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1.
nBu2Sn[O2CCH2CH(4-ClC6H4)Ge(OCH2CH2)3N]2.H2O(Mr=1053.66) is an air-stable compound which crystallizes in the monoclinic space group C2/c with a=21.182(5), b=12.174(3), c=17.108(4) , β=99.59(2)°, V=4350(3) 3, Z=4, F(000)=2104, μ=2.104 mm-1. The refinement of structure with I≥3σ(I) for 1819 reflections converged at R=0.045. The coordination geometry around the Sn atom is best described as an askew-pentagonal bipyramid, in which four carboxylate oxygen atoms( Sn(1)-O(5), Sn(1)-O(5a)=2.099 and Sn(1)-O(4), Sn(1)-O(4a)=2.158 ) and an oxygen atom from an aqua ligand comprise the pentagonal plane, with two butyl groups occupying axial positions.  相似文献   

2.
Relative rate techniques were used to study the kinetics of the reactions of Cl atoms and OH radicals with ethylene glycol diacetate, CH3C(O)O(CH2)2OC(O)CH3, in 700 Torr of N2/O2 diluent at 296 K. The rate constants measured were k(Cl + CH3C(O)O(CH2)2OC(O)CH3) = (5.7 +/- 1.1) x 10(-12) and k(OH + CH3C(O)O(CH2)2OC(O)CH3) = (2.36 +/- 0.34) x 10(-12) cm3 molecule-1 s-1. Product studies of the Cl atom initiated oxidation of ethylene glycol diacetate in the absence of NO in 700 Torr of O2/N2 diluent at 296 K show the primary products to be CH3C(O)OC(O)CH2OC(O)CH3, CH3C(O)OC(O)H, and CH3C(O)OH. Product studies of the Cl atom initiated oxidation of ethylene glycol diacetate in the presence of NO in 700 Torr of O2/N2 diluent at 296 K show the primary products to be CH3C(O)OC(O)H and CH3C(O)OH. The CH3C(O)OCH2O* radical is formed during the Cl atom initiated oxidation of ethylene glycol diacetate, and two loss mechanisms were identified: reaction with O2 to give CH3C(O)OC(O)H and alpha-ester rearrangement to give CH3C(O)OH and HC(O) radicals. The reaction of CH3C(O)OCH2O2* with NO gives chemically activated CH3C(O)OCH2O* radicals which are more likely to undergo decomposition via the alpha-ester rearrangement than CH3C(O)OCH2O* radicals produced in the peroxy radical self-reaction.  相似文献   

3.
1INTRODUCTIONThestudiesoforganotincompoundsareofcurentinterestowingtotheirwiderangeofapplications〔14〕suchasbiocidesandhomogen...  相似文献   

4.
The new tin(IV) species (CH(3))(2)SnCl(OTeF(5)) was prepared via either the solvolysis of (CH(3))(3)SnCl in HOTeF(5) or the reaction of (CH(3))(3)SnCl with ClOTeF(5). It was characterized by NMR and vibrational spectroscopy, mass spectrometry, and single crystal X-ray diffraction. (CH(3))(2)SnCl(OTeF(5)) crystallizes in the monoclinic space group P2(1)/n (a = 5.8204(8) A, b =10.782(1) A, c =15.493(2) A, beta = 91.958(2) degrees, V = 971.7(2) A(3), Z = 4). NMR spectroscopy of (CH(3))(3)SnX, prepared from excess Sn(CH(3))(4) and HX (X = OTeF(5) or N(SO(2)CF(3))(2)), revealed a tetracoordinate tin environment using (CH(3))(3)SnX as a neat liquid or in dichloromethane-d(2) (CD(2)Cl(2)) solutions. In acetone-d(6) and acetonitrile-d(3) (CD(3)CN) solutions, the tin atom in (CH(3))(3)SnOTeF(5) was found to extend its coordination number to five by adding one solvent molecule. In the strong donor solvent DMSO, the Sn-OTeF(5) bond is broken and the (CH(3))(3)Sn(O=S(CH(3))(2))(2)(+) cation and the OTeF(5)(-) anion are formed. (CH(3))(3)SnOTeF(5) and (CH(3))(3)SnN(SO(2)CF(3))(2) react differently with water. While the Te-F bonds in the OTeF(5) group of (CH(3))(3)SnOTeF(5) undergo complete hydrolysis that results in the formation of [(CH(3))(3)Sn(H(2)O)(2)](2)SiF(6), (CH(3))(3)SnN(SO(2)CF(3))(2) forms the stable hydrate salt [(CH(3))(3)Sn(H(2)O)(2)][N(SO(2)CF(3))(2)]. This salt crystallizes in the monoclinic space group P2(1)/c (a = 7.3072(1) A, b =13.4649(2) A, c =16.821(2) A, beta = 98.705(1) degrees, V = 1636.00(3) A(3), Z = 4) and was also characterized by NMR and vibrational spectroscopy.  相似文献   

5.
Seven novel R2Sn(IV)-oxydiacetate (oda) and -iminodiacetate (ida) compounds of the form [R2Sn(oda)(H2O)]2 (R = Me, nBu, and Ph) (1-3), [(R2SnCl)2(oda)(H2O)2]n (R = Et, iBu, and tBu) (4-6), and [Me2Sn(ida)(MeOH)]2 (7) have been synthesized and characterized by IR, 1H, 13C, and 119Sn NMR (solution), solid-state 119Sn CPMAS NMR, and (119m)Sn M?ssbauer spectroscopy. The crystal structure of [Me2Sn(oda)(H2O)]2, 1, shows it to be dinuclear (centrosymmetric), with two seven-coordinated tin atoms, bridged by one arm of the carboxylate group from each oda. By contrast, the crystal structure of [(Et2SnCl)2(oda)(H2O)2]n, 4, comprises a zigzag polymeric assembly containing a pair of different alternating subunits, {Et2SnCl(H2O)} and {Et2SnCl(H2O)(oda)}, which are connected by way of bridging oda carboxylates, thus giving seven-coordinate tin centers in both components. Finally, the structure of [Me2Sn(ida)(MeOH)]2, 7, also centrosymmetric dinuclear, is comprised of a pair of mononuclear units with seven-coordinate tin. The 119Sn solid-state CPMAS NMR and (119m)Sn Mossbauer suggest the presence of seven-coordinate Sn metal atoms in some derivatives and the existence of two different tin sites in the [(R2SnCl)2(oda)(H2O)2]n compounds.  相似文献   

6.
报道2,4-Br2C6H3OCH(CN3)CO2Sn(C6H11)2CU3(1)和2-OCH3-4-CH3CH=CHC6H3OCH2CO2Sn(C6H11)2CH3(H2O)(Ⅱ)的晶体结构和分子结构。(Ⅰ)单斜晶系,空间群P21/c,a=13.067(3),b=10.594(3),c=18.157(4),β=106.99(2)°,Z=4,Dc=1.672g/cm3,V=2403.73,μ=43.731cm-1,Mr=622.99,F(000)=1232;(Ⅱ)单斜晶系,空间群P21/n,a=10.409(1),b= 12.570(2),c=20.664(2),β=83.51(1)°,Z=4,Dc=1.281g/cm3,V=2686.4A3,μ=9.761cm-1,Mr=539.28,F(000)=1120.最后的偏离因子,化合物(Ⅰ)R=0.046,Rω=0.046;化合物(Ⅱ)R=0.049,Rω=0.047。晶体结构解析表明,化合物(Ⅰ)和(Ⅱ)中的锡均被配体的3个碳和2个氧原子配位,配位原子呈畸变三角双锥构型;化合物中的环己基均为椅式构象;化合物(Ⅱ)中,配位水分子和另一分子的羰基氧与芳环上的甲基氧?  相似文献   

7.
A facile and credible strategy was demonstrated to synthesize two new Sn-O clusters 1 and 2 by the reactions of nBu2SnO with esters directly under mild conditions.Cluster 1 crystallizes in the triclinic system,space group P1 with a = 13.054(3),b = 13.137(3),c = 15.077(3) ,α = 80.009(9),β = 77.187(10),γ = 76.075(11)°,Z = 2,V = 2427.3(9) 3,Dc = 1.565 g/cm3,μ(MoKα) = 2.076 mm-1,F(000) = 1152,the final R = 0.0335 and wR = 0.0664 for 9416 observed reflections(I 2σ(I)).Cluster 2 belongs to the monoclinic system,space group P21/c with a = 13.673(3),b = 13.342(3),c = 16.296(4) ,β = 104.385(5)o,Z = 4,V = 2879.7(10) 3,Dc = 1.347 g/cm3,μ(MoKα) = 1.751 mm-1,F(000) = 1176,the final R = 0.0306 and wR = 0.0706 for 6390 observed reflections(I 2σ(I)).The crystal structures of the clusters consist of cen-trosymmetric [RCOOSnnBu2OSnnBu2OH)]2 molecules with an almost planar Sn4O4 framework.Each pair of exo-and endo-cyclic tin atoms was linked by one bridge-OH only.In addition,a novel structure of nBu2SnO different from the previous reports was proposed on the basis of 1H-NMR,TG analysis and X-ray diffraction.  相似文献   

8.
Li2Sn(OH)6     
Hydro­thermally prepared dilithium tin hexa­hydro­xide crystallizes in the monoclinic system (space group P21/n), with the Sn atom at a site with symmetry and all other atoms in general positions. The Sn coordination polyhedron is made up of six hydro­xide groups. The Li atom is tetrahedrally coordinated by oxy­gen, with the tetrahedra sharing two corners and one edge with the adjacent Sn octahedra. Hydro­gen bonds between the OH groups provide additional bonds in the framework.  相似文献   

9.
The title complex {[nBu2Sn(2-OHC6H4CH=NC6H4COO)]2O}2·2H2O was synthesized by the reaction of N-(4-carboxyphenyl)-salicylideneimine with dibutyltin(IV) oxide in 1∶1 molar ratio. The compound has been characterized by elemental analysis, IR, 1H NMR spectra and X-ray single crystal diffraction. It crystallizes in triclinic system with space group P1. The crystal data are: a=1.242 9(2) nm, b=1.261 3(2) nm, c=1.594 9(3) nm, α=102.06(2)°, β=92.884(3)°, γ=95.939(3)°, Z=2, Dc=1.342 g·cm-3, F(000)=1 000, V=2.425 2(7) nm3, R1=0.041 5, wR2=0.104 4. The compound is in centro-symmetric dimer structure mode with a four-member central endo-cyclic Sn2O2 unit in which the bridging oxygen atoms are tri-coordinated. All the tin atoms are five-coordinated with geometry of distorted trigonal bipyramid. CCDC:286105.  相似文献   

10.
The Crystal Structure of Trimethyltin Methanesulfinate, (CH3)3SnO2SCH3 Trimethyltin methanesulfinate, (CH3)3SnO2SCH3 crystallizes orthorhombie in the space group A2122. The lattice constants are: a = 7.98 ± 0.01, b = 12.59 ± 0.02 and c = 17.83 ± 0.02 Å Within the crystal structure the Sn atoms are linked together via bridging RSO2 groups to form a helical chain along [l00]. Each Sn atom is surrounded by three C and two 0 atoms in a trigonal bipyramidal arrangement. The Sn? C distances are in the range from 2.09 to 2.18 Å the Sn? 0 distance amounts to 2.23 Å.  相似文献   

11.
1 INTRODUCTION Recently, the researches on inorganic-organic hy-brid compounds represent an advanced field in mate-rial science[1]. At the molecular level, the combina-tion of two extremely different components providesan avenue to design new hybrid materials as well asthe ability to modulate properties of one or more ofthe components[2~6]. Some attractive properties, suchas efficient luminescence[2~4], ideal thermal and me-chanical stability, interesting magnetic[5], non-linearoptical[…  相似文献   

12.
Mixed-ligand diorganotin esters, [R 2Sn(OP(O)(OH)Ph)(OS(O) 2R (1))] n [R = n-Bu, R (1) = Me ( 1), n-Pr ( 2); R = Et, R (1) = Me ( 3)], have been synthesized by reacting the tin precursors, R 2Sn(OR (1))OS(O) 2R with an equimolar amount of phenylphosphonic acid under mild conditions (room temperature, 6-8 h, CH 2Cl 2). These have been characterized by IR, multinuclear ( (1)H, (13)C{ (1)H}, (31)P, and (119)Sn) NMR, and single crystal X-ray diffraction studies. The asymmetric unit of 1 is comprised of a tetramer with four crystallographically unique tin atoms. The structure reveals a central eight-membered (Sn-O-S-O) 2 cyclic ring with two exocyclic tin atoms, which results from micro 3-binding of the two methanesulfonate groups. The remaining two sulfonates are monodentate and contribute in O...HO(P) hydrogen bonding. The molecular structure is extended into a 3D coordination polymer with the aid of hydrogenphenylphosphonate group on each tin atom, acting in a micro 2-O 2P mode and forms a series of eight-membered (Sn-O-P-O) 2 rings in the structural framework. 2 and 3 are isostructural and represent linear 1D coordination polymers via micro 2-binding mode of both alkanesulfonate and hydrogenphenylphosphonate groups.  相似文献   

13.
The novel complexes [Zn(L)Cl] (1), [Cd(L)Cl] (2), [Hg(L)Cl] (3), {[Hg(L)Cl].NaOH.2H2O} (3.NaOH.2H2O), and {[Hg3(HL)2Cl6].2H2O} (4) (L = -SCH2CH2NH2) were prepared and investigated by means of IR spectroscopy and single-crystal X-ray diffraction. The crystal structures of 1, 2, and 3.NaOH.2H2O show chelating N,S-coordination of the cysteaminate ligand, bridging S, and terminally coordinating Cl. Apart from these common features, the coordination geometries and modes of intermolecular association are different. 1 forms a cyclic tetramer with a Zn4S4 ring, and 3.NaOH.2H2O contains one-dimensional [Hg(L)Cl]n chains with S-bridged Hg atoms. Zn and Hg atoms in 1 and 3.NaOH.2H2O are tetracoordinate with a distorted tetrahedral M(ClNS2) geometry (M = Zn, Hg). Each Cd atom of 2 binds to three S atoms and vice versa, such that layers of distorted Cd3S3 hexagons are formed. 2 is the first example for a compound exhibiting a group 12-group 16 layer structure, which can be described as an analogue of a graphite layer. Additionally, each Cd atom binds to a chlorine atom and a nitrogen atom from a cysteaminate ligand resulting in pentacoordination with a distorted trigonal bipyramidal Cd(ClNS3) geometry. 4 contains two differently coordinate Hg atoms. One displays a distorted trans-octahedral Hg(Cl4S2) geometry, while the other is coordinated by four Cl atoms and one S atom and additionally forms a long Hg...Cl contact.  相似文献   

14.
A model compound for the active sites of Fe-only hydrogenases,[Fe2(SCH2)2N(3-PhCF3)(CO)6]2,has been synthesized and structurally characterized by single-crystal X-ray diffraction.It crystallizes in tetragonal,space group P43,with a = 12.6324(3),b = 12.6324(3),c=24.0453(12) (A),V = 3837.1(2) (A)3,Z = 4,Fe4S4N2C30O12F6H16,Mr= 1062.09,Dc= 1.839 g/cm3,μ(MoKa) = 1.791 mm-1,F(000) = 2112,T= 293(2) K,Flack = 0.034(9),R= 0.0282 and wR =0.0685 for 8148 observed reflections with I > 2σ(I).In the title compound,each Fe1 atom is coordinated by three terminal carbonyl C atoms (Fe-C:1.783(3)~ 1.816(3)(A)),two bridging S atoms (Fe-S:2.2609(7)~2.2757(8)(A)) and another Fe atom (Fe-Fe 2.5011(5) (A)),adopting a distorted octahedral geometry with trans angles ranging from 152.45( 11 ) to 157.77(10)°.  相似文献   

15.
A new mononuclear tin(IV) complex [Sn(edt)2L]·CH2Cl2 (edt = ethane-1,2-dithio- late, L = di-2-pyridyl-ketone p-phenyldiamine) was obtained by a one-pot reaction which involves in situ formation of a new Schiff-base ligand L. The title compound (C22H24Cl2N4S4Sn) crystallizes in monoclinic, space group P21/n with a = 13.438(1), b = 12.2657(10), c = 17.1477(13) (A), β = 99.323(1)o, V = 2789.1(4) (A)3, Z = 4, Mr = 662.28, Dc = 1.577g/cm3, F(000) = 1328, μ = 1.426 mm(1, the final R = 0.0450 and wR = 0.1077 for 3868 observed reflections (I > 2σ(I)). In the title compound, Sn4+ ion is six-coordinated with four sulfur atoms of two edt ligands and two nitrogen atoms of the ligand di-2-pyridyl-ketone p-phenyldiamine to form a highly distorted octahedron.  相似文献   

16.
Combination of 2-aminoethanethiol hydrochloride and HgI2 in water in the presence of a base yielded a cyclic molecular structure, [Hg4I4(SCH2CH2NH2)4] (1). For the same reaction in the absence of the base, a similar structure with protonated amines was expected; however, polymeric [Hg4I8(SCH2CH2NH3)2]n.nH2O2 was formed instead. The structures are quite variable despite similar reaction conditions. For instance, there is an additional Hg-N interaction in 1 due to the use of base. The environment around tetracoordinate Hg in 1 is comprised of S, N, and I atoms, with the ligand forming a five-membered chelate and the I atoms present alternate to each other. In the repeating unit of 2, three independent types of Hg atoms are observed, with HgSI3, HgS2I2, and HgI4 bonding environments that have both bridging and terminal I atoms. A simple mechanistic pathway for the formation of 1 and 2 is proposed that includes the presence of three- and four-coordinate Hg intermediates in the solution. Intermolecular hydrogen bonding involving N, I, and S in 1 and N, I, and O atoms in 2 create extended three-dimensional networks. The shortest Hg... Hg distances are found to be intrachain in the range 3.938-3.962 A and indicate no interaction between these atoms. The solution studies (UV-vis and NMR) along with solid-state (IR, Raman, and X-ray) studies for 1 and 2 confirm retention of the structural configuration in the solution. The thermal study of 2 indicates that degradation of the complex occurs in a single step, in contrast to 1, which takes a more complicated decomposition pathway.  相似文献   

17.
The structure of bis[tris(cyclohexyl)tin] azide hydroxide, (Cy3Sn)2N3(OH) ( 1 ), contains infinite chains of molecules linked by regularly alternating and µ2 bridging azide and hydroxide groups that create trigonal bipyramidal tin centres. The bridges, with Sn? N 2.436(11) and 2.385(11) Å and Sn? O 2.199(8) and 2.197(8) Å, are relatively symmetrical. This structure is similar to that of catena bis(trimethyltin) azide hydroxide, (Me3Sn)2N3(OH) ( 2 ). In the structure of 1 , each terminal nitrogen atom of the azide is bonded to a different tin atom (1,3 or α,γ bridge formation). In the structure of 2 , however, only one nitrogen atom of each azide is involved in bridging and bonds to two different tin atoms (1,1 or α,α bridge formation). In this case, the remaining terminal nitrogen atoms act as acceptors for O? H?N hydrogen bonds that link the chains to form infinite sheets. It appears then, from these two examples, that in such compounds the size of the organic species bonded to tin can affect the azide bridging mode and also the packing of the polymeric chains Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

18.
采用表面改性和离子交换相结合的方法制备了Ni2(OCH3)2/SiO2负载型双核金属甲氧基配合物催化剂,利用红外光谱(IR)、程序升温脱附(TPD)、程序升温表面反应(TPSR)和微反技术考察了催化剂的表面结构以及CO2和CH3OH的化学吸附和反应性能.结果表明:Ni2(OCH3)2/SiO2中Ni2+与载体SiO2表面O2-以双齿配位形式键合,甲氧基以桥基形式联结双金属离子形成双核物种Ni2(OCH3)2;CO2在催化剂表面存在甲氧碳酸酯基物种和桥式两种吸附态,CH3OH则只有一种分子吸附态;在100~200℃条件下,CO2和CH3OH在催化剂上的反应产物主要是DMC和H2O;根据反应结果,讨论了催化反应机理.  相似文献   

19.
A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2),has been synthesized and characterized by X-ray structure determination. It crystallizes in the triclinic system, space group P1-, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) (A), α = 81.338(3),β= 88.173(4), γ = 66.199(3)°, V = 718.9(2) (A)3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3,μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I> 2σ(Ⅰ)). In the title complex, each copper(Ⅱ) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions,and one chlorine atom). Two copper(Ⅱ) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(Ⅱ)-Cu(Ⅱ) binuclear entity, and the distance between two copper(Ⅱ)atoms is 3.0144(15) (A).  相似文献   

20.
Fifteen new tris[(4-fluorophenyldimethylsilyl)methyl]tin O,O-dialkyldithiophosphates were synthesized and characterized by IR, 1 H NMR, MS spectroscopy, x-ray diffraction, and elemental analysis. The crystal structure of [(4-FC 6 H 4 SiMe 2 CH 2 ) 3 Sn] 2 O has been determined. The structure consists of four-coordinated tin atoms in a slightly distorted tetrahedral geometry with an O atom bridge between the two Sn atoms.  相似文献   

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