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 31 毫秒
1.
The ammoniates [K(18‐crown‐6)(NH3)2]3Sb11 · 5.5NH3 ( 1 ) and [Cs(18‐crown‐6)]2CsAs11 · 8NH3 ( 2 ) (18‐crown‐6 = 18C6: 1,4,7,10,13,16‐Hexaoxacyclooctadecan) were synthesized by either the reaction of K3Sb7 with SbPh3 in liquid ammonia or by extraction of Cs3As11 with liquid ammonia. Single crystals were isolated and characterized by low temperature X‐ray structure analysis. [K(18‐crown‐6)(NH3)2]3Sb11 · 5.5NH3 crystallizes in the space group with a = 13.31(2) Å, b = 15.161(2) Å, c = 22.521(3) Å, α = 99.23(1)°, β = 100.99(1)° and γ = 105.03(1)°. [Cs(18‐crown‐6)]2CsAs11 · 8NH3 crystallizes in the monoclinic space group C2/c with a = 20.009(3) Å, b = 17.024(1) Å, c = 19.838(2) Å and β = 119.732(9)°. While 1 contains isolated [Sb11]3? anions and [K(18‐crown‐6)(NH3)2]+ complexes, cesium–arsenic contacts lead to one–dimensionally infinite chains in 2 .  相似文献   

2.
Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of K2[IrCl5(NH3)] The X-ray structure determination of K2[IrCl5(NH3)] (orthorhombic, space group Pnma, a = 13.426(4), b = 10.015(2), c = 6.8717(7) Å, Z = 4) revealed the Cs point symmetry of the complex anion [IrCl5(NH3)]2? (Ir? Cl = 2.337–2.365, Ir? N = 2.067(10); N? H = 0.73–0.79 Å). Using the molecular parameters the IR and Raman spectra are assigned by normal coordinate analysis. The valence force constants are fd(NH) = 5.88, fd(IrN) = 2.66, fd(IrCl) = 1.68 mdyn/Å.  相似文献   

3.
The compound [NH4(NH3)4][Co(C2B9H11)2] · 2 NH3 ( 1 ) was prepared by the reaction of Na[Co(C2B9H11)2] with a proton‐charged ion‐exchange resin in liquid ammonia. The ammoniate 1 was characterized by low temperature single‐crystal X‐ray structure analysis. The anionic part of the structure consists of [Co(C2B9H11)2] complexes, which are connected via C‐H···H‐B dihydrogen bonds. Furthermore, 1 contains an infinite equation/tex2gif-stack-2.gif[{NH4(NH3)4}+(μ‐NH3)2] cationic chain, which is formed by [NH4(NH3)4]+ ions linked by two ammonia molecules. The N‐H···N hydrogen bonds range from 1.92 to 2.71Å (DHA = Donor···Acceptor angles: 136‐176°). Additional N‐H···H‐B dihydrogen bonds are observed (H···H: 2.3‐2.4Å).  相似文献   

4.
The reaction of ammonium heptamolybdate with hydrazine sulfate in an aqueous solution of glycine at room temperature yielded colorless crystals of (NH4)4[(NH3CH2CO)2(Mo8O28)] · 2 H2O. The crystal is monoclinic, space group C2/c (no. 15), a = 17.234 Å, b = 10.6892 Å, c = 18.598 Å, β = 108.280°, V = 3253.2 Å3, Z = 4. The crystal structure contains ammonium cations and isolated octamolybdate(4–) anions, [(NH3CH2CO)2(Mo8O28)]4–, with two zwitterionic glycine molecules as ligands.  相似文献   

5.
Conformation and Cross Linking of (CuCN)6‐Rings in Polymeric Cyanocuprates(I) equation/tex2gif-stack-8.gif [Cu2(CN)3] (n = 2, 3) The alkaline‐tricyano‐dicuprates(I) Rbequation/tex2gif-stack-9.gif[Cu2(CN)3] · H2O ( 1 ) and Csequation/tex2gif-stack-10.gif[Cu2(CN)3] · H2O ( 2 ) were synthesized by hydrothermal reaction of CuCN and RbCN or CsCN. The dialkylammonium‐tricyano‐dicuprates(I) [NH2(Me)2]equation/tex2gif-stack-11.gif[Cu2(CN)3] ( 3 ), [NH2(iPr)2]equation/tex2gif-stack-12.gif[Cu2(CN)3] ( 4 ), [NH2(Pr)2]equation/tex2gif-stack-13.gif[Cu2(CN)3] ( 5 ) and [NH2(secBu)2]equation/tex2gif-stack-14.gif[Cu2(CN)3] ( 6 ) were obtained by the reaction of dimethylamine, diisopropylamine, dipropylamine or di‐sec‐butylamine with CuCN and NaCN in the presence of formic acid. The crystal structures of these compounds are built up by (CuCN)6‐rings with varying conformations, which are connected to layers ( 1 ) or three‐dimensional zeolite type cyanocuprate(I) frameworks, depending on the size and shape of the cations ( 2 to 6 ). Crystal structure data: 1 , monoclinic, P21/c, a = 12.021(3)Å, b = 8.396(2)Å, c = 7.483(2)Å, β = 95.853(5)°, V = 751.4(3)Å3, Z = 4, dc = 2.728 gcm—1, R1 = 0.036; 2 , orthorhombic, Pbca, a = 8.760(2)Å, b = 6.781(2)Å, c = 27.113(5)Å, V = 1610.5(5)Å3, Z = 8, dc = 2.937 gcm—1, R1 = 0.028; 3 , orthorhombic, Pna21, a = 13.504(3)Å, b = 7.445(2)Å, c = 8.206(2)Å, V = 825.0(3)Å3, Z = 4, dc = 2.023 gcm—1, R1 = 0.022; 4 , orthorhombic, Pbca, a = 12.848(6)Å, b = 13.370(7)Å, c = 13.967(7)Å, V = 2399(2)Å3, Z = 8, dc = 1.702 gcm—1, R1 = 0.022; 5 , monoclinic, P21/n, a = 8.079(3)Å, b = 14.550(5)Å, c = 11.012(4)Å, β = 99.282(8)°, V = 1277.6(8)Å3, Z = 4, dc = 1.598 gcm—1, R1 = 0.039; 6 , monoclinic, P21/c, a = 16.215(4)Å, b = 13.977(4)Å, c = 14.176(4)Å, β = 114.555(5)°, V = 2922(2)Å3, Z = 8, dc = 1.525 gcm—1, R1 = 0.070.  相似文献   

6.
Crystals of the zwitterionic copper(I) π‐complex [(HC≡CCH2NH3)Cu2Br3] have been synthesized by interaction of CuBr with [HC≡CCH2NH3]Br in aqueous solution (pH < 1) and X‐ray studied. The crystals are monoclinic: space group P21/n, a = 6.722(4), b = 12.818(8), c = 9.907(3) Å, β = 100.25(4)°, V = 840.0(8) Å3, Z = 4, R = 0.0592 for 3015 reflections. The crystal structure of the π‐complex contains isolated [(HC≡CCH2NH3)+(Cu2Br3)?]2 units which are incorporated into a framework by strong hydrogen N–H···Br and C≡C–H···Br bonds. The length of π‐coordinated propargylammonium C≡C bond is equal 1.216(8) Å and Cu(I)–(C≡C) distance equals 1.958(5) Å.  相似文献   

7.
A one‐dimensional aluminum phosphate, [NH3(CH2)2NH2(CH2)3NH3]3+ [Al(PO4)2]3—, has been synthesized hydrothermally in the presence of N‐(2‐Aminoethyl‐)1, 3‐diaminopropane (AEDAP) and its structure determined by single crystal X‐ray diffraction. Crystal data: space group = Pbca (no. 61), a = 16.850(2), b = 8.832(1), c = 17.688(4)Å, V = 2632.4(2)Å3, Z = 8, R1 = 0.0389 [5663 observed reflections with I > 2σ(I)]. The structure consists of anionic [Al(PO4)2]3— chains built up from AlO4 and PO4 tetrahedra, in which all the AlO4 vertices are shared and each PO4 tetrahedron possesses two terminal P=O linkages. The cations, which balances the negative charge of the chains, are located in between the chains and interact with the oxygen atoms through strong N—H···O hydrogen bonds. Additional characterization of the compound by powder XRD and MAS‐NMR has also been performed and described.  相似文献   

8.
The hydrothermal reaction of VOSO4, As2O5, piperazine and H2O produces [H2N(CH2)4NH2]4[β‐As8V14O42(SO4)]·2HSO4 ( 1 ), which is the first arsenic‐vanadium cluster containing a spherical β‐As8V14O42 shell. The structure of this compound was characterized by single crystal X‐ray diffraction, elemental analysis, TG, and IR spectrum. Crystal data for 1 : Orthorhombic, Cmcm, a = 15.369(1) Å, b = 16.404(1) Å, c = 25.772(1) Å, V = 6497.4(9) Å3, Z = 4.  相似文献   

9.
The blue copper complex compounds [Cu(phen)2(C6H8O4)] · 4.5 H2O ( 1 ) and [(Cu2(phen)2Cl2)(C6H8O4)] · 4 H2O ( 2 ) were synthesized from CuCl2, 1,10‐phenanthroline (phen) and adipic acid in CH3OH/H2O solutions. [Cu(phen)2‐ (C6H8O4)] complexes and hydrogen bonded H2O molecules form the crystal structure of ( 1 ) (P1 (no. 2), a = 10.086(2) Å, b = 11.470(2) Å, c = 16.523(3) Å, α = 99.80(1)°, β = 115.13(1)°, γ = 115.13(1)°, V = 1617.5(5) Å3, Z = 2). The Cu atoms are square‐pyramidally coordinated by four N atoms of the phen ligands and one O atom of the adipate anion (d(Cu–O) = 1.989 Å, d(Cu–N) = 2.032–2.040 Å, axial d(Cu–N) = 2.235 Å). π‐π stacking interactions between phen ligands are responsible for the formation of supramolecular assemblies of [Cu(phen)2(C6H8O4)] complex molecules into 1 D chains along [111]. The crystal structure of ( 2 ) shows polymeric [(Cu2(phen)2Cl2)(C6H8O4)2/2] chains (P1 (no. 2), a = 7.013(1) Å, b = 10.376(1) Å, c = 11.372(3) Å, α = 73.64(1)°, β = 78.15(2)°, γ = 81.44(1)°, V = 773.5(2) Å3, Z = 1). The Cu atoms are fivefold coordinated by two Cl atoms, two N atoms of phen ligands and one O atom of the adipate anion, forming [CuCl2N2O] square pyramids with an axial Cl atom (d(Cu–O) = 1.958 Å, d(Cu–N) = 2.017–2.033 Å, d(Cu–Cl) = 2.281 Å; axial d(Cu–Cl) = 2.724 Å). Two square pyramids are condensed via the common Cl–Cl edge to centrosymmetric [Cu2Cl2N4O2] dimers, which are connected via the adipate anions to form the [(Cu2(phen)2Cl2)(C6H8O4)2/2] chains. The supramolecular 3 D network results from π‐π stacking interactions between the chains. H2O molecules are located in tunnels.  相似文献   

10.
Potassium Amido Trioxo Germanates(IV) – Hydrogen Bridge Bonds in K3GeO3NH2 and K3GeO3NH2 · KNH2 Colorless crystals of K3GeO3NH2 and of K3GeO3NH2 · KNH2 were obtained by the reaction of KNH2 with GeO2 in supercritical ammonia at 450°C and p = 6 kbar in high-pressure autoclaves within 15 resp. 5 days. The crystal structures of both compounds were solved by X-ray single crystal methods. K3GeO3NH2: P1 , a = 6.390(1) Å, b = 6.684(1) Å, c = 7.206(1) Å, α = 96.47(1)°, β = 101.66(1)°, γ = 91.66(1)°, Z = 2, R/Rw = 0.020/0.022, N(I) ≥ 2σ(I) = 3023, N(Var.) = 82 K3GeO3NH2 · KNH2: P21/c, a = 10.982(6) Å, b = 6.429(1) Å, c = 12.256(8) Å, β = 106.12(1)°, Z = 4, R/Rw = 0.022/0.029, N(F) ≥ 3σ(F) = 1745, N(Var.) = 107. In K3GeO3NH2 tetrahedral ions GeO3NH23? are connected to chains by N? H …? O bridge bonds with 2.18 Å ≤ d(H …? O) ≤ 2.40 Å for d(N? H) ? 1.0 Å and by potassium ions while in K3GeO3NH2 · KNH2 bridge bonds between NH2 groups of GeO3NH23? and NH2? ions as acceptors occur with 2.41 Å ≤ d((N? )H …? NH2?) ≤ 2.61 Å for d(N? H) ? 1.0 Å.  相似文献   

11.
Reactions of rubidium or barium salts of the ortho‐selenostannate anion, [Rb4(H2O)4][SnSe4] ( 1 ) or [Ba2(H2O)5][SnSe4] ( 2 ) with Zn(OAc)2 or ZnCl2 in aqueous solution yielded two novel compounds with different ternary Zn/Sn/Se anions, [Rb10(H2O)14.5][Zn4(μ4‐Se)2(SnSe4)4] ( 3 ) and [Ba5(H2O)32][Zn5Sn(μ3‐Se)4(SnSe4)4] ( 4 ). 1 – 4 have been determined by means of single crystal X‐ray diffraction: 1 : triclinic space group lattice dimensions at 203 K: a = 8.2582(17) Å, b = 10.634(2) Å, c = 10.922(2) Å, α = 110.16(3)°, β = 91.74(3)°, γ = 97.86(3)°, V = 888.8(3) Å3; R1 [I > 2σ(I)] = 0.0669; wR2 = 0.1619; 2 : orthorhombic space group Pnma; lattice dimensions at 203 K: a = 17.828(4) Å, b = 11.101(2) Å, c = 6.7784(14) Å, V = 1341.5(5) Å3; R1 [I > 2σ(I)] = 0.0561; wR2 = 0.1523; 3 : triclinic space group ; lattice dimension at 203 K: a = 17.431(4) Å, b = 17.459(4) Å, c = 22.730(5) Å, α = 105.82(3)°, β = 99.17(3)°, γ = 90.06(3)°, V = 6563.1(2) Å3; R1 [I > 2σ(I)] = 0.0822; wR2 = 0.1782; 4 : monoclinic space group P21/c; lattice dimensions at 203 K: a = 25.231(5) Å, b = 24.776(5) Å, c = 25.396(5) Å, β = 106.59(3)°, V = 15215.0(5) Å3; R1 [I > 2σ(I)] = 0.0767; wR2 = 0.1734. The results serve to underline the crucial role of the counterion for the type of ternary anion to be observed in the crystal. Whereas Rb+(aq) stabilizes a P1‐type Zn/Sn/Se supertetrahedron in 3 like K+, the Ba2+(aq) ions better fit to an anionic T3‐type Zn/Sn/Se cluster arrangement as do Na+ ions. It is possible to estimate a radius:charge ratio for the stabilization of the two structural motifs.  相似文献   

12.
>From Small Fragments to New Poly‐alkoxo‐oxo‐metalate Derivatives: Syntheses and Crystal Structures of K4[VIV12O12(OCH3)16(C4O4)6], Cs10[VIV24O24(OCH3)32(C4O4)12][VIV8O8(OCH3)16(C2O4)], and M2[VIV8O8(OCH3)16(VIVOF4)] (M = [N(nBu)4] or [NEt4]) By solvothermal reaction of ortho‐vanadicacid ester [VO(OMe)3] with squaric acid and potassium or caesium hydroxide the compounds K4[VIV12O12(OCH3)16(C4O4)6] ( 2 ) and Cs10[VIV24O24(OCH3)32(C4O4)12][VIV8O8(OCH3)16(C2O4)] ( 3 ) could be syntesized. With tetra‐n‐butyl‐ or tetra‐n‐ethylammonium fluoride [N(nBu)4]2[VIV8O8(OCH3)16(VIVOF4)] ( 4 ) and [N(Et)4]2[VIV8O8(OCH3)16(VIVOF4)] ( 5 ) could be isolated. In 2 and 3 the corners of a tetrahedron or cube resp. are occupied by {(VO)3(OMe)4} groups and connected along the edges of the tetrahedron resp. cube by six or twelve resp. squarato‐groups. The octanuclear anions in the compounds 3 , 4 , and 5 are assumedly built up by fragments of the ortho‐vanadicacid ester [VO(OMe)3]. Around the anions C2O42— or VOF4 these oligormeric chains are closed to a ring . Crystal data: 2 , tetragonal, P43, a = 18.166(3)Å, c = 29.165(7)Å, V = 9625(3)Å3, Z = 4, dc = 1.469 gcm—3; 3 , orthorhombic, Pbca, a = 29.493(5)Å, b = 25.564(4)Å, c = 31.076Å, V = 23430(6)Å3, Z = 4, dc = 1.892 gcm—3; 4 , monoclinic, P21/n, a = 9.528(1)Å, b = 23.021(2)Å, c = 19.303(2)Å, β = 92.570(2)°, V = 4229.8(5)Å3, Z = 2, dc = 1.391 gcm—3; 5 , monoclinic, P21/n, a = 16.451(2)Å, b = 8.806(1)Å, c = 23.812(1)Å, β = 102.423(2)°, V = 3368.7(6)Å3, Z = 2, dc = 1.534 gcm—3.  相似文献   

13.
The novel compound K2Na[InSb2] was synthesized from the elements at 900 K in sealed niobium ampoules. The compound forms plate-like crystals with silver metallic luster, which are very unstable in air and moisture. The crystal structure of K2NaInSb2 has been determined using single-crystal X-ray diffraction methods (space group Cmca (No. 64); a = 14.032(2), b = 16.399(3), c = 7.009(1) Å; Z = 8; Pearson symbol oC48). The structure contains pairs of edge-sharing InSb4 tetrahedra which are linked to four other pairs via common vertices and form a two-dimensional [In2Sb2Sb4/2]6? anionic partial structure. The resulting pairs of tetrahedral holes are filled by Na+ cations. These [In2Sb2Sb4/2]6? layers are stacked along the b-axis and are interconnected by K+ cations. The whole structure can be considered as an ordered derivative of the KMnP structure (PbFCl type).  相似文献   

14.
The title compound was prepared by the reaction of Mo_3S_4(dtp)_4(H_2O)[ctp=S_2P(OEt)_2]with NaOAc·3H_2O and C_4H_8NCS_2NH_4.Crystallographic data:[Mo_3(μ_3-S)(μ-S)_2(μ-OAc)-(S_2CNC_4H_8)_3(O)_2]·0.5CH_2CI_2·2H_2O,Mr=980.18,triclinic,space group P,α=12.360(3),b=16.653(6),c=9.206(2)A,α=101.97(2),β=108.32(2),γ=86.14(3)°.V=1759.6(9)A~3,Z=2,Dc=1.85 g/cm~3,F(000)=962,μ(Mo K_α)=16.53 cm~(-1).Final R=0.044 for 4301 reflections with I≥3σ(I).This compoundmay be regarded as a mixed-valent trinuclear molybdenum cluster{Mo_2(V)Mo(Ⅳ)(μ_3-S)(μ-S)_2-(μ-OAc)(S_2CNC_4H_8)_3(O)_2}.The Mo-Mo distances are 2.783(1),2.833(1)and 3.374(2)A in the Mo_3non-equilateral triangle and there exist only two Mo-Mo bonds.The cluster was obtained by oxi-dation and ligand substitution of{Mo_3(μ_3-S)(μ-S)_3[μ-S_2P(OEt_2)][S_2P(OEt)_2]_3(H_2O)}.  相似文献   

15.
A solution of sodium in liquid ammonia reacts with Sb2S3 to form large colorless crystals of the composition Na3SbS3⋅10 NH3. The trigonal‐pyramidal SbS33− anion is ion‐paired with three Na+ counter ions, the coordination spheres of which are completed by eight ammine ligands. The resulting neutral [Na(NH3)3]2[Na(NH3)2]SbS3 molecules crystallize together with two ammonia molecules of solvation in the space group P21/c (a=9.828(2), b=6.0702(4), c=33.4377(6) Å, β=91.362(7)°, V=1994.2(5) Å3, Z=4).  相似文献   

16.
Crystal Structures of Octacyanomolybdates(IV). IV Dodecahedral [Mo(CN)8] Coordination of the Cyano‐Bridged Cobalt and Nickel Ammin Complexes MII2(NH3)8[Mo(CN)8] · 1.5 H2O (MII = Co, Ni) and Ni2(NH3)9[Mo(CN)8] · 2 H2O At single crystals of the hydrated cyano complexes Co2(NH3)8[Mo(CN)8] · 1.5 H2O (a = 910.0(4), b = 1671(2), c = 1501(1) pm, β = 93.76(6)°) and Ni2(NH3)8[Mo(CN)8] · 1.5 H2O (a = 899.9(9), b = 1654.7(4), c = 1488(1) pm, β = 94.01°), isostructurally crystallizing in space group P21/c, Z = 4, and of trigonal Ni2(NH3)9[Mo(CN)8] · 2 H2O (a = 955.1(1), c = 2326.7(7) pm, P31, Z = 3), X‐ray structure determinations were performed at 168 resp. 153 K. The [Mo(CN)8]4– groups of the three compounds, prepared at about 275 K and easily decomposing, show but slightly distorted dodecahedral coordination (mean distances Mo–C: 216.3, 215.4 and 216.1 pm). Within the monoclinic complexes the anions twodimensionally form cyano bridges to the ammin cations [M(NH3)4]2+ and are connected with the resulting [MN6] octahedra (Co–N: 215.1 pm, Ni–N: 209.8 pm) into strongly puckered layers. The trigonal complex exhibits a chain structure, as one [Ni(NH3)5]2+ cation is only bound as terminal octahedron (Ni–N: 212.0 pm). Details and the influence of hydrogen bridges are discussed.  相似文献   

17.
Two new hybrid fluorides, {[(C2H4NH3)3NH]4+}2 · (H3O)+ · [Al7F30]9– ( I ) and {[(C2H4NH3)3NH]4+}2 · [Al7F29]8– · (H2O)2 ( II ), are synthesized by solvothermal method. The structure determinations are performed by single crystal technique. The symmetry of both crystals is triclinic, sp. gr. P 1, I : a = 9.1111(6) Å, b = 10.2652(8) Å, c = 11.3302(8) Å, α = 110.746(7)°, β = 102.02(1)°, γ = 103.035(4)°, V = 915.9(3) Å3, Z = 1, R = 0.0489, Rw = 0.0654 for 2659 reflections, II : a = 8.438(2) Å, b = 10.125(2) Å, c = 10.853(4) Å, α = 106.56(2)°, β = 96.48(4)°, γ = 94.02(2)°, V = 877.9(9) Å3, Z = 1, R = 0.0327, Rw = 0.0411 for 3185 reflections. In I , seven corner‐sharing AlF6 octahedra form a [Al7F30]9– anion with pseudo 3 symmetry; such units are found in the pyrochlore structure. The aluminum atoms lie at the corners of two tetrahedra, linked by a common vertex. In II , similar heptamers are linked in order to build infinite (Al7F29)n8– chains oriented along a axis. In both compounds, organic moieties are tetra protonated and establish a system of hydrogen bonds N–H…F with four Al7F309– heptamers in I and with three inorganic chains in II .  相似文献   

18.
Synthesis and Molecular Structure of [Al(SiMe3)3(DBU)] (DBU = 1,8-Diazabicyclo[5.4.0]undec-7-ene) [Al(SiMe3)3(OEt2)] reacts with DBU (DBU = 1,8-diazabicyclo[5.4.0]undec-7-ene) at 0 °C yielding [Al(SiMe3)3 · (DBU)] ( 1 ). 1 was characterised spectroscopically (1H, 13C, 29Si, 27Al NMR, IR, MS) and by X-ray structure determination [monoclinic, C2/c, a = 33.053(2), b = 9.307(1), c = 20.810(1) Å, β = 124.07(2)°, V = 5302.4(5) Å3, Z = 8, 218(2) K]. 1 does not react with [Cp2ZrCl2] even in boiling toluene.  相似文献   

19.
Colourless block‐shaped crystals of [(NH4)2(2.2.2‐cryptand)2][P2S8] ( 1 ) and [(NH4)2(18‐crown‐6)2][P2S8]·H2O ( 2 ) could be obtained by the reaction of an aqueous solution of ammonium hexathiohypodiphosphate, (NH4)4P2S6·2 H2O, with sulfur and 2.2.2‐cryptand or 18‐crown‐6. The crystal structures of both compounds have been determined by single‐crystal X‐Ray diffraction analysis. Compound 1 crystallizes in the monoclinic space group C2/c with a = 2032.7(2), b = 1243.6(2), c = 2244.6(2) pm, β = 98.64(1)°, and Z = 8, whereas compound 2 crystallizes also monoclinic in the space group P21/c with a = 2121.3(2), b = 865.5(1), c = 2345.4(2) pm, β = 91.96(1)°, and Z = 4. It could be established that the title compounds contain a new type of six‐membered [1,2‐P2S4] ring with P – P bond and three S – S linkages. The tetrahedral environment of each phosphorus is completed by a (formally) single and double bonded sulfur atom attached externally to the [1,2‐P2S4] ring. These terminal PS2 units are mesomerically stabilized according to their P – S distances. FT‐IR and FT‐Raman spectra of the title compounds are recorded and interpreted.  相似文献   

20.
K3[DyIII(nta)2(H2O)]·5H2O and (NH4)3[DyIII(nta)2] have been synthesized in aqueous solution and characterized by IR, elemental analysis and single-crystal X-ray diffraction techniques. In K3[DyIII(nta)2(H2O)]·5H2O the DyIII ion is nine coordinated yielding a tricapped trigonal prismatic conformation, and its crystal belongs to monoclinic system and C2/c space group. The crystal data are as follows: a = 15.373(5) Å, b = 12.896(4) Å, c = 26.202(9) Å; β = 96.122(5)°, V = 5165(3) Å3, Z = 8, D c = 1.965 g·cm?3, μ = 3.458 mm?1, F(000) = 3016, R 1 = 0.0452 and wR 2 = 0.1025 for 4550 observed reflections with I ≥ 2σ(I). In (NH4)3[DyIII(nta)2] the DyIII ion is eight coordinated yielding a usual dicapped trigonal anti-prismatic conformation, and its crystal belongs to monoclinic system and C2/c space group. The crystal data are as follows: a = 13.736(3) Å, b = 7.9389(16) Å, c = 18.781(4) Å; β = 104.099(3)°, V = 1986.3(7) Å3, Z = 2, D c = 1.983 g·cm?3, μ = 3.834 mm?1, F(000) = 1172, R 1 = 0.0208 and wR 2 = 0.0500 for 2022 observed reflections with I ≥ 2σ(I). The results indicate that the difference in counter ion also influences coordination numbers and structures of rare earth metal complexes with aminopolycarboxylic acid 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