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1.
Cs[Na(NH3)6][B10H10]·NH3 was synthesised from cesium and disodium‐decahydro‐closo‐decaborate Na2B10H10 in liquid ammonia, from which it crystallized in form of temperature sensitive colorless plates (triclinic, P1¯, a = 8.4787(7) Å, b = 13.272(1) Å, c = 17.139(2) Å, α = 88.564(1)°, β = 89.773(1)°, γ = 81.630(1)°, V = 1907.5(3) Å3, Z = 4). The compound is the first example of an alkali metal boranate with two different types of cations. The decahydro‐closo‐decaborate dianions [B10H10]2— and the cesium cations form a equation/tex2gif-stack-1.gif[Cs2(B10H10)2]2— layer parallel to the ac plane. These layers are separated by N—H···N‐hydrogen bonded hexamminesodium cations.  相似文献   

2.
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   

3.
The ammoniate [K17(Sb8)2(NH2)] · 17.5NH3 was synthesized by reduction of antimony with potassium in liquid ammonia. Single crystals were isolated and characterized by low temperature X‐ray structure analysis. [K17(Sb8)2(NH2)] · 17.5NH3 crystallizes in the space group P21/c (No. 14) with a = 12.976(1) Å, b = 24.536(1) Å, c = 22.858(1) Å and β = 99.17(1)°. The ammoniate contains crown‐shaped [Sb8]8? Zintl anions which are analogous to S8 rings. The presence of amide NH2? as an additional anion is deduced from coordination observations and the close similarity of structural features to the structure of KNH2.  相似文献   

4.
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   

5.
Preparation, properties, and crystal structure of Na3[Yb(NH2)6] Na3[Yb(NH2)6] was prepared by the reaction of Na and Yb in the atomic ration 3:1 with ammonia at 150°C and 200 atm as a light grey microcrystalline powder. Colourless single crystals were obtained at 180°C and ~6000 atm. It decomposes rapidly at temperature above 140°C. At 250°C NaNH2 nd a nitride phase results which crystallizes in the Nacl lattice type with a = 4.86 Å. Na3[Yb(NH2)6] crystallizes orthorhombically with the lattice spacings a = 6.492 Å, b = 12.24 Å, and c = 21.33 Å with 8 formula units per unit cell. The space group is D–Pbca (No.61). The amide ions have a distorted close-packed arrangement with the layer sequence ABAC in the direction [010]. Ytterbium occupies on sixth, sodium one half of the octahedral interstices.  相似文献   

6.
The two novel thioantimonate(V) compounds [Mn(C6H18N4)(C6H19N4)]SbS4 ( I ) and [Mn(C6H14N2)3][Mn(C6H14N2)2(SbS4)2]·6H2O ( II ) were synthesized under solvothermal conditions by reacting elemental Mn, Sb and S in the stoichiometric ratio in 5 ml tris(2‐aminoethyl)amine (tren) at 140 °C or chxn (trans‐1, 2‐diaminocyclohexane, aqueous solution 50 %) at 130 °C. Compound I crystallises in the triclinic space group P1¯, a = 9.578(2), b = 11.541(2), c = 12.297(2)Å, α = 62.55(1), β = 85.75(1), γ = 89.44(1)°, V = 1202.6(4)Å3, Z = 2, and II in the monoclinic space group C2/c, a = 32.611(2), b = 13.680(1), c = 19.997(1)Å, β = 117.237(5)°, V = 7931.7(8)Å3, Z = 4. In I the Mn2+ cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS4]3— anion yielding a distorted octahedral environment. In II one unique Mn2+ ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn2+ ion is coordinated by two chxn ligands and two monodentate [SbS4]3— units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods.  相似文献   

7.
Synthesis and Crystal Structure of Ammonium Tetraamminelithium Amidotrithiophosphate‐Ammonia(1/1)(NH4)[Li(NH3)4][P(NH2)S3]·NH3 Colourless crystals of (NH4)[Li(NH3)4][P(NH2)S3]·NH3 were prepared by the reduction of P4S10 with a solution of lithium in liquid ammonia. The X‐ray structure determination shows them to contain the pseudo‐tetrahedral amidotrithiophosphate anion [P(NH2)S3]2− (point group CS), which is the hitherto unknown final member of a series of previously characterized amidothiophosphates. The ammonium ion and the ammonia molecule of solvation form an diamminehydrogen(1+)‐ion N2H7+ with a short, nearly linear hydrogen bond of 2.864(3) Å.  相似文献   

8.
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   

9.
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   

10.
We present the low‐temperature synthesis of potassium hexaamido zirconate(IV) from the transition metal tetrafluoride and thealkali metal dissolved in liquid ammonia at –40 °C. Potassium hexaamido zirconate(IV) K2[Zr(NH2)6] is the first ternary amide reported for elements of group 4 of the periodic table It crystallizes with a novel structure type in the trigonal space group R$\bar{3}$ c with a = 6.5422(2) Å, c = 32.824(2) Å, V = 1216.66(9) Å3, Z = 6 and c/a = 5.017. The structure can be derived from the K2PtCl6 type. The compound contains discrete D3‐symmetric [Zr(NH2)6]2– anions which differ significantly from octahedral shape. Quantum chemical calculations show the distortion to arise from a splitting of degenerate d‐orbitals on the zirconium atom leading to a significant gain in energy.  相似文献   

11.
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   

12.
Dissolution of solid AgNCO (silver isocyanate) in aqueous ammonia (25 %) and subsequent crystal growth at T = –9 °C furnished the new ammoniate (NH3)Ag(NCO) as colorless crystals [P21/c (no. 14); a = 4.1817(3) Å, b = 14.445(1) Å, c = 6.1988(5) Å, β = 102.0(4)°, V = 365,6(2) Å3; Z = 4]. In the molecular monammine complex, which is only stable at temperatures below T = 0 °C, silver is in a twofold, however, asymmetrical coordination by the isocyanate anion and ammonia. At the reaction conditions applied, AgNCO does not form an ionic diammine species (e.g. [Ag(NH3)2]+) as known from related silver salts. In this sense, the solvation chemistry of AgNCO exhibits a rarely observed feature.  相似文献   

13.
(LiI)2Li3SbS3 was prepared by solid‐state reaction of stoichiometric amounts of LiI, Li, Sb, and S in the ratio 2 : 3 : 1 : 3. The product is air and moisture sensitive. The crystal structure was determined from single crystals at room temperature. Colourless to pale yellow (LiI)2Li3SbS3 crystallizes in the orthorhombic system, space group Pnnm (no. 58) with a = 10.436(1)Å, b = 13.509(1)Å, c = 7.530(1)Å, V = 1061.6(1)Å3, and Z = 4 (data at 20 °C). The crystal structure of (LiI)2Li3SbS3 is closely related to that of (CuI)2Cu3SbS3 and (AgI)2Ag3SbS3, at least for the positions of I, Sb, and S. Thus, iodine forms an eutactic arrangement which resembles the structure of hexagonal diamond. [SbS3]3— units are embedded in this framework in a way that the sulphur atoms of two adjacent trigonal pyramids form distorted octahedral voids. The lithium ions are tetrahedrally coordinated and fully ordered within the anionic framework. The three‐dimensional connectivities in (LiI)2Li3SbS3 are significantly different from the homologous copper and silver compound due to the bonding necessities of Li and slightly different radii of the monovalent cations. Thus, a novel three‐dimensional network of edge sharing tetrahedra is observed in (LiI)2Li3SbS3. It exhibits strands of eight‐membered rings of edge sharing tetrahedra which are linked by common vertices and cross linked by double tetrahedra.  相似文献   

14.
NaPPh2, prepared from sodium and PClPh2 in refluxing dioxane, crystallises from dioxane as [Na4(μ‐dioxane)8/2(μ‐dioxane)(PPh2)4] ( 1 ), in which the basic structural features are eight‐membered Na4P4 rings, linked by intermolecularly bridging dioxane molecules to give a three‐dimensional network, and inclusion of one dioxane molecule inside the eight‐membered ring. 1 crystallises in the orthorhombic space group Cmc21 (no. 36), T = 203(2) K, a = 27.377(1) Å, b = 10.579(1) Å, c = 23.608(1) Å, V = 6837.3(6) Å3, Z = 4, and the absolute structure parameter 0.3(2). The refinement converged to R1 = 0.0632, wR2 = 0.1701 (for reflections with I > 2σ(I)), R1 = 0.0707, wR2 = 0.1781 (all data).  相似文献   

15.
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   

16.
A Comparison of the Crystal Structures of the Tetraammoniates of Lithium Halides, LiBr·4NH3 and LiI·4NH3, with the Structure of Tetramethylammonium Iodide, N(CH3)4I Crystals of the tetraammoniates of LiBr and LiI sufficient in size for X‐ray structure determinations were obtained by slow evaporation of NH3 at room temperature from a clear solution of the halides in liquid ammonia. The compounds crystallize in the space group Pnma (No. 62) with four formula units in the unit cell: LiBr·4NH3: a = 11.947(5)Å, b = 7.047(4)Å, c = 9.472(3)Å LiI·4NH3: a = 12.646(3)Å, b = 7.302 (1)Å, c = 9.790(2)Å For N(CH3)4I the structure was now successfully solved including the hydrogen positions of the methyl groups. N(CH3)4I: P4/nmm (No. 129), Z = 2, a = 7.948(1)Å, c = 5.738(1)Å The ammoniates of LiBr and LiI crystallize isotypic in a strongly distorted arrangement of the CsCl motif. Even N(CH3)4I has an CsCl‐like structure. Both structure types differ mainly in their orientation of the [Li(NH3)4]+ — resp. [N(CH3)4]+ — cations with respect to the surrounding “cube” of anions.  相似文献   

17.
Cs2Ba(O3)4 · 2 NH3, the First Ionic Alkaline Earth Metal Ozonide Cs2Ba(O3)4 · 2 NH3 is the first ionic ozonide containing an alkaline earth metal cation. Its synthesis has been achieved via partial cation exchange of CsO3 dissolved in liquid ammonia. According to a single crystal X‐ray structure determination (Pnnm; a = 6.312(2) Å, b = 12.975(3) Å, c = 8.045(2) Å; Z = 2; R1 = 4.6%; 848 independent reflections) ozonide anions, cesium cations and ammonia molecules form a CsCl‐type arrangement, where Cs+ and NH3 occupy one half of the cation sites, each. Ba2+ is coordinated by four ozonide groups and two ammonia molecules. Because of a short hydrogen bond to one of the terminal oxygen atoms, the respective O–O‐distance in the ozonide ion is longer than the other. The shortest intermolecular O–O‐distance ever observed in ionic ozonides has been found in this compound, which can be taken as a first clue for the radical ozonide anion to dimerize like the isoelectronic SO2 does.  相似文献   

18.
The monoammoniate of lithium amidoborane, Li(NH3)NH2BH3, was synthesized by treatment of LiNH2BH3 with ammonia at room temperature. This compound exists in the amorphous state at room temperature, but at ?20 °C crystallizes in the orthorhombic space group Pbca with lattice parameters of a=9.711(4), b=8.7027(5), c=7.1999(1) Å, and V=608.51 Å3. The thermal decomposition behavior of this compound under argon and under ammonia was investigated. Through a series of experiments we have demonstrated that Li(NH3)NH2BH3 is able to absorb/desorb ammonia reversibly at room temperature. In the temperature range of 40–70 °C, this compound showed favorable dehydrogenation characteristics. Specifically, under ammonia this material was able to release 3.0 equiv hydrogen (11.18 wt %) rapidly at 60 °C, which represents a significant advantage over LiNH2BH3. It has been found that the formation of the coordination bond between ammonia and Li+ in LiNH2BH3 plays a crucial role in promoting the combination of hydridic B? H bonds and protic N? H bonds, leading to dehydrogenation at low temperature.  相似文献   

19.
Potassium Triamidostannate(II), K[Sn(NH2)3] – Synthesis and Crystal Structure Rusty‐red crystals of K[Sn(NH2)3] were obtained by the reaction of SnBr2 and KNH2 in a 1 : 3 molar ratio in liquid ammonia at 233 K in the form of platelets. The structure was determined from single crystal X‐ray diffractometer data: Space group P3; Z = 2; a = 6.560(1) Å, c = 7.413(2) Å. The structure contains trigonal pyramidal complex anions [Sn(NH2)3] and potassium cations. These ions are arranged to one another following the motif of a strongly distorted hexagonal close packing of sequence A(Sn) B(Sn) A′(K) B′(K) …  相似文献   

20.
Synthesis and Crystal Structures of [P(C6H5)4][1-(NH3)B10H9] and Cs[(NH3)B12H11] · 2CH3OH The reduction of [1-(NO2)B10H9]2? with aluminum in alkaline solution yields [1-(NH3)B10H9]? and by treatment of [B12H12]2? with hydroxylamine-O-sulfonic acid [(NH3)B12H11]? is formed. The crystal structures of [P(C6H5)4][1-(NH3)B10H9] (triclinic, space group P1 , a = 7.491(2), b = 13.341(2), c = 14.235(1) Å, α = 68.127(9), β = 81.85(2), γ = 86.860(3)°, Z = 2) and Cs[(NH3)B12H11] · 2CH3OH (monoclinic, space group P21/n, a = 14.570(2), b = 7.796(1), c = 15.076(2) Å, β = 111.801(8)°, Z = 4) reveal for both compounds the bonding of an ammine substituent to the cluster anion.  相似文献   

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