。