CRYSTAL STRUCTURE OF Fe4S4[SC（CH3）3]4[（C4H9）4N]2

<正> Fe_4S_4[SC(CH_3)_3]_4[(C1H_9)_2,Mr=1193. 23,tetragonal,142d,a = 23. 272(2), c= 13. 080(5) A ,V=7084(3) A3,Z=4,DC=1. 12g·cm-3,UUUU(MoKa) = 10. 8cm-1,F(000) = 2568,R=0. 058 for 1005 observed reflections. The cluster anion contains a cubane-type Fe4S4 core compressed along the 4 axis which is crystallographically imposed. Compared to other salts with different cations ,the core is subject to slight structural distortions in different crystalline environments and crystallographic symmetry of the anion is related to that of the cation.     

STRUCTURE OF PLATINUM HYDRIDE WITH BULKY PHOSPHINE LIGANDS trans-PtH (PCy_3)_2 {S_2CN (CH_2C_6H_5)_2}

<正> trans-PtH(PCy3)2[S2CN(CH2C6H5)2] crystallizes in triclinic space group P1 with a=10. 961 (9),b= 13. 247 (6), c= 18. 331(4) A ,α=82. 97(2) ,β= 103. 89(5),γ=103. 79(7)°,Mr=1029. 39,V = 2503(4)A3,Z = 2,Dc = 1. 366g/cm3, μ= 30. 06cm-1,F(000) = 1068,R=0. 033 and Rw = 0. 039 for 6940 unique observed reflections. The platinum atom is coordinated by one hydrogen,one sulfur and two phosphorus atoms to form a distorted square plane.     

[(C_5H_4CH_3)_2HoN_4CPh]_2·[(C_5H_4CH_3)(C_5H_5)HoN_4CPh]_2的合成和晶体结构

（C5H4CH3）3Ho和（C5H4CH3）2Ho（C5H5）与5-苯基四唑（HN4CPh）在THF中反应，得到复合产物[（C5H4CH3）2HoN4CPh]2·[（C5H4CH3）（C5H5）HoN4CPh]2，该晶体属三斜晶系，P1空间群，晶胞参数为a=9．386（3），b=13．071（3），c=16.571（2）A，a=86．90（1），β=74．61（2），γ=77.30（2）°，V=1912．2（8）A3，Z=1，Dc=1.602g／cm3，Mr=922．61，μ=41．92cm－1，F（000）=896，最终偏离因子R=0．041，Rw=0．056．晶体数据显示，在同一个晶胞里有两个组成不同的分子，每一个分子都是具有对称中心的四唑基桥二聚体结构，其桥环单元-HoN3HoN3-是平面型的。每个钬原子分别被两个茂基和3个四唑基氮原子配位，形成1个边桥变形四面体构型。     

SYNTHESIS AND CRYSTAL STRUCTURES OF {Pr[(C_2H_5O)_2POO]_3}_n

The synthesis, characterization and crystal structure of rare earth coordination complex of {Pr[(C_2H_5O)_2POO]_3}_n has been studied. It is triclinic with space group P1 in a unit cell of dimensions a=11.788(5), b=12.536(3), c=10.262(2.) , α=112.21(2), β=93.01(3), γ=109.94(3)°; V=1290.9(8)~3, Z=2. As shown in Fig. 1, each Pr atom is connected with other two Pr atoms through three "O-P-O" bridging groups to form a long chain polymer. The coordination number of Pr is six. The six coordinated O atoms form an octahedron. The average bond distance of Pr-O is 2.333 A. The complex has been also studied by infrared spectroscopy and thermal analyses.     

CRYSTAL STRUCTURE OF {Ni[(C_4H_9O)_2PS_2](C_(12)H_8N_2)_2} -[(C_4H_9O)_2PS_2]

<正> {Ni C(C4H9O)2PS2] (C12H8N2)2} [C(C4H9O)2PS2], Mr= 795. 60, Monocinic,P2,/n,a=16. 806(2), b=12. 720(2), c=21. 248(2) A. β=98. 454(7)°, V = 4493A3,Z=4,Dc= 1. 18g·cm-3,Mo Ka radiation,A=0. 71069A ,F(000) = 1664, R=0. 102 for 4154 reflections with I≥3σ(I).The crystal structure consists of complex cation {NiC(C4H9O)2PS2](C12H8N2)2}+ and complex anion C(C4H9O)2PS2]-. In the cation, nickel (Ⅱ) atom is coordinated by four nitrogen atoms and two sulfur atoms to form a distorted octahedron.     

(C5H7S2)2[Cu3I5]的合成和晶体结构

我们曾经对二硫代乙酰丙酮和多种金属离子的配合反应进行了系统的研究.在成功合成(C_5H_7S_2)_2[CuBr_3]的基础上,最近我们试图用类似方法合成(C_5H_7S_2)[CuI_3].但对产物晶体的X 射线衍射分析结果却表明,所得到的化合物的分子式为(C_5H_7S_2)_2[Cu_3I_5].[Cu_3I_5]~(2-)是以[CuI_3]配位三角形和两个相邻[CuI_4]配位四面体连接的无限链状配合阴离子形式存在.     

SYNTHESIS AND STRUCTURE OF THE FIRST TUNGSTEN-IRON-SULFUR CUBANE-LIKE CLUSTER [WFe_3S_4(S_2CNC_4H_8)s]·2DMF CONTAINING DITHIOCARBAMATO LIGANDS

<正> The title compound (Mr =1236.54) crystallizes in monoclinic space group C2/c with a =12.553(4),b=20.121(6),c=19.659(2)A,β=102.96(2)°,V=4839.1A3, Z = 4 and DC -1.697g/cm3. The structure was solved by direct methods.A full matrix least-squares refinement for 2197 reflections with I>3σ(I) gave final R and Rw of 0.064 and 0.076,respectively. The [WFe3S4] core of the cluster can be considered to be a [WFe3] tetrahedron capped by a sulfur atom on each face to fora a distorted cubane. The 57Fe Mossbauer spectrum indicates that there are two types of Fe atoms of ratio 2:1 in the cluster.     

CRYSTAL STRUCTURE OF Na[Nd(S_2CN(C_2H_5)_2)_4]·CH_3CN

<正> Triclinic, PI, a=10.204(3), b=ll.384(2), c=18.399(4) X, a=84.19 (2), 6=106.15(2), Y=116.71(2)? V=1833.1(6)S3, Z=2, y=18.76cm, A=0.71069&, F(OOO)=809.91, room temperature, .R=0.059. In, the title compound the neodym-ium ion is coordinated by eight sulphur atoms from S2CNEt2ligands with the average distances of 2.88A and 2.<.Et2N桟桟\(:S桸Et2-Nb-\\C 桸Et2     

STRUCTURE OF {Mo4S4（μ—OAc）2[S2P（OC2H5）2]4H}

<正> {Mo4S4(μ-OAc)2(dtp)4H}3,(dtp=S2P(OEt)2),Mr=1371.60,Or-thorhombic, space group Pcab, a = 18. 90 (2) ,b = 21. 678 (4 ) , c = 24. 491 (4 ) A , V = 10031(7)A3,Z=8,Dc=1.818g/cm-3,F(000)=5464,λ(MoKa)=0.71073A,finalR= 0. 069 for 3738 independent reflections. This is a successful example of the formation of [Mo4S4]5+ from[3+1] reaction mode. The results of the structure determination indicate that the configuration of the title compound exhibits a tetranuclear cubane-type core [Mo4S4]5+ with six Mo - Mo distances in the range 2. 685~2. 969A and is very similar to that of the previously characterized compound {Mo4S4(μ-OAc)2(dtp)4}2, [Mo4S4]6+, which was obtained directly by the reaction of MoCl3·3H2O with dtp. Some notable differences, however, can be found when six Mo - Mo bond distances and bonding parameters of the four terminal bidentate ligands (dtp) are compared between these two compounds , That can be attributed to the difference in the oxidation state of these two clusters .     

Synthesis and structure of {Mo_3S_7[S_2P(OC_2H_5)_2]_3}{Mo_3S_4[S_2P(OC_2H_5)_2]_4(SCN)} and interaction between their cluster units

Ｔｈｅｔｒｉｍｏｌｙｂｄｅｎｕｍｃｌｕｓｔｅｒｓｗｉｔｈｇｅｎｅｒａｌｆｏｒｍｕｌａ[Ｍｏ3(μ3Ｓ)(μＳ)3(μｄｔｐ)(ｄｔｐ)3Ｌ](ｄｔｐ=(Ｓ2Ｐ(ＯＣ2Ｈ5)2)-,Ｌ=Ｈ2Ｏ,ｐｙ,ＳＣ(ＮＨ2)2ｅｔｃ.)[1](ｒｅｆｅｒｒｅｄｔｏａｓＭ1ｔｙｐｅ[2]),ａｎｄ[Ｍｏ3(μ3Ｓ)(μＳ2)3(ｄｔｐ)3]Ｘ(Ｘ=Ｃｌ,Ｉ)[3](ｒｅｆｅｒｒｅｄｔｏａｓＭ2ｔｙｐｅ),ａｒｅｔｗｏｍａｉｎｔｙｐｅｓｏｆｔｒｉｍｏｌｙｂｄｅｎｕｍｃｌｕｓｔｅｒｓｅｖｅｒｉｎｖｅｓｔｉｇａｔｅｄｂｙｏｕｒｒｅｓｅａｒｃｈｇｒｏｕｐ.Ａｓｗｅｈａｖｅａｌｒｅａｄｙ…     

Synthesis and Structureof［（C_2H_5）_4N］［Mo_3（μ_3－O）（μ－Cl）_3（μ－CH_3CH_2COO）_3Cl_3］

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ［（Ｃ_２Ｈ_５）_４Ｎ］［Ｍｏ_３（μ_３－Ｏ）（μ－Ｃｌ）_３（μ－ＣＨ_３ＣＨ_２ＣＯＯ）_３Ｃｌ_３］ＺｈｕａｎｇＨｏｎｇ－Ｈｕｉ；ＷｕＤｉｎｇ－Ｍｉｎｇ；ＨｕａｎｇＪｉａｎ－Ｑｕａｎ；ＨｕａｎｇＪｉｎ－Ｌ...     

SYNTHESIS AND CRYSTAL STRUCTURE OF A MOLYBDENUM-COPPER-SULFUR CLUSTER COMPLEX WITH DITHIOBENZOATE LIGAND [Bu_4N]_2[MoCu_2S_4(C_6H_5CS_2)_2]

<正> The title compound has been synthesized by the reaction of (Bu4N)2MoS4, CuCl and (C6H5CS2)(Bu4N) in DMF and recrystallized from DMF/ Et2O. The red black crystal belongs to the triclinic space group P1 with a = 12. 021 (6), b = 17.045(8), c=17. 136(7)(?) , α=110.05(3), β=108.64(4), γ=103.87 (4)°, V = 2873(3)(?)3, Dc=1. 321gcm-3, Z = 2. The structure was refined to R = 0. 065 for .4783 reflections. The anion of the title compound can be described as a MoS42- tetrahedron coordinated by two [Cu(C6H5CS2)] units with the three metal atoms lying on a line. The coordination number of each Cu atom is three.     

Structures that should be Described in Higher-Symmetry, Centrosymmetric Space Groups. Part 1. The Disordered Structures of [(CH_3CH_2)_4N]_3{[(SCH_2CH_2S)MoS_3]_2Fe}, [(CH_3CH_2)_4N]_2{[S_2CN(C_2H_5)_2]_4Fe_4S_4} and [(CH_3CH_2)_4N]_3{[(SCH_2C

1　ＩＮＴＲＯＤＵＣＴＩＯＮＡｍｅｔｈｏｄｏｆｓｐａｃｅｇｒｏｕｐｒｅｖｉｓｉｏｎｂｙｗｈｉｃｈｔｈｅｓｔｒｕｃｔｕｒｅｆａｃｔｏｒｓｏｆｔｈｅｌｏｗｅｒ ｓｙｍｍｅｔｒｙｓｔｒｕｃｔｕｒｅａｒｅｇｅｎｅｒａｔｅｄａｎｄｔｈｅｓｔｒｕｃｔｕｒｅｉｓｔｈｅｎｓｏｌｖｅｄｆｒｏｍｔｈｅｓｉｍｕｌａｔｅｄｉｎｔｅｎｓｉｔｙｄａｔａｈａｓｂｅｅｎｒｅｃｅｎｔｌｙｒｅｐｏｒｔｅｄ[1].Ｔｈｉｓｍｅｔｈｏｄｉｓｎｏｗａｐｐｌｉｅｄｔｏｔｈｅｒｅｖｉ ｓｉｏｎｏｆｔｈｅｓｐａｃｅｇｒｏｕｐｏｆｔｈｅｍｅｔａｌ ｃｌ…     

STRUCTURE OF NEODYMIUM TRINITRATE WITH DIPHENYL SULFOXIDE LIGANDS, Nd(N0_3)_3·[(C_6H_5SO]_4

<正> Mr=2278, triclinic, Pl, a=11.154(1), b=14.310(2), c=17.295(2) A, α=84.09(1)°, β=72.97(1)°, r=69:37(1)°, V=2470.2(5)A3, Z=2; 2(MoKα)=12.9cm-1 F(000)=1154, Dx=1.53 g/cm3, room temperature. The final R=0.039, Rw=0.039 with wt=1, S=2.57 for 5710 independent reflections with | Fα|≥2.5σ(F0). The molecular configuration of the Nd-complex is similar to those of the Sm-complex and Pr-complex except for the difference in distances between central metal and the coordinated oxygen atoms.     

Crystal Structure of Complex （Et4N）[VFe3S4Cl3（CH3CN）3]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅ1980,ｍａｎｙＶ/Ｆｅ/Ｓｈｅｔｅｒｏｍｅｔａｌｌｉｃｓｕｌｆｕｒｃｌｕｓｔｅｒｃｏｍｐｏｕｎｄｓｈａｖｅｂｅｅｎｒｅｐｏｒｔｅｄ.ＲａｕｃｈｆｕｓｓｅｔａｌｏｂｔａｉｎｅｄｔｗｏｋｉｎｄｓｏｆＶ/Ｆｅ/Ｓｃｏｍｐｏｕｎｄｓ[1]ｕｓｉｎｇ(ＣＨ3Ｃ5Ｈ4)2Ｖ2Ｓ4ａｓａｎｏｒｇａｎｏｍｅｔａｌｌｉｃｌｉｇａｎｄ,ｏｎｅｉｓ(ＭｅＣｐ)2Ｖ2Ｆｅ2(ＮＯ)2Ｓ4ｗｉｔｈａｃｕｂａｎｅｌｉｋｅｓｔｒｕｃｔｕｒｅａｎｄａｎｏｔｈｅｒｉｓ(ＭｅＣｐ)2Ｖ2Ｓ4Ｆｅ(ＮＯ)2ａｎｄ(ＭｅＣｐ)2Ｖ2Ｓ4…     

MASS SPBCTRA OF CUBAN-LIKE CLUSTER COMPOUND [MoFe_3S_4 (S_2CN■)_5]

<正> INTRODUCTION. We have previously reported the mass spectra of a single MoFe_3S_4 cubane-like cluster compound (Et_4N)MoFe_3S_4(Et_2NCS_2)_5. Its analogue MoFe_3S_4(C_4HaNCS_2)_5 having the same core structure has rently been synthesized and characterized structurally. In this paper, the results of its mass spectra investigation using an electron impact (EI) ionization mass spectrometer are offered and identified by metastable technique, isotopic     

Crystal Structure of (γ-CH_3C_5H_4N)_2Zn(S_2C_2(CN)_2)and the Second Harmonic Effect

1mrnODUCTIONMetallorganiccompoundisconsideredtobehighlyprospectiveasnonlinearoptical(NLO)materials.NLOpropertiesofmanymetallorganiccompoundshavebeenstudiedsince1986[h,clearlyshowingthepracticalmeaningofthiskindofresearch,especiallyforapplicationsinthevisiblefield.ForametallorganicNLOcrystaltobetransparentinthevisibleregion,generally,atleastthefollowingprerequisites"'mustbesatisfiedwithmolecularandcrystalstructurerespects.Firstly,theelectronconfigurationofcentricionsoftransitionmetalmustb…     

[（t—BuCp）2GdCl]2的合成及晶体结构

Wayda最近报道,无水氯化稀土LnCl_3和叔丁基环戊二烯钠(t-BuCp)Na进行交换反应时,由于歧化反应得不到单取代或双取代的轻稀土氯化物衍生物,只能得到中稀土和重稀土氯化物衍生物,并且没有测得这些配合物的晶体结构。我们采用提高反应温度和延长反应时间,使交换反应进行完全,有效地避免了歧化反应的发生,成功地分离到了单取代或双取代的叔丁基环戊二烯基轻稀土氯化物。并测得(t-BuCp)_2LnCl·nTHF(Ln=Pr,n=2;Ln=Yb,n=1)     

SYNTHESIS AND STRUCTURE OF A NEW LINEAR TETRANUCLEAR Mo-Fe-S CLUSTER (Et_4N)_2[(Et_2NCSSMoS_2)_2O_3Fe_2S_2]·DMF

<正> (Et4N)2[Et2NCSSMoS2)2O3Fe2S2]·DMF(1) ,Mr= 1174. 10,mono-clinic,space group P21/n,a = 9. 608(3),b=17. 962(2),c=15. 312(3) A ,β=95. 03 (3)°,V=2632. 4 A3,Dc= 1. 48 g/cm3 and Z=2. The structure was solved from 2499 reflections with I>3σ(Ⅰ) and refined by full-matrix least squares method to R(Rw) = 0. 073(0. 087). The anion of 1 has linear Mo -Fe -Fe-Mo array. The oxidation states of metal atoms in this cluster are 2Mo(Ⅵ) + 2Fe(Ⅲ).     

四核钼簇合物的配体取代反应及产物Mo_4S_4(μ-OAc)_2(dtp)_4的晶体结构

标题化合物(Ⅰ)经由Mo_4S_4(μ-dtp)_4(Ⅱ)[dtp=S_2P(OEt)_2]和Ni(OAc)_2反应而得。(Ⅰ)晶体属单斜晶系,空间群P2/c,a=13.176(4),b=11.699(3),c=18.526(4)(?),β=116.11(3)°,V=2564(3)(?)~3,Z=2,D_c=1.776g·cm~(-3)。晶体结构由直接法解出,最终偏离因子R=0.085。本文结果表明,可由已知的四核钼簇合物经过配体置换反应,合成得到其簇骼中心[Mo_4S_4]保持不变并具有-OAc作为桥式配体和-dtp作为端基配体的混合配体类立方烷[Mo_4S_4]簇合物。