CRYSTAL STRUCTURE OF [Et_4N]_2[Mo_2O_2(μ-S)_2(S_2)_2]

<正> [(C2H5)4N]2[Mo2o2S2(S2)2], Mr = 676. 74, monoclinic, P21/c, a = 13.510(2), b = 14.373(2), c=14. 777(3)(?), β = 97.53(2)°, V = 2844.7(9) (?)3, Z = 4, Dc= 1. 58g/cm3, μ(MoKα) = 13.0cm-1, F(000) = 1384, R =0. 033 for 1803 observed reflections. The structure contains discrete [Mo2O2S2(S2)2]2- anions and Et4N+ cations. The two oxygen atoms bonded to the Mo atoms are in cis-form with respect to the Mo2S2 bridging unit, with an average Mo- O distance of 1. 678 (?), The Mo…Mo distance is 2. 832(1)(?).     

Synthesis and Structure of [Cu（OH）2（H2O）2（4—C5H4N—COOH）2]

1 INTRODUCTION Supramolecular chemistry and crystal engineering of coordination compounds have attracted considerable interests nowadays owing to the fascinating structural diversity and potential applications as functional materials[1,2]. Generally, architectures of supramolecules are formed through hydrogen bonds, ?- ?stacking interaction or other weak interactions between the molecules. Recently, many supramolecular compounds containing silver(I) and copper(II) species have been re-…     

Crystal Structure of [Cd（pom）2Cl2]

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｃｄ（ｐｏｍ）_２Ｃｌ_２］ＷｕＷｅｎ－Ｓｈｉ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ，Ｈｕａ－ｑｉａｏＵｎｉｖｅｒｓｉｔｙ，Ｆｕｊｉａｎ，Ｃｈｉｎａ，３６２０１１）ＤｏｎｇＭｅｉ－Ｂｉｎ；ＬｉＳｏｎｇ－Ｘｉａ...     

[Et_4N]_2[Zn_2(OPh)_2Cl_4]的合成和晶体结构

ZnCl2, PhONa和Et4NCl稨2O在乙腈溶剂中反应合成了一种二核锌配合物[Et4N]2[Zn2(OPh)2Cl4]。X射线衍射结果表明,晶体属单斜晶系,C2/m空间群,晶胞参数 a = 14.1366(2), b=13.6985(5), c=9.3308(3)牛?107.851(2)o, V=1719.92(9)?,C28H50O2N2Zn2Cl4,Mr=721.24,Z=2,Dx=1.393g/cm3,μ(MoKα)=1.732mm—1,F(000)=756, R=0.0552, wR=0.1534, S=1.027。 配合物是由2个阳离子Et4N+和1个阴离子[Zn2(OPh)2Cl4]2—组成。阴离子[Zn2(OPh)2Cl4]2—包含着1个中心Zn2O2菱形平面。配合物中的2个锌原子通过2个苯酚中的氧原子桥连,每个锌原子还与2个氯原子配位形成变形四面体结构。     

Synthesis and Crystal Structure of [Mn（DPMT）2Cl2（H2O）2]

The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1-[[2-(2,4-dichlorophenyl)- 1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2·4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 23.913(4), b = 7.8883(13), c = 8.6291(14) , β = 95.816(3)o, V = 1619.4(5) 3, Z = 2, C24H26Cl6MnN6O6, Mr = 762.15, Dc = 1.563 g/cm3, μ = 0.950 mm-1, S = 1.045, F(000) = 774, R = 0.0462 and wR = 0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.     

Synthesis and Crystal Structure of[Li(dme)3][(t-BuC_5H_4)_2Gd(NPh_2)_2]·1/2dme

1INTRODUCTIONIntherecentyears,organolanthanideamideshaveattractedagreatdealofat-tention.Forexample,theyareabletoreactwithCOtogiveinsertionproduct[(C,Me,)2SinjZt(PhN)OCCO(NPh)jti},withaminoolefinstoyieldcorrespondingheterocyclestZ),withmethylmethacrylate(MMA)toleadtoMMApolymeriza-tiont3'43.Inordertoexplorefurthertheirchemistry,wesynthesizedsomeanionicandneutrallanthanoceneamidestoinvestigatetheirchemicalreactivities(5--7).Inthispaper,wewouldliketodescribethepreparationofanotheranio…     

Synthesis and Structural Characterization of Manganese Carbonyl Incorporated Polyoxomolybdate (n-Bu_4N)_2[Mo_6O_(16)(OCH_3)_2{HOCH_2C(CH_2O)_3}_2{Mn(CO)_3}_2]

The polyoxoanion incorporated {Mn(CO)3+} complex, (n-Bu4N)2[Mo6O16(OCH3)2{HOCH2C(CH2O)3}2· {Mn(CO)3}2](1), has been synthesized by the reaction of (n-Bu4N)4[Mo8O26] with Mn(CO)5Br in methanol, in the presence of C(CH2OH)4. The complex 1 has been characterized by IR, UV-Vis, X-ray single crystal diffraction, and TG. Crystal data for the complex 1: C25H48MnMo3NO16 (1), Triclinic P1, a=0.9405(3) nm, b=1.3351(4) nm, c=1.5455(4) nm, α=103.206(5)o, β=102.165(5)o, γ=100.784(5)o, V=1.7896(9) nm3, Z=2, R1=0.0703, wR...     

Crystal Structure of Binuclear Bridging Complex[(dppf)_2Pd_2 (Ⅱ) (μ-Cl)_2] [PF_6]_2

1INTRODUCTIoNFerrocenecontainingtransitionmeta1complexeshasarousedtheinterestofchemistsbecauseofitsnovelstructureandproperties"',Huangetal[2'3isynthesizedsomechainandbridgeformcomplexesandstudiedtheirIRandCV.Linetal[4isyn-thesizedthecrystalof[(dppf)PdCl,jO.5[(CH3),COj(dppf=1,11-(diphenylphosphine)-ferrocene)anddeterminedthestructurebyX-raydiffraction.Inthisarticlewereportthesynthesisandcrystalstructureof[(dppf),Pd,(ll)(p-Cl),j[PF,j2.2EXPERIMENTAL2.1PreparationAsolutionofO.86mm…     

〔NH_4（15－C－5）_2〕〔Cd_2（SCN）_5〕配合物的晶体和分子结构

用凝胶法合成了标题化合物［ＮＨ４（１５－Ｃ－５）２］［Ｃｄ２（ＳＣＮ）５］（１５－Ｃ－５＝Ｃ１０Ｈ２０Ｏ５）的晶体，并对其进行了红外光谱、元素分析等各项物理性质的测试，并经Ｘ射线单晶结构分析得到了配合物的全部晶体学数据：Ｍｒ＝９７３．７８，正交晶系，空间群Ｐｎｍａ，晶胞参数ａ＝１０．５０７（１）Ａ，ｂ＝１６．５８４（２）Ａ，ｃ＝２３．４９４（２）Ａ，Ｖ＝４０９３．８（３）Ａ３，Ｚ＝４，Ｄｃ＝２．５８０ｇ／ｃｍ３，μ＝１３．３１ｃｍ（－１），Ｆ（０００）＝１９６８，Ｒ＝０．０７０，Ｒω＝０．０８５。结构分析结果表明，配阳离子是由一个ＮＨ４＋和两个１５－Ｃ－５组成的，ＮＨ４＋没有进入１５－Ｃ－５空腔内，而是位于两个１５－Ｃ－５之间，呈夹心结构；配阴离子是以［Ｃｄ２（ＳＣＮ）５］为单元的阴离子长键，其中一组ＳＣＮ－被四个Ｃｄ离子共享，其余两组ＳＣＮ－被两个Ｃｄ离子共享，呈变形八面体构型。配阳离子［ＮＨ４（１５－Ｃ５）２］＋和配阴离子［Ｃｄ２（ＳＣＮ）５］－间靠静电力结合成配合物晶体。     

STRUCTURE STUDIES OF [Et_4N]_4[Cu_8(i-mnt)_6] (i-mnt=S_2C=C(CN)_2) AND [Me_4N]_4[Cu_5Ag_3(i-mnt)_6]·H_2O

<正> [Me4N]6[Ag6(i-mnt)6].H2O(1),[Et4N]4[Cu8(i-mnt)6](2) and [Me4N]4-[Cu5Ag3(i-mnt)6].H2O(3)(i-mnt=S2C=C(CN)2) were synthesized. The crystal and molecular structure of the complex 1 was reported by us.The structure of the complex 2 was determined from single crystal X-ray diffraction data. [Et4N]4[Cu8(i-mnt)s] 2, Mr=1870.46, monoclinic, P21/n, a=14.724(6), b = 17.228(3), c=15.59(1)A,β= 100.75(7)°,V=3886.3A3;Z = 2,Dc= 1.598 g/cm3. Complex 3 has been characterized by ICP elemental analyses and IR spectrum.     

CRYSTAL STRUCTURE OF [Sm(CCl_3COO)_3(H_2O)_2]·2H_2O

<正> Biaqua-trichloroacetate-samarium dihydrate, [Sm(CCl3COO)3(H2O)2]-2H2O, Mr=707.54, orthorhombic, space group Pnne, with a = 19.158(5), b = 22.176(4), c= 9.798(4)A, Z= 8, V= 4162.7A3.F{000)= 2696,λ(MoKα)=0.71069A, Dx = 2.258 g/cm3, final R=0.061. The title compound has non-molecular structural character, and its structural units Sm(μ-CCl3COO)s/2-(H2O>2 constitute 2-dinensional infinite chains of Sm(μ-CCl3COO)4Sm(μ-CCl3-COO)2Sm.The Sa(Ⅲ) atom in each unit is bound to two O atoms from aqua-molecules and six 0 atoms from six bridging CCl3COO groups (four of which are shared with the SB atom of another unit, two shared with the Sm atom of a third unit) forming a square antiprism.     

CRYSTAL STRUCTURE OF W_4(μ_(3-)S)_4[S_2P(OEt)_2]_6

<正> W4S4 [S2P (OEt)2]6, Mr= 1974. 94, triclinic, P1, a = 14. 063 (5) , b = 16. 289(4), c= 13. 377(3) A ,α=92. 06 (2), β=95. 24(3), γ= 73. 06(2)°, V= 2919(3)A3,Z=2,DC=2. 18g/cm3, Moka radiation,λ =0. 71069A ,μ = 90. 64cm-1, F(000) = 1764,R=0. 053 and Rw = 0. 069 for 5422 reflections with I≥3σ(I).The title compound is comprised of a cubane-like cluster core [W4S4] in which every W atom is coordinated by six S atoms to form a distorted octahedron.     

CRYSTAL STEOCTURE OF [Cu(HCOO)_2(HCOOH)_2]n

<正> Mr=245.6, monoclinic, V2l/c, a=7.778(4), b=7.946(4), c=8.008(4) X, B=115.31(4)? V=447.483, Z=2, Dx=1.82 g/cm3, X(Mokct)=0.710698, y=25.5cm~1 F(000)=245.96, T=293 K. The final R=0.059 for 423 unique observed reflections. Cu2-' is coordinated by six oxygen atoms to form a distorted octahedron. Cu2^ ions are linked together by formate groups in an anti-anti bridging arrangement to form a two dimensional polymer. Two oxygen atoms in a formate group are equivalent with C(l)-0(l)=l.25(1) and C(l)-0(2) = l. 2.5(1)8.     

CRYSTAL STRUCTURE OF（Bu4N）2[Pt（C3S5）2]

<正> The title compound C38H72N2PtS10(Mr=1072.74)crystallizes in triclinic system,space group P1 with cell constants a=11.994(4),b=18.117(7),c=11.855(6)A,α=95.55(4),β=99.14(3),γ=75.71(3)°,V=2460.0A3,Z=2 and Dc=1.45 gcm-3.The structure is solved by direct methods and refined by full-matrix least-squares technique to final R=0.046 and Rw=0.045 based on 5919 independent reflections with I≥3.0(I).The anion [Pt(C3S5)2]2-is approximately planar,of which the platinum-sulfur coordination polyhedron takes a square form with mean Pt-S bond length of 2.310(4)A.     

Crystal Structure of[Ru(taab)(DMF)_2]·[(CIO_4)_2]

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｒｕ（ｔａａｂ）（ＤＭＦ）_２］·［（ＣＩＯ_４）_２］￥ＤｕａｎＣｈｕｎ－Ｙｉｎｇ；ＬｕＺｈｏｎｇ－Ｌｉｎ；ＴｉａｎＹｕ－Ｐｅｎｇ；ＹｏｕＸｉａｏ－Ｚｅｎｇ；ＣｈｅｎＹａｏ（ＣｏｏｒｄｉｎａｔｉｏｎＣｈｅｍｉｓｔ?..     

镉－硫氰酸根与铵－苯并15－冠－5配合物的合成与结构研究

用凝胶法生长了标题配合物［ＮＨ_４（Ｂ１５Ｃ５）_２］［Ｃｄ（ＳＣＮ）_３］的晶体，并对其进行了红外光谱，元素分析等各项物理性质的测试。经Ｘ射线单晶结构分析得到了配合物的全部晶体学数据：Ｍ_ｒ＝８４１．３１，正交晶系，空间群Ｐ２_１２_１２_１，晶胞常数ａ＝１０．９７０（３），ｂ＝２１．８３４（３），ｃ＝１５．５６３（４），Ｖ＝３７２７（３），Ｚ＝４，Ｄ_ｘ＝１．５０ｇ／ｃｍ￣３，Ｆ（０００）＝１７３６，μ＝７．０９ｃｍ￣（－１），Ｒ＝０．０７０，Ｒ_ｗ＝０．０６３。结构分析结果表明，配阳离子［ＮＨ_４（Ｂ１５Ｃ５）_２］￣＋和配阴离子［Ｃｄ（ＳＣＮ）_３］￣－间靠静电力结合成配合物。     

CRYSTAL STRUCTURE OF Mo_3(μ3-S)(μ-S)_2[S_2P(OEt)_2]_3][SOP(OEt)_2](0)_2

<正> M=1140.85, monoclinic, P21/c. a=12.748(2), b=14.320(2), c=23.118 (3)A,β=101.07(1)°, V=4141(2)A3, Z=4, Dc=1.830 g.cm-3. Final R=0.039 for 4160 reflections.The title compound is a rather irregular trinuclear molybdenum cluster having only two M-M bonds with two shorter Mo-Mo distances of 2.808(1), 2.839(1), and one longer Mo-Mo distance of 3.337(1)8. The existence of two Mo-Mo bonds is coincident with the electron counting for {Mo3} cluster core, and may be regarded as a result of the oxidation of a compound Mo3(μ3-S)(μ-S)2 (μ-L)[S2P(OEt)2]4(L') (L'=neutral ligands)1 characterized by us previously.     

CRYSTAL STRUCTURES OF [Bu4N]2[M2Ag3（ μ3—S）2（μ—S）4S2Et2dtc]（M=W,Mo）

<正> The title compounds were prepared from the reation of (NH4)2MS4 (M=W,Mo),AgNO3,NadtcEt2 and Et4NBr in CH3CN-H2O solution. The isomorphous compounds [Bu4N]2[W2Ag3S8Et2du] ( I ) and [Bu4N]2[Mo2Ag3S8Et2dtc] (Ⅱ) crystallize in triclinic space qroup Pi with the following crystal parameters:α=13. 043(4),b = 21. 640(6),c=10. 757(6)A ,α=95. 09(5),β = 91. 90(4),γ = 98. 57(3)°,Z = 2,V = 2987A3,Dc=1. 76g/cm3 for I 5;a= 12. 989(2) ,b=21. 574 (9) ,c= 10. 7/1(1) A .α= 95. 06(7), β=91. 61(4), γ=98. 52(2)°, Z = 2,V = 2961 A3.Dc= 1. 58g/cm3 for Ⅱ . The final R and Rw values are 0. 061 and 0. 072 for Ⅰ ,and 0. 062 and 0. 076 for Ⅱ The M2Ag3 (M = W, Mo) unit in anion M2Ag3S8Et2dtc forms a five-membered ring.     

［Vmo_3O_4（O_2CEt）_8］_2Na_2的合成与结构

［ＶＭｏ３Ｏ４（Ｏ２ＣＥｔ）８］２Ｎａ２（１），三斜晶系，Ｐ１空间群，ａ＝１２．９７７（７），ｂ＝１４．０７０（６），ｃ＝１２．３３８（８），α＝１０９．８１（４），β＝１１７．２０（４），γ＝９０．５１（５）°，Ｖ＝１８４８．８３，Ｍｒ＝２０２０．６，Ｄｃ＝１．８１ｇ／ｃｍ３，Ｚ＝１，Ｆ（０００），μ＝１２．９ｃｍ１（ＭｏＫα）对３７４２个可观测反射点（Ｉ＞３σ（Ｉ））最终一致性因子为Ｒ＝０．０１８，Ｒω＝０．０５４。单晶结构分析表明，簇阴离子中两个［Ｍｏ３Ｏ４］４＋单元通过两个＂桥＂金属Ｖ原子连接成一个奇特的环状结构，Ｍｏ－Ｍｏ平均键长为２．５１９（１），Ｍｏ…Ｖ间平均距离为３．６５４。簇阴离子通过Ｎａ＋连成一个一维长链，Ｎａ原子与氧原子形成一个少见的五配位三角双锥结构，Ｎａ－Ｏ距离仅为２．３１２，Ｎａ－Ｏ间较强的相互作用以及无限长链的晶体结构很好地解释了簇合物（１）的稳定性和不溶性。     

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex[La(betaine)_2(H_2O)_6Fe(CN)_6]·2H_2O

1 INTRODUCTION In the last decade, cyano-bridged Prussian Blueanalogues[1] have been intensively studied from theviewpoint of application as functionalized molecule-based magnets[2], chemical sensor materials[3], fluo-rescent materials[4] and zeolitic-type materials[5, , 6]etc. In 1976, a series of cyano-bridged three-dimen-sional rare earth hexacyanometalates(IIILnM(CN)6?nH2O (M = Fe or Cr, n = 4 or 5) were crystallized andsubjected to single-crystal X-ray analysis[7]. …