H_(3+n)[AsMo_(12-n)V_nO_(40)]·9H_2O(n=2—4)的结构

X光晶体结构分析证实H_(3+n)[AsMo_(12-n)V_+nO_(40)]·9H_2)(n=2—4)的晶体同构,空间群为P,Z=2。n=2时,a=13.951(5),b=14.137(5),c=13.556(4),α=112.44(2),β=109.49(3),γ=60.77(3)°,V=2120.2,M_r=1943.36,D_c=3.044g.cm~(-3),μ=40.90cm~(-1),F(000)=1828。用6216个I>3σ(I)的独立衍射精修结构,R=0.082;n=3时,a=13.891(7),b=14.076(5),c=13.483(5)A,α=112.34(3),α=109.26(3),γ=60.82(3)°,V=2094.5,M_r=1899.37,D_c=3.011g.cm~(-3),μ=40.63cm~(-1),F(000)=1792。用6699个I>3σ(I)的独立衍射精修结构,R=0.054;n=4时,a=13.854(3),b=14.099(2),c=13.501(4),α=112.09(2),β=109.13(2),γ=61.03(2)°,V=2103.0,M_r=1855.38,D_c=2.92(悬浮法),D_c=2.930g.cm~(-3),μ=39.71cm~(-1),F(000)=1756。用7613个I>3σ(I)的独立衍射精修结构,R=0.044。实验采用MoKα辐射,λ=0.71073,T=296K。杂多阴离子均呈准Keggin结构,12个金属原子呈无序分布,可以M(Mo/V)表示。AsO_4四面体中As—O键长1.66—1.68,O—As—O键角均在109.5°左右。畸变的MO_6八面体中,M—O键长分布在1.63—2.36范围。水分子无序处在晶胞中十四个位置上,除O_w(12)和O_w(13)外的水分子均与杂多阴离子形成氢键,且水分子间形成如沸石中那样的复杂?     

CRYSTAL STRUCTURE OF [Eu(μ-CH_3COC-O)(CH3COO)_2(H_2O)_2]_2·4H_2O

<正> C12H34O20Eu2,Mr=802.30 triclinic, space group P1, a= 8.955(2), b=9.328(1), c=10.536(2) A,α= 91.74(2),β=113.87(2),γ=118.23(2), V=681.7(2)A,Dm(flotation in CC14/ BrCH2CH2Br)=1.95,DX(Z=1) =1.954g cm-3,λ(MoKα)=0.71069 A,μ=6.41 cm-1,F(OOO)=391.92, T =. 295°K,final RF= 0.032 for 7483 observed reflections with |F0|>3a(|Fo|). The compound is isostructural with the known erbium complex,the basic unit being a centrosymmetric dimer composed of two nine-coordinate polyhedra sharing a common edge. An O atom in one or the three bidentate acetato groups about each europium atom serves as a bridge between the metal centars. The dimeric units are linked by hydrogen bonds involving both ligand and lattice water molecules to form a three-dimensional network.     

STRUCTURE OF CHLORO [2-2''''-PYRIDYL)-6-MSTHYLBEHZOTHIAZOLE] PYROCATECHOLATOANTIMONY(Ⅲ)

<正> C19H14N2O2ClSSb,Mr = 491.6, space group P1, a = 5.977(1), b= 8.708(1), c = 8.962(1) X, a=93.91(1),B= 103.25(1),r=94.80(1), V = 450.6 A3, Z = 1, Do = 1.79, DC = 1.812 g.cm-3,F(000) = 242,u(MoKa)= 18.1 cm-1,R=0.024 for 2903 reflections. The Sb atom is situated in a distorted square- pyramidal ( octahedral) environment, with Sb-Cl 2.546(2), Sb-0 2.004(2)/2.038(3), and Sb-N 2.442(3)/2.526(3)A.     

CRYSTAL STRUCTURE OF A SILVER COMPLEX Ag（PPh3）2（S2P—（OCH3）2）

<正> The crystal structure of the title silver complex has been determined by the single crystal X-ray diffraction method.The white plate crystal is tri-clinic.space group P1 with a=12.289(1),b=13.330(2),c=14.846(1)A.α=59.78(1),β=70.33(1),γ=64.01(1)°,V=1867.9A3,Z=2,Dc=1.404 g/ cm3,Mr=789.6,F(000)=808,MoKa radiation,μ(MoKa)=7.891 cm-1,final R=0.049 and Rw=0.051 for 5753 observed reflections.The silver(I)is surrounded by two P and two S atoms in a distorted tetrahedral coordination.     

Synthesis and Crystal Structure of Cluster 〔C_6H_4-1,2-(CO_2CH_2C_2H-μ)_2〕〔Co_2(CO)_6〕_2

１ＩＮＴＲＯＤＵＣＴＩＯＮＯｃｔａｃａｒｂｏｎｙｌｄｉｃｏｂａｌｔｉｓａｖｅｒｙｃｏｎｖｅｎｉｅｎｔｓｔａｒｔｉｎｇｍａｔｅｒｉａｌｆｏｒｔｈｅｐｒｅｐａｒａｔｉｏｎｏｆａｌｍｏｓｔａｎｙｃｏｂａｌｔｃｏｍｐｏｕｎｄ〔１〕．Ｔｈｅｒｅａｃｔｉｏｎｓｏ...     

STRUCTURE OF [Et4N]2[Mo2（CO）8（SCH2C6H4CH2SH）]

<正> Mr =1015.05, P21/c, a= 10.912(4), b= 12.088(3), c= 18.807(8) A.β=103.57(3)° ,V= 2411.4 A3, Z = 2, DC = 1.40 g/cm3.λ(MoKα)= 0.71073 A, μ=7.2 cm-1,F(000)=1048.Room temperature, final R=0.069, Rw=0.091. The geometry around the Mo atom is a distorted octahedron. The equatorial Mo-C distances are shorter than the axial ones. The Mo...Mo distance is 3.949A.     

Crystal and Molecular Structures of［Cu_2（OAc）_4（Ur）_2］．2H_2O and｛［Cu（H_2Y）］．Ur·H_2O｝_n（Ur＝urea； H_4Y＝EDTA）

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｓｏｆ［Ｃｕ_２（ＯＡｃ）_４（Ｕｒ）_２］．２Ｈ_２Ｏａｎｄ｛［Ｃｕ（Ｈ_２Ｙ）］．Ｕｒ·Ｈ_２Ｏ｝_ｎ（Ｕｒ＝ｕｒｅａ；Ｈ_４Ｙ＝ＥＤＴＡ）￥ＺｈａｎｇＨａｎ－Ｈｕｉ；ＹｅＺｈａｏ；ＹａｎｇＲｏｎｇ...     

CRYSTAL STRUCTURE OF TRIS(2-THENOYLTRIFLUOROACETONATO)BIS(TRIPHENYLPHOSPHINE OXIDE)EUROPIUM(Ⅲ), Eu(TTA)_3.(Ph_3PO)_2

<正> C60H42O8F9S3P2Eu,Mr=1372.07 triclinic, space group Pl,a = 11.191(1), b = 12.121(2), c = 23.529(3) A,α=80.08(1),β=76.51(1),γ=70.46(1)°,V=2909.3(6)A3, Dm(flotation in CCl4/BrCH2CH2Br) = 1.566, Dx(Z=2) = 1.562 g cm-3,λ(MoKα) =0.71073 A,μ=13.16 cm-1, F(OOO)=1376, T =295 °K, final RF=0.033 for 9104 observed reflections with |Fσ|>3σ(|Fσ|).The compound is isostructural with the known neodymium(Ⅲ) complex. The metal atom in the monomeric molecule is coordinated dodecahedrally by the eight 0 atoms of the surrounding ligands with Eu-0 bond distances in the range 2.361(2)-2.457(3) A.     

Crystal Structure of 3－hydroxyl－1，5－diazacycloheptane Dihydrobromide C_5H_（12）N_2O·2HBr

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ３－ｈｙｄｒｏｘｙｌ－１，５－ｄｉａｚａｃｙｃｌｏｈｅｐｔａｎｅＤｉｈｙｄｒｏｂｒｏｍｉｄｅＣ_５Ｈ_（１２）Ｎ_２Ｏ·２ＨＢｒＬＩＵＹｏｎｇ；ＸＵＥＧｕｏ－Ｐｉｎｇ；ＷＵＣｈｅｎｇ－Ｔａｉ（Ｄｅｐａｒｔｍｅｎｔｏｆ?..     

CRYSTAL STRUCTURE OF A NEW STEROIDAL ALKALOID FROM PEIMINE,C_(27)H_(43)NO_2·H_2O

<正> Mr = 431,.6 orthorhombic,P212121,a = 8.526(2), b = 9.970(2), c= 29.787(6)X,Z=4,V=2532.0A3,Dc=1.132g.cm-3,λ(MoKα)=0.71073A,μ=0.67cm-1, F(000) = 952, final R= 0.069 for 1733 observed reflections with I>1σ(I). All six-membered rings in this free base are in the chair form and the five-membered ring C takes the envelope conformation, with the ring fusions A/B traps, B/C trans, C/D cis, D/E trans and E/F trans. There is one crystal water whose oxygen atom joins the adjacent alkaloid molecules by the inter-molecular hydrogen bonds O(1)-H... 0(3)-H(31)...0(2)=C(6). Pertinent parameters for the hydrogen bonding system are: .0(1)...0(3) 2.878(6), 0(2)...O(3) 2.917(6)A,O(1)-H...O(3) 178.3(3)°,and 0(3)-H(31)...0(2) 165.6(3)°.     

Crystal Structure of trans－2－（1－Naphthyl）－1－（p－（4＇，4＇，5＇，5＇－tetramethyl－4＇，5＇－dihydro－1＇H－imidazolyl－1＇－oxy－3＇－oxide）－phenyl）－imine，C_（24）H_（24）N_3O_2

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆｔｒａｎｓ－２－（１－Ｎａｐｈｔｈｙｌ）－１－（ｐ－（４＇，４＇，５＇，５＇－ｔｅｔｒａｍｅｔｈｙｌ－４＇，５＇－ｄｉｈｙｄｒｏ－１＇Ｈ－ｉｍｉｄａｚｏｌｙｌ－１＇－ｏｘｙ－３＇－ｏｘｉｄｅ）－ｐｈｅｎｙｌ）－ｉｍ...     

Crystal and Molecular Structure of 5，6，7，8，9，10－Hexahydro－3－（4－methylphenylamino）－2－thioxoquinoxaline

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆ５，６，７，８，９，１０－Ｈｅｘａｈｙｄｒｏ－３－（４－ｍｅｔｈｙｌｐｈｅｎｙｌａｍｉｎｏ）－２－ｔｈｉｏｘｏｑｕｉｎｏｘａｌｉｎｅＳｕｎＤａ－Ｑｉｎｇ；ＬａｎｇＪｉａｎ－Ｐｉｎｇ；ＬｕＺｈ...     

Crystal Structure of Quaternary Mixed Anion Complex of Labthanide [Ce(CH_3COO)_2(NO)_3(phen)]_2

11NTRODUrmNSomequaternarymixedanioncomplesesoflanthanidesweresynthesized.karasavetalsynthesized">Eu(acac)(NO3)(bipy)2.3H2OandJin[2ietal.Synthe-sizedEu(m-MBA)(NO3)(phen)andEu(o-MBA)(NO,)(phen).Onlyacrystalstructureofceriumcontainingphenwasstudied,Ce(CH,COCHCOCH,)3(phen),fromCambridgeStructureDatabase.SowesynthesizedthecomplexoftCe(CH,Coo)z(Noa)(phen)J,andthecrystalstructure.2EXPERmENTAL2.1Cry8talpreparationThecrystalwasseparatedfromtheethanol/waterso-lutionofceriumnitrate…     

STUDY ON TETRANUCLEAR TRANSITION METAL CLUSTER WITH μ_3-O BRIDGES I . SYNTHESIS AND CRYSTAL STRUCTURE OF [Fe_4O_2(O_2CCH_3)_7(2,2''''-bipy)_2]Cl

INTRODUCTION.The first tetranuelear oxo一bridged manganese eomplex eon-taining〔Mn4OZ〕“+eore was reported on its synthesis,strueture and magnetie proper-ties in 1 987〔‘〕,representing the best available model for the photosynthetie water oxi-dation eentre.In order to find out the relationship of aetivity with eonfiguration ofthis kind of eomplexes,a series of dual oxo一bridged tetranuelear eomplexes have beensynthesized in our laboratory〔2〕.In this paper the aeetato一bridged tetran…     

Solid State Synthesis and Structural Characterization of Binuclear Cu(I)-SbPh3 Complex [Cu(SbPh3)2I]2

Dimeric complex [Cu(SbPh3)2I]2 has been synthesized by a solid state reaction at a low heating temperature and its crystal structure has been analyzed by X-ray crystallography. The crystal is monoclinic, space group P21/a (#14), a = 20.436(5), b=14.125(3), c=24.683(3)(A), β=110.67(1)°, Z=4, V=6666(2)(A)3; C72H60Sb4I2Cu2, Mr = 1792, Dc = 1.787 g.cm-3, μ(MoKα) = 31.88 cm-1, F(000)=3440, R=0.038 and Rw=0.043 for 5632 observed reflections (I≥3.0σ(I)) and 361 refined parameters. The result reveals the copper and the bridging iodide atoms form an approximately planar rhomboid array. Effects of the bulkiness of the ligands upon the structures of the analogous complexes are discussed.     

Crystal structure of di-(2,7-disubstituted-9 fluorenyl)glutamate

The title compound, di-(2,7-disubstituted-9 fluorenyl)glutamate, C82 H86 O12 has been characterized thus: triclinic, P 1, a=16.173(5)A, b=16.233(5)A, c=14.320(5)A, alpha=91.124(5), beta=105.098(5), gamma=92.270(5), V=3625(1)A3, Z=2 and F.W.=1248.54, Dm=1.125 gcm-3, Dc=1.169g cm-3. F000=1356.00, lambda(Mo- K)=0.71069 A, mu=0.77cm-1,final R1 and omegaR2 are 0.094 and 0.28 respectively.     

Synthesis and Crystal Structure of MnSm_4(SiO_4)_3O

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＭｎＳｍ_４（ＳｉＯ_４）_３Ｏ￥ＣｈｉＬｉ－Ｓｈｅｎｇ；ＤｅｎｇＳｈｕｉ－Ｑｕａｎ；ＺｈｕａｎｇＨｏｎｇ－Ｈｕｉ；ＨｕａｎｇＪｉｎ－Ｓｈｕｎ；（ＳｔａｔｅＨｅｙｌａｂｏｒａｔｏｒｙｏｆＳｔｒ?..     

STRUCTURE OF 1-PHENYL-3,4-BENZO-7,10-DIMETHYL-2,8,9-TRIOXA-5-A2A- SILATRICYCLO(3.3.3.0~(1,5))UNDECANE

<正> Mr=327.49, monoclinic,C2/c,a=17.211(11), b=12.300(7),c=17.079(10)A,β=99.41(5)°,V=3567(4)A3,Z=8,μ(MoKα)=1.5cm-1,F(000)=1392,Dx=1.22g/cm3, room temperature.The final R=0.085,Rw=0.077 and s=1.27 for 1471 independent reflections with |Fo|>2.5σ(|Fo|).The length of the dative bond N→Si is 2.193(5)A.The structure Is disordered at C(7),C(13),C(10), C(12)positions.     

CRYSTAL AND MOLECULAR STRUCTURE OF BIS(2-ME-THOXYETHYL-CYCLOPENTADIENYL) ERBIUM CHLORIDE

<正> Complex Cp'2 ErCl(Cp'=2-methoxyethylcyelopentadienyl)(I)has been synthesized by the reaction of Cp' Na and ErCl3 in THF It crystallizes in space group Pnma with a=12.269(0),b=11.742(6),c=11.197(2)A,V=1613.1A3,Dc=1.849 g/cm3,Z=4,A=0.71073 A,μ(MoKa)=54.38 cm-1,F(000)=876,R=0.043,Rw=0.046.The Er atom is formally nine-coordinated with a pseudo-trigonal bipyramidal geometry with the "equatorial" plane composed of the Er atom,the Cl atom and the centers(1)and(2)of the two Cp rings(Cp=cy-clopentadienyl).The molecule is located at the crystallographic mirror plane through the atom C(3),C(4),C(S),Er,O(1)and C(6).The atom Cl and the atoms of Cp'(2)(except C(16)and C(16'))are disordered with an occupancy of 0.5 each.     

Crystal Structure of[PrAl(CF3COO)2(CF3CHOO)(C2H5)2(C4H8O)2]2

[PrAl(CF3COO)2(CF3CHOO)(C2H5)2(C4H8O)2]2 Mr=1420.56, monoclinic, P21/n, a=10.651(6), b=24.276(9), c=11.110(5)(), β=107.650(4)°, V=2737.4(1)()3, Z=2, Dc=3.45 g/cm3, F(000)=2816, T=233K, MoKα radiation (λ=0.71069()), μ(MoKα)=38.017 cm-1, R=0.048 for 2847 observed reflections (I≥3σ(I)). It is isostructural with [LnAl(CF3COO)2(CF3CHOO)-R2(C4H8O)2]2 (Ln=Ho, R=Et; Ln=Nd, Y, R=iBu). Pr3+ is coordinated by eight oxygen atoms from five bridging ligands and two THF forming a distorted bicap-prism.