Crystal and molecular structure of cesium isothiocyanatotrimethylaluminate,Cs[Al(CH3)3NCS]

The crystal structure of the title compound has been determined from three-dimensional X-ray diffraction data, and refined by full-matrix least-squares techniques. The crystals belong to the monoclinic space groupP2₁/c, witha = 8.849(4),b = 13.798(5),c = 7.943(4) Å, = 102.98(3) °, andD _x = 1.85g cm^–3 forZ = 4. The finalR factor for 1283 observed reflections is 0.046. The aluminum atom is bonded to the nitrogen atom of the thiocyanate ligand, where the Al-N bond length is 1.94(1) Å. The SCN is linear, and the CN-Al angle is 175(1) °. The cesium ion exhibits four contacts less than 3.60 Å: Cs C(thiocyanate) = 3.39(1) Å, Cs C(methyl) = 3.52(1) Å, Cs C.(methyl) = 3.56(1) Å, and Cs N = 3.575(9) Å. The closest Cs S is 3.772(3) Å.     

Crystal structure and phase transition in the compound [C6H5CH2NH(CH3)2]TlCl4

The N‐N dimethyl benzylammonium tetrachlorothallate (III) [C₆H₅CH₂NH(CH₃)₂]TlCl₄ crystallizes in the monoclinic system P2₁/n at room temperature with the following unit cell dimensions: a = 7.725(3) Å, b = 14.080(5) Å, c = 13.697(4) Å, β = 91.2(2)° with Z = 4. The structure shows a layer arrangement perpendicular to the b axis: planes of [TlCl₄]^‐ tetrahedra alternate with planes of [C₆H₅CH₂NH(CH₃)₂]⁺ cations. The cohesion of the atomic arrangement is ensured by hydrogen bonds N‐H…Cl. Differential scanning calorimetric and optical birefringence measurements reveals a phase transition at T = 339K. Raman spectroscopic study and dielectric measurements were performed to discuss the mechanism of the phase transition. (© 2007 WILEY ‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of NH3(CH2)2NH3(BiI4)2·4H2O

The ethylenediammonium bis tetraiodobismuthate(III) tetrahydrate salt is monoclinic with the following unit cell dimensions:a=7.476(3)Å,b=13.194(3)Å,c=13.916(9)Å, β=95.22(6)°, space groupP2₁ lc withZ=2. The structure consists of disordered ethylenediammonium cations, water molecules and polynuclear anions in which slightly distored [BiI₆]^3? octahedra sharingcis edges are interconnected into chains. The [BiI₄]^? anions are connected through O(W2)?H...I hydrogen bonds, so that infinite two dimensional chains parallel to thea axis with anionic period [BiI₄(H₂O)]^? are formed in the structure. These chains are themselves interconnected by means of the O?H...I and N...O(I) bonds originating respectively from the water molecules and the ethylenediammonium entities, forming a three-dimensional network.     

Hydrothermal Synthesis,Crystal Structure,and Photoluminescent Properties of Li[UO2(CH3COO)3]3[Co(H2O)6]

Crystallography Reports - Single crystal of Li[UO2(CH3COO)3]3[Co(H2O)6] was prepared and found to crystallize in the monoclinic crystal system in the sp. gr. C2/c, with Z = 2, and unit cell...     

[(CH3)2NH]3[H3PMo12O40]的合成、结构及表征

通过水热合成法,成功合成了化合物[(CH3)2NH]3[H3PMo12O40],并通过单晶X射线衍射,IR,XRD,元素分析和电化学分析对该化合物进行表征.该化合物中,Keggin型磷钼酸之间通过氢键形成二维折叠层,这些层按照ABCD沿c轴方向堆积.二甲胺分子分布在层间,通过氢键连接相邻的来自不同层的两个Keggin型磷钼酸,将二维折叠层进一步拓展成三维超分子骨架.     

孔道结构钒铝磷酸盐(NH3CH2CH2NH2)[(VO)Al(PO4)2]的水热合成及热稳定性

用XRD,TG-DTA,FT-IR和SEM对水热法合成的孔道结构钒铝磷酸盐(NH3CH2CH2NH2)[(VO)Al(PO4)2]进行了热性能表征.该化合物中有机组份的分解温度,在氧化气氛中为305～529℃,在惰性气氛中为411～593℃.有机组分的分解逸出导致了结构的破坏,但晶体的微形貌没有发生明显的变化;温度继续升高,发生相变.该化合物热稳定性较其它含有机模板的孔道结构钒磷酸盐要高,主要原因在于结构中存在[AlO4]和[PO4]共顶连接而成的一维链,这种链增加了骨架的强度.     

N-亚水杨基正丁胺锌配合物的合成、谱学表征和晶体结构

以乙酸锌、正丁胺及水杨醛为原料在甲醇介质中反应,合成得到了席夫碱配合物N-亚水杨基正丁胺锌[Zn(CH3CH2 CH2CH2N=CHC6H4O)2],用元素分析、红外光谱、核磁共振氢谱和热重分析进行了谱学表征,培养了该配合物的单晶,并通过单晶X射线衍射测得其晶体结构为四方晶系, 空间点群为P-4,a=1.4380(2)nm,b=1.4380(2)nm,c=0.53803(18)nm,α=β =γ=90°,V=1.1126(4)nm3 ;Dc =1.247 g/cm3;Z=2;F(000) = 400;μ =1.12mm-1.锌离子位于变形四面体的中心,分别与两个席夫碱N原子和两个酚氧负离子形成配合物.     

Synthesis and molecular structure of [Al(CH3)2]2[C10H22N4] [Al(CH3)3]2: Condensation product of trimethylaluminum and a multidentate open-chain amine

The crystalline condensation product [Al(CH₃)₂]₂[C₁₀H₂₂N₄][Al(CH₃)₃]₂ is prepared from reaction of the multidentate open-chain amine 1,4-bis(3-aminopropyl)piperazine with trimethylaluminum in methylene chloride. The compound crystallized in the monoclinic space groupC2/c with unit cell parametersa=25.166(12),b=7.268(4),c=17.316(4) Å,=115.3(4)°, andD _c =1.06 g cm^–3 forZ=4. Least-squares refinement based on 1054 observed reflections with intensitiesI 3(I) in the range 2<2<45° led to a finalR factor of 0.053 (R _w =0.064). The title compound resides on a crystallographic center of symmetry with independent Al-N distances of 1.889(5), 2.058(5), and 2.030(5) Å.     

Molecular and crystal structures of halopentaamminerhodium-(III) complexes, [Rh(NH3)5Cl]Cl2 and [Rh(NH3)5Br]Br2

The crystal and molecular structures of the title compounds have been determined by three-dimensional single-crystal X-ray techniques. All crystallographic details are fully reported. The major chemical conclusion for the pair, [Rh(NH₃)₅Cl]Cl₂ and [Rh(NH₃)Br]Br₂, is that neither Cl nor Br exert a static intramoleculartrans effect. Furthermore, the two halogens have the same static electronic structural effect on the [Rh^III(NH₃)₅] fragment. The conclusions shed much light on spectroscopic, thermodynamic and kinetic data of other compounds.Work supported in part by NSF-traineeship (E.A.H.).The term trans effect will be employed to refer to static and kinetic behavior-the distinction will be apparent from the context of the discussion.     

Interaction of aromatic hydrocarbons with organometallic compounds of the main group elements: VI. Synthesis and crystal structure of cesium diiododimethylaluminatep-xylene solvate,Cs[Al(CH3)2I2]·C6H4(CH3)2

The crystal structure of thep-xylene solvate of cesium diiododimethylaluminate has been determined from counter data, and refined by full-matrix least-squares techniques. The crystals belong to the orthorhombic space groupC222₁ witha = 12.577(4),b = 9.311(3),c = 14.256(4) Å, andD _x = 2.19 g cm^–3 forZ = 4. The finalR value for 481 observed reflections is 0.036. The anion resides on a two-fold axis; the Al-I bond length is 2.647(4) Å, and the Al-C distance, 1.98(2) Å. Important bond angles include I-Al-I, 102.3(2) °; C-Al-C, 115(1) °; I-Al-C, 114(3) °; and I-Al-C, 106(3) °. The cesium ion also lies on the two-fold axis. Throughout the crystal the cesium ions are separated byp-xylene molecules. The Cs C distances average 3.84 Å. In the lattice the iodine atoms reside on thea,b face diagonals (and symmetry-related positions) and are situated almost exactly between the cesium ions. The Cs I contact, 3.925(1) Å, is consistent with a significant bonding interaction.For Part V see Atwood et al. (1978).     

Crystal structure of bis 4-benzyl piperidinium monohydrogenmonophosphate pentahydrate, [C6H5CH2CHCH2CH2NH2CH2CH2]2HPO4·5H2O

The salt bis 4-benzyl piperidinium monohydrogenmonophosphate pentahydrate is orthorhombic with the following unit cell dimensions: a = 11.235(2) Å, b = 27.924(6) Å, c = 9.321(4) Å space group Pca2₁ with Z = 4. The structure was solved by the Patterson method and refined to final R value of 0.049 for 1802 independent reflections. The flack parameter is 0.14 with an e.s.d. of 0.23. The structure consists of infinite parallel two-dimensional [110] planes built of mutually connected ions and water molecules by strong O—H,...,O and N—H,...,O hydrogen bonding. There are no contacts other than normal van der Waals interactions between the layers.     

Crystal structure of pentakis ethylenediammonium bis undecachlorodiantimonate(III) tetrahydrate, (NH3(CH2)2NH3)5(Sb2Cl11)2·4H2O

The pentakis ethylenediammonium bis undecachlorodiantimonate(III) tetrahydrate salt is monoclinic with the following unit cell dimensions:a=16.271(5) Å,b=13.004(4) Å,c=13.932(4) Å, β=111.72(2)°, space groupP2₁/c withZ=2. The structure was solved by Patterson methods and refined to a finalR value of 0.023 for 4435 reflections withF ₀>4σ(F ₀). The structure shows a layer arrangement perpendicular to thea axis: planes of the [Sb₂Cl₁₁]⁵⁻ bioctahedra alternate with planes of [NH₃(CH₂)₂NH₃]²⁺ dications. The [Sb₂Cl₁₁]⁵⁻ bioctahedra are connected through O−H...Cl hydrogen bonds, such that infinite chains of composition [Sb₂Cl₁₁(H₂O]_n ⁵ⁿ⁻ are formed in the structure, parallel to the twofold axis. These chains are themselves interconnected by means of N−H...Cl and O−H...Cl bonds originating from the [NH₃(CH₂)₂NH₃]²⁺ entities and the water molecules, respectively, and form a threedimensional network.     

Molecular structure of AlH3[N(CH2CH2)3CH]2

Reaction of AlH₃[N(CH₂CH₂)₃CH] with hexamethyltrisiloxane, (OSiMe₂)₃, gives rise to the bis-quinuclidine complex AlH₃[N(CH₂CH₂)₃CH]₂, which has been characterized by ¹H and ¹³C NMR spectroscopy and X-ray crystallography. The molecular structure of AlH₃[N(CH₂CH₂)₃CH]₂ consists of a trigonal bipyramidal aluminum with axial coordination of the quinuclidine ligands. Crystal data: orthorhombic, space group Pbcn, a = 10.6895(9), b = 12.266(1), c = 12.3794(9) Å, V = 1623.2(2) ų, and Z = 4.     

Crystal structure of [Co(o-SC6H4NH2){P(OMe)3}3]PF6

A cobalt-thiolato-phosphite complex [Co(o-SC₆H₄NH₂){P(OMe)₃}₃]PF₆ has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic space group with a = 10.590(4), b = 11.122(3), c = 13.577(5) Å, = 101.85(1), = 108.50(1), = 101.75(1)°, V = 1420.6(8) ų, and Z = 2. The structure comprises discrete [Co(o-SC₆H₄NH₂){P(OMe)₃}₃]⁺ cations and PF ₆ ^– anions where the metal atom is coordinated in a highly distorted square-pyramidal environment by one chelate o-SC₆H₄NH ₂ ^– (abt) and two P(OMe)₃ ligands in the basal positions, and a third P(OMe)₃ in the axial site with Co–N,, 1.847(5), Co–S, 2.166(2), Co–P, 2.157(2), 2.147(2), and 2.125(2) Å.     

Ether cleavage of [2.2.2]cryptand: synthesis and X-ray crystal structure of [NH(CH2CH2I)3][I5]

Treatment of [2.2.2]cryptand1 in toluene with HI(g) has resulted in the formation of a twophase liquid clathrate solution from which the complex [NH(CH₂CH₂I)₃][I₅]2 has been isolated and crystallographically characterized. Crystal data for2: triclinic, space group $P\bar 1$ ,a=9.301(3) Å,b=10.419(3) Å,c=11.078(3) Å, α=90.20(2)^o, β=103.28(2)^o γ=96.50(2)^o,D _c =3.57g/cm³,Z=2,R _f =0.054,R _w =0.054. The salt is a product of an ether cleavage of the macrobicycle. The crystal structure of2 contains [NH(CH₂CH₂I)₃]⁺ ions and zigzag chains of [I₅]^? ions which self-assemble to form alternating layers, of cations and anions.     

Synthesis and crystal structure of N-benzylmethy- lammonium pentachlorothallate (III), [C6H5CH2NH2CH3]2TlCl5

N-Benzylmethylammonium pentachlorothallate (III) salt crystallizes in the monoclinic system P2₁/c with the following unit cell dimensions: a = 10.9540 (8), b = 12.559(1), c = 18.099(2)Å, = 112.1(3)° and Z = 4. The examination of the structure shows an alternate stacking of inorganic layers of pentachlorothallate (III) anions and organic layers of [C₆H₅CH₂NH₂CH₃]⁺ cations parallel to the c axis. The cohesion forces of the packing of N-benzylmethylammonium units in the layer and between two adjacent layers are provided by hydrogen bonds (N—HsCl) and van der Waals contacts.