Preparation and Structure of A Novel Ethanolamine-occluding Aluminoarsenate

An aluminoarsenate, Al2As2O3.EAN, denoted as AlAsO4-1 was synthesized from EAN(EAN= ethanolamine), pyroarsenic acid and aluminium-iso-propylate systems. The crystal structure of AlAsO4-1 was determined by single crystal X-ray diffraction method. The compound crystallizes in orthorhombic space group Pcab with the unit cell constants:0 = 8.781(3), 6=10.261(3), c=20. 433(11) A .V = 1840.9 A3, 2=8. The final R and Rw factors are 0. 0401 and 0. 0344, respectively. The framework of AlAsO4-1 contains two types of Al atoms. It is interesting that in the asymmetric unit one of two Al atoms is strictly 4-coordinated and the other is 6-coordinated. The three-dimensional framework is built of two-dimensional nets which consist of 4-membered rings and 8-membered rings. The biggest open channel in the framework runs along [100], in which EAN template is located. Arsenic atoms can function as a component element for construction of three-dimensional net with topological novelty.     

Synthesis and Crystal Structure of {(PPh_3)_2CIRuCIRu(PPh_3) B_(10)H_8[OCH(CH_3)_2)]_2}

1INTRODUCTIONAlthoughseveralhundredpolyhedralmetallaboraneshavebeencharacterized,theincidenceofruthenaboranesisparticularlysurprising.(hThefirstpolyhedralruthenaboraneisstructurallytypifiedbythecompound[(PPh,)2RuB,,HS(OEt),j,whichisobtainedin40%yieldsfromthereactionbetweentRuCI,(PPh,),jandcloso-tB,,H,,j'--inCHCI,/EtOH.tZiWithCH,COOH/THFt'iandC,H,COOH/CH,CI,">insteadofCHCI,/EtOH,twocompoundsF{(PPh,)2Ru}~(p-MeCO,)3--(pH)z-{RuB,,H,}jand[(PPh,)2(PhCOO)RuB,,HSCljhav…     

The Crystal structure of Hexakisammonium Diacetyloctamolybdate Tetrahydrate

1　ＩＮＴＲＯＤＵＣＴＩＯＮＴｈｅｓｔｕｄｉｅｓｏｎｏｒｇａｎｉｃｐｏｌｙｏｘｏｍｅｔａｌｌａｔｅｓｈｅｌｐｔｏｕｎｄｅｒｓｔａｎｄｔｈｅｒｏｌｅｓｏｆｐｏｌｙｏｘ ｏｍｅｔａｌｌａｔｅｓｏｎｃａｔａｌｙｓｉｓ.Ａｓｅｒｉｅｓｏｆｏｃｔａｍｏｌｙｂｄａｔｅｓｗｉｔｈｄｅｓｃｒｉｐｔｉｏｎ〔Ｍｏ8Ｏ2 6Ｘ2 〕2ｎ -4(ｎｉｓｔｈｅｎｏｒｍａｌｃｈａｒｇｅｏｆｔｈｅｃｏｏｒｄｉｎａｔｅｄｂａｓｅＸ)ｈａｖｅｂｅｅｎｒｅｐｏｒｔｅｄｉｎｌｉｔｅｒａｔｕｒｅｓ .Ｔｈｅｉｒｓｔｒｕｃｔｕｒｅｓｏｆｔｈｅα ,β ,γ …     

Synthesis and Crystal Structure of 4-tert-Butyl-6-（4-chlorophenyl）-3,6- dihydro-2H-1,3-thiazin-2-iminium Chloride

The title compound, 4-tert-butyl-6-（4-chlorophenyl）-3,6-dihydro-2H-1,3-thiazin- 2-iminium chloride （C14H18C12N2S）, has been synthesized by the reaction of 1-（4-chlorophenyl）- 4,4-dimethylpent-1-en-3-one with thiourea, and its crystal structure was determined by single- crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P211c with a = 16.3064（11）, b = 9.4471（6）, c = 11.2626 （8）A, β = 108.400（1）°, Z = 4, V = 1646.28（19） A^3, Mr = 317.26, Dc = 1.280 g/cm^3, S = 1.078,μ = 0.510 mm^-1, F（000） = 664, the final R = 0.0514 and wR = 0.1412 for 3210 observed reflections （I 〉 2σ（I））. The thiazine ring system displays a twisted boat conformation, and three N-H,..Cl hydrogen bonds exist in the crystal. The combination of two N-H...Cl hydrogen bonds generate an R2^1 （6） ring.     

Synethesis and Crystal Structure of Bi(ethylenediamine)copper Tetracyanonickelate(Ⅱ)

The crystal structure of the title compound C8H16CuN8Ni has been determined by single crystal X-ray diffraction. The crystal is triclinic with space group P1, a=6.494(3), b=7.270(4), c=7.936(5) .A, α=106.67(3), β=91.33(4), γ=106. 80(6)°, V=341. 3(3) A3, Z==1, Mr=346. 54, F(000)=177, μ=2. 933mm-1, Dc= 1. 686 Mg/m3. The final R factor is 0. 0603 for 1214 unique ob24- served reflections [I≥2σ(I)]. The structure consists of [Cu(en)2]2+ (eh=ethylenedi amine) cations and [Ni(CN)4]2- anions linked together by two of the CN groups (the remaining two act as unidentate ligands) to form infinite chains, in the chain, the hy between the interchains also exist, with distances of 3. 160 and 3. 124 A , so it forms a three-dimensional structure of the title compound.     

Crystal Structure of Diethyl 1-(p-toluenesulfonamido)-p-chlorophenylmethylphosphonate

1mrnODUCTIoNThederivativesofa-aminophosphonicacidhavebeenwidelystudiedduetotheinterestintheirvariousbiologicalactivitiestl)-Forthepurposeofsearchingfornewkindsofherbicides,aseriesofdiethyl1-(P-toluenesulfonamido)-(substituted)phenylmethylphosphonates1havebeensynthesizedbyathree-comPonentreaction'ofHtoluenesulfonamide,a(substituted)benzaldehydeanddiethylphosphite(2).Howev-er,thelHNMRsPectraofalltheproductsshowedthatthetwoethoxygroupsintheirstructuresaremagneticallynonequivalent.Inordertoe…     

Synthesis and Crystal Structure of Compound [ZnS6 (C12H8N2)]

The title compound ZnS6(C12H8N2) was obtained by reaction of zinic powder with sulfur and 1,10-phenathtroline in DMF solvent, and its structure has been determined by single crystal X-ray diffraction analysis. The crystal data for the compound: triclinic, P-1, Z = 2, a = 8. 159(2), b = 9. 485(2), c = 11. 997(2)A , α =110. 00(3)°,β = 99.22(3)°, γ = 100.57(3)°, V = 832A3, Dc =1. 748g/cm3, μ(MoKa)=0. 2219 cm-1, F(000)=440. The structure was refined to R = 0. 0723 and Rw = 0. 0865 for 1427 independent observed reflections. The tilte crystal consists of a discrete molecules, in which the core of ZnS2N2 shows a distorted tetrahedral geometry.     

Crystal Structure of 2-Germatranylmethyl-N-(4'-methylphenyl) succinimide

1INrnODUCTIONItiswell-knownthatitaconicacidderivativesandgermatraneshavemanybioac-tivitiest1.23.lnordertoinvestigatethestructureandantitumoractivitiesofnewger-maniumcompounds,wesynthesizedaseriesofpolycycliccompoundsbythereactionoftrichlorogermanewith2-succinimidesor2-methylenesuccinamicacids[3i.Aspartofthiswork,n0wwereP0rtinthispaPerthecrystalstructureofthetitlec0mpound.2EXPERIMENTAL2-Germatranylmethyl-N-(4'-methylphenyl)succinimidewassynthesizedasacolourlesscrystal,anditsstructureh…     

THE CRYSTAL AND MOLECULAR STRUCTURE OF N,N~'-DI-n-BUTYL-29,30-DIMBTHOXY-13,27-DICHLORO-6,20-DIAZA-3,9,17,23-TETRAOXA TRICYCLIC (23.3.1.1~(11,15))-CYCLOTRIACONTANE-1(29),11,13,15(30),25,27-HEXENE

<正> C34H52N2O6Cl2, Mr=655.70, triclinic, Pl,a=8.909(5),b=9.158(5), c=11.841(9) A,α=73.41(5)°,β=76.51(8)°,γ=80.38(6)°, V = 895.1 A3, Z=l, DC=1.223 gcm-3,λ= 0.7107 A,μ=2.299 cm-1.Full matrix least-squares refinement, final R = 0.088, Rw= 0.084 for 1039 (I>36) unique reflections. The crystal is composed of separate molecules having an approximate inversion center. The molecule is shaped like an ellipse. The distances of 0(31)-0(32), 0(41)-0(42), and N(31)-N(41) are 4.254, 4.136 and 10.930 A, respectively.     

Crystal Structure of Co（S2CPh）3

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＣｏ（Ｓ_２ＣＰｈ）_３ＬｕＳｈａｏ－Ｆａｎｇ；ＣｈｅｎＨｏｎｇ－Ｂｉｎ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ（ＦｕｊｉａｎＩｎｓｔｉｔｕｔｅｏｆＲｅｓｅａｒｃｈｏｎｔｈｅＳｔｒｕｃｔｕｒｅｏｆＭａｔｔｅｒ，Ａｃａｄｅｍｉａ...     

单、双核镍(II)配合物的晶体结构、光谱和磁性

报道2个具有三足四齿配体,三(2-甲基吡啶)胺(缩写TPA)的单、双核镍(II)配合物。X射线晶体结构分析结果表明,双核镍配合物(1)晶体(C~3~6H~3~6N~8Ni~2Cl~2).11/6(ClO~4).1/6(OH).8/6(H~2O)属三方晶系,空间群为R-3,a=2.8425(4)nm,b=2.8425(4)nm,c=1.4385(5)nm,α=β=90.00ⅲ,γ=120.00ⅲ,Z=18,最终因子R=0.078,Rw=0.078。单核配合物晶体C~2~0H~1~8N~6NiS~2.0.5(H~2O),属三斜晶系,空间群P1,a=0.9467(1)nm,b=1.5566(3)nm,c=1.5913(3)nm,α=73.59(4)ⅲ,β=87.37(3)ⅲ,γ=76.27(2)ⅲ,Z=4,最终因子R=0.0784,Rw=0.238。双核配合物的变温磁化率(4-300K)数据表明,用最小二乘法进行理论拟合(H=-2JS~1.S~2),得出交换积分J=6.72cm^-^1,θ=-0.60cm^-^1,表明双核镍之间为弱的铁磁相互作用,分子间为弱的反铁磁相互作用。     

Crystal and Molecular Structure of 2-(2, 6-Dinitro-4-Trifluoromethyl) phenylthio-5, 7-Dimethyl-1,2,4-Triazolo [1, 5-a] Pyrimidine

1INTRoDUCTIONItwasreportedthattheheterocycliccompoundscontainingl,2,4-triazolo[1,5-ajpyrimldinyldisplayedpotentialbioIogicalactivities['2i.Howeverltheherbicidalac-tivityofthethio-etherderivativesof1,2,4xtriazolo[1,5-ajpyrimidinewasrarelyre-ported"'.Inourpreviouspaper"',wedesignedandsynthesizedaseriesof2-arylthio-l,2,4-triazolo{l,5-ajpyrimidines,someofwhichdisplayedgoodherbicidalactivity.Inordertostudythestructure-activityrelationshipofthesecompounds,thestructureofthetitlecompound(1)wasan…     

Synthesis and Crystal Structure of a Three-dimensional Mn(Ⅱ) Coordination Polymer with 3-(Pyrazin-2-yloxy)-pyridine and Azide Anion as Mixed Bridge Ligand

A three-dimensional coordination polymer [Mn2(μ1,3-N3)4(μ-PP)2]n(PP = 3-(pyra-zin-2-yloxy)-pyridine) has been synthesized with 3-(pyrazin-2-yloxy)-pyridine and azide anion as mixed bridge ligand,and its crystal structure was determined by X-ray crystallography.The crystal data:triclinic system,space group P,with a = 6.794(4),b = 9.885(6),c = 9.947(6) ,α = 64.170(6),β = 84.190(8),γ = 85.319(8)°,V = 597.7(6) 3,Z = 1,C18H14Mn2N18O2,Mr = 624.35,Dc = 1.735 g/cm3,F(000) = 314 and μ = 1.117 mm-1.In the crystal,the azide anion acts as a bridge ligand and makes adjacent Mn(II) ions connect into a two-dimensional sheet on the ab plane,then 3-(pyrazin-2-yloxy)-pyridine serves as a bidentate bridge ligand to connect neighboring sheets along the c axis,and finally a three-dimensional structure is formed.     

Excision of the

The synthesis of new molybdenum cluster selenocyanide anionic complexes [Mo6Se8(CN)6]7- and [Mo6Se8(CN)6]6- is reported. The [Mo6Se8(CN)6]7- ion was obtained by excision of the cluster core [Mo6Se8] from a Chevrel phase in the reaction of Mo6Se8 with KCN at 650 degrees C; the [Mo6Se8(CN)6]6- ion is formed by oxidation of [Mo6Se8(CN)6]7-. New cluster salts K7[Mo6Se8(CN)6] x 8H2O (1) and (Me4N)4K2[Mo6Se8(CN)6] x 10H2O (2) were isolated and their crystal structures were solved. Compound 1 crystallizes in the cubic space group Fm3m (a=15.552(2) A, Z=4, V=3761.5(8) A3), compound 2 crystallizes in the triclinic space group P1 (a=11.706(2), b=11.749(2), c=12.459(2) A, alpha=72.25(1), beta=77.51(1), gamma=63.04(1), Z=1, V=1448.5(4) A3). Compound 1 is paramagnetic due to an availability of 21 electrons per Mo6 cluster; cyclic voltammetry reveals a quasi-reversible transition [Mo6Se8(CN)6]7- <--> [Mo6Se8(CN)6]6-, E1/2=0.63 V.     

N─苯基邻苯二甲酰亚胺和N─对甲苯基邻苯二甲酰亚胺的晶体和分子结构

报道一种新类型的有机电子晶体Ｎ－苯基邻苯二甲酰亚胺（１）（Ｃ＿（１４）Ｈ＿９ＮＯ＿２）和Ｎ－对甲苯基邻苯二甲酰亚胺（２）（Ｃ＿（１５）Ｈ＿（１１）ＮＯ＿２）的晶体和分子结构，（１）属正交晶系，空间群为Ｐｃａｂ，ａ＝７．６４９（４），ｂ＝１１．６５９（２），ｃ＝２３．７３９（３）Ａ，Ｖ＝２１１７．０Ａ￣３，Ｚ＝８，Ｄ＿ｃ＝１．４０１ｇ／ｃｍ￣３，Ｍ＿ｒ＝２２３．２３，μ＝０．８８５ｃｍ￣（－１），最终偏离因子Ｒ＝０．０５３，Ｒ＿ω＝０．０４８；（２）属正交晶系，空间群为Ｐｎａ２＿１，ａ＝７．６２４（２），ｂ＝１１．２３７（１），ｃ＝１３．８５６（２）Ａ，Ｖ＝１１８７．０　Ａ３，Ｚ＝４，Ｄ＿ｃ＝１．３２８ｇ／ｃｍ￣３，Ｍｒ＝２３７．２６，μ＝２．７６４ｃｍ－１，最终偏离因子Ｒ＝０．０３６，Ｒ＿ω＝０．０３２。晶体结构测定结果表明，邻苯二甲酰亚胺的内酰亚胺碳、氮、氧原子与其苯并环共平面。化合物（２）中的甲基碳原子与取代基苯环共平面，苯并酰亚胺平面与取代苯环平面间的夹角分别为５８．４°（化合物１）和５６．２°（化合物２）。     

DETERMINATION OF CRYSTAL STRUCTURE OF C6H5GdCl2（THF）4

<正> By X-ray (λ=0. 71069A) diffraction of single crystal,we have determined the crystal structure of C6H5GdCl2 (THF)4,C22H37Cl2O4Gd, MT=593. 2,or-thorhombic space group Ccm2;with lattice parameters a=12. 776(6),b=12. 954(6), c=15. 802(3)A ;V=2615. 4(1. 8)A3;Z=4,Dc=2. 43gcm-3,μ=29. 3cm-1,F(000) = 1120. The structure was solved by heavy-atom method and Fourier techniques and refined by least-squares to a final R=0. 051 ,Rw = 0. 049 for 839 reflections with I≥1. 5σ (I). The results revealed that the bond length of Gd-C is 2. 437(22) A ,the average bond lengths of Gd-Cl 2. 678(6) A ,Gd-O 2. 499(12) A, C-C from phenyl group 1. 376(40)A. This crystal structure is the first organolanthanide complex with only one Ln-C bond in the molecule.     

1,2-二甲基-3-吲哚甲叉(异丙叉)丁二酸酐(1)和1,2-二甲基-3-吲哚乙叉(异丙叉)丁二酸酐(2)的晶体结构

1.2-二甲基-3-吲哚甲叉(异丙叉)丁二酸酐(1)(C_(18)H_(17)NO_3)与1.2-二甲基-3-吲哚乙叉(异丙叉)丁二酸酐(2)(C_(19)H_(19)NO_3)同属于吲哚俘精酸类化合物,它们的分子结构非常类似,只是(1)中为吲哚甲叉,(2)中为吲哚乙叉.但它们的光色性却差别很大.化合物(1)无光致变色性,化合物(2)则表现为良好的光致变色性.其原因在于结构的不同。     

SOLID STATE PHOTOCHEMICAL SYNTHESIS OF A NOVEL HOST COMPOUND METHYL 4-(DI-3-INDOLYL) METHYLBENZOATE AND X-RAY CRYSTAL STRUCTURE OF ITS 1:1 INCLUSION COM-PLEX WITH ACETONE

<正> A novel host compound methyl 4-(di-3-indolyl) methylbenzoate p-CH3OCOC6H4CH (C8H6N)2(3) was prepared by irradiation of the mixed crystals of methyl p-formylbenzoate (1) and indole (2.). The crystal structure of 1:1 inclusion complex (3' ) formed by compound (3) and acetone has been examined by X-ray diffraction analysis. The crystal belongs to triclinic system, space group P1, with cell parameters: a = 9.902(3), b = 10. 626(2), c=12. 945(2) A , α=70. 69(2),β = 72.56(2), γ = 69. 53(2)°, V = 1177. 82(?)3, Mr = 438. 53, Z = 2, Dx = 1. 236g/ cm3, μ = 0. 75cm-1, F (000) = 464. The final R is 0. 041 for 2006 observed unique reflections. There are three main planes in one molecule of this compound, the dihedral angles between them are 62. 37°, 89. 12° and 83. 308, respectively.     

Crystal Structures of N，N＇－Bis（4－chlorophenyl）－1，10－diaza－18－crown－6 and Its Complexwith Ba（SCN）_2

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｓｏｆＮ，Ｎ＇－Ｂｉｓ（４－ｃｈｌｏｒｏｐｈｅｎｙｌ）－１，１０－ｄｉａｚａ－１８－ｃｒｏｗｎ－６ａｎｄＩｔｓＣｏｍｐｌｅｘｗｉｔｈＢａ（ＳＣＮ）_２￥ＺｈａｎｇＬｉ－Ｊｕａｎ；ＬｉｕＸｉａｏ－Ｌａｎ；ＭａＳｈｉ－Ｋｕ?..     

[Co(2,3-tri)(men)Cl][ZnCl4] 体系中三个经式异构体的晶体结构

在[Co(2,3-tri)(men)Cl][ZnCl₄](2,3-tri = N-(2-氨乙基)-1,3-丙二胺;men=N-甲基乙二胺)体系中可能的几何异构体的数目多达二十个,其中经式异构体八个,面式异构体十二个。用单晶 X-射线衍射分析方法解析了三个获得单晶的经式异构体,它们的晶体学参数:(1)m3-[ZnCl₄](monoclinic P2₁/c,a=8.0874(18),b=1