首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 62 毫秒
1.
The crystal and molecular structure of catena-[(-acetato) (-phthalazine)-silver(I)dihydrate], {[Ag(O2CCH3) (C8H6N2)(H2O)2]2}n, has been determined by single crystal X-ray analysis: the space group is P21/n,a=16.150(8) Å,b=3.886(5) Å,c=18.716(9) Å, =96.02(5)°,V=1168 Å3. Phthalazine (PHZ) bridges the silver atoms to form {Ag--PHZ]2 dimeric subunits. These dimeric subunits are planar and stack by bridging acetates to form a polymeric lattice. The acetates also form an asymrnetric chelate ring with the silver atoms which result in a distorted, square pyramidal configuration. The complex is further characterized by its IR and thermal properties.  相似文献   

2.
The structure of diaquobis--(dimethylsulfoxo)bis(dimethylsulfoxo)dilithium tetraphenyl- borate, [Li2(Me2SO)4(H2O)2][BPh4]2, has been determined at 293 K. The compound crystallizes in the triclinic P-1 space group (a = 11.429(2) Å, b = 14.068(3) Å, c = 19.215(4) Å, = 69.31(3), = 88.98(3), = 89.03(3)). The lithium is coordinated to the oxygens of an aquo ligand, a terminal dimethylsulfoxo ligand, and two bridging dimethylsulfoxo ligands. The coordination geometry of each lithium is significantly distorted from a tetrahedron by the twisting of the plane containing the lithium ion and the two bridging dimethylsulfoxo oxygens relative to the plane containing the lithium ion and the terminal dimethylsulfoxo and aquo oxygen atoms. Hydrogen bonding between the aquo hydrogens and the phenyls of the tetraphenylborate anion is observed but does not result in a polymeric structure as has been observed in other lithium tetraphenylborate salts because of the 1:1 ratio of aquo ligands and tetraphenylborate anions.  相似文献   

3.
The title compound crystallizes in the centrosymmetric triclinic unit cell, a = 6.6662(8) Å, b = 8.8584(6) Å, c = 13.574(2) Å, = 71.468(7)°, = 82.182(9)°, = 75.270(7)°, Z = 1. Refinement converged at R = 0.0396 for 1383 observed reflections. The molecule consists of two W(CO)5 fragments bridged centrosymmetrically by the 2,2,9,9-tetramethyl-3,7-dithiadecane ligand.  相似文献   

4.
[Cu2(bet)4Cl2]Cl2·4H2O (bet = betaine: IUPAC name: trimethylammonioacetate) is monoclinic, space group P21/c, a = 11.0510(10) Å, b = 14.7140(4) Å, c = 11.1620(15) Å, = 107.40(2)°. The dinuclear copper(II) cation [Cu2(bet)4Cl2]2+ is counterbalanced by two naked Cl ions. The copper(II) ions have a square bipyramidal environment with oxygen atoms from the acetato groups in the basal planes and a chlorine and a copper atom occupying the apical positions. The metal atoms are 2-bridged by four acetato groups and the molecular symmetry is close to C 2h. The two symmetry-independent chelating betaine molecules are present in their zwitterionic, neutral form.  相似文献   

5.
[(C2H4N3S) (C2H3N3S) BiI4]; [(HL) (L) BiI4] (L=2-amino-1,3,4-thiadiazole),M r=919.86. monoclinic, P 1 21/a 1,a=7.622(1),b=18.977(2),c=12.821(1) Å, =102.77(1)°, finalR=0.033. The crystals consist of HL+ cations, neutral L molecules and polymeric [BiI4] anions built up of edge-sharing [BiI6]3– octahedra, with Bi–I(bridging) distances in the range 3.320(1)–3.057(1) Å and Bi–I(terminal) distances in the range 2.917(1)–2.929(1) Å. The1H and13C spectra in DMSO-d6 solution are used in conjunction with the X-ray structural results to establish the preferred protonation site of the thiadiazole ring.  相似文献   

6.
The reaction of [Ru3(CO)10(-dppm)] 1 with PPhCl2 in refluxing CHCl3 results in the isolation of [(-H)Ru3(CO)8(-Cl)(-dppm)] 3 in 10% yield. Compound 3, which has been structurally characterized by crystallographic methods, is also formed from the reaction of 1 with H2 in refluxing CCl4. The compound crystallizes in the monoclinic space group P21/c with a = 16.814(2), b = 18.7590(12), c = 11.486(2) Å, = 97.745(11)°, V = 3589.8(8) Å3, and Z = 4. The hydride and chloride ligands bridge the same edge of the triruthenium cluster as the dppm ligand.  相似文献   

7.
The reaction between the dianion [Fe2(CO)6(2-S)2]2– and NiCl2(dppf) occurs readily at room temperature to give the mixed-metal cluster Fe2(CO)6(3-S)2Ni(dppf) in moderate yield. Fe2(CO)6(3-S)2Ni(dppf) was isolated by preparative chromatography and its solid-state structure established by X-ray diffraction analysis. Fe2(CO)6(3-S)2Ni(dppf) crystallizes in the monoclinic space group C2/c, a = 20.320(6), b = 13.114(2), c = 15.622(2) Å, = 110.25(2)°, V = 3905.4(11) Å3, Z = 4, and d calc = 1.630 g/cm.3 The X-ray structure of Fe2(CO)6(3-S)2Ni(dppf) exhibits an Fe2S2Ni arachno polyhedral core, with the pendant dppf ligand attached to an essentially square planar Ni center. The redox chemistry of Fe2(CO)6(3-S)2Ni(dppf) was investigated by cyclic voltammetry which showed a reversible, one-electron oxidation localized on the Fe2S2 core along with an irreversible, one-electron reduction that is antibonding with respect to the Fe—Fe and Fe—S bonds. The electrochemical assignments were confirmed by carrying out extended Hückel MO calculations on the model cluster Fe2(CO)6(3-S)2Ni(H4-dppf).  相似文献   

8.
Treatment of the azavinylidene-bridged cluster Ru3(-H)(-N=CPh2)(CO)10 (1) with the diphosphine ligand bis(dimethylphosphino)ethane (dmpe) gives Ru3( -H)(-N=CPh2)(CO)8(dmpe) (2) in moderate yield, while the ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) reacts with Ru3( -H)(-N=CPh2)(CO)10 in the presence of Me3NO to furnish Ru3( -H)(-N=CPh2)(CO)8(bpcd) (3) in low yield. Each new cluster has been isolated and characterized in solution by IR and NMR (1H and 31P) spectroscopies, and the coordination mode exhibited by the ancillary diphosphine ligand in 2 and 3 has been established by X-ray crystallography. Ru3( -H)(-N=CPh2)(CO)8(dmpe) crystallizes in the monoclinic space group P2(1)/c, a = 10.791(1) Å, b = 16.377(1) Å, c = 18.148(1) Å, = 96.675(2)°, V = 3185.3(4) Å3, Z = 4, D cacl = 1.791 Mg/m3; R = 0.0360, R w = 0.0866 for 7522 observed reflections with I > 2(I). Ru3(-H)(-N=CPh2)(CO)8(bpcd) crystallizes, as the CH2Cl2 solvate, in the triclinic space group , a = 11.956(1) Å, b = 14.228(1) Å, c = 31.409(3) Å, = 89.377(2)°, = 79.344(2)°, = 77.235(2)°, V = 5118.4(8) Å3, Z = 2, D calc = 1.670 Mg/m3; R = 0.0557, R w = 0.1069 for 10977 observed reflections with I > 2(I). The structural details of clusters 2 and 3 are contrasted with Ru3(-H)(-N=CPh2)(CO)7(-dppm)(-dppm), which is the only known structurally characterized phosphine-substituted cluster of this genre.  相似文献   

9.
The title compound, catena-[bis(azido-N)-copper(II)-(bis(2-benzimidazolyl)butane), [Cu(C18H18N4)(N3)2]n, was obtained from the reaction of the ligand bis(2-benzimidazolyl)butane and Cu(N3)2. The x-ray crystal structure is reported. The compound crystallizes in the monoclinic space group P21/c with a = 8.2524(10), b = 12.765(5), c = 9.1125(15) Å, = 106.423(12)°, Z = 2. The Cu(II) ions are square-planar coordinated with trans-oriented end-on binding azido ligands. The structure is a polynuclear chain with the benzimidazole bridging at each end. In addition a N(ligand)-H···N(azido) H-bridge [N(ligand)···N(azido) = 2.994(7) Å] is present, resulting in a pseudo 2-dimensional lattice. The characteristic azido infrared vibrations are found at 2060 and 2077 cm–1 (as(N3)) and 1284 and 1297 cm–1 ((N3)).  相似文献   

10.
The reaction of equal millimolar quantities of CdBr2 and 2-hydroxyethyl sulfide in 31 CH3CNCH3OH produced [Cd(OH2)2(Br)4 (Cd(2-hydroxy ethyl sulfide) (-Br))2]n. The compound crystallizes as a bromide-bridged polymer with hydrogen bonding interactions between the polymeric chains. Each of the two unique metal centers has a distorted octahedral geometry. The thioether ligand is bidentate to one cadmium position with one alcoholic terminus uncoordinated. The uncoordinated portion of the molecule is disordered with each conformation participating in slightly different hydrogen bonding environments. The other unique cadmium center is coordinated to four bridging bromides and twotrans water molecules.  相似文献   

11.

Abstract  

Tetrakis-(μ2-phenylacetato-O,O′)-bis(caprolactam-O)copper(II) (1) was synthesized and characterized by X-ray crystallography, magnetic susceptibility and FT-IR spectroscopy. The title compound (1) crystallized in the monoclinic space group P21/n with unit cell parameters a = 18.2242(4) ?, b = 10.0994(2) ?, c = 23.0696(5) ?, β = 101.117(2)°; V = 4166.37(15) ?3; Z = 4. The molecular structure of (1) consists of a copper dimer bridged by four phenylacetate ligands in the paddlewheel geometry with caprolactam coordinated in both axial sites. The copper dimers of (1) are organized into one-dimensional columns by N–H···O interactions between bound caprolactam ligands. Magnetic susceptibility studies indicate antiferromagnetic coupling between the Cu+2 ions with a singlet ground-state and triplet excited-state separated by |2J = 319(1) cm−1 |.  相似文献   

12.
The triruthenium cluster ( -H)Ru3( 33-CHCHCMe)(CO)9 reacts with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) in the presence of Me3NO to afford ( -H)Ru3( 33-CHCHCMe)(CO)7(bpcd) in moderate yield. This new cluster has been isolated and characterized in solution by IR and NMR (1H, 31P) spectroscopies, and the solid-state structure has been established by X-ray crystallography. ( -H)Ru3( 33-CHCHCMe)(CO)7(bpcd) MeOH crystallizes in the triclinic space group P , a = 11.2426(8) Å, b = 11.7141(8) Å, c = 16.195(1) Å, = 102.041(5)°, = 95.128(5)°, = 102.553(6)°, V = 2008.4(3) Å3, Z = 2, d calc. = 1.733 g/cm3; R = 0.0488, R w = 0.0546 for 2212 observed reflections with I > 3 (I). The X-ray structure reveals that the bpcd ligand is bound exclusively to the Ru3 core at the ruthenium center coordinated by the terminal CH unit of the -allylic 33-CHCHCMe moiety.  相似文献   

13.
Crystals of [Co(C2H8N2)2(C3H6NO2)]PbCl4 · H2O [a = 7.627(1) Å, b = 11.238(1) Å, c = 11.444(1) Å, α = 99.125(1)°, β = 103.80(1)°, γ = 94.739(1)°, V = 933.09(1) Å3, Z = 2, and space group $P\bar 1$ ] contain the octahedral PbCl6 groups that share edges to form infinite [Cl2Pb(μ-Cl)2] n 2n chains, in which the terminal Cl atoms occupy the cis positions. The Pb-Cl bond lengths are 2.763(1)–3.180(3) Å. In the discrete cationic complexes, the Co atom is coordinated by two ethylenediamine molecules and the 3-aminopropionate anion. In the enantiomeric complex with the Δ absolute configuration, the ethylenediamine rings have the λ and δ configurations and the aminopropionate ring has the λ configuration.  相似文献   

14.
Reaction of CuSCN with 2,5-dimethylpyrazine (2,5-me2pyz) yields a polymeric material, [Cu2(SCN)2(2,5-me2pyz)], which has been crystallographically characterized. The compound crystallizes in the monoclinic space group P21/N with a = 5.6850(2) Å, b = 6.92877(3) Å, c = 14.3575(6) Å, = 93.435(1), and Z = 2. It contains [Cu(SCN)] sheets in which each thiocyanate ligand acts in a -N,S,S-bridging mode. The sheets are bridged by 2,5-dimethylpyrazine ligands to generate a three dimensional network. The compound has also been characterized by infrared spectroscopy and thermogravimetric analysis.  相似文献   

15.
The reaction of the terminal alkyne methyl propiolate with the heterometallic dimers CoRu(CO)7(μ-PPh2) (1) and CoRu(CO)5[(Z)-Ph2PCH=CHPPh2](μ-PPh2) (2) has been investigated at 65°C in toluene. In the reaction of 1, chromatographic purification afforded a minor band, from which the two species RuCo(CO)4(μ-CO)[μ-PPh2C(O)CHC(CO2Me)] and RuCo(CO)4(μ-CO)[μ-PPh2CHC(CO2Me)] were observed by 1H NMR spectroscopy, and one major band, whose 1H NMR spectrum revealed the presence of multiple species. The identity of one of the compounds in the major component has been established as that of CoRu(CO)4(μ-CO)[μ-PPh2C(O)CH(CCO2Me)C(O)CHC(CO2Me)] (3) by X-ray diffraction analysis. The solid-state structure of 3 confirms the double insertion of CO and head-to-head coupling of the methyl propiolate that accompanies the formation of this product. Compound 3 crystallizes in the triclinic space group P-1, a = 8.4035(4), b = 9.6721(5), c = 17.678(1) Å, α = 94.135(2), β = 103.318(2), γ = 101.336(2)°, V = 1360.5(1) Å3, Z = 2, D calc = 1.732 Mg/m3; R = 0.0300, R w = 0.0760 for 8630 reflections with I > 2σ(I). The ruthenium-bound diphosphine ligand in 2 exerts a controlling influence on the reaction with added alkyne insomuch as only the mono-insertion product CoRu(CO)3(μ-CO)[(Z)-Ph2PCH=CHPPh2][μ-PPh2C(O)C(CO2Me)CH] (4) is formed as a single regioisomer. The molecular structure of 4 was established by X-ray diffraction analysis and 4 was found to crystallize in the monoclinic space group P21/c, a = 19.483(7), b = 11.905(4), c = 20.131(7) Å, β = 110.455(6)°, V = 4375(3) Å3, Z = 4, D calc = 1.466 Mg/m3; R = 0.0961, R w = 0.1683 for 6262 reflections with I > 2σ(I). The reactivity of methyl propiolate with 1 and 2 is compared with the known reactivity that has been reported for other alkynes.  相似文献   

16.
The title compound, [Cu2(II)(4-Cl-3-NO2–C6H3CO2)4(CH3OH)2] or [Cu2(4-chloro-3-nitrobenzoate)4(MeOH)2] has been prepared and its structure determined using X-ray crystallography. The complex crystallizes in the triclinic space group P-1 with a = 9.6887(9)Å, b = 10.6448(9)Å, c = 11.4194(10)Å, = 108.094(2), = 110.682(2), = 105.055(2), V = 952.691(15)Å3, and Z = 1. The structure consists of centrosymmetric dimers in which the Cu(II) atoms display a square pyramidal CuO5 coordination, with four carboxylate O atoms in the basal plane [CuO 1.951(2)–1.968(2)Å] and the methanol O atoms in the apical position [CuO 2.170(2)Å]. The Cu atoms are 2.614(1)Å apart and are bridged by four benzoate groups. The discrete dimers are extended into 1D chains that result from hydrogen bonding between the coordinated methanol on one Cu(II) dimer and the nitro substituent on an adjacent Cu(II) dimer. The chains are interdigited and held by – stacking interactions forming 3D supramolecular array.  相似文献   

17.
The reaction between the tricobalt cluster Co3(CO)9(3-CCl) (1) and AlCl3, followed by treatment with ethyl diazoacetate, N2CHCO2Et, affords a complex mixture of products in low yields. Column chromatography has allowed the isolation of the four cluster compounds Co3(CO)9(3-CH) (2), Co3(CO)9(3-CCO2Et) (3), Co3(CO)9(3-CCH2CO2Et) (4), and [Co3(CO)9(3-CCHCO2Et)]2 (5). Clusters 4 and 5 are new and have been fully characterized in solution by IR and 1H NMR spectroscopy. The molecular structures of clusters 3–5 have also been determined by single-crystal X-ray diffraction analysis. Co3(CO)9(3-CCO2Et) crystallizes in the triclinic space group P , a = 8.8393(5), b = 14.727(1), c = 15.272(1) Å, = 93.361(6), = 105.509(5)°, = 100.336(6)°, V = 1872.6(2) Å3, Z = 4, and d calc = 1.823 g/cm3. Co3(CO)9(3-CCH2CO2Et) crystallizes in the monoclinic space group P21/n, a = 9.3806(7), b = 9.2617(8), c = 22.455(2) Å, = 94.483(7)°, V = 1944.9(3) Å3, Z = 4, and d calc = 1.803 g/cm3. [Co3(CO)9(3-CCHCO2Et)]2 crystallizes in the monoclinic space group C2/c, a = 21.585(2), b = 8.7977(7), c = 20.784(1) Å, = 104.807(6)°, V = 3815.8(5) Å3, Z = 4, and d calc = 1.835 g/cm3. Plausible pathways leading to the formation of clusters 2, 4, and 5 are discussed.  相似文献   

18.
Abstract  The complex, [Mn6O2(OOCCMe3)10(HOOCCMe3)3(py)], has a hexanuclear structure with a Mn6O2 core. This complex crystallizes in the monoclinic space group P21/n with a = 17.757(5) ?, b = 27.413(5) ?, c = 22.348(5) ?, β = 90.233(5)°, V = 9,040(4) ?3 and Z = 4. It contains a [Mn6O2]10+ core that can be described as two edge-sharing Mn4 tetrahedra at the centre of each of which tetrahedron lies a μ4-O2− ion. All Mn atoms are six-coordinate and possess distorted octahedral geometry. Mn4 exhibits butterfly arrangement with both μ4-O atoms on the same side of the molecule. The complex is mixed-valence , and the MnIII centers are assigned as the two central metal ions bridged by two O2− ions. Index abstract  The complex, [Mn6O2(OOCCMe3)10(HOOCCMe3)3(py)], has a hexanuclear structure with a Mn6O2 core. This complex crystallizes in the monoclinic space group P21/n with a = 17.757(5) ?, b = 27.413(5) ?, c = 22.348(5) ?, β = 90.233(5)°, V = 9040(4) ?3 and Z = 4. It contains a [Mn6O2]10+ core that can be described as two edge-sharing Mn4 tetrahedra at the centre of each of which tetrahedron lies a μ4-O2− ion. All Mn atoms are six-coordinate and possess distorted octahedral geometry. Mn4 exhibits butterfly arrangement with both μ4-O atoms on the same side of the molecule. The complex is mixed-valence , and the MnIII centers are assigned as the two central metal ions bridged by two O2− ions.   相似文献   

19.
The barium salt of 1-oxyethylidenediphosphonatohydroxogermanium acid Ba3[Ge(μ-OH)(μ-Oedph)]6 · 25H2O (I) (H4Oedph is 1-oxyethylidenediphosphonic acid) was synthesized and studied by X-ray diffraction. The complex was characterized by elemental analysis, thermogravimetry, and IR spectroscopy. The hexanuclear cyclic complex anions [Ge(μ-OH)(μ-Oedph)] 6 6-t- ] cations, and water molecules of crystallization are the structural units of the crystal of I.  相似文献   

20.

Abstract  

Complexes [Zn(NCS)2(2-AMP)2] (2-AMP = 2-aminopyrimidine) 1 and [Cd(SCN)2(2-AMP)2]n 2 are prepared and characterized by X-ray crystallographic methods. 1 crystallizes in the monoclinic, space group C2/c, with a = 13.5761(14), b = 8.3330(10), c = 13.5962(15) ?, β = 99.5450(10)°, V = 1516.8(3) ?3, Z = 4. In 1, the zinc atom is coordinated by four N atoms from two AMP and two NCS. 2 crystallizes in the monoclinic, space group C2/c, with a = 9.7259(11), b = 19.332(2), c = 8.2149(9) ?, β = 99.817(2)°, V = 1522.0(3) ?3, Z = 4. Complex 2 is made up of 1D chains along a-axis. Each Cd is attached to four NCS bridges and two pendant 2-AMP ligands.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号