Crystal structure of triethylentetraammonium bis monohydrogenmonophosphate dihydrate, [NH3(CH2)2NH2(CH2)2NH2(CH2)2NH3](HPO4)2 · 2H2O

The salt triethylentetraammonium bis monohydrogenmonophosphate dihydrate is monoclinic with the following unit cell dimensions: a = 8.462(1), b = 10.500(1), c = 9.520 Å, = 99.297(1)°, space group P2₁/n with Z = 2. The structure was solved by the Patterson method and refined to final R value of 0.043 for 1590 independent reflections. The structure consists of infinite parallel two-dimensional [ 01] planes built of mutually connected ions and water molecules by strong O—H···O and N—H···O hydrogen bonding.     

Crystal structure of triethylentetraammonium bis monohydrogen-monophosphate dihydrate β-NH3(CH2)2NH2(CH2)2NH2(CH2)2NH3(HPO4)2·2H2O

The salt triethylentetraammonium bis monohydrogen-monophosphate dihydrate is orthorhombic Pbca with unit cell dimensions a = 8.963(2), b = 10.326(2), c = 17.381(4)Å; Z = 4; D_m = 1.540 g cm^–3; D _x = 1.562 g cm^–3. The examination of the structure shows a layer arrangement parallel to the axis: planes of [HPO₄]^2– tetrahedra alternate with planes of [(NH₃(CH₂)₂NH₂CH₂)₂]⁴⁺. The [HPO₄]^2– tetrahedra are connected through O(W)s--H···O hydrogen bonds, so that infinite chains of the composition [HPO₄(H₂O)]_n ^2n– are formed in the structure parallel to the axis. The structure of this compound is built from [HPO₄]^2– anions, [(NH₃(CH₂)₂NH₂CH₂)₂]⁴⁺ cations and zeolitic water molecules connected by hydrogen bonds.     

Crystal structure of NH3(CH2)2NH3BiCl5·2H2O

The ethylenediammonium pentachlorobismuthate(III) dihydrate salt is monoclinic with the following unit cell dimensions: a = 10.902(8)Å, b = 7.926(6)Å, c = 15.199(6)Å, = 96.40(1)°, space group P2₁/n with Z = 4. The structure shows a layer arrangement parallel to the axis: planes of the [Bi₂Cl₁₀]^4– bioctahedra alternate with planes of [NH₃(CH₂)₂NH₃]²⁺ dications. The [Bi₂Cl₁₀]^4– bioctahedra are connected through O(W)–H··· Cl hydrogen bonds, so that infinite unidimensional chains of composition [Bi₂Cl₁₀(H₂O)₂] _n ^4n– are formed in the structure parallel to the axis. These chains are themselves interconnected by means of the N–H···Cl bonds originating from the [NH₃(CH₂)₂NH₃]²⁺ entities, forming a three-dimensional network.     

Crystal structure of Al(tBu)3(NH2CH2CH2Ph): A molecular “slinky”

The molecular structure of Al(^tBu)₃(NH₂CH₂CH₂Ph) is determined by the crystal packing of the phenyl rings and the pseudo spherical Al(^tBu)₃ units, and may be viewed as a layered structure consisting of double sheets of the phenyl rings and the Al(^tBu)₃ units. The Al–N–C–C linkage shows severe disorder as a result of its flexibility. The structure of Al(^tBu)₃ (NH₂CH₂CH₂Ph) can be likened to a molecular slinky, in which the rigid ends are fixed in space by molecular packing forces, leaving the interior link to adopt multiple orientations. Crystal data: orthorhombic, Cmca,a=13.282(9),b=25.01(1),c=13.210(9), Å,V=4388(10) ų,Z=4,R=0.0957,R _w=0.0957.     

Copper(I) nitrate π-complexation: Synthesis and crystal structure of [(CH2=CH−CH2)2NH2][Cu(NO3)2] compound

By means of alternating current electrochemical synthesis, triclinic crystals of [(C₃H₅)₂NH₂][Cu(NO₃)₂] -complex were obtained: space group ,a=7.218(2),b=7.536(2),c=10.231 (3) Å, =74.75(3), =82.47(3), .=77.22(3)°, andD _meas=1.80(1)g cm^–3 forZ=2. The structure consists of diallylammonium cations which form two -coordinate bonds to the same copper atom. Oxygen atoms from NO₃-anions complete the trigonal pyramidal metal environment. The coordinated C=C bonds are lengthened to 1.349(5) and 1.369(5) Å.     

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.     

Cyclic dithiophosphate salts [Et3NH+[(OCH2CMe2CH2O)P(S)S]− and [Et3NH]+[CH2{6-t-Bu-4-Me-C6H4O}2P(S)S]−

X-ray structures of the cyclic dithiophosphate salts [Et₃NH]⁺[(OCH₂CMe₂CH₂O)P(S)(S)]^– (1) and [Et₃NH]⁺[CH₂{6-t-Bu-4-Me-C₆H₄O}₂P(S)S]^– (2) have been determined. Crystal data for 1: Tetragonal, P4₂/m, a = 13.416(7), b = 13.416(2), c = 9.153(2) Å, and Z = 4. Crystal data for 2 = Monoclinic, P2₁/c, a = 19.1112(17), b = 14.649(9), c = 22.7166(19) Å, = 102.883(7)°, and Z = 8. The six- and eight-membered rings in 1 and 2 have chair and boat-chair conformations respectively. Both of these compounds show weak N—H······S hydrogen bonds; interestingly, in 2 both two-center and three-center hydrogen bonds are observed in the solid state.     

Synthesis, Structure and Properties of (H2NCH2CH2NH3)3 {(VO)6 [B10O16 (OH)6]2} · 11H2O

Abstract A new polyoxovanadoborate cluster (H₂NCH₂CH₂NH₃)₃ {(VO)₆[B₁₀O₁₆(OH)₆]₂} · 11H₂O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA. The crystal of the new compound belongs to monoclinic system, space group C2/c with a = 20.198(1) ?, b = 13.4476(8) ?, c = 21.602(1) ?, β = 97.067(1)°, V = 5822.8(5) ?³, Z = 4, D _c = 1.956 g cm⁻³, M = 1714.4, μ = 1.066 mm⁻¹, S = 1.905, R = 0.059, R _w = 0.0966. Index Abstract A new polyoxovanadoborate cluster (H2NCH2CH2NH3)3{(VO)6 [B10O16(OH)6]2} · 11H2O was prepared by hydrothermal technique and characterized by single crystal X-ray diffraction analysis, IR and TGA.      

Crystal and molecular structure of [(C6H5)2P(=0)(CH2CH2N(CH3)3 +][I−]

The title compound crystallizes in the centrosymmetric triclinic space group withZ=4. The crystallographic asymmetric unit contains two independent cations; interatomic distances within these include P=O=1.47(1) and 1.47(1) Å, P–C₆H₅=1.78(2)–1.81(1)Å and P–CH₂CH₂NMe₃ ⁺=1.80(1) and 1.81(1) Å. The phosphine oxide moiety is involved in intermolecular hydrogen bonding ()...H–C, with O...H2.42Å) and the iodide is involved in I...H–C contacts with I...H3.10Å.     

Low-temperature X-ray studies of a [(CH3)2NH2]2 · CuCl4 crystal

The a, b, c lattice parameters of a [(CH₃)₂NH₂]₂ · CuCl₄ crystal have been measured by the X-ray diffraction method within the temperature range of 100–300 K. The temperature dependences of thermal expansion coefficients α_a = f(T), α_b = f(T), and α_c = f(T) along the principal crystallographic axes and thermal expansion coefficient of the unit-cell volume αV = f(T) are determined. It is found that all the three parameters, a, b, and c, vary with temperature in a complicated way and show jumplike anomalies in the a = f(T), b = f(T), and c = f(T) curves at phase-transition temperatures T _c1 = 255 K and T _c2 = 279 K. An incommensurate phase with the modulation wave vector q _i = (1/2 + δ)(a* + c*) is revealed in the temperature range 279–296 K. It is shown that the incommensurability parameter δ increases with an increase in temperature.     

Hydrothermal synthesis and X-ray structure: A reduced titanic molybdenum(V) phosphate (NH3CH2CH2NH2)5Na [Ti2Mo12O30(PO4)(HPO4)4(H2PO4)3]⋅6H2O

A novel titanic molybdenum(V) phosphate (NH₃CH₂CH₂NH₂)₅Na [Ti₂Mo₁₂O₃₀(PO₄) (HPO₄)₄(H₂PO₄)₃]6H₂O crystallizes in the triclinic space group P1 with a = 12.057(3) Å, b = 14.668(2) Å, c = 21.2680(10) Å, = 80.840(10)°, = 82.960(10)°, = 76.65(2)°, and D _c = 2.707 g cm^–3 for Z = 2, Refinement based on 12,037 observed reflections led to R = 0.0609. The result of single crystal x-ray diffraction revealed the presence of a tunnel and two crystallographically independent clusters in the solid state structure. The plane layers in its solid-state structure are interconnected in-sheet (axial) through multipoint hydrogen bonding between the ethylenediamine nitrogen atoms and the cluster oxygen atoms.     

Neutron refinement of the crystal structure of partially exchanged taurine, (ND 3 + )0.65(NH 3 + )0.35(CH2)2SO 3 −

Refinement of neutron-diffraction data from a partially deuteriated single crystal of taurine, 2-aminoethylsulfonic acid, confirms the zwitterion structure, ND ₃ ⁺ (CH₂)₂SO ₃ ^? , at room temperature; the S?C?C?N torsion angle of thegauche configuration in the solid state is ?69.4⁰. Hydrogen positions have been located more precisely than in the earlier X-ray analysis to yield apparent bond lengths N?D/H=1.02(1) Å and C?H=1.08(1) Å.     

Structural characterization of a series of cyclohexaphosphates: M0.5((C6H5CH2)2NH2)5P6O18·H2O (M = Co, Cu, Cd)

Three new cyclohexaphosphates with general formula M_0.5((C₆H₅CH₂)₂NH₂)₅P₆O₁₈·H₂O (M=Co, Cu, Cd) are reported. They crystallize with monoclinic unit-cells and are isotropic. We have determined their structure from the salt M=Co. This later exhibits the following unit-cell parameters: a = 22.739(5), b = 17.682(3), c = 18.342(3) Å, = 91.22(1)°, Z = 4,P2₁/n, V = 7373 ų, and Dx = 1.373 g cm^–3. The atomic arrangement can be described as layers containing P₆O₁₈ ring anions and CoO₆ octahedra spreading in the (101) planes and intercalated by the dibenzylammonium groups and the water molecules. Synthesis and characterization by X-ray diffraction, IR absorption, and TA are described.     

三维孔道结构钒磷酸盐[H3N(CH2)3NH3]2[H3N(CH2)3NH2][H2N(CH2)3NH2]-[V(H2O)2(VO)8(OH)4(PO4)4(HPO4)4]·4H2O的水热合成和结构表征

以1,3-丙二胺为模板,水热合成了三维孔道结构钒磷酸盐[H3N(CH2)3NH3]2[H3N(CH2)3NH2][H2N(CH2)3NH2][V(H2O)2(VO)8(OH)4(PO4)4(HPO4)4]·4H2O(DAP-V9P8).用单晶X射线衍射、红外光谱和热重法对该化合物的晶体结构进行了表征.DAP-V9P8的无机骨架由[VO5]、[VO6]、[PO4]和[HPO4]通过共顶点连接而成.孔道中充填的丙二胺分子随所处结晶学位置不同,有三种完全不同的分子构象.其中,位于//b轴直径达1.82nm椭圆形孔道中心的丙二胺分子碳链呈独特的直线状分布.晶体学参数:a=1.4820(9)nm,b=1.0255(4)nm,c=1.8181(9)nm,β=90.391(8)°;P21/n(No.14);R1=0.0772,wR2=0.2004(I＞(2σI)).与等结构的其它化合物进行了系统的结构比较.     

Crystal structure of N-benzylmethylammonium dihydrogen-monophosphate monohydrate, [C6H5CH2NH2CH3]H2PO4·H2O

The salt N-benzylmethylammonium dihydrogenmonophosphate monohydrate is monoclinic with the following unit cell dimensions: a = 6.356(1)Å, b = 8.385(7)Å, c = 11.472(5)Å, = 104.32(1)°, space group P2₁ with Z = 2. 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.     

Growth and Study of Properties of Mixed Crystals (NH4)2NixCo1 –x(SO4)2 · 6H2O

Crystallography Reports - Mixed crystals (NH4)2NixCo1 –x(SO4)2 · 6H2O have been grown from aqueous solutions of different compositions by reducing the solution temperature in two growth...     

Synthesis and structural analysis of (μ-SCH2CH2CH2S-μ)Fe2(CO)5(2-C5H4NPPh2)

Treatment of (μ-SCH₂CH₂CH₂S-μ)Fe₂(CO)₆ with equimolar 2-C₅H₄NPPh₂ in the presence of Me₃NO·2H₂O in CH₂Cl₂/MeCN solutions gave the title complex (μ-SCH₂CH₂CH₂S-μ)Fe₂(CO)₅(2-C₅H₄NPPh₂) in 76% yield. The title complex was characterized by spectroscopy as well as by single crystal X-ray diffraction analysis. The molecular structure consists of a butterfly [Fe₂S₂] cluster with propane, five carbonyls, and 2-C₅H₄NPPh₂. In the crystal packing diagram, intermolecular C–H···O hydrogen bonds between phenyl and carbonyl groups stabilize the solid state.     

Synthesis,Structure, and Properties of the Tris(ethylendiamine)nickel(II) Dichloride Dihydrate [Ni(H2NCH2CH2NH2)3]Cl2 ⋅ 2H2O Crystals

Crystallography Reports - The conditions for synthesis of [Ni(H2NCH2CH2NH2)3]Cl2 ⋅ 2H2O ([Ni(en)3]Cl2 ⋅ 2H2O) crystals from aqueous solutions have been considered. The synthesized...     

Crystal structure of radical cation salt (BEDT-TTF)4(GaCl4)2 · C6H5CH3

A new radical cation salt based on bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF) with the tetrahedral anion GaCl ₄ ^? , namely, (BEDT-TTF)₄(GaCl₄)₂ · C₆H₅CH₃, has been synthesized. The crystal structure of this salt is determined by X-ray diffraction analysis [a = 31.757(2) Å, b = 6.8063(3) Å, c = 34.879(2) Å, β = 90.453(4)°, V = 7538.8(7) ų, space group I2/c, and Z = 4]. In the structure, the radical cation layers alternate with the anion layers along the c-axis. The anion layers consist of the GaCl ₄ ^? tetrahedra and solvent molecules. The packing of BEDT-TTF molecules in the radical cation layer differs from that in the structure of the known salt (BEDT-TTF)₂GaCl₄, even though both compounds exhibit semiconductor properties.     

Molecular structure of [CpRu(PPh3)2(C6H11SH)]BF4·CH2Cl2

The structure of the [CpRu(PPh₃)₂(C₆H₁₁SH)]BF₄·CH₂Cl₂ complex was determined by X-ray diffraction techniques; triclinic space group ,a=12.567(1),b=13.409(1),c=14.733(1) Å, =95.380(7), =111.041(7), =96.454(8)°,V=2278.5(4) ų,Z=2,R=0.056,R _w=0.088. The Ru is attached to two triphenylphosphine ligands, a cyclopentadienyl and the S atom of the cyclohexylthiol. The Ru–S distance is 2.389(2) Å and the S–H distance is 1.23 Å.