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1.
In the title complex salt, tetra­kis[hexa­ammine­cobalt(III)] hexa­chloro­cadmate(II) bis­[aqua­tetra­chloro­thio­cyanato­cad­mate(II)] dichloride dihydrate, the discrete ions, i.e. [Co(NH3)6]3+, Cl, [CdCl6]4− (located on an inversion centre) and [CdCl4(SCN)(H2O)]3−, together with cocrystallized water mol­ecules, are assembled by means of a network of hydrogen‐bonding inter­actions. This is the first X‐ray structure determination of a hexa­amminecobalt(III) salt with two different complex chloro­cadmium anions.  相似文献   

2.
Crystal Structures of „Supramolecular”︁ Benzo‐18‐crown‐6 Potassium Tetrathiocyanato Metallates: A Dimeric Complex {[K(Benzo‐18‐crown‐6)]2[Hg(SCN)4]}2 and Two Isomeric Complexes [K(Benzo‐18‐crown‐6)][Cd(SCN)3] Containing Trithiocyanato Cadmate Anions with Chain Structures By reaction of potassium thiocyanatomercurate(II) complexes with benzo‐18‐crown‐6 (2,3‐benzo‐1,4,7,10,13,16‐hexaoxacyclooctadec‐2‐ene) crystals of {[K(benzo‐18‐crown‐6)]2[Hg(SCN4)]}2 ( 1 ) were obtained. 1 crystallizes monoclinic, space group P21/n (non‐standard setting of P21/c), a = 1737.35(2), b = 1377.16(2), c = 1984.12(3) pm, β = 100.637(1)°, Z = 2. With potassium tetrathiocyanatocadmate(II) two modifications of a complex [K(benzo‐18‐crown‐6)][Cd(SCN)3] ( 2 , 3 ), of different symmetry were formed. 2 crystallizes monoclinic, P21/c, a = 1158,31(3), b = 1096,55(2), c = 2028,46(2) pm, β = 99,5261(2)°, Z = 4, 3  orthorhombic, P21cn, a = 1105,95(3), b = 1413,07(4), c = 1617,10(5) pm, Z = 4. 1 has a dimeric structure, built up from a dication K2(benzo‐18‐crown‐6)2]2+ and two [K(benzo‐18‐crown‐6)]+ cations, which are bridged by two [Hg(SCN)4]2– anions. In 2 and 3 triply bridged infinite [{Cd(SCN)3}n] zigzag chains, stretching along screw axes, are to be found as anions. In 2 these chains exist in two conformations related by inversion symmetry, whereas in 3 only one form can be found. [K(benzo‐18‐crown‐6)]+ cations are linked to the anion chains via K · · · S interactions of different lengths.  相似文献   

3.
18‐crown‐6(18‐C‐6) complexes with K2[M(SeCN)4] (M = Pd, Pt): [K(18‐C‐6)]2[Pd(SeCN)4] (H2O) ( 1 ) and [K(18‐C‐6)]2[Pt(SeCN)4](H2O) ( 2 ) have been isolated and characterized by elemental analysis, IR spectroscopy and single crystal X‐ray analysis. The complexes crystallize in the monoclinic space group P21/n with cell dimensions: 1 : a = 1.1159(3) Å, b = 1.2397(3) Å, c = 1.6003(4) Å, β = 92.798(4)°, V = 2.2111(8) Å3, Z = 2, F(000) = 1140, R1 = 0.0418, wR2 = 0.0932 and 2 : a = 1.1167(3) Å, b = 1.2394(3) Å, c = 1.5968(4) Å, β = 92.945(4)°, V = 2.2071(9) Å3, Z = 2, F(000) = 1204, R1 = 0.0341, wR2 = 0.0745. Both complexes form one‐dimensionally linked chains of [K(18‐C‐6)]+ cations and [M(SeCN)4]2— (M = Pd, Pt) anions bridged by K‐O‐K interactions between adjacent [K(18‐C‐6)]+ units.  相似文献   

4.
In the title compound, 4,7,13,16,21,24‐hexa­oxa‐1,10‐diazo­nia­bicyclo­[8.8.8]hexa­cosane dioxo[7,13,21,27‐tetra­phenyl‐3,17‐di­oxa­penta­cyclo­[23.3.1.15,9.111,15.119,23]ditriaconta‐1(29),5,7,9(30),11(31),12,14,19(32),20,22,25,27‐dodeca­ene‐29,30,31,32‐tetra­olato]uranium dimethyl sulfoxide tri­solvate, (C18H38N2O6)[U(C54H40O6)O2]·3C2H6OS, the uranyl ion is bound to the four phenoxide groups of the deprotonated p‐phenyl­tetra­homodioxacalix[4]arene ligand in a cone conformation, resulting in a dianionic complex. The diprotonated [2.2.2]cryptand counter‐ion is located in the cavity defined by the eight aromatic rings of the homooxacalixarene, where it is held by cation–anion, cation–π and possibly C—H⋯π inter­actions. Dimerization in the packing leads to the formation of sandwich assemblages in which two diprotonated [2.2.2]cryptands are encompassed by two uranyl complexes.  相似文献   

5.
The title salt, (1,4,7,10,13,16‐hexa­oxa­cyclo­octa­decane‐κ6O)[(iso­thio­cyanato)­tri­phenyl­borato‐κS]­potassium(I), [K(C19H15BNS)(C12H24O6)] or [K(SCNBPh3)(18‐crown‐6)], where 18‐crown‐6 is 1,4,7,10,13,16‐hexaoxa­cyclo­octa­decane and [SCNBPh3] is the (iso­thio­cyanato)­tri­phenyl­borate anion, exhibits a supramol­ecular structure that is best described as a helical coordination polymer or molecular screw. This unusual supramolecular structure is based on a framework in which the SCN ion bridges the chelated K+ ion and the B atom of BPh3 in a μ2 fashion. The X‐ray crystal structure of the title salt has been determined at 100 (1) and 293 (2) K. The K+ ion exhibits axial ligation by the S atom of the [SCNBPh3] anion, with a K—S distance of 3.2617 (17) Å (100 K). The trans‐axial ligand is an unexpected η2‐bound C=C bond of a phenyl group (meta‐ and para‐C atoms) that belongs to the BPh3 moiety of a neighboring mol­ecule. The K—C bond distances span the range 3.099 (3)–3.310 (3) Å (100 K) and are apparently retained in CDCl3 solution (as evidenced by 13C NMR spectroscopy). By virtue of the latter interaction, the supramolecular structure is a helical coordination polymer, with the helix axis parallel to the b axis of the unit cell. IR spectroscopy and semi‐empirical molecular orbital (AM1) calculations have been used to investigate further the electronic structure of the [SCNBPh3] ion.  相似文献   

6.
The novel complex [K(18-C-6)]2[Cd(mnt)2][18-C-6-18-crown-6,nmt=1,2-dicyanoethene-1,2-dithiolate,C2S2-(CN)2^2-] was synthesized and characterized by elemental analysis,IR spectrum and X-ray diffraction analysis.The complex displays two-dimensional network structure of [K(18-C-6)] complex segments and [Cd(nmt)2] complex segment bridged by S-K-S,S-K-N and N-K-N interactions between adjacent[K(18-C-6)] and [Cd(mnt)2]units.  相似文献   

7.
From the reduction of heptamolybdate, a polyoxomolybdate was obtained with the formula [Na(H2O)16(NH2CH2­COO)]4+·{Na+[H9MoMoO56(NH2CH2COO)]5?}4?­·20H2O, i.e. hepta­sodium nona­hydrogen tetra­car­bam­ate hexa­deca­aqua­hexa­penta­conta­oxa­octa­deca­molyb­date(V,VI) icosa­hydrate. The 18 Mo atoms are connected by bridging O atoms to form a centrosymmetric girdle‐like structure, in which MoV–MoV units are found. An Na+ cation occupies the central hole of the girdle, while four Na+ cations are bonded to the O atoms on the girdle edge. The girdles are linked into a one‐dimensional chain by the other Na+ cations.  相似文献   

8.
The title compounds, bis­(ammonium) naphthalene‐1,5‐di­sul­fon­ate, 2NH4+·C10H6O6S22−, and bis­[1‐(hydroxy­methyl)‐3,5,7‐tri­aza‐1‐azoniatri­cyclo­[3.3.1.13,7]­decane] 1,5‐naphthalene­di­sul­fon­ate, 2C7H15N4O+·C10H6O6S22−, were prepared from the acid‐promoted reaction of hexa­methyl­enetetr­amine. In both structures, the di­sulfonate anion is positioned on an inversion center, with each sulfonate group contributing to the supramolecular assemblies via hydrogen bonds. The ammonium cations are linked to sulfonate groups by four distinct N+—H⃛O—S contacts [N⃛O = 2.846 (2)–2.898 (2) Å and N—H⃛O = 160 (2)–175 (2)°], whereas the 1‐(hydroxy­methyl)‐3,5,7‐tri­aza‐1‐azoniatri­cyclo­[3.3.1.13,7]­decane cations form one O—H⃛O—S [O⃛O = 2.628 (2) Å and O—H⃛O = 176°] and three C—H⃛O—S [C⃛O = 3.359 (2)–3.380 (2) Å and C—H⃛O = 148–155°] interactions to neighboring sulfonate groups.  相似文献   

9.
The [2.2]­para­cyclo­phane groups of the title compounds, chiral and meso‐bis­(tri­cyclo­[8.2.2.24,7]­hexa­deca‐4,6,10,12,13,15‐hexa­en‐5‐yl)­methane (the former as a racemate), C33H32, and meso‐bis­(tri­cyclo­[8.2.2.24,7]­hexa­deca‐4,6,10,12,13,15‐hexa­en‐5‐yl) sulfide, C32H30S, show the characteristic structural features of the parent compound [2.2]­para­cyclo­phane and the related compound di­methylbis([2.2]­para­cyclo­phan‐4‐yl)­silane, C34­H36­Si: the aromatic rings are puckered, resulting in a boat conformation. The planes of the four coplanar C atoms are slightly twisted with respect to each other. The Csp3—Csp3 bond lengths of the ethyl­ene bridges are elongated by the electronic and steric effects of the skeleton.  相似文献   

10.
The title complex, (diethyl 3,4,8,15,19,20‐hexa­methyl‐21,22,23,24‐tetraazopenta­cyclo­[16.2.1.12,5.17,11.114,17]­tetracosa‐1(20),2(22),3,5,7,9,11,13(24),14,16,18‐undecaene‐9,14‐dicarb­oxyl­ate‐κ4N)­iodo­iron(III) chloro­form solvate, [Fe(C32H32­N4O4)I]·­CHCl3, shows an almost planar arrangement of the corrphycene moiety with a slightly distorted trapezoid pyramidal core; the FeIII atom is 0.416 (1) Å from the plane of the C20N4 system. The Fe—N distances are 2.049 (3), 2.044 (3), 2.079 (3) and 2.075 (3) Å. The solvated chloro­form forms a C—H?O hydrogen bond [C?O 3.107 (10) Å] to an adjacent carbonyl O atom. This is the first X‐ray structure analysis of a corrphycenatoiron(III) derivative.  相似文献   

11.
In the two compounds (borohydrido)(1,4,7,10,13,16‐hexa­oxacyclo­octa­decane‐κ6O)potassium, [K(BH4)(C12H24O6)], (I), and (borohydrido)(1,4,7,10,13,16‐hexa­oxa‐2,3:11,12‐di­benzo­cyclo­octa­deca‐2,11‐diene‐κ6O)(tetra­hydro­furan)­potassium, [K(BH4)(C4H8O)(C20H24O6)], (II), the K atom is bound to the six O atoms of the crown ether and to a tridentate borohydride group, with further coordination to a tetra­hydro­furan mol­ecule in (II). The alkali metal ion environment is thus distorted hexa­gonal–pyramidal in (I) and bipyramidal in (II).  相似文献   

12.
A new complex compound, [K2(18-crown-6)2[K(18-crown-6)(EtOH)]2[Er(NCS)6](SCN) (I), was synthesized and its crystal structure was studied by X-ray diffraction. In this work, the synthes and X-ray difraction stady of the crystals of a new complex, hexakis (isothiocyanato) erbiu(III) thiocyanate bis(18-crown-6) dipotassium bis(18-crown-6) ethanolpotassium], [K2(18-crown-6)2][K(18-crown-6)(ETON)]2[Er(NCS)6(SCN)(I)] are described. In crystal I, the alternating [Er(NCS)6]3? anions and binuclear complex cation [K(18-crown-6)2]2+ from infinite chains via the F-S bonds, while two complex cations [K(18-crown-6)(ETON)]+ and the statistically disordered SCN? anion between them are linked by the hydragen bonds O-H…S and O-H…N. Complex I contains the host-guest complex cations [K2(18-crown-6)2)]2+ and [K(18-crown-6)(ETON)]+ [1]. The alternating octabedral [Er(NCS)6]3? anions and binuclear complex cations [K2(18-crown-6)2]2+of crystal I form infinite chains via the K-S bonds, while two complex cations [K(18-crown-6)(EtOH)]+ and the statistically disordered SCN? anion lying between them are linked by interionic hydrogen bonds O-H…S and O-H…N. Complex I contains the host-guest complex cations [K2(18-crown-6)2]2+ and [K(18-crown-6)(EtOH)]+ [1].  相似文献   

13.
In 8a‐azonia­[6]­helicene hexa­fluoro­phos­phate or 8a‐azoniaphenanthro[3,4‐c]phen­an­threne hexa­fluoro­phos­phate, C25H16N+·PF6, replacement of an outer bridgehead carbon of hexahelicene by a quaternary Nsp2 atom results in a geometrical change in the helical structure. The racemic heterohelicene forms homochiral columnar stacks through intermolecular π–π donor–acceptor interactions in the crystalline state.  相似文献   

14.
The title compound, tetra­ethyl­ammonium dodeca‐μ‐cyano‐hexa­cyano­tetrakis­(ethyl­ene­di­amine)­tetra­cadmium(II)­tri­fer­rate(III), (C8H20N)[Cd4Fe3(CN)18(C2H8N2)4], was pre­pared from a reaction mixture containing CdCl2, K3[Fe(CN)6], ethyl­ene­di­amine (en) and [Et4N]Br in a 1:1:3:1 molar ratio. The crystal structure consists of a negatively charged three‐dimensional framework of {[Cd(en)]4[Fe(CN)6]3} anions, with [Et4N]+ cations located in the cavities of the framework. The Cd atom is octahedrally coordinated by one disordered chelating en mol­ecule [mean Cd—N = 2.35 (3) Å] and four N‐­bonded bridging cyano groups [Cd—N distances are in the range 2.283 (2)–2.441 (2) Å]. There are two crystallographically independent [Fe(CN)6]3− anions in the structure and in each the Fe atom lies on a twofold axis. In the first [mean Fe—C = 1.941 (5) Å], all the cyano groups are bridging ligands, while in the second [mean Fe—C = 1.945 (2) Å], there are two terminal cyano ligands in trans positions. The Cd—N—C angles range from 128.6 (2) to 172.8 (2)°.  相似文献   

15.
A hydrogen‐bonded coordination supramol­ecule, (meso‐5,7,­7,­12,14,14‐hexa­methyl‐1,4,8,11‐tetra­aza­cyclo­tetra­decane‐κ4N)­nickel(II) [N,No‐phenylenebis­(oxamato)­‐κ4O,N,N′,O′]nickelate(II) dihydrate, [Ni(C16H36N4)][Ni(C10H4N2O6)]·2H2O or [Ni(meso‐cth)]­[Ni(opba)]·2H2O, has been prepared and characterized by X‐ray crystallographic analysis. The two complex ions, i.e. [Ni(meso‐cth)]2+ and [Ni(opba)]2?, are hydrogen bonded to each other, resulting in two‐dimensional neutral supramolecular sheets. The sheets stack along the a direction to produce a three‐dimensional architecture with one‐dimensional channels in which hydrogen‐bonded chains of water mol­ecules are included.  相似文献   

16.
A new orthorhombic polymorphic modification of the title compound (alternative name: cistransoidcis‐2,5,8,15,18,21‐hexaoxatri­cyclo­[20.4.0.09,14]­hexa­cosane), C20H36O6, has been found and is compared with the previously known monoclinic modification. In the structures of the two polymorphs, the crown‐ether mol­ecules are centrosymmetric and reveal essen­tially the same molecular shape but different packing motifs.  相似文献   

17.
The syntheses and crystal structures of the title Pt2II and Pt2III dimers doubly bridged with N,N‐dimethyl­guanidinate ligands, namely bis­(μ‐N,N‐dimethyl­guanidinato)bis­[(2,2′‐bipyridine)platinum(II)](Pt—Pt) bis­(hexa­fluoro­phosphate) acetonitrile disolvate, [Pt2II(C3H8N3)2(C10H8N2)2](PF6)2·2CH3CN, (I), and guanidinium bis­(μ‐N,N‐dimethyl­guanidinato)bis­[(2,2′‐bipyridine)sulfatoplatinum(III)](Pt—Pt) bis­(hexa­fluoro­phosphate) nitrate hexa­hydrate, (C3H10N3)[PtIII2(C3H8N3)2(SO4)2(C10H8N2)2]NO3·6H2O, (II), are reported. The oxidation of the Pt2II dimer into the Pt2III dimer results in a marked shortening of the Pt—Pt distance from 2.8512 (6) to 2.5656 (4) Å. The change is mainly compensated for by the change in the dihedral angle between the two Pt coordination planes upon oxidation, from 21.9 (2) to 16.9 (3)°. We attribute the relatively strong one‐dimensional stack of dimers achieved in the Pt2II compound in part to the strong PtII⋯C(bpy) associations (bpy is 2,2′‐bipyridine) in the crystal structure [Pt⋯C = 3.416 (10) and 3.361 (12) Å].  相似文献   

18.
A novel two‐dimensional network dibenzo‐18‐crown‐6 (DB18‐C6) complex: [Na (DB18‐C‐6) (H2O)2] [Na (DB18‐C‐6) (SCN)2] has been isolated and characterized by elemental, IR and X‐ray diffraction analysis. The crystal structure belongs to monoclinic, space group P21/c with cell dimensions a = 1.06178(7), b = 1.40243(8), c = 3.03496(19) nm, β = 90.4220(10)°, V = 4.5292(5) nm3, Z=4, Dcalcd =1.351 g/ cm3, F(000) = 1936, R1 = 0.0369, wR2 = 0.0821. The most interesting feature in this structure is that complex cation and complex anion form a two‐dimensional network via τ‐τ stacking interactions, hydrogen bonds and electrostatic interactions.  相似文献   

19.
The crystal structure of the title compound, K[Ag(CN)2]·C12H24O6, conventionally denoted K(18‐crown‐6)Ag(CN)2, where 18‐crown‐6 is 1,4,7,10,13,16‐hexa­oxa­cyclo­octa­decane, is characterized by closely packed linear chains formed by the coordination of the nitrile N atoms of the [Ag(CN)2] anions to the K+ cations. The K atoms lie on centers of inversion and are additionally bound to the six O atoms of the crown ether.  相似文献   

20.
The title PtII complexes, viz. (2,2′‐bi­pyridine‐κ2N,N′)[(1R,2R)‐1,2‐di­amino­cyclo­hexane‐κ2N,N′]­platinum(II) bis­(hexa­fluoro­phosphate), [Pt(C6H14N2)(C10H8N2)](PF6)2, and [(1R,2R)‐1,2‐di­amino­cyclo­hexane‐κ2N,N′](1,10‐phenanthroline‐κ2N,N′)platinum(II) bis­(hexa­fluoro­phosphate), [Pt(C6H14N2)(C12H8N2)](PF6)2, containing an aromatic α‐di­imine and a non‐planar di­amino­cyclo­hexane, both form a ladder‐type structure, which is constructed via loose π–π stacking on the α‐di­imine ligands and hydrogen bonding between the cyclic amines and the counter‐anions. In the former compound, there are two independent complex cations, both of which have a twofold axis through the Pt atom.  相似文献   

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