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1.
The substituted reactions of (μ-FcC≡CH)Co2(CO)6 with PPh3, AsPh3 and dppm have been studied and three new substituted derivatives have been obtained. The compounds were characterized by elemental analysis, IR, 1H NMR, MS and X-ray crystallography. They have the following formula: (μ-FcC≡CH)Co2(CO)6-nL[n=1, L=PPh32), AsPh33); n=2, L=dppm (4)]. The cluster 2 crystallizes in monoclinic, space group P21/n, with a=1.342 4(8) nm, b=1.305 4(8) nm, c=1.875 0(9) nm, β=103.084(9)°, V=3.201(3) nm3, Z=4, F(000)=1 480, Dc=1.515 g·cm-3, μ=15.62 cm-1; final R indices [I > 2σ(I)]: R1=0.040 9, ωR2=0.076 9; S=1.007, Δρmax=463e·nm-3, Δρmin=-395 e·nm-3. The cluster 3 crystallizes in monoclinic, space group P21/n, with a=1.341 0(4) nm, b=1.307 9(4) nm, c=1.912 0(5) nm, β=103.043(5)°, V=3.267(15) nm3, Z=4, F(000)=1 552, Dc=1.574 g·cm-3, μ=24.87 cm-1; final R indices[I> 2σ(I)]:R1=0.0437, ωR2=0.078 2; S=0.995, Δρmax=530 e·nm-3, Δρmin=-444 e·nm-3. CCDC: 221860, 2; 221863, 3.  相似文献   

2.
用Co2(CO)8分别与两个杂环配体C(S)NHP(S)(C6H4OCH3)OC(Ph)CH (L1)和C(S)NHC(CH3)2P(S)(Cl)N(Ph) (L2)反应,合成两个新的三核钴羰基硫簇合物Co3(CO)73-S)[μ,η2-CNP(S)(C6H4OCH3)OC(Ph)CH]()和Co3(CO)73-S)[μ,η2-SCNC(CH3)2P(S)(Cl)N(Ph)]()。用元素分析,IR, 1H NMR, 31P NMR及MS谱表征了它们的结构,同时用X射线衍射法测定了它们的晶体分子结构,二者属于三斜晶系,空间群P1,的晶胞参数为:a=0.84768(1)nm,b=1.19049(3)nm,c=1.43639(1)nm,α=86.926(1)°,β=81.601(3)°,γ=88.535(2)°,V=1.4318(5)nm3,Z=2,Dc=1.641g·cm-3,F(000)=716,μ=1.893mm-1,R=0.0602,Rw=0.1515。的晶胞参数为:a=1.2050(2)nm,b=1.2448(2)nm,c=0.8951(2)nm,α=97.49(1)°,β=93.552(4)°,γ=108.432(3)°,V=1.2554(3)nm3,Z=2,Dc=1.841g·cm-3,F(000)=690,μ=2.419mm-1,R=0.0423,Rw=0.1075。的分子骨架Co3S为三角锥构型,S作为面桥基配体,所有CO作为端基配体与三个Co原子成键。中含有CoCoCN四元环组件,中含有CoCoSCN五元环组件。  相似文献   

3.
Treatment of the lithium β-diketiminate [Li{N(R)C(NMe2)C(H)C(NMe2)N(R)}]2 (1) (R=SiMe3) with KOBut, KOH·H2O and CoCl2 in tetrahydrofuran gave in good yields the RO bridged β-diketiminato Co(Ⅱ) complex [Co{N(H)C(NMe2)C(H)C(NMe2)N(R)-( μ-OR)}]2 (2) at ambient condition. The crystal data of (2) are as follows: crystal system, monoclinic; space group, P121/n1; a=0.963 9(3) nm, b=1.077 2(3) nm, c=2.025 0(6) nm, V=2.102 5(10) nm3, Z=2, Dc=1.186 g·cm-3, F(000)=804, μ(Mo )=0.934 mm-1, R1=0.047 8, wR2=0.097 9. In solid state, complex (2) is a dimer bridged by RO (R=SiMe3) group and the two Co2+ are in distorted tetrahedron. CCDC: 249253.  相似文献   

4.
Ag(Ⅰ)、Pd(Ⅱ)异核金属簇合物的制备和晶体结构研究   总被引:2,自引:2,他引:2  
The complexes of [Ag2Pd2(μ-dppm)2(μ-S2CNC4H8)23-S2CNC4H8)2](SbF6)2·Et2O (1) and [AgPd(S2CN C4H8)(μ-dppm)2](SbF6)·H2O (2)were synthesized and their single crystal structures were determined by X-ray diffraction. The complex 1 is monoclinic system, space group P21/c with a=1.14370(3)nm, b=1.39025(4)nm, c=2.93579(8)nm, β=95.173(1)°, V=4.6490(2)nm3, Z=4, Dc=1.716g·cm-3, μ(Mo Kα)=1682cm-1, F(000)=2384, Mr=2401.98, R=0.0662, wR=0.1302. The complex 2 is monoclinic system, space group Cc with a=2.74136(6)nm, b=1.04317(2)nm, c=2.523990(10)nm, β=95.173(1)°, V=4.6490(2)nm3, Z=4, Dc=1.716g·cm-3, μ(Mo Kα)=1682cm-1, F(000)=2384, Mr=2401.98, R=0.0662, wR=0.1302. CCDC: 1, 213613; 2, 213612.  相似文献   

5.
以三齿吡唑-三嗪(类蝎型)化合物2,4-二(3,5-二甲基吡唑)-6-二乙基胺-1,3,5-三嗪(bpz*eaT)为配体,在无水乙醇和甲醇溶剂中,合成了2个配合物Cu2(mpz*eaT-EtO)2(N3)2Cl2(1)和Cu2(mpz*eaT-MeO)2(N3)4(2)(mpz*eaT-EtO:2-(3,5-二甲基吡唑)-4-乙醇-6-二乙基胺-1,3,5-三嗪;mpz*eaT-MeO:2-(3,5-二甲基吡唑)-4-甲醇-6-二乙基胺-1,3,5-三嗪)。通过元素分析、红外光谱、紫外光谱、热重分析以及X-ray单晶衍射方法对配合物进行了表征,并分析了其光谱及结构特征。晶体结构表明,配合物1属于三斜晶系,P1空间群,a=0.9949(2)nm,b=1.0216(2)nm,c=1.1480(2)nm,α=115.11(3)°,β=106.99(3)°,γ=100.39(3)°,V=0.9460(3)nm3,Z=1;配合物2属于单斜晶系,P21/c空间群,a=1.5464(5)nm,b=1.4008(5)nm,c=0.8905(3)nm,β=103.227(5)°,V=1.8779(10)nm3,Z=2。配合物12中的中心铜原子均为五配位,形成扭曲的四角锥构型。  相似文献   

6.
夏军  张明  赵斌  程鹏 《无机化学学报》2006,22(8):1406-1410
本文分别用N,N′-二(2-吡啶基)-2,6-吡啶二酰胺(H2L)和2-吡啶酸得到了2种具有一维链结构的铜配合物。通过X-射线单晶衍射,测定了晶体的结构。配合物1,{Cu3L2(C4H4O4)·10H2O}n,属于三斜晶系,空间群是P1,晶胞参数如下:a=0.706(1) nm,b=1.113(8) nm,c=1.288(7) nm,α=110.810(5)°,β=90.422(6)°,γ=101.183(6)°,V=0.926 2(2) nm3Z=1。配合物2,{Cu(pic)2·2H2O}n,也属于三斜晶系,空间群是P1,晶胞参数如下:a=0.513(6) nm,b=0.765(0) nm,c=0.924(6) nm,α=74.839(4)°,β=84.386(5)°,γ=71.401(5)°,V=0.332 3(0) nm3Z=1。通过分子中未配位的水分子的氢键作用,配合物1构成了1个三维结构;而配合物2通过弱配位键作用形成了一维的链状结构。CCDC:603470,1;608265,2。  相似文献   

7.
Two novel substituted derivatives ( μ3-S)( μ-H)Fe2Co(CO)7Ln (n=2, L=AsPh3 (3) n=1, L=dppm (4)) have been synthesized and characterized by IR, 1H NMR, 31P NMR, MS and X-ray crystallography . The cluster 4 crystallizes in monoclinic space group C2/c, with a=1.589 1(7), b=1.814 9(8), c=2.277 8(11) nm, β=96.861(8), V=6.522(5) nm3, Z=8, Dc=1.552 g·cm-3, F(000)=3 094, μ=12.95 cm-1. Final R indices [i>2σ(I)]: R1=0.054 3, wR2=0.101 1. The cyclic voltammetric behavior for the parent cluster 1 and its substituted derivatives were investigated, the results show that the order of σ-donator ability is CO < PPh3 < AsPh3 < dppm. CCDC: 221867.  相似文献   

8.
Copper(Ⅱ) complexes Cu(C6H6N2)2(ClO4)2 (1) and Cu2(OAc)4(C5H5ClN2)2 (2) with amino-pyridine deriva-tives ligands have been synthesized and characterized by elemental analysis and IR spectrum. Their crystal struc-tures are determined by X-ray diffraction method. Compound 1, C12H16C12CuN4O8Mr=478.73, triclinic, space group , a=0.7641(1)nm, b=0.7987(1)nm, c=0.7990(1)nm, α=106.78(1)°,β=95.71(1)°, γ=108.85(1)°, V=0.4317(1)nm3Z=1, Dc=1.841g·cm-3, μ=1.627mm-1F(000) =243,R1=0.0264, ωR2=0.0641 (I>2σ(I)). In 1, the center metal ion Cu(Ⅱ) possesses distorted octahedral geometry. Compound 2, C18H22C12Cu2N4O8Mr=620.38,monoclinic, space group C2/ca=1.9888(3), b=0.9158(1), c=1.4241(2)nm, β=115.89(1)°, V=2.3336(5)nm3Z=4, Dc=1.766mg·cm-3, μ=2.104mm-1F(000)=1256, R1=0.0263, wR2=0.0676 (I>2σ(I)). Compound 2 is dinuclear structure, in which each Cu(Ⅱ) adopts five-coordinated distorted square pyramid geometry. CCDC: 193109; 193110.  相似文献   

9.
Three tin (Ⅳ) complexes with N,N-dialkyl dithiocarbamates Ph3SnS2CN(CH3)C6H5 (1),Ph3SnS2CN(C4H8NH) (2) and Sn(Cl)2(S2CNEt2)2 (3) have been synthesized. The crystal structures have been determined by X-ray sin- gle crystal diffraction. A crystal of the complex 1 is triclinic with space group P1, a=0.9485(3)nm, b=1.0491(3)nm, c=1.3631(4)nm, α=70.996(4)°, β=72.294(4)°, γ=79.609(4)°, Z=2, V=1.2168(6)nm3, Dc=1.453g·cm-3, μ=1.234mm-1, R=0.0442, wR=0.0858. A crystal of the complex 2 is monoclinic with space group P2(1)/c, a=1.2214(2)nm, b=1.1651(2)nm, c=1.5769(3)nm,β=99.039(2)°, Z=2, V=2.2162(7)nm3, Dc=1.532g·cm-3, μ=1.352mm-1, R=0.0267, wR=0.0591. A crystal of the complex 3 is triclinic with space group P1, a=0.7179(2)nm, b=0.9256(3)nm, c=1.5327(5)nm,α=93.857(4)°,β=98.992(4)°, γ=109.481(4)°, Z=2, V=0.9405(5)nm3, Dc=1.717g·cm-3, μ=2.076mm-1, R=0.0263, wR=0.0662. In the complexes 1 and 2 the tin atoms rendered five-coordination in a distorted tigonal bipyramidal structure and in the complex 3 the tin atom rendered six-coordination in a distorted octahedron structure. CCDC: 1, 179918; 2, 180024; 3, 180004.  相似文献   

10.
利用水热技术,合成了2个新的配合物{[Co(Hbtc)(Pyphen)(H2O)]·H2O}n (1)和{[Cd2(btc)(Pyphen)2Cl]·2H2O}n(2) (H3btc=1,2,4-苯三酸,Pyphen=[2,3-f]吡嗪并[1,10]-菲咯啉),并通过X-射线单晶衍射、元素分析、热重分析和荧光进行了表征。配合物1属三斜晶系,空间群P1,a=0.643 44(13) nm,b=1.202 9(2) nm,c=1.371 6(3) nm,α=95.03(3)°,β=90.46(3)°,γ=103.54(3)°,V=1.027 7(4) nm3,Z=2,CoC23H16N4O8,Mr=535.31,Dc=1.730 g·cm-3,μ(MoKα)=0.900 mm-1,F(000)=546,GOOF=1.089,R=0.099 2,wR=0.249 0;配合物2属三斜晶系,空间群P1,a=0.968 93(8) nm,b=1.223 82(10) nm,c=1.592 21(14) nm,α=67.486 0(10)°,β=73.158 0(10)°,γ=78.468 0(10)°,V=1.660 9(2) nm3,Z=2,Cd2C37H23N8O8Cl,Mr=967.88,Dc=1.935 g·cm-3,μ(MoKα)=1.432 mm-1,F(000)=956,GOOF=1.051,R=0.077 9,wR=0.141 2。结构分析表明:配合物1为无限一维双链结构,配合物2为二维层状结构。此外,氢键和π-π相互作用在加固配合物的结构中起到重要作用。  相似文献   

11.
用Ru3(CO)12与顺-2,4二(叔丁基胺基)-1,3,-二(叔丁基)-1,3,2,4-环偶磷氮烷cis-[P(NHBut)NBut]2反应,得到两个新的含偶磷氮环的三核钌羰基簇合物:Ru3(CO)11[{P(NHBut)NBut}2] Ⅰ和Ru3(CO)11[P(NHBut)(NBut)2P(O)H] Ⅱ。对它们进行了元素分析,IR和1H NMR谱表征,并用X-ray单晶衍射法测定了晶体结构。Ⅰ:正交晶系,Pna2(1)空间群,a=2.7574(9) nm,b=0.8981(3) nm,c=1.5272(5) nm, V=3.782(2) nm3,Dc=1.686 g·cm-3,Z=4;Ⅱ:三斜晶系,P1空间群,a=0.96384(19) nm,b=1.1705(2) nm,c=1.5589(3) nm,α=101.72(3) °,β=91.54(3) °,γ=108.20(3) °,V=1.6282(6)nm3,Dc=1.845g·cm-3,Z=2;两个簇合物均为Ru3(CO)12的单取代衍生物,配位基环偶磷氮烷以单齿P原子配位在一个Ru原子的赤道位置上。中,偶磷氮环上未配位P(Ⅲ)被氧化成具有膦酰基结构(=P(O)H)的P(Ⅴ)。  相似文献   

12.
合成了两种具有新型结构的苄基锡化合物:一维链状μ-氯-三苄基锡(1)和一维链状μ-氧-三苄基锡(2),经X-射线方法测定了化合物的晶体结构。晶体结构(1)属正交晶系,空间群为P212121,晶体学参数:a=0.855 3(3) nm,b=1.081 4(4) nm,c=1.968 1(7) nm,V=1.820 4(11) nm3Z=4,Dc=1.560 g·cm-3,μ(Mo )=15.47 cm-1F(000)=856,R1=0.059 7,wR2=0.141 5。晶体结构(2)属正交晶 系,空间群为P212121,晶体学参数:a=1.982 3(4) nm,b=1.089 1(2) nm,c=0.861 1(17) nm,V=1.859 0(6) nm3Z=4,Dc=1.458 g·cm-3, μ(Mo )=13.76 cm-1F(000)=820,R1=0.032 7,wR2=0.064 8。配合物中锡原子均呈五配位畸变三角双锥构型。  相似文献   

13.
In this article we report the synthesis of (R,S)-4,4′-biquinoline-6,6′-dimethyl-3,3′-dicarboxylate (DBBD) (1) and the formation of copper(I) coordination polymer [CuI(DBBD)2]n (2) by inducing a bidentate organic ligand (DBBD). The crystal 1 belongs to monoclinic system with space group P21, and a=0.881 30(19) nm, b=1.966 0(6) nm, c=1.478 1(4) nm, β=119.429(12)°, V=2.230 5(10) nm3, Dc=1.276 g·cm-3. The crystal 2 belongs to orthogonal system with space group Fmm2, and a=2.044 41(17) nm, b=1.543 06(13) nm, c=1.652 45(13) nm, V=5.212 9(7) nm3, Dc=1.669 g·cm-3, Z=8. CCDC: 292931, 1; 292934, 2.  相似文献   

14.
三核锌配合物的合成及结构表征   总被引:1,自引:0,他引:1  
A trinuclear Zn(Ⅱ) complex [Zn3(L)2(Cl)2(OSO3)2(H2O)2]·2H2O (1) (L=N1-(2-aminoethyl)-N1-(2-imidazolethyl)-ethane-1,2-diamine) was synthesized by reaction of ligand L with ZnSO4·7H2O at pH=9 in air. The complex has been characterized by elemental analysis, FTIR and X-ray single crystal diffraction. It reveals that the crystal of complex 1 belongs to monoclinic C2/c space group, a=3.516 9(7) nm, b=0.676 57(14) nm, c=1.502 2(3) nm, β=110.955(4)°, V=3.337 9(12) nm3, Z=4. In complex 1, two ligands L bridge three Zn(Ⅱ) centers to form trinuclear structure which was further connected by hydrogen bonding to form two-dimensional structure. CCDC: 609515.  相似文献   

15.
合成了一对结构类似的双核铜和锌配合物,Cu2(L1)2(1)和[Zn2(L2)2(CH3OH)2] (2),其中L1和L2分别是2-溴-N''-(2-羟基-5-甲基苯亚甲基)苯甲酰肼(H2L1)和2-氯-N''-(2-羟基-5-甲基苯亚甲基)苯甲酰肼(H2L2)的二价阴离子,通过元素分析、红外光谱以及单晶X射线衍射表征了它们的结构。配合物1以三斜晶系P1空间群结晶,其晶体学参数:a=0.91411(6) nm,b=1.18004(7) nm,c=1.35936(9) nm,α=101.928(2)°,β=91.399(2)°,γ=107.873(2)°,V=1.3593(2) nm3,Z=2,R1=0.0540,wR2=0.1189,GOF=0.970。配合物2以单斜晶系P21/c空间群结晶,其晶体学参数:a=1.21697(9) nm,b=1.21496(9) nm,c=1.21283(9) nm,β=110.939(1)°,V=1.6748(2) nm3,Z=2,R1=0.0341,wR2=0.0689,GOF=1.024。X射线分析表明2个化合物都是中心对称的双核配合物,其中配合物1中的Cu原子是平面正方形配位构型,配合物2中的Zn原子是四方锥配位构型。还通过MTT法研究了这两个配合物的抗细菌(大肠杆菌,金黄色葡萄球菌,枯草芽孢杆菌和铜绿色假单胞菌)和抗真菌(白假丝酵母菌和黑曲霉菌)活性。  相似文献   

16.
The new compound, [Ni(TSSB)(Phen)(H2O)]·4H2O (TSSB=Taurine Salicylic Schiff Base, phen=O-Phenanthroline) has been synthesized and characterized by IR, elemental analysis and X-ray diffraction. The compound crystal data: triclinic, space group P1, a=1.049 7(2), b=1.122 5(2), c=2.384 3(4) nm, α=87.676(3)°, β=82.957(3)°, γ=62.924(3)°; V=2.482 3(7) nm3, Z=4; Dc=1.488 g·cm-3, μ=0.920 mm-1, F(000)=1 160, Goof=1.032, (Δρ)max=899 e·nm-3, (Δρ)min=-624 e·nm-3. The compound is a dimmer. In the complex, two Ni(Ⅱ) were coordinated by three oxygen atoms and three nitrogen atoms while the O atoms of Ac- groups did not coordinate. The Ni(Ⅱ) formed a distorted octahedron geometry. The compound is an three dimensional net connecting with hydrogen bonding. CCDC: 275474.  相似文献   

17.
Reactions of CuBr with equimolar PyHBr or γ-MePyHBr afforded two novel one-dimensional bromocuprate(Ⅰ)polymers {(PyH)3[Cu3Br6]} (1) and {(γ-MePyH)2[Cu2Br4]}(2), respectively. Both 1 and 2 were charac-terized by IR, elemental analysis, and X-ray crystallography. Crystal data for 1: monoclinic, space group P21/na=0.93262(12)nm, b=1.3497(2)nm, c=1.9149(2)nm, β=93.465(7)°, V=2.4060(5)nm3, Z=4. Crystal data for 2: orthorhombic, space group Pbcma=0.8659(4)nm, b=1.5669(6)nm, c=1.2849(5)nm, V=1.7432(2)nm3, Z=4. The structure of 1 has a unique helical chain composed of [Cu3Br5] units and μ-bromide anions while that of 2 shows a linear chain consisted of [Cu2(μ-Br)2] units bridged by pairs of μ-Br atoms. CCDC: 1, 208412; 2, 208413.  相似文献   

18.
The reaction of Ru3(CO)12 with five-membered cyclic SP(S)(Fc)N(Ph)NC(Me) gave two novel trinuclear and tetranuclear ruthenium carbonyl clusters containing capping S atoms in Ru3(CO)83-S)2[P(Fc)N(Ph)NC(Me)S] 1 and Ru4(CO)7(μ-CO)34-S)2[P(Fc)N(Ph)NC(Me)S] 2 (Fc=C5H5FeC5H4). During the reaction, the ligand precursor cleaved only in its P=S bond to give the fragments S and [P(Fc)N(Ph)NC(Me)S], and then coordinated to the ruthenium atoms to form the clusters as listed above. The clusters have been characterized by elementary analysis, IR, 1H NMR and MS spectroscopy. The crystal structure of cluster 2 has been determined by X-ary diffraction techniques. The crystal belongs to monoclinic with space group P21/c. The unit cell parameters are as follows: a=1.18744(7) nm, b=1.36041(11) nm, c=2.20026(18) nm, β=104.126(3) °, V=3.4468(5) nm3, Dc=2.175 g·cm-3, Z=4. In the molecule, the three bridging carbonyls and Ru4 are planar and with a pseudo-octahedral Ru4S2 skeleton. The terminal carbonyl of Ru1 was substituted by the cyclic ligand [P(Fc)N(Ph)NC(Me)S]. CCDC: 217076.  相似文献   

19.
陈正军  张道  金国新 《无机化学学报》2005,21(12):1775-1783
选择含有烯丙基亚胺酚为辅助配体,设计合成了5个ⅣB族钛锆金属络合物[{CH2=CHCH2N=CH-C6H3(3-R)O}2MCl2](4aR=t-Bu,M=Zr;4bR=t-Bu,M=Ti;4cR=Ph,M=Zr;4dR=Ph,M=Ti)和[{(CH3)2CHCH2N=CH-C6H3(3-t-Bu)O}2ZrCl2] (5),对它们进行了红外光谱、核磁共振及元素分析表征。并用X-射线单晶衍射法测定了化合物4a4d的晶体结构。部分配合物在助催化剂MMAO的作用下对烯烃聚合显示了较好的催化活性,其中自固载催化剂4a生成了双峰分布的聚烯烃产品 (Mw/Mn=15.3~31.9)。  相似文献   

20.
以双(4-吡啶-4-苯基)胺(BPPA)和4,4-(六氟)双(苯甲酸)(H2hfipbb)或对苯二甲酸(p-H2bdc)为配体,采用溶剂热法与M(NO3)2·6H2O(M=Co、Zn)组装合成了2个新的配合物{[Co2(BPPA)(hfipbb)2·(H2O)3]·6H2O}n(1)、{[Zn2(BPPA)2(p-bdc)2]·H2O·DMF}n(2),X射线单晶衍射测定结果表明:配合物12均为二维结构。配合物1具有新的拓扑结构。配合物2的二维结构又可以组成三维框架结构。配合物1为正交晶系,Pnna空间群,a=2.6409(2) nm,b=1.71578(13) nm,c=1.50411(11) nm,V=6.8154(9) nm3,Z=4,μ=0.571 mm-1,F(000)=2592,Dc=1.245 g·cm-3,Mr=1383.76,R1=0.0666,ωR2=0.2089(I>2σ(I));配合物2为单斜晶系,C2/c空间群,a=2.79670(9) nm,b=1.81482(6) nm,c=2.30313(7) nm,β=102.1360(10)°,V=11.4283(6) nm3,Z=8,μ=0.906 mm-1,F(000)=4944,Dc=1.391 g·cm-3,Mr=1196.85,R1=0.0398,ωR2=0.1064(I>2σ(I))。此外,热重分析表明配合物12均具有良好的热稳定性。  相似文献   

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