COMPLEX SALTS [Pd(NH3)4][Pd(NH3)3NO2] [CrOx3]·H2O AND [Pd(NH3)4][Pd(NH3)3NO2] [CoOx3]·H2O AND SOLID SOLUTIONS [Pd(NH3)4] [Pd(NH3)3NO2][CoOx3]x[RhOx3]1–x·H2O : PROMISING PRECURSORS FOR POROUS NANOALLOYS

Journal of Structural Chemistry - New complex salts [Pd(NH3)4][Pd(NH3)3NO2][CrOx3]·H2O I, [Pd(NH3)4][Pd(NH3)3NO2][CoOx3]·H2O II, and a series of solid solutions...     

Structure of [NH3(CH2)4NH3]2P4O12·2H2O

After a short survey of what is the present state of the cyclophosphates associated with the organic molecule NH₂(CH₂)₄NH₂, we report chemical preparation and crystal structure for a new example of such compounds. [NH₃(CH₂)₄NH₃]₂P₄O₁₂.2H₂O is monoclinic (S.G. : P2₁/n), with Z = 2 and the following unit-cell parameters : a = 7.6728(8) Å, b = 18.962(3) Å, c = 7.9789(9) Å β = 111.751(9)°. Bidimensional layer arrangement of P₄O₁₂ rings connected to the water molecules thanks to weak H-bonds run parallel to the ab plane. The organic groupements located between these inorganic planes perform the three-dimensional cohesion by NH····O hydrogen bonds.     

Synthesis and structure of [Cr3O(CH3COO)6(H2O)3][UO2 (CH3COO)3] · 3H2O

Crystals of [Cr₃O(CH₃COO)₆(H₂O)₃][UO₂(CH₃COO)₃]·3H₂O (I) were synthesized for the first time and studied by X-ray crystallography. The crystals of I are orthorhombic: a = 8.3561(3) ?, b = 16.8421(5) ?, c = 25.7448(9) ?, V = 3623.2(2) ?³, space group P2₁2₁2₁, Z = 4, R = 0.0409. The structure is composed of trinuclear [Cr₃O(CH₃COO)₆(H₂O)₃]⁺ complexes and mononuclear [UO₂(CH₃COO)₃]^? complexes classified with crystal-chemical groups A₃M³B ₆ ² M ₃ ¹ (A = Cr³⁺, M³ = O^2?, B² = CH₃COO^?, M¹ = H₂O) and AB ₃ ⁰¹ (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^?), respectively. The complexes are bound to each other by electrostatic interactions and hydrogen bonds involving outer-sphere water molecules. The results of IR spectroscopic study of I are in good agreement with the structural data for the crystal.     

Synthesis and Characterization of [NH3（CH2）2NH2（CH2）2NH3]BiCl6

1 INTRODUCTION During the past decade, a series of organic-inor- ganic hybrid compounds based on metal halide units have been prepared and studied[1]. The combination of organic and inorganic components at the mole- cular level affords us the opportunity to design new hybrid materials and modulate the properties of components[2]. As a result, some interesting proper- ties, such as non-linear optical[3], interesting magne- tic[4], efficient luminescence[2], ideal thermal and mechanical sta…     

Dawson结构多金属氧酸电荷转移化合物[CH3NH2CH3]2[CH3NHCH3]4H4[P2W18O62]·H2O的合成、表征及晶体结构

钨磷酸;二甲胺;Dawson结构多金属氧酸电荷转移化合物[CH3NH2CH3]2[CH3NHCH3]4H4[P2W18O62]·H2O的合成、表征及晶体结构     

Synthesis, Structure Characterization and Biological Activity of Layered Vanadium Oxides [ NH3 （ CH2 ）2 NH （ CH2 ）2 NH3 ] [ V6 O14 ]

Introduction Over the past decades, polyoxometalates(POMs)have been attracting extensive interestowing to the widerange of their topological properties and potential appli-cations in catalysis, photochemistry, electrochromism,and magnetism[1,2]. Meanwhile, owing to the potentialapplication of polyoxometalaes as anticancer and antivi-ral drugs, their complexes have attracted increasing in-terest of both inorganic chemists and biochemists[3]. Itis well known that polyoxometalates are excellent …     

Solvothermal Synthesis and Crystal Structure of [H2N（CH2）2NH3]{Co[H2N（CH2）2NH2]3}[SbSe4]

1 INTRODUCTION The chalcogenidometallates with open frame- works have attracted considerable interest as pos- sible zeolite-like materials, of which highly interes- ting properties could be expected. Over the last de- cades a large number of thioanti…     

The Synthesis and Characterization of [4-CH3OC6H4CH2NH3]4P2O7·6H2O

Inorganic–organic hybrid compounds exhibit interesting properties in several application areas. In this regard, chemical preparation and characterization by X-ray diffraction, thermal analysis, and IR spectroscopy are given for a new organic cation diphosphate [4-CH₃OC₆H₄CH₂NH₃]₄P₂O₇·6H₂O. This later crystallizes in a C2/c unit cell with a = 38.238(6)Å, b = 6.453(1)Å, c = 16.942(7)Å; β = 97.60(4)°; Z = 4; and V = 4144(2)ų and D_x = 1.377 g·cm^?3. Its crystal structure has been determinated and refined to R = 0.044, using 7978 independent reflections. This atomic arrangement consists of inorganic layers built up from P₂O₇ ^4? anions and water molecules. On these layers, which are parallel to the (b, c) planes, the (4-CH₃OC₆H₄CH₂NH₃)⁺ cations are anchored through multiple hydrogen bonds.     

同多化合物[C6H5CH2NH(CH3)2]4[Mo8O26]·4H2O的合成与晶体结构

以MoO3和C6H5CH2N(CH3)2为原料,制得[C6H5CH2NH(CH3)2]4[Mo8O26]·4H2O,并通过扩散法得到无色透明晶体.X射线单晶衍射表明,晶体属三斜晶系,空间群为P墿,晶胞参数a=1.0685(2)nm,b=1.4050(3)nm,c=1.0643(2)nm,α=93.12(3)°,β=110.26(3)°,γ=71.41(3)°,V=1.4179(5)nm3,R=0.0383.     

[(CH3)2NH2]3[NSiMo12O40]·2DMF·4H2O的合成和晶体结构

电荷转移盐;[(CH3)2NH2]3[NSiMo12O40]·2DMF·4H2O的合成和晶体结构     

Synthesis and Structure of Trinuclear Iron Acetate [Fe3O(CH3COO)6(H2O)3][AuCl4]·6H2O

Iron acetate of composition [Fe₃O(CH₃COO)₆(H₂O)₃][AuCl₄]·6H₂O (I) was synthesized and investigated by X-ray diffraction analysis and Mössbauer spectroscopy. The [Fe₃O(CH₃COO)₆(H₂O)₃]⁺ complex cation has a structure typical for ₃-O bridged trinuclear ferric compounds with iron atoms lying at the vertices of a regular triangle with an oxygen atom at the center. The iron atoms are each coordinated by 4 oxygen atoms of the four bridging carboxylic groups, the ₃-O bridging atom, and the coordinated water molecule in the trans-position to the latter. In the trinuclear cation, the Fe(III) ions are coupled by antiferromagnetic exchange interactions with the exchange parameter J = -29.0 cm ^–1 (HDVV model for D _3h symmetry). The specific role of the solvate water molecules in structure formation is discussed.     

Hydrothermal synthesis,crystal structure and thermal stability of a new 2D layered metal(II) phosphonate: [NH3CH2CH2NH3][Fe2(O3PCH(OH)CO2)2(H2O)2]·2H2O

In the presence of ethylenediamine template agents, a metal(II) phosphonate, [NH₃CH₂CH₂NH₃][Fe₂(O₃PCH(OH)CO₂)₂(H₂O)₂]?·?2H₂O (1) has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction as well as infrared spectroscopy, elemental analysis and thermogravimetric analysis. The compound crystallines in the monoclinic space group P2₁/n: Crystal data for 1: a?=?8.4523(8)?Å, b?=?9.8196(9)?Å, c?=?10.9217(10)?Å, β?=?105.9500(10)°, V?=?871.58(14)?Å, Z?=?2, D _c?=?2.103?g?cm^?3, R ₁?=?0.0290, wR ₂?=?0.0811. The Fe (II) cation is octahedrally coordinated by six oxygen atoms from the three ligands and one coordinated water molecule to form a 2D layered structure with a one-dimensional channel system in the a-axis direction.     

Structural and Physicochemical Studies of [4-ClC6H4CH2NH3]4Li2P6O18·4H2O

The crystal structure of a new organic cation cyclohexaphosphate, [4-ClC ₆ H ₄ CH ₂ NH ₃ ] ₄ Li ₂ P ₆ O ₁₈ .4H ₂ O, is reported. It crystallizes in the triclinic system (space group P-1) with the following unit-cell parameters: a = 9.628(8), b = 12.801(9), c = 19.528(6) Å, α = 78.60(4)°, β = 83.00(5)°, β = 89.98(4)°, Z = 2, and V = 2341(3)Å ³ . The structure has been solved using direct methods and refined by least-squares analysis [R ₁ = 0.043, wR ₂ = 0.108]. The structure can be described as infinite anionic layers with composition of [Li ₂ (P ₆ O ₁₈ )(H ₂ O) ₄ ] ^{4 ?} and parallel to the ac plane. The organic groups are located in the accessible voids. The molecules are stabilized by O─H…O and N─H…O types of intermolecular hydrogen bonds in the unit cell in addition to Van der Waals forces.     

Macro-, Micro-, Nano- and Crystal Structures of a Homodinuclear Complex [NH3（ CH2）3NH3]2{Na2[（C6H4O2）2]（C6H4O2H）2}

A homodinuclear complex （NH3CH2CH2CH2NH3）2 {Na2[（C6H4O2）2] （C6H4O2H）2} （1） has been synthesized by a solution-based self-assembly route. It crystallized in monoclinic system with space group P21/c. Every sodium ion coordinates in a tetragonal prism fashion with two O atoms of a terminal chelating catecholate ligand and three O atoms from two bridging catecholate ligands. Two neighboring NaO5 tetragonal prisms are edge-shared and centrosymmetric with regard to the inversion center to form a binuclear cluster {Na2[（C6H4O2）2]（C6H4OOH）2}^4- anion. The complex anions were aligned parallelly by n-n interaction and linked with the protonated 1,3-propylenediamine through hydrogen bonds which were assembled into a multi-lamellar structure with channels. The crystal exhibits rectangular geometry with an interior triangle hollow structure under optical microscopy. And the scanning electron microscopy （SEM） indicates that the wall of the tubes shows multi-lamella morphologies. Further, the transmission electron microscopy （TEM） reveals that the crystal is composed of multi-lamellar nano-tubes with diameters less than 100 nm. The molecular structure of the complex was compared with that of its isomer complex 2.     

二维配位聚合物(NH3+CH2CH2NH3+)(NH2CH2CH2NH3+)2[(VO)4(PO4)4(H2O)2]·2H2O的水热合成及晶体结构

无机-有机杂化钒氧酸盐由于其结构的多样性以及在催化、医药、光、电、磁等材料领域中的应用前景而受到人们的广泛关注。近年来这一研究领域的重大进步是将有机氮配体或者过渡金属配合物直接连接到矾氧骨架上以获得各种新奇结构。合成出许多属于L/V/O、MXLY/V/O、L/P/V/O和MXLY     

Synthesis and X-ray diffraction study of cs3[UO2(CH3COO)3]2[UO2(CH3COO)(NCS)2(H2O)] and Cs5[UO2(CH3COO)3]3[UO2(NCS)4(H2O)] · 2H2O

Cs₃[UO₂(CH₃COO)₃]₂[UO₂(CH₃COO)(NCS)₂(H₂O)] (I) and Cs₅[UO₂(CH₃COO)₃]₃[UO₂ (NCS)₄(H₂O)] · 2H₂O (II) have been synthesized via the reaction between uranyl acetate and cesium thiocyanate in aqueous solution. According to single-crystal X-ray diffraction data, both compounds crystallize in monoclinic system with the unit cell parameters a = 18.7036(5) Å, b = 16.7787(3) Å, c = 12.9636(3) Å, β = 92.532(1)°, space group C2/c, Z = 4, R = 0.0434 (I); and a = 21.7843(3) Å, b = 24.6436(5) Å, c = 13.1942(2) Å, β = 126.482(1)°, space group Cc, Z = 4, R = 0.0273 (II). Uranium-containing structural units of compound (I) are mononuclear [UO₂(CH₃COO)₃]^? and [UO₂(CH₃COO)(NCS)₂(H₂O)]^? moieties, which correspond to the AB ₃ ⁰¹ and AB⁰¹M ₃ ¹ crystallochemical groups (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^?, M¹ = NCS^? and H₂O). The structure of compound II is built of [UO₂(CH₃COO)₃]^? and [UO₂(NCS)₄(H₂O)]^2? complexes, which belong to the AB ₃ ⁰¹ and AM ₅ ¹ crystallochemical groups, respectively. Uranium-containing complexes in both structures are linked into a framework by hydrogen bonds and electrostatic interactions with cesium cations. The IR spectra of compounds I and II agree well with X-ray diffraction data.     

Crystal structures of [Pd(NH3)3(NO2)][Rh(NH3)2(NO2)4] and [PdEn2][Rh(NH3)(NO2)5]·0.75H2O

The structure of double complex salts [Pd(NH₃)₃(NO₂)][Rh(NH₃)₂(NO₂)₄] and [PdEn₂][Rh(NH₃)(NO₂)₅]·0.75H₂O is determined by single crystal X-ray diffraction. In the structures, the main structural moieties are identified.     

Crystal structure and thermal properties of [Pt(NH3)5Cl][ReCl6]Cl·H2O

The crystal structure of double complex salt [Pt(NH₃)₅Cl][ReCl₆]Cl·H₂O is determined. Crystallographic characteristics are: a = 23.9502(4) Å, b = 7.5963(1) Å, c = 8.9016(2) Å, V = 1619.49(5) ų, space group Pnma, Z = 4, d _x = 3.150 g/cm³. The packing of structural fragments is studied. It is shown that on heating the salt in a helium atmosphere up to 840 °C a mixture of two solid solutions of fcc Pt_0.90Re_0.10 and hcp Pt_0.25Re_0.75 forms.     

Synthesis and Structure of [Pd(NH3)4][cis-Pd(NH3)2(SO3)2][Pd(NH3)3(SO3)] · H2O

A new palladium compound [Pd(NH₃)₄][cis-Pd(NH₃)₂(SO₃)₂][Pd(NH₃)₃(SO₃)] · H₂O (I) was synthesized and its structure was studied by X-ray powder diffraction method. In the course of the synthesis, the initial trans-diamminesulfite anionic complex is transformed into the cis-configuration. Further heating in aqueous solution results in isomerization of a substance into a neutral complex [Pd(NH₃)₃(SO₃)]. Crystals I are triclinic: a = 10.3297(2) Å, b = 14.1062(3) Å, c = 6.8531(1) Å, = 101.36(0)°, = 92.74(0)°, = 92.71(0)°, space group P1¯. Structure I consists of the columns with alternating cis-[Pd(NH₃)₂(SO₃)₂]^2– and [Pd(NH₃)₃(SO₃)] complexes and [Pd(NH₃)₄]²⁺ ions between the columns.     

Synthesis,Crystal and Molecular Structures of [Co(MH)2(Thio)2][BF4] · H2O and [Co(DH)2(NH3)2][BF4]

Crystal structures of [Co(MH)₂(Thio)₂][BF₄] · H₂O (I) and [Co(DH)₂(NH₃)₂][BF₄] (II), where MH^– is H₃C–C(NOH)–C(NO^–)–H and DH^– is H₃C–C(NOH)–C(NO^–)–CH₃, were determined by X-ray diffraction. The crystals are monoclinic, space group C2/c, unit cell parameters (for I and II, respectively): a = 22.018(2) Å, b = 7.943(1) Å, c = 11.681(1) Å, = 92.68(1)° and a = 21.436(2) Å, b = 6.400(2) Å, c = 12.389(2) Å, = 113.13(1)°. In both cases, the Co(III) coordination polyhedron is a centrosymmetrical trans-octahedron, N₄S₂ for I and N₆ for II. In the crystals of I and II, the complex cations and the outer-sphere [BF₄]^– anions (and the crystal water molecules in I) form elaborate hydrogen bonding system.