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1.
From the 1:1 system of [Cu(dien)2](NO3)2 and K[Ag(CN)2] in water (dien is diethyl­enetri­amine, C4H13N3), the novel compound catena‐poly­[bis­[[μ‐cyano‐1:2κ2C:N‐diethyl­enetri­amine‐2κ3N‐copper(II)silver(I)]‐μ‐cyano‐1:2′κ2C:N] di­cyano­silver(I) tri­cyanodisilver(I)], [CuAg(CN)2(dien)]2[Ag(CN)2][Ag2(CN)3], has been isolated. The structure is formed from positively charged [–Cu(dien)–NC–Ag–CN–]nn+ chains and two isolated centrosymmetric [Ag(CN)2]? and [Ag2(CN)3]? anions. In the cationic chains, the Cu atoms are linked by bridging di­cyano­argentate groups, and the deformed square‐pyramidal coordination polyhedron of the CuII cation is formed from a tridentate chelate‐like bonded dien ligand and two N‐bonded bridging cyano groups. One of the bridging cyano groups occupies the apical (ap) position [mean Cu—­Neq = 2.02 (2) Å, and Cu—Nap = 2.170 (3) Å; eq is equatorial]. Short argentophilic interactions in the range 3.16–­3.30 Å are present in the crystal structure.  相似文献   

2.
The crystal structures of two square tetracyanocomplexes were determined. [Ni(dien)2][Ni(CN)4]·2H2O (NDNCH) and [Ni‐(dien)2][Pd(CN)4] (NDPC) (dien = diethylene triamine) exhibit ionic structures consisting of mer‐[Ni(dien)2]2+ cations and [Ni(CN)4]2‐ or [Pd(CN)4]2‐ anions, respectively. Moreover, the structure of NDNCH is completed by two water molecules of crystallisation. In both compounds hydrogen bonds contribute to the stabilisation of the structure. NDNCH dehydrates on air quickly yielding anhydrous [Ni(dien)2][Ni(CN)4] (NDNC). Its thermal decomposition proceeds in a complicated process followed by aerial oxidation of metallic nickel to NiO.  相似文献   

3.
Two special manganese complexes [Mn(II)(acac?)2(4,4′‐bipy)]n (bipy=4,4′‐bipyridine) (complex 1 ) and [Mn(III)(acac?)3]·4CO(NH2)2 (acacH=acetylacetone) (complex 2 ) were synthesized in the same strategy by solvothermal method. Single crystal X‐ray diffraction revealed the complex 1 consists of one‐dimensional infinite coordination chain, with the manganese centers bridged by 4,4′‐bipy. And free carbamides of complex 2 connect with each other through the hydrogen bonds to form a 14‐membered carbamide ring and a zig‐zag plane. Both enantiomers of Mn(III)(acac?)3 exist in the structure, forming a racemate. Furthermore, these enantiomers and those zig‐zag planes are linked with hydrogen bonds to form an unique spatial network.  相似文献   

4.
Synthesis, Vibrational Spectra, and Crystal Structures of the Nitrato Argentates (Ph4P)[Ag(NO3)2(CH3CN)]·CH3CN and (Ph4P)[Ag2(NO3)3] Tetraphenylphosphonium bromide reacts in acetonitril suspension with excess silver nitrate to give (Ph4P)[Ag(NO3)2(CH3CN)]·CH3CN ( 1 ), whereas (Ph4P)[Ag2(NO3)3] ( 2 ) is obtained in a long‐time reaction from (Ph4P)Br and excess AgNO3 in dichloromethane suspension. Both complexes were characterized by vibrational spectroscopy (IR, Raman) and by single crystal structure determinations. 1 : Space group P21/c, Z = 4, lattice dimensions at 193 K: a = 1781.5(3), b = 724.8(1), c = 2224.2(3) pm, β = 96.83(1)°, R1 = 0.0348. 1 contains isolated complex units [Ag(NO3)2(CH3CN)]?, in which the silver atom is coordinated by the chelating nitrate groups and by the nitrogen atom of the solvated CH3CN molecule with a short Ag—N distance of 220.7(4) pm. 2 : Space group I2, Z = 4, lattice dimensions at 193 K: a = 1753.4(4), b = 701.7(1), c = 2105.5(4) pm, R1 = 0.072. In the polymeric anions [Ag2(NO3)3]? each silver atom is coordinated in a chelating manner by one nitrate group and by two oxygen atoms of two bridging nitrate ions. In addition, each silver atom forms a weak π‐bonding contact with a phenyl group of the (Ph4P)+ ions with shortest Ag···C separations of 266 and 299 pm, respectively, indicating a (4+1) coordination of silver atoms.  相似文献   

5.
The title compound, bis[di­aqua­bis­(ethyl­enedi­amine‐κ2N,N′)copper(II)­] hexa­cyano­iron(II) tetrahydrate, [Cu(C2H8N2)2(H2O)1.935]2[Fe(CN)6]·4H2O, was crystallized from an aqueous reaction mixture initially containing CuSO4, K3[Fe(CN)6] and ethyl­enedi­amine (en) in a 3:2:6 molar ratio. Its structure is ionic and is built up of two crystallographically different cations, viz. [Cu(en)2(H2O)2]2+ and [Cu(en)2(H2O)1.87]2+, there being a deficiency of aqua ligands in the latter, [Fe(CN)6]4− anions and disordered solvent water mol­ecules. All the metal atoms lie on centres of inversion. The Cu atom is octahedrally coordinated by two chelate‐bonded en mol­ecules [mean Cu—N = 2.016 (2) Å] in the equatorial plane, and by axial aqua ligands, showing very long distances due to the Jahn–Teller effect [mean Cu—O = 2.611 (2) Å]. In one of the cations, significant underoccupation of the O‐atom site is observed, correlated with the appearance of a non‐coordinated water mol­ecule. This is interpreted as the partial contribution of a hydrate isomer. The [Fe(CN)6]4− anions form quite regular octahedra, with a mean Fe—C distance of 1.913 (2) Å. The dominant intermolecular interactions are cation–anion O—H⋯N hydrogen bonds and these inter­actions form layers parallel to (001).  相似文献   

6.
Crystal Structure and Vibrational Spectrum of (H2NPPh3)2[SnCl6]·2CH3CN Single crystals of (H2NPPh3)2[SnCl6]·2CH3CN ( 1 ) were obtained by oxidative addition of tin(II) chloride with N‐chloro‐triphenylphosphanimine in acetonitrile in the presence of water. 1 is characterized by IR and Raman spectroscopy as well as by a single crystal structure determination: Space group , Z = 2, lattice dimensions at 193 K: a = 1029.6(1), b = 1441.0(2), c = 1446.1(2) pm, α = 90.91(1)°, β = 92.21(1)°, γ = 92.98(1)°, R1 = 0.0332. 1 forms an ionic structure with two different site positions of the [SnCl6]2? ions. One of them is surrounded by four N‐hydrogen atoms of four (H2NPPh3)+ ions, four CH3CN molecules form N–H···N≡C–CH3 contacts with the other four N‐hydrogen atoms of the cations. Thus, 1 can be written as [(H2NPPh3)4(CH3CN)4(SnCl6)]2+[SnCl6]2?.  相似文献   

7.
Two new salts of the cation [CuI(dmp)2]+ (dmp is 2,9‐dimeth­yl‐1,10‐phenanthroline, C14H12N2), namely bis­[bis­(2,9‐dimeth­yl‐1,10‐phenanthroline‐κ2N,N′)copper(I)] bis­(hexa­fluorophos­phate) hemi[bis­(4‐pyridylmethyl­idene)hydrazine] acetonitrile solvate, [Cu(C14H12N2)2]2(PF6)2·0.5C12H10N4·C2H3N or [Cu(dmp)2]2(PF6)2·0.5(bpmh)·CH3CN [bpmh is bis­(4‐pyridylmethyl­idene)hydrazine, C12H10N4], (I), and bis­(2,9‐dimeth­yl‐1,10‐phenanthroline‐κ2N,N′)copper(I) dicyanamide, [Cu(C14H12N2)2](C2N3) or [Cu(dmp)2][N(CN)2], (II), are reported. The Cu—N bond lengths and the distortion from idealized tetra­hedral geometry of the dmp ligands are discussed and compared with related compounds. The bpmh molecule in (I) is π–π stacked with a dmp ligand at a distance of 3.4 Å, rather than coordinated to the metal atom. The molecule lies across an inversion center in the crystal. In (II), the normally coordinated dicyanamide mol­ecule is present as an uncoordinated counter‐ion.  相似文献   

8.
Coordination Polymeric 1, 2‐Dithiooxalato and 1, 2‐Dithiosquarato Complexes. Syntheses and Structures of [BaCr2(bipy)2(1, 2‐dtox)4(H2O)2], [Ni(cyclam)(1, 2‐dtsq)]·2DMF, [Ni(cyclam)Mn(1, 2‐dtsq)2(H2O)2]·2H22, and [H3O][H5O2][Cu(cyclam)]3[Cu2(1, 2‐dtsq)3]2 1, 2‐Dithioxalate and 1, 2‐dithiosquarate ions have a pair of soft and hard donor centers and thus are suited for the formation of coordination polymeric complexes containing soft and hard metal ions. The structures of four compounds with building blocks containing these ligands are reported: In [BaCr2(bipy)2(1, 2‐dtox)4(H2O)2] Barium ions and pairs of Cr(bipy)(1, 2‐dtox)2 complexes form linear chains by the bisbidentate coordination of the dithiooxalate ligands towards Ba2+ and Cr3+. In [Ni(cyclam)(1, 2‐dtsq)]·2DMF short NÖH···O hydrogen bonds link the NiS2N4‐octahedra with C2v‐symmetry to an infinite chain. In [Ni(cyclam)Mn(1, 2‐dtsq)2(H2O)2]·2H2O the 1, 2‐dithiosquarato ligand shows a rare example of S‐coordination towards manganese(II). The sulfur atoms of cis‐MnO2S4‐polyedra are weakly coordinated towards the axial sites of square‐planar NiN4‐centers, thus forming a zig‐zag‐chain of Mn···Ni···Mn···Ni polyhedra. [H3O][H5O2][Cu (cyclam)]3[Cu2(1, 2‐dtsq)3]2 contains square planar [CuII(cyclam)]2+ ions and dinuclear [CuI2(1, 2‐dtsq)3]4— ions. Here each copper atom is trigonally planar coordinated by S‐donor atoms of the ligands. The Cu…Cu distance is 2.861(4)Å.  相似文献   

9.
Phosphorane Iminato Complexes of Antimony. The Crystal Structures of [Sb2Cl5(NPMe3)2][SbCl6] · CH3CN and [SbCl(NPPh3)]2[SbCl6]2 · 6 CH3CN The title compounds are formed by reaction of antimony pentachloride in acetonitrile solution with the phosphorane iminato complexes SbCl2(NPMe3) and SbCl2(NPPh3), respectively, which themselves are synthesized by reaction of antimony trichloride with Me3SiNPR3 (R = Me, Ph). The complexionic compounds are characterized by 121Sb Mössbauer spectroscopy and by crystal structure determinations. [Sb2Cl5(NPMe3)2][SbCl6] · CH3CN: Space group P41, Z = 4, 3 698 observed unique reflections, R = 0.022. Lattice dimensions at ?60°C: a = b = 1 056.0(1), c = 2 709.6(2) pm. The structure consists of SbCl6? ions and cations [Sb2Cl5(NPMe3)2(CH3CN)]+, in which one SbIII atom and one SbV atom are bridged by the N atoms of the phosphorane iminato ligands. [SbCl(NPPh3)]2[SbCl6]2 · 6 CH3CN: Space group P1 , Z = 2, 5 958 observed unique reflections, R = 0.033. Lattice dimensions at ?60°C: a = 989.4(11), b = 1 273(1), c = 1 396(1) pm, α = 78.33(7), β = 77.27(8)°, γ = 86.62(8)°. The structure consists of SbCl6? ions and centrosymmetric cations [SbCl(NPPh3)(CH3CN)2]22+, in which the antimony atoms are bridged by the N atoms of the phosphorane iminato ligands.  相似文献   

10.
Preparation and Crystal Structures of Ag[N(CN)2](PPh3)2, Cu[N(CN)2](PPh3)2, and Ag[N(CN)2](PPh3)3 The coordination compounds Ag[N(CN)2](PPh3)2 ( 1 ), Cu[N(CN)2](PPh3)2 ( 2 ), and Ag[N(CN)2](PPh3)3 ( 3 ) are obtained by the reaction of AgN(CN)2 or CuN(CN)2 with triphenylphosphane in CH2Cl2. X‐ray structure determinations were performed on single crystals of 1 , 2 , and 3 · C6H5Cl. The three compounds crystallize monoclinic in the space group P21/n with the following unit cell parameters. 1 : a = 1216.07(9), b = 1299.5(2), c = 2148.4(3) pm, β = 99.689(13)°, Z = 4; 2 : a = 1369.22(10), b = 1257.29(5), c = 1888.04(15) pm, β = 94.395(7)°, Z = 4; 3 · C6H5Cl: a = 1276.6(4), b = 1971.7(3), c = 2141.3(5) pm, β = 98.50(3)°, Z = 4. In all structures the metal atoms have a distorted tetrahedral coordination. The crystal structure of 3 · C6H5Cl shows monomeric molecular units with terminal coordinated dicyanamide. The crystal structure of 1 is built up by dinuclear units, which are bridged by dicyanamide ligands. However, the crystal structure of 2 corresponds to a onedimensional coordination polymer, bridged by dicyanamide anions.  相似文献   

11.
A new cyano‐bridged binuclear 4f‐3d complex Sm(DMSO)4‐(H2O)3Cr(CN)6 was synthesized and characterized by single crystal structure analysis. It crystallizes in monoclinic, space group P21 with a=0.9367(2) nm, b = 1.3917(3) nm, c = 1.1212(2) run, β = 99.88(3)° and Z = 2. In this binuclear complex, Sm atom is eight coordinated and linked to the Cr atom by a cyano bridge. The molecules packs to form 3D structure due to the hydrogen bonds among them. [K3(18‐C‐6)3(H2O)4]Cr(CN)6·3H2O (18‐C‐6 represents 18‐crown‐6‐ether) that was synthesized as a byproduct in the preparation of a Gd—Cr complex is also structurally characterized. Crystal data: triclinic, space group P‐l with a = 1.0496(7) nm, b= 1.1567(14) nm, c = 1.3530(13) nm, a = 94.15(9)°, β = 96.04(8)°, γ = 95.25(9)° and Z = l. [K3(18‐C‐6)3(H2O)4]‐Cr(CN)6·3H2O consists of ionic [K3(18‐C‐6)3(H2O)4]3+ and [Cr(CN)6]3‐ pairs, of which the [K3(18‐C‐6)3(H2O)4]3+ ion is a trinuclear duster connected by water, and K atoms are eight coordinated by eight oxygen atoms of one 18‐C‐6 and two water molecules.  相似文献   

12.
Polysulfonylamines. CLXV. Crystal Structures of Metal Di(methanesulfonyl)amides. 14. Cs3Ag[(MeSO2)2N]4 and CsAg[(MeSO2)2N]2: A Three‐Dimensional and a Layered Coordination Polymer Containing Bis(dimesylamido‐N)argentate Building Blocks Serendipitous formation pathways and low‐temperature X‐ray structures are reported for the coordination compounds Cs3A2[AgA2] ( 1 ) and Cs[AgA2] ( 2 ), where A— represents the pentadentate dimesylamide ligand (MeSO2)2N—. Both phases (monoclinic, space group C2/c, Z′ = 1/2) contain inversion‐symmetric bis(dimesylamido‐N)argentate units displaying exactly linear N—Ag—N cores and short, predominantly covalent Ag—N bonds [ 1 : 213.5(2), 2 : 213.35(12) pm]; in each case, the coordination number of the silver ion is extended to 2 + 6 by four internal and two external Ag···O secondary interactions. The three‐dimensional coordination polymer 1 is built up from alternating layer substructures [{Cs(1)}{A}4/2]— with Cs(1) lying on twofold rotation axes and [{Cs(2)}2{AgA2}4/4]+ with Cs(2) occupying general positions. Within the substructural layers, both types of cesium cation have approximately planar O4 environments, whereas the final coordination spheres including interlayer bonds are extended to O6 for Cs(1) and to O8N for Cs(2). Compound 2 , in contrast, forms a genuine layer structure. The layers are constructed from Cs+ chains located on twofold rotation axes, alternating with [AgA2]— stacks reinforced by Ag···O secondary interactions and weak C—H···O hydrogen bonds; Cs+ is embedded in an O8 environment. Both structures are pervaded by a three‐dimensional C—H···O network.  相似文献   

13.
Gadolinium dicyanamide dihydrate Gd[N(CN)2]3 · 2 H2O was prepared by ion exchange in aqueous solution followed by evaporation of the solvent at room temperature. Gd[N(CN)2]3 · 2 H2O was characterized by single‐crystal structure analysis, FTIR spectroscopy and DSC analysis. In the crystal there are three crystallographically independent [N(CN)2]? ions and Gd3+ which are coordinated by six N atoms from six different [N(CN)2]? ions and two O atoms from two water molecules forming an irregular quadratic antiprism. Four H bonds have been identified in the structure of Gd[N(CN)2]3 · 2 H2O, two of them running to terminal N atoms and two to the bridging N atoms of dicyanamide ions (Gd[N(CN)2]3 · 2 H2O: P21/n (no. 14), a = 7.4845(15) Å, b = 11.529(2) Å, c = 13.941(3) Å, β = 93.98(3)°, Z = 4, 1948 reflections, 175 parameters, R1 = 0.0493). The DSC analysis indicates that Gd[N(CN)2]3 · 2 H2O looses the crystal water at temperatures around 130 – 140 °C forming anhydrous Gd[N(CN)2]3, the structure of which has been refined by the Rietveld method based on X‐ray powder diffraction data. Gd[N(CN)2]3 was found to be isotypic with Ln[N(CN)2]3 (Ln = La, Ce, Pr, Nd, Sm and Eu) which previously have been described in the literature.  相似文献   

14.
Ag/CuI Mixed Occupancy in the Crystal Structures of the Copper(II) Cyanoargentates Cu(NH3)(py)Ag3?xCux(CN)5 · py From pyridine and ammonia containing CuII solutions, to which K[Ag(CN)2] and in part KCu(CN)2/KCN has been added, we obtained single crystals of mixed-valent copper compounds of variable composition Cu(NH3)-(py)Ag3-xCux(CN)5 · py. The phases corresponding to x = 0.39(1) ( I ) and to x = 1.243(6) ( II ) were characterized by X-ray structure analysis. They are isomorphous and crystallize with Z = 4 in the monoclinic space group P21/c. The lattice constants for I [and II , resp.] are: a = 923.8(2) [901.4(2)], b = 1226.8(2) [1227.3(2)], c = 1809.8(4) [1783.5(2)] pm, β = 91.41(3) [91.02(1)]°. The CuII cation shows trigonal bipyramidal [CuN5] coordination, with the neutral ligands in axial positions (mean value Cu? N for II : 201 pm), three N atoms of cyano bridges in equatorial ones (Cu? N: 206 pm). One of these bridges stems from a trigonal unit [AgCN(NC)2], the central atom of which is substituted by CuI to an extent of 39% in I , and completely in II . The two other bridges originate from two [Ag(CN)2]? groups, of which the more bent one may be partially occupied by CuI as well (24% in II ). The units mentioned are connected into meshes of elongated hexagons and further into puckered layers within the (010) plane, interpenetrating each other in pairs. A threedimensional linking of layers occurs by the trigonal Ag/CuI species forming centrosymmetric dimers, in which the metal coordination is completed to tetrahedral by a C-atom of the corresponding neighbouring group and short metal-metal distances of 279.1(3) pm in I and 264.1(1) pm in II appear. Details and relations are discussed.  相似文献   

15.
Structures of Ionic Di(arenesulfonyl)amides. 8. Sodium Bis[di(4‐fluorobenzenesulfonyl)amido‐N]argentate: A Heterobimetallic Complex Exhibiting a Lamellar Layer Structure and Short C–H···F–C Interlayer Contacts Na[Ag{N(SO2–C6H4–4‐F)2}2] (monoclinic, C2/c, Z′ = 1/2) is the first heterobimetallic representative in a well‐documented class of layered inorgano‐organic solids where the inorganic component is comprised of metal cations and coordinating N(SO2)2 groups and the outer regions are formed by the aromatic rings of the di(arenesulfonyl)amide entities, which adopt a folded conformation approximating to mirror symmetry. The inversion‐symmetric bis(amido)argentate unit of the novel compound displays an exactly linear N–Ag–N core and short Ag–N bonds of 217.55(17) pm (at ?140 °C); the coordination number of the silver ion is extended to 2 + 6 by four internal and two external Ag···O secondary interactions. The polar lamella is constructed from rows of Na+ ions located on twofold axes, alternating with bis(amido)argentate strands reinforced by Ag···O interactions and weak C–H···O hydrogen bonds; Na+ is embedded in an O6 environment. Adjacent layers are cross‐linked via short C–H···F–C contacts suggestive of weak hydrogen bonding enhanced by cooperativity.  相似文献   

16.
The complexes [Ag12(Spz)12(N‐triphos)2][Ag3(Spz)3(N‐triphos)]2 · (DMF)6 ( 1 ) and [Ag18(Spz)12(N‐triphos)4(CF3CO2)6] ( 2 ) were synthesized and structurally characterized by X‐ray diffraction [HSpz = pyrazine‐2‐thiolate, N‐triphos = tris((diphenylphosphanyl)methyl)amine]. The central [Ag6] ring with chair‐conformation in 1 and the ideally octahedral [Ag6] cluster core in 2 are both stabilized by the tripodal building units of neutral [Ag3(Spz)3(N‐triphos)] compound. The Ag ··· Ag distances of the [Ag6] moieties in 1 and 2 are 3.07 and 2.81 Å, respectively, exhibiting intermetallic interactions, which can enhance the stability of [Ag6] conformations. In addition, the π ··· π interactions between parallel pyrazine rings could impose on the building and the Ag ··· Ag interactions of these Ag–S clusters.  相似文献   

17.
The title compound, catena‐poly[[bis[(triazacyclononane‐κ3N,N′,N′′)copper(II)]‐di‐μ‐cyanido‐κ4N:C‐palladate(II)‐di‐μ‐cyanido‐κ4C:N] dibromide bis[[(triazacyclononane‐κ3N,N′,N′′)copper(II)]‐μ‐cyanido‐κ2N:C‐[dicyanidopalladate(II)]‐μ‐cyanido‐κ2C:N] monohydrate], {[Cu2Pd(CN)4(C6H15N3)2]Br2·[Cu2Pd2(CN)8(C6H15N3)2]·H2O}n, (I), was isolated from an aqueous solution containing tacn·3HBr (tacn is 1,4,7‐triazacyclononane), Cu2+ and tetracyanidopalladate(2−) anions. The crystal structure of (I) is essentially ionic and built up of 2,2‐electroneutral chains, viz. [Cu(tacn)(NC)–Pd(CN)2–(CN)–], positively charged 2,4‐ribbons exhibiting the composition {[Cu(tacn)(NC)2–Pd(CN)2–Cu(tacn)]2n+}n, bromide anions and one disordered water molecule of crystallization. The O atom of the water molecule occupies two unique crystallographic positions, one on a centre of symmetry, which is half occupied, and the other in a general position with one‐quarter occupancy. One of the tacn ligands also exhibits disorder. The formation of two different types of one‐dimensional structural motif within the same structure is a unique feature of this compound.  相似文献   

18.
Crystal Structures of the Hexachlorometalates NH4[SbCl6], NH4[WCl6], [K(18‐crown‐6)(CH2Cl2)]2[WCl6]·6CH2Cl2 and (PPh4)2[WCl6]·4CH3CN The crystal structures of the title compounds were determined by single crystal X‐ray methods. NH4[SbCl6] and NH4[WCl6] crystallize isotypically in the space group C2/c with four formula units per unit cell. The NH4+ ions occupy a twofold crystallographic axis, whereas the metal atoms of the [MCl6]— ions occupy a centre of inversion. There exist weak interionic hydrogen bridges. [K(18‐crown‐6)(CH2Cl2)]2[WCl6]·6CH2Cl2 crystallizes in the orthorhombic space group R3¯/m with Z = 3. The compound forms centrosymmetric ion triples, in which the potassium ions are coordinated with a WCl3 face each. In trans‐position to it the chlorine atom of a CH2Cl2 molecule is coordinated so that, together with the oxygen atoms of the crown ether, coordination number 10 is achieved. (PPh4)2[WCl6]·4CH3CN crystallizes in the monoclinic space group P21/c with Z = 4. This compound, too, forms centrosymmetric ion triples, in which in addition the acetonitrile molecules are connected with the [WCl6]2— ion via weak C—H···Cl contacts.  相似文献   

19.
Although pure hydrogen cyanide can spontaneously polymerize or even explode, when initiated by small amounts of bases (e.g. CN?), the reaction of liquid HCN with [WCC]CN (WCC=weakly coordinating cation=Ph4P, Ph3PNPPh3=PNP) was investigated. Depending on the cation, it was possible to extract salts containing the formal dihydrogen tricyanide [CN(HCN)2]? and trihydrogen tetracyanide ions [CN(HCN)3]? from liquid HCN when a fast crystallization was carried out at low temperatures. X‐ray structure elucidation revealed hydrogen‐bridged linear [CN(HCN)2]? and Y‐shaped [CN(HCN)3]? molecular ions in the crystal. Both anions can be considered members of highly labile cyanide‐HCN solvates of the type [CN(HCN)n]? (n=1, 2, 3 …) as well as formal polypseudohalide ions.  相似文献   

20.
The three new thioantimonates(V) [Ni(chxn)3]3(SbS4)2·4H2O ( I ), [Co(chxn)3]3(SbS4)2·4H2O ( II ) (chxn is trans‐1,2‐diaminocyclohexane) and [Co(dien)2][Co(tren)SbS4]2·4H2O ( III ) (dien is diethylenetriamine and tren is tris(2‐aminoethyl)amine) were synthesized under solvothermal conditions. Compounds I and II are isostructural crystallizing in space group C2/c. The structures are composed of isolated [M(chxn)3]2+ complexes (M = Ni, Co), [SbS4]3? anions and crystal water molecules. Short S···N/S···O/O···O separations indicate hydrogen bonding interactions between the different constituents. Compound III crystallizes in space group and is composed of [Co(dien)2]2+ and [Co(tren)SbS4]? anions and crystal water molecules. In the cationic complex the Co2+ ion is in an octahedral environment of two dien ligands whereas in [Co(tren)SbS4]? the Co2+ ion is in a trigonal bipyramidal coordination of four N atoms of tren and one S atom of the [SbS4]3? anion, i.e., two different coordination polyhedra around Co2+ coexist in this compound. Like in the former compounds an extended hydrogen bonding network connects the complexes and the water molecules into a three‐dimensional network.  相似文献   

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