Synthesis and Structure of Mixed Distannoxane Dimers [ClR2SnOSnR2′Cl]2

Mixed distannoxane dimers [ClR2SnOSnR2′Cl]2 were synthesized by the reaction of R2SnO(R=Bu,Pr) and R2SnCl2(R=Me,Ph,Cy,Oct). The crystal structures of compound 1 and 5 show they are ladder-type dimers that contain a central planar Sn2O3 four-membered ring. Both endo-and exo-Sn atoms are five-coordinate.     

Diorgano, Dichloro－tin （IV） Complexes of 4－X－Benzohydroxamic Acid （X=CI, OCH3）： Synthesis, Characterization, Antitumor Activity in Vitro and the Crystal Structure of trans－ [Me2Sn（L2） 2]

A series of diorganotin (IV) derivatives of R2SRL2 (R = Me, Et, n-Bu, ph or CI; L = Ll or L2) and their corresponding mixed-ligand complexes RESn (L1)(L2) have been prepared and the structure of trans-MeESn (L2)2 was characterized by FT-IR, ^1H, ^13C and ^ll9Sn NMR spectroscopies,MS, elemental analysis, melting points and X-ray diffIaction. The structure-activity relationships were discussed.     

Synthesis, Crystal Structure, UV-vis and EPR Studies of（ NH3CH2CH2NH2 ） 2.5 [ Mo0.5^（V）W0.5^（VI）O2 （ OC6H4O ） 2]

Cis-dioxo-metal complex ( NH3CH2CH2NH2 ) 2.5 [ Mo0.5^(V)W0.5^(VI)O2 ( OC6H4O ) 2] 1 was obtained by the reaction of tetra-butyl ammonium hexamolybdotungstate with 1, 2-dihydroxybenzene in the mixed solvent of CH3OH, CH3CN and ethylenediamine,and characterized by X-ray diffraction, UV-vis and EPR analysis. Compared with its analogous complexes (NH3CH2CH2NH2)3[Mo^(V)O2(OC6H40)2] 2 and (NH3CH2CH2NH2)2[W^(VI)O2(OC6H4O)2] 3, the results show that tungsten(VI) is less active in redox than molybdenum (VI) and that the change of the valence induced by substitution of W(VI) for Mo(V) in EMO2(OC6H40)2]n- does not influence the coordination geometry of the complex anion in which the metal center exhibits distorted octahedral coordination with cis-dioxo catechol. The responses to EPR of complexes 1 and 2 are active but complex 3 is silent,and the UV-vis spectra exhibited by the three complexes are obvious different because of the different electronic configuration between the central Mo(V) and W(VI) ions in the complexes.It is noteworthy that complexes 1 and 2 have the similar EPR signal to flavoenzyme, suggesting that the three complexes have the same coordination geometry feature with the co-factor of flavoenzyme.     

Hydrothermal Synthesis and Crystal Structure of [（CH3CH2）4N]4[（La12（OH）12MoO29）],A Novel Cluster Compound with a MoO5 Hexahedron Center surrounded by La—O Octahedron

IntroductionRecently,the molecular designs of polyox-ometalates( POM) with basic oxometal clusterbuilding blocks are of great interest[1,2 ] . Hy-drothermal synthesis,with the characteristic ofone- pot reaction,provides a convenient method toobtain novel structures of POM compounds[3— 6] . Inthe Ln/Mo/O system ( Ln=rare earth) ,somecompounds containing La and Mo elements havebeen reported[7— 17] . However,these compoundshave all been synthesized under the highly restrict-ed synthetic co…     

Synthesis and Crystal Structure of Drum Organooxotin Clusters from Heteroaromatic Carboxylic Acid [PhCH2Sn（O）（O2CC5H4N）]6 and[PhCh2Sn）（O）（O2CC4H3O）]6

IntroductionRecentlywehaveinvestigatedthestructuralchemistryofanumberofdi ortri organotinheteroaromaticcarboxyl ates.1 5Thesestudieshaveshownthatthestructureoforgan otinheteroaromaticcarboxylatesisdependentonboththena tureofthealkylorarylsubstituentboundtothetinatomandthetypeofcarboxylateligand .Inparticular,majorstructuralvariationsareobservedwhencarboxylateligandcontainsanadditionaldonoratom ,suchasapyridineNatom ,availableforcoordinationtotheSnatom .1 3,5 8Wehavenowturnedtothemonoorganotin…     

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 aNovelPolythiotungstate Compound[PPh4]2[（S）2W（μ—S）2（O）W（THF）（μ—S）2W（S）2]

1 INTRODUCTION Polythiotungstate complexes can be prepared from the protonation of one sulfur atom of [WS4]2－ and subsequent intramolecular redox reactions[1,2]. For example, [(S)2W(m-S)2W(m-S)2W(S)2]2 was formed by the acidification of a diluted aqueous solution of (NH4)2[WS4] with dilute H2SO4[3]. When a diluted aqueous solution containing [WS4]2 was acidified with 0.1mol/L HCl, [(S)2W(m-S)2(O)- W(H2O)(m-S)2W(S)2]2 was formed[4]. [(S)2W- (m-S)2(S)W(m-S)2W(S)2]2 was form…     

Synthesis and Structure of [Cu2（μ—NO2）（aepy）4]（ClO4）3 （aepy=2—（2—Aminoethyl）pyridine）

1 INTRODUCTION There has been great and considerable interest in the study of copper nitrite complexes because they are relevant to the study of copper-containing enzymes involved in the denitrification process[1]; in particular, copper-nitrite complexes are potentially relevant to the nitrite reductases[2] (the enzyme from Achromobacter Cycloclastes) which convert NO2－ to NO and/or N2O. Many attempts have been made to synthesize a variety of copper-nitrite complexes, in which the n…     

Synthesis, Structure and Conductivity of （PyH）[Ni（dmit）2]2

A new molecular conductor (PyH)[Ni(dmit)2]2 (dmit = 4, 5-dimercapto-1, 3-dithiole-2-thione) has been prepared and its crystal structure has been determined. Crystallographic parameters for (PyH)[Ni(dmit)2]2: C17H6NNi2S20; triclinic system; P-1 space group; a = 5.9227 (4) , b =8.2279 (6), c = 16.7535 (9) A, a = 90.233 (5) , 0 = 92.107 (6) , y= 104.654 (6) ; V= 789.25 (9) A3; Z = 1; Dc = 2.068 g/cm3; F (000) = 491. The conductivity at one direction on (001) plane at room temperature was measured to be 0.13 ii^-cmf1. The resistivity-temperature curve in the temperature range of 90-290 K shows that this compound behaves as a semiconductor.     

Synthesis and Structure of Mixed Distannoxane Dimers [ClR_2SnOSnR''''_2Cl]_2

1,1,3,3-Tetraorganodistannoxanes [XR2SnOSnR2X]2 (R = alkyl, Ph; X = halogen, NCS, OAc, OR) are a kind of organotin oxo clusters. They have received considerable attention because they are useful catalysts for many reactions1-5. And recently S. W. Ng reported that [XR2SnOSnR2X]2 (R = Bu, X = OOCCH2SC(O)N(CH2CH2)2O) had more active antitumor activity than cis-platin in vitro6. A characteristic feature of symmetric tetraorganodistannoxanes in the solid state is their dimeriz…     

1,3-二氯-1,1,3,3-不对称四烃基二锡氧烷的合成及结构表征

通过氧化二烃基锡与二氯二烃基锡的反应,合成了不对称四烃基二锡氧烷[ClR₂SnOSnR'₂Cl]₂ (R=Bu,Pr; R'=Me,Ph,Cy,Oct).通过对化合物1和5的X-衍射晶体结构分折,表明该类化合物在晶体状态 时是含有中心对称Sn₂O₂四元环的梯状二聚体,内环锡与外环锡均为五配位的畸变三角双锥构型.     

Synthesis,Crystal Structure and Quantum Chemical Study of the Ladder Organotin Compound {[（C6H5CH2）2Sn]2（O）（Cl2）}2

The title compound {[（C6H5CH2）2Sn]2（O）（Cl2）}2 has been synthesized by the reaction of bisbenzyltin dichloride with NaOH dilute solution, and its structure was determined by X-ray diffraction. The crystal belongs to monoclinic, space group C2/c, with a = 2.5081（17）, b = 1.0089（7）, c = 2.0909（14） nm, β = 94.267（8）°, V= 5.276（6） nm^3, Z = 4, De= 1.734 g/cm^3,μ（MoKa） = 21.55 cm^-1, F（000） = 2704, R = 0.0398 and Rw = 0.1024. According to structural analysis, the tin atom adopts a distorted five-coordinate trigonal bipyramidal geometry, and the ladder-like structure is shaped by one planar four-membered Sn2O2 ring together with two planar four-membered Sn2OCl rings.     

有机锡氧羧酸簇合物[PhCH_2Sn(O)(O_2CCH=CHAr)]_6的合成、表征和[PhCH_2Sn(O)(O_2CCH=CHPh)]_6的晶体结构

利用(PhCH_2)_3Sn]_2O与ArCH=CHCO_2H反应，合成6个新的[PhCH_2Sn(O) (O_2CCH=CHAr)]_6簇合物。通过元素分析、红外光谱和X射线单晶衍射对其结构进 行了表征。用X射线单晶衍射测定了[PhCH_2Sn(O)(O_2CCH=CHPh)]_6的晶体结构， 结果表明，该簇合物为三斜晶系，空间群P1, a = 1.6771(3) nm, b = 1.8020(4) nm, c = 2.1073(4) nm, α = 108.111(3)°β = 103.614(3)°,γ = 104.679 (3)°,Z = 2, V = 5.5033(18) nm~3, D_c = 1.350 g/cm~3, μ = 1.396 mm~(-1) , F(000) = 2208, R = 0.0606, wR = 0.698。该化合物为鼓型簇状结构，锡原子 呈畸变的八面体构型。     

Crystallographic report: Dimeric tetraphenyl‐1‐hydroxo‐3‐trifluoromethanesulfonatodistannoxane, [Ph2(HO)SnOSn(O3SCF3)Ph2]2

The molecular structure of the title compound, obtained by an adventitious phenyl group cleavage of Ph₃SnOSnPh₃ with triflic acid, reveals discrete centrosymmetric units of [Ph₂(HO)SnOSn(O₃SCF₃)Ph₂]₂ that are loosely associated via hydrogen bonding. Copyright © 2004 John Wiley & Sons, Ltd.     

固相配位化学反应研究(LXI)——[Cu(SC(Ph)NHPh)(PPh_3)_2X](X+Cl,Br,I)的固相合成和晶体结构(X=Cl)

SC(Ph)NHPh,CuX(X=Cl,Br,I)和PPh_3的固相反应产物经CS_2处理得红黄色立方晶体[Cu(SC(Ph)NHPh)(PPh_3)_2X],其中X=Cl的单晶用X射线衍射法收集晶胞参数,此晶体属单斜晶系,空间群P2_1/c,α=1.8013(5)nm,b=1.4588(5)nm,c=1.7222(4)nm,β=105.54(3)°,F=4.3601nm~3,Z=4。中心铜离子以扭曲四面体配位,Cu原子周围的平均键角为109.4°,其中Cu—S键、Cu—Cl键、Cu—P(1)键和Cu—P(2)键的键长分别为0.2352(3)nm、0.2375(4)nm、0.2297(4)nm和0.2282(3)nm.     

Crystal Structure of {(PPh_3)_2RuB_(10)H_8[(CH_3)_2CHO]_2}

1INTRODUCTIONFromreactionsof[RuCl,(PPh,),jwithcloso-[B,,H,,j'-respectivelyinEtOH/CH,Cl,t'i,CH,COOH/THF"'andC,H,COOH/CH,Cl,">solution,itcanbefoundthatbothalcoholandorganicacidcanreplacehydrogenatomsinborane.Further-more,accordingtotheirdifferentreactiontime(3h,1OOhand113hrespectively),wecanknowthatalcoholismoreactivetoreplacehydrogenatomsinborane.NowinordertoconfirmthisrulefurtherweusePhCH(OH)COOH/(CH3)2CHOHsolutioninsteadofabove-mentionedsolutions.Newcompounds(I)and(II…     

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 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...     

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?..