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1.
In the presence of Et4NCl·H2O, reaction of AgCl with TabHPF6 in MeCN afforded the title complex {(Tab-Tab)[Ag2(μ-Cl)4]-2MeCN}n 1. 1 crystallizes in the orthorhombic space group Pbcn with a = 16.782(3), b = 6.8358(14), c = 26.194(5) A, V = 3004.9(10) A3, Z = 8,μ = 1.817 mm^-1, Dc = 1.711 g/cm3, T= 223 K, C1lH16AgCl2N2S, Mr= 387.10, F(000) = 1544, S= 1.160, R = 0.0528 and wR = 0.0896 for 2732 observed reflections with I 〉 2σ(I). 1 contains a 1D linear [Ag2Cl4]n^2n- chain coupled with the [Tab-Tab]2+ dications. Intermolecular hydrogen bonding interactions between the protons of methyl groups from the Tab-Tab dications and the chlorides result in the formation of a 2D hydrogen-bonded network.  相似文献   

2.
Two binuclear silver complexes, [Ag2{μ-S2P(OCH2Ph)2}2(phen)2](1) and [Ag2{μ-S2P(OCH2CH2Ph)2}2(phen)2](2), were synthesized and characterized by elemental analysis, infrared spectrum, thermo-gravimetric analysis and X-ray single-crystal diffraction. Complex 1 crystallizes in the triclinic system, space group P1 with a = 9.7881(4), b = 10.7726(4), c = 13.1952(6) , a= 103.686(4), γ = 99.477(3), γ = 107.494(4)°, V = 1246.88(9) 3, Dc = 1.591 g·m-3 and Z = 1; Complex 2 is of monoclinic system, space group P21/n with a = 10.6014(8), b = 24.3969(15), c = 11.5353(10) , β = 14.125(10)°, V = 2722.9(4) 3, Dc = 1.526 g·m-3 and Z = 2. In the molecules of 1 and 2, O,O'-dialkyldithiophosphate anions,(PhCH2O)PS2- and(PhCH2CH2O)PS2- act as bridging ligands and connect two Ag(I) centers into a binuclear unit with Ag2S4P2 eight-membered rings in "chair" conformations. In both crystal structures, face-to-face π-π stacking interactions between the adjacent paralleling aromatic rings of 1,10-phenanthroline play a prominent role in the crystal packing and result in a 1D chain. And such 1D chains are further linked into 3D networks by weak intermolecular C–H···π interactions for 1.  相似文献   

3.
The reaction of [Et4N]2WOS3 with three equiv.of CuI and dmpzm in MeCN afforded [WOS3Cu3I(dmpzm)2]·2(MeCN)0.5(1·2(MeCN)0.5) while that of [PPh4]2WS4 with four equiv.of CuI in DMF/MeCN followed by the addition of two equiv.of dmpzm in MeOH gave rise to [WS4Cu4I2(dmpzm)2]·DMF(2·DMF).Both compounds were characterized by elemental analysis,IR,and single-crystal X-ray diffraction analysis.1·2(MeCN)0.5 crystallizes in triclinic,space group P1-with a = 11.4552(5),b = 11.6735(3),c = 16.2278(9) ,α = 99.537(9),β = 101.986(2),γ = 118.464(13)o,V = 1775.5(3)3,Z = 2,μ = 6.080 mm-1,Dc = 1.983 Mg/m3,T = 193(2) K,C24H35Cu3IN9OS3W,Mr = 1063.22,F(000) = 1018,S = 1.060,R = 0.0376 and wR = 0.0870.2·DMF belongs to the orthorhombic system,space group Pmn21 with a = 22.145(4),b = 11.464(2),c = 7.7370(15) ,V = 1964.2(6)3,Z = 2,μ = 6.865 mm-1,Dc = 2.189 Mg/m3,T = 193(2) K,C25H39Cu4I2N9OS4W,Mr = 1301.72,F(000) = 1226,R = 0.0632,wR = 0.1706 and S = 1.130.1·2(MeCN)0.5 consists of one CuI and two [Cu(dmpzm)]+ fragments that are linked by [WOS3]2-species via six Cu-S bonds,forming a nido-like [WS3Cu3] core.2·DMF contains a saddle-shaped [WS4Cu4] core with two iodides coordinated at two Cu centers in a cis position and two dmpzm ligands being chelated at another two Cu centers in a cis position.  相似文献   

4.
The reaction of [(η5-C5Me5)2Mo2(μ3-S)4(CuCl)2] 1 with Na2S in MeCN produced a trinuclear cluster [(η5-C5Me5)2Mo2(μ3-S)(μ-S)3(CuCl)] 2. 2 crystallizes in the monoclinic system, space group P21/c with a = 15.563(3), b = 8.9547(18), c = 17.846(4) , β = 101.29(3)o, V = 2438.9(9) 3, Z = 4, Dc = 1.878 g/cm3, T = 193(2) K, C20H30ClCuMo2S4, Mr = 689.60, F(000) = 1376, μ(MoKα) = 2.335 mm–1, S = 1.050, R = 0.0305 and wR = 0.0688 for 4033 observed reflections with I > 2σ(I). In the structure of 2, one [(η5-C5Me5)2Mo2(μ-S)2S2] moiety and one CuCl unit are assembled into an incomplete cubane-like [Mo2S4Cu] core framework, in which the Cu center adopts a distorted tetrahedral geometry coordinated by one μ3-S atom, two μ-S atoms and one terminal chloride. The two Mo…Cu contacts are 2.7519(7) and 2.7689(8) , respectively.  相似文献   

5.
The self-assembly reactions of MIICl2 (M = Ni, Co) with the flexible bix ligand [bix = 1,4-bis(imidazole-1-ylmethyl)benzene] yielded a 2D network [NiII(bix)2Cl2]n 1 and a 1D chain [CoII(bix)Cl2]n 2. Their crystal structures have been determined by X-ray single-crystal diffraction analysis. Complex 1 characters a two-dimensional grid-type structure and crystallizes in monoclinic, space group P21/c with a = 7.7231(7), b = 12.7787(9), c = 13.9374(13) , β = 105.419(4)o, C28H28Cl2N8Ni, Mr = 606.19, Ζ = 2, V = 1326.0(2) 3, Dc = 1.518 g/cm3, μ = 0.969 mm-1, F(000) = 628, R = 0.0429 and wR = 0.0783 for 2503 observed reflections (I > 2σ(I)). Compound 2 is a one-dimensional chain and crystallizes in orthorhombic, space group Pbca with a = 11.3696(6), b = 10.2128(6), c = 14.4943(9) , C14H14Cl2CoN4, Mr = 368.12, Z = 4, V = 1683.01(17) 3, Dc = 1.453 g/cm3, μ = 1.334 mm-1, F(000) = 748, R = 0.0317 and wR = 0.0800 for 1778 observed reflections (I > 2σ(I)). Magnetic properties of the title complexes were also investigated.  相似文献   

6.
The solvothermal reaction of 3-amino-1H-1,2,4-triazole (ttr) with Zn(ClO4)2·6H2O and NaCl in a 1:1:1 molar ratio gave a new complex [Zn(ttr)Cl]n with a 3-connected (4.82) 2-D struc- ture. The layers stack in the -ABAB- way along the c axis with abundant hydrogen bonding interac- tions to form the crystal structure. The complex [Zn(ttr)Cl]n crystallizes in the orthorhombic space group Pbca with a = 9.369(1), b = 10.049(1), c = 11.905(1) , V = 1120.9(3) 3, Z = 8.00, C2N4H3ZnCl, Mr = 183.90, Dc = 2.180 g/cm3, μ = 4.740 mm-1, F(000) = 720, S = 1.059 and T = 293(2) K. The final R = 0.0662 and wR = 0.2457 for 956 observed reflections with I > 2σ(I), and R = 0.0689 and wR = 0.2504 for all data.  相似文献   

7.
Introduction Polynuclear Ag(I)-thiolate compounds are of interests due to their unique molecular structures and metal-metal interactions. There were some such compounds reported in literatures, including Ag8(6-S)(dtp)6 [dtp=S2P(OEt)2] with [Ag8] cube,1 {Ag[S2P(OC3H7)2]}6 with a [Ag6] distorted octahedron,2 Ag11S(Et2dtc)9 [Et2dtc=S2CN(C2H5)2] with a [Ag11] cage of a 3-fold axis,3 and Ag14(6-S)(SPh)12(PPh3)8 4CH3OH13H2O with a [Ag14S12] cage composed of a staggered [Ag6] octahedr…  相似文献   

8.
A new 3D Ag(I) coordination polymer, [Ag8(btc)2(bpp)2]n(1, H4btc = biphenyl- 2,2ˊ,4,4ˊ-tetracarboxylic acid, bpp = 1,2-bis(4-pyridyl)propane), has been hydrothermally synthesi- zed and characterized by single-crystal X-ray diffraction analysis, elemental analysis and IR spectroscopy. Complex 1 crystallizes in the triclinic system, space group P1 with a = 13.4899(8), b = 13.4928(8), c = 16.4575(10) , α = 102.7640(10), β = 108.8100(10), γ = 101.4940(10)°, V = 2644.1(3) 3, Z = 2, Dc = 2.401 Mg·m-3, μ = 2.978 mm-1, F(000) = 1840, the final R = 0.0481 and wR = 0.0955 for 6794 observed reflections with I 2σ(I). Complex 1 features a 3D framework formed by Ag(I)-carboxylate chains containing [Ag16(COO)16] secondary building block. Furthermore, thermal stability and electrochemical property of 1 are also investigated in detail.  相似文献   

9.
雷晓武  岳呈阳 《结构化学》2011,30(6):805-810
A new intermetallic compound,Tb3Co4Sn13,has been synthesized by solid-state reaction of the corresponding pure elements in a welded tantalum tube at high temperature.Its crystal structure was established by single-crystal X-ray diffraction.Tb3Co4Sn13 crystallizes in cubic,space group Pm3n(No.223) with a = 9.5072(2) ,V = 859.33(3) 3,Z = 2,Mr = 2255.45,Dc = 8.717 g/cm3,μ = 34.369 mm-1,F(000) = 1906,and the final R = 0.0140 and wR = 0.0312 for 199 observed reflections with I > 2σ(I).The structure of Tb3Co4Sn13 belongs to the Yb3Rh4Sn13 type.It is isostructural with RE3Co4Sn13(RE = La,Ce),featuring a 3D [Co4Sn12] framework based on [CoSn6] trigonal prisms.The [CoSn6] trigonal prisms are interconnected via corner-sharing and Sn-Sn bonds to form a 3D [Co4Sn12] framework.The other Sn and Tb atoms are located in the spacers of the 3D framework.Band structure calculations indicate that Tb3Co4Sn13 is metallic.  相似文献   

10.
An inorganic-organic hybrid thioantimonate(Ⅲ) [CH3(CH2)3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method.1 crystallizes in the triclinic system, space group P with a = 7.0124(11), b = 11.919(2), c = 14.879(3) (A), α = 108.791(3), β = 102.441(3), γ = 92.846(2)o, V = 1140.1(3) (A)3, Mr = 859.71, Z = 2, Dc = 2.504 g/cm3, μ= 5.324 mm-1, F(000) = 804, S = 1.013, the final R = 0.0297 and wR = 0.0618 for 3534 observed reflections with I>2σ(I). 1 consists of [C4H9NH3] cations and two-dimensional [Sb4S7]n2n-anion which is composed of three SbS3 trigonal pyramids and one SbS4 unit joined by sharing common corners. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3] cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.  相似文献   

11.
The title complex [Ag(carbene)2]2[Ag2Br4] has been synthesized by the reaction of Ag2O with 1-ethyl-3-benyl-imidazolium bromide in DMSO at room temperature, and characterized by elemental analysis, 1H NMR and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P with a = 10.1597(10), b =11.0646(11), c = 13.0245(14) , α = 102.230(2), β = 90.606, γ = 113.9250(10)o, V = 1300.3(2) 3, Mr = 748.06, Z = 2, Dc = 1.911 g/cm3, μ(MoKα) = 4.60 mm-1 and F(000) = 728. The structure was refined to R = 0.0316 and wR = 0.0835 for 3744 observed reflections with I > 2σ(I). The title compound crystallizes as a centrosymmetric tetranuclear compound. One half of the molecule comprises the asymmetric unit of the structure. The Ag(1) atom is nearly linear or T-shaped when the Ag(1)-Ag(2) interaction is taken into consideration, which is bi-coordinated by two carbene carbon atoms. The Ag(2) atom adopts tetrahedral geometry. The catalytic behavior of the title complex has been investigated, and the results indicate it has a highly catalytic activation for L-lactide polymerization.  相似文献   

12.
An inorganic-organic hybrid thioantimonate(Ⅲ) [CH3(CH2)3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system,space group P1 with a=7.0124(11),b=11.919(2),c=14.879(3),α=108.791(3),β=102.441(3),γ=92.846(2)o,V=1140.1(3)3,Mr=859.71,Z=2,Dc=2.504 g/cm3,μ =5.324 mm-1,F(000)=804,S=1.013,the final R=0.0297 and wR=0.0618 for 3534 observed reflections with I > 2σ(I). 1 consists of [C4H9NH3]+ cations and two-dimensional [Sb4S7]n2n- anion which is composed of three SbS3 trigonal pyramids and one SbS4 unit joined by sharing common corners. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]+ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.  相似文献   

13.
The reaction of [Fe2S2(CO)6] with one equiv.of o-OCH3C6H4CH2Br under the re-duction of LiBHEt3 in dry THF afforded a tetranuclear cluster [(μ4-S){(μ-SCH2(o-OCH3)Ph)Fe2(CO)6}2](1).Complex 1 crystallizes in monoclinic,space group P21/n with a = 16.5623(6),b = 12.8265(5),c = 18.2702(7) ,β = 115.95(1)o,V = 3489.9(4) 3,Z = 4,μ = 1.87 mm-1,Dc = 1.709 Mg/m3,T = 296(2) K,C28H18Fe4O14S3,Mr = 898.03,F(000) = 1800,S = 1.10,R = 0.032 and wR = 0.058.Complex 1 consists of two diiron fragments possessing a {Fe2(CO)6} core.The two diiron units are bridged by an inorganic sulfide in a μ4-S binding mode and the sulfide is in a distorted tetrahedral geometry with the four iron atoms at each corner of the distorted tetrahedral.In its solid state,two types of non-classic intermolecular hydrogen bonding interactions plus a weak π-π stacking interaction led to a 2-D network.  相似文献   

14.
A new O,O'-bis(4-tert-butylphenyl)dithiophosphate complex Ni[SSP(OC6H4But- p)2]2 (1) was synthesized and characterized by elemental analysis, IR, 1H NMR, thermogravimetric analysis (TGA) and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 12.8440(3), b = 6.18686(12), c=26.3018(5) , β=92.6135(18)°, V = 2087.87(7) 3, Z = 2, Dc = 1.345 g/cm3, μ = 0.780 mm-1, the final R = 0.0316 and wR = 0.0748 (Ⅰ >2σ(Ⅰ)). A total of 4269 unique reflections were collected, of which 3621 with Ⅰ > 2σ(Ⅰ) were observed. The NiII atom lies on an inversion center and is chelated by two (p-ButC6H4O)2PSS-ligands in a [NiS4] square-planar geometry with Ni-S bonds of 2.2408(5) and 2.2444(5) , respectively. A stepwise 1D chain structure is constructed via intermolecular S…S and C-H…S interactions. According to our knowledge this is the first case that intermolecular S…S interaction is observed in mononuclear transition metal complex of O,O'-dialkyldithiophosphates.  相似文献   

15.
A new infinite three-dimensional framework structure of the title compound [H6MoVI8O27]·3C4N2H10 has been synthesized under mild hydrothermal conditions and charac-terized by elemental analyses,IR,fluorescent spectra and single-crystal X-ray diffraction.C12H36Mo8N6O27 crystallizes in the triclinic system,space group P 1 with a = 8.820(3),b = 9.534(3),c = 10.993(4) ,α = 99.985(17),β = 106.65(2),γ = 101.650(14)o,V = 840.6(5) 3,Mr = 1463.99,Z = 1,Dc = 2.892 g/cm3,μ = 2.993 mm-1,F(000) = 702,the final R = 0.0676,wR = 0.1920 and S = 1.074 for 2196 observed reflections with I > 2σ(I).The title compound exhibits a novel infinite three-dimensional(3D) framework composed of a [H6MoVI8O27] subunit and three dissociated piperazine fragments.The complex exhibits two strong fluorescent emission bands at ca.417 and 440 nm(λex = 378 nm) in the solid state at room temperature.  相似文献   

16.
One new coordination polymer with the chemical formula [CoCu2L2·K2·1.5C2H5OH]n(H4L = 2-hydroxy-3-[(E)-({3-[(2-hydroxybenzoyl)amino]propyl}imino)methyl] benzoic acid) has been synthesized based on the slow diffusion method,and characterized by IR spectroscopy,thermalgravimetric and X-ray diffraction analysis.It crystallizes in the monoclinic system,space group P21/n with a = 11.98860(10),b = 24.4279(3),c = 14.9008(2) ,β = 104.7490(10)°,V = 4220.01(8) 3,Z = 2,Mr = 1009.94,Dc = 1.590 g/cm3,F(000) = 2056,μ(MoKα) = 1.649 mm-1,the final R = 0.0411 and wR = 0.1178 for 5920 observed reflections with I 2σ(I).The compound possesses a 2D brick wall structure constructed from trinuclear units.  相似文献   

17.
A novel pillared-layer framework with a (52.6)(53.63.73.8) Schl fli symbol, [Mn(H2O)(Htrz)(Hbtc)]n (1), was prepared by the reaction of 1,2,4-triazole (Htrz), 1,3,5-benzenetricarboxylic acid (H3 btc), and Mn Ⅱ salt and structurally and magnetically characterized. It crystallizes in the orthorhombic system, space group P212121 with a=7.1618(5), b=9.0356(6), c=10.9740(13) , V=1292.54(15) 3 , D c=1.799 g/cm3 , Mr=350.15, Z=4, F(000)=708, μ=1.064 mm -1 , and the final R=0.0177 and wR=0.0462 for 2273 observed reflections with I > 2σ(I). The unique octahedral Mn Ⅱ ion in 1 is periodically linked into a two-dimensional (2D) magnetic layer by μ2 -N1 , N4 -Htrz and syn, anti-COO of doubly deprotonated Hbtc 2anion, which is further supported by the phenyl backbone of Hbtc 2ligand to generate a 3D pillared-layer framework. Magnetically, complex 1 displays an antiferromagnetic ordering below 5.0 K due to the cooperative antiferromagnetic couplings mediated by the mixed heterobridges within the magnetic layer.  相似文献   

18.
Two new Schiff base complexes of nickle(Ⅱ) [C18H20NiN2O4]·1.5H2O(1) and [C18H20N2NiO4]·H2O(2) were synthesized and characterized by elemental analysis,IR,UV-Vis and X-ray crystal structure analysis.Both 1 and 2 crystallize in the orthorhombic system.Crystal 1:space group Pbcn with a = 12.8591(19),b = 14.779(2),c = 19.749(3) ,V = 3753.3(10) 3,C18H23N2NiO5.5,Mr = 414.07,Z = 8,Dc = 1.445 g/cm3,μ = 1.067 mm-1,F(000) = 1712,S = 1.037,the final R = 0.0741 and wR = 0.2101 for 4353 observed reflections(I > 2σ(I)) and R = 0.1157 and wR = 0.2380 for all data.Crystal 2:space group P21 with a = 9.4673(17),b = 11.559(2),c = 16.347(3) ,V = 1788.9(6) 3,C18H22N2NiO5,Mr = 405.07,Z = 4,Dc = 1.497 g/cm3,μ = 1.116 mm-1,F(000) = 840,S = 1.085,the final R = 0.0330 and wR = 0.0869 for 3151 observed reflections(I > 2σ(I)) and R = 0.0362 and wR = 0.0887 for all data.Each Ni atom of 1 and 2 is six-coordinated with two nitrogen atoms and four oxygen atoms from two salicylidene-2-ethanolamine ligands yielding a distorted octahedral geometry.Dimer structure is observed in the packing diagram of 1.The thermal stability of complex 2 is also studied.  相似文献   

19.
Two new 1,3-oxazin derivatives, C22H24N2O5(3I) and C19H16N2O5(3II), have been synthesized via an unusual cascade reaction. The attractive aspect of this cascade reaction is that the novel construction of 1,3-oxazine and the direct C-N bond formation from C-C bond can be easily achieved via pyridine-mediated acylation in a one-pot operation. Both compounds have been synthesized and characterized by elemental analysis, IR, NMR spectra and X-ray single-crystal diffraction. Compound 3I crystallizes in monoclinic, space group P21/n with a = 16.282(4), b = 7.4117(18), c = 17.256(5) , β = 103.193(9)°, V = 2027.4(9) 3, Mr = 396.43, Z = 4, Dc = 1.299 g/cm3, F(000) = 840, MoKa radiation(λ = 0.71073 ), the final R = 0.0771 and wR = 0.1582 for 3662 were observed reflections with I 2σ(I). Compound 3II crystallizes in triclinic, space group P1 with a = 7.1265(9), b = 10.1071(13), c = 23.529(3), α = 97.463(9), β = 96.981(9), γ = 94.345(9)°, V = 1600.5(4) 3, Z = 4, Dc = 1.409 g/cm3, F(000) = 736, CuKa radiation(λ = 1.54186 ), the final R = 0.0515 and wR = 0.1241 for 4920 observed reflections with I 2σ(I). The preliminary antibacterial activities of 2 and 3 against E. coli and S. aureus were investigated. The results showed that the inhibiting effect of 3 was higher than that of 2.  相似文献   

20.
A new lanthanum coordination polymer formulated as {[La2(pyda) 2(μ4-SO4) ·5H2O]· 2H2O}n(1,H2pyda = 2,6-pyridine-dicarboxylic acid) has been synthesized from the reaction of H2pyda with lanthanide nitrate in the presence of sulfate as a counter anion. The compound was characterized by elemental analysis,IR spectroscopy and X-ray single-crystal diffraction. It crystallizes in the orthorhombic system,space group Pna21,with a = 18.8558(19) ,b = 6.5831(7) and c = 18.7543(19) . The compound is a 2D hybrid,in which the La(Ⅲ) ions were doubly connected by the carboxylic group of pyda2-ligand to form the La(Ⅲ) dimer followed by being grafted into 1D zig-zag chains which are further connected into a 2D network containing {[La(SO4) ]+}n helical chains. The interchain hydrogen bonding and π-π stacking interactions extended the 2D networks into a 3D supramolecular edifice.  相似文献   

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