Preparation and X-ray structure of [(methyl quinaldate)2H]+ [AuBr4]−

The crystal structure of the title complex (R _F =0.051 for 2384 observed MoK data) consists of a packing of tetrabromoaurate(III) anions and [(methyl quinaldate)₂H]⁺ cations in which the two planar heterocyclic ring moieties are interlinked by a proton to form a NHN hydrogen bond of length 2.88(1) Å; the dihedral angle of the planes is 79.5°. The infrared spectrum of the compound is also discussed.     

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.     

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.     

Synthesis and structural characterization of [VS4(CuPPh3)4Br]·CH2Cl2

Heating a solid mixture of (NH₄)₃VS₄, CuCl, PPh₃, and NEt₄Br at 100°C for 10 h and extraction with CH₂Cl₂ yielded [VS₄(CuPPh₃)₄Br]·CH₂Cl₂. Crystallographic data: Triclinic, P1¯, a = 15.189(3), b = 20.093(6), c = 12.031(3) Å, = 102.39(2), = 100.05(2), = 82.86(2)°, V = 3517(3) ų, and Z = 2. The configuration of the VS₄Cu₄Br core can be described as a distorted cubane with an additional face. The V atom has retained the tetrahedral geometry of the free [VS₄]^3– moiety. The four Cu atoms have three different coordination environments, strongly distorted tetrahedral, nearly trigonal planar, and strictly trigonal planar. The infrared, electronic, and ⁵¹V NMR spectra have also been reported.     

Structure of tetrasodium nitrilotrimethylenetriphosphonatozincate tridecahydrate Na4[N(CH2PO3)3Zn] · 13H2O,an inhibitor of scaling and corrosion

The structure of a crystal hydrate of tetrasodium nitrilotrimethylenetriphosphonatozincate Na₄[N(CH₂PO₃)₃Zn] · 13H₂O is determined (space group $P\bar 1$ , Z = 2, a = 11.2208(2) Å, b = 11.2666(3) Å, c = 12.3286(3) Å, α = 108.455(2)°, β = 97.168(2)°, and = 117.103(2)°, Z = 2). The complex has a chelate structure; the inner coordination sphere includes three five-membered N-C-P-O-Zn cycles, which share the Zn-N bond. An oxygen atom of a neighboring complex completes a distorted trigonal bipyramidal coordination of the Zn atom.     

Synthesis and structure of (NH4)3[UO2(C3H2O4)2(NCS)] · 2H2O

Malonate-thiocyanate complex (NH₄)₃[UO₂(C₃H₂O₄)₂(NCS)] · 2H₂O is synthesized and studied by X-ray diffraction. The compound crystallizes in the monoclinic system: a = 13.9983(4) Å, b = 8.1947(2) Å, c = 16.4678(4) Å, β = 100.846(1)°, space group Cc, Z = 4, and R = 0.0158. The main structural units of the crystal are mononuclear [UO₂(C₃H₂O₄)₂(NCS)]^3? groups belonging to the AB ₂ ⁰¹ M ₁ crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ , B ⁰¹ = C₃H₂O ₄ ^2? , M ¹ = NCS^?). Discrete uranium-containing groups are connected by electrostatic interactions with ammonium ions and by hydrogen bonds. Some specific structural features of crystals containing [UO₂(L)₂(NCS)]^3? complexes, where L is the oxalate or malonate ion, are discussed.     

Molecular structure and hydrogen bonding of 4-dimethylaminopyridinioacetate in its crystalline dihydrate and hydrochloride trihydrate,L·2H2O and [L2H]Cl·3H2O (L=p-Me2NC5H4N+CH2CO2 −)

The crystalline dihydrate and hydrochloride trihydrate of a new betaine, namely, L·2H₂O (1) and [L₂H]Cl·3H₂O(2) (L=p-Me₂NC₅H₄N⁺CH₂CO₂), have been synthesized and characterized by X-ray crystallography. Molecule L in compound1 [space groupPbcn, witha=15.732(3),b=7.894(2),c=18.304(4) Å, andZ=8] possesses approximateC _s symmetry. The formation of hydrogen bonds by water molecules bridging neighboring carboxy oxygen atoms leads to an infinite two-dimensional network composed of a packing of two different kinds of 12-membered rings. In compound2 [space group PT witha=7.341(2),b=9.543(2),c=17.010(4) Å, =82.43(2)°, =80.34(2)°, =74.05(2)°, andZ=2], the carboxylate groups of a pair of betaine molecules are bridged by a proton to form a dimeric cation L₂H⁺ with a very strong asymmetric hydrogen bond of length 2.464(7) Å. The crystal structure features a hydrogen-bonded corrugated ribbon comprising an alternate arrangement of edge-sharing centrosymmetric (H₂O)₄(Cl^–)₂ and (H₂O)₄ rings running parallel to thea axis.     

[Co(H2O)6](C18H15O4SO3)2·4H2O的合成和晶体结构

以芒柄花素为先导化合物,合成了水溶性的[Co(H2O)6](C18H15O4SO3)2·4H2O,并采用IR, 1H NMR, TG-DTA, XRD和单晶X射线衍射法对其结构进行了表征.单晶X射线衍射结果表明:[Co(H2O)6]2+、C18H15O4SO 3和H2O之间存在多种氢键,形成晶体结构中的亲水区.异黄酮骨架间反平行排列,面对面和边对面芳香堆积作用同时存在于其中,构成晶体结构中的疏水区.磺酸根是连接亲水区和疏水区的桥梁.氢键、芳香堆积作用以及阴阳离子之间的静电引力共同将标题化合物组装成具有三维网络结构的超分子.     

On the Crystal Structures of the Polymorphs of Manganese(II) Chloride Tetrahydrate: α-MnCl2·4H2O and β-MnCl2·4H2O

Journal of Chemical Crystallography - The manganese(II) chloride tetrahydrate MnCl2·4H2O (α-form) crystallizes in the space group P21/n with a?=?6.1918(4) Å,...     

2-pyridylbis(diphenylphosphino)methane chemistry. Synthesis and structures of [Cu(μ−η2:η1(Ph2P)2−CHC5H4N)(THF)]2(BF4)2 and [Ni(Ph2PCH2C5H4N)2]-[NiCl4]·0.85CH2Cl2and [Ni(Ph2PCH2C5H4N)2]-[NiCl4]·0.85CH2Cl2

Reaction of 2-pyridylbis(diphenylphosphino)methane (NPP) with [Cu(NCMe)₄]BF₄ and with [Ni(H₂O)₆]Cl₂ forms [Cu(NPP)(THF)]₂(BF₄)₂ (after recrystallization in the presence of THF) (1) and NiCl₂(NPP) (2) respectively Attempts to recrystallize2 led ultimately to the ligand cleavage product [Ni(Ph₂PCH₂C₅H₄N)₂][NiCl₄]·0.85CH₂Cl₂ (3). Complex1 crystallizes in the monoclinic space groupP2₁/n witha=13.148(2),b=19.221(2),c=13.458(2) ų, β=108.61(1)^o,V=3222.6(8) ÅZ=2. The structure was refined onF ² toR1=0.11,wR2=0.14 (R1=0.044 forI≥2σ(I)) for 5661 observed reflections. Complex3 crystallizes in the triclinic space groupP1 witha=12.795(2),b=17.535(1),c=10.203(1) Å, α=107.564(6), β=114.260(8), γ=78.435(8)^o,V=1982.1(8) ų;Z=2. The structure was refined onF toR1=0.044,R _w=0.059 for 3534 observed reflections. Dinuclear complex1 has crystallographically imposed centrosymmetry with the NPP ligands arranged in a head-to-tail fashion. The Cu...Cu separation of 3.372(1) Å is too long to support significant metal-metal interaction. Complex3 results from the cleavage of a {PPh₂} unit from the NPP ligand and contains an approximately square nickel atom surrounded by two Ph₂PCH₂C₅H₄N ligands coordinated in a head-to-head fashion.     

Crystal Packing of Potentially Mesomorphic Azobenezene Derivatives R1–C6H4–N=N–C6H4–R2 (R1, R2 = CH3COO,C2H5O; CH2=C(CH3)COO,C2H5; C6H13COO,C2H5O)

Crystallography Reports - The structure and thermal properties of azobenzene derivatives R1–C6H4–N=N–C6H4–R2, where R1/R2 = CH3COO/C2H5O (I), CH2=C(CH3)COO/C2H5 (II), or...     

Synthesis,crystal structure and spectral studies of the complex [Ni(C3H4N2)4(H2O)2]·(C6H4COSO2N)2

The title compound has been synthesized and its crystal structure determined at room temperature.M _r =731.39, triclinic, space groupP¯1,a=9.020(3),b=11.280(7),c=7.784(2)Å,=97.05(4),=97.08(2), =105.32(4)°, U=748(1)ų,Z=1,D _calc.=1.624 g/cm³. The finalR is 0.030 for 3095 independent observed reflections withI3(I). The crystal structure consists of repeated [Ni(im)₄(H₂O)₂]²⁺ cations and noncoordinated saccharin anions. In the complex cation [Ni(im)₄(H₂O)₂]²⁺, Ni² is bonded to four N atoms from four imidazole molecules and two O atoms from two water molecules forming an approximately square octahedral stereochemistry. The d-d transition spectrum of the title compound is also reported and is explained perfectly with the scaling radial theory which was proposed by us.     

Crystal and molecular structure of complex compound [Fe3O(CH3COO)6(H2O)3]2[ZnCl4] ⋅ 2H2O

The X-ray crystal structure of trinuclear iron acetate [Fe₃O(CH₃COO)₆(H₂O)₃]₂ [ZnCl₄] ? 2H₂O was determined. The crystal has a ionic structure. It is monoclinic, a = 25.363(7), b = 14.533(4), c = 15.692(4) Å, β = 103.11(2)°, space group _C2/c, and R = 0.0685. The structure of the cationic complex [Fe₃O(CH₃COO)₆(H₂O)₃]⁺ is typical of trinuclear iron(III) compounds containing a μ₃-O bridge: the iron atoms are situated at the vertices of an almost equilateral triangle with the O atom at the center. Each Fe atom is coordinated by four O atoms of bridging carboxy groups, the μ₃-bridging O atom, and the water molecule in the trans position to the latter O atom. Mössbauer spectroscopy evidence indicates the high-spin state (_S = 5/2) of the iron(III) ions.     

Structure of chlorotris(1,3,5-triaza-7-phosphaadamantane)platinum(II) chloride hydrate methanolate, [Pt(PTA)3Cl] [Cl]·H2O·CH3OH

The title compound chlorotris(PTA)platinum(II) chloride hydrate methanolate (PTA=1,3,5-triaza-7-phosphaadamantane), [C₁₉H₄₂Cl₂N₉O₂P₃Pt] is monoclinic, witha=10.832(1),b=21.306(7),c=12.702(3)Å,=100.42(5)°,V=2883(2)ų,Z=4,D _x=1.814 g cm^–3,=53.0 cm^–1,F(000)=1568,T=298K in space groupP2₁/c. The structure was solved by heavy atom and Fourier methods and refined toR=0.051 for 4319 unique observed reflections. The complex exhibits approximately square-planar geometry about the Pt atom and a significant trans effect, with bond lengths Pt-Cl1=2.3371(2), Pt-C12 (ionic)=4.463(4), Pt-P _{trans(to cl)}=2.233(2), Pt-P _cis,ave=2.323(3)Å and bond angles Cl-Pt-P _cisave 83.60(3), P _trans -Pt-P _cis,ave 96.49(6)°. The H₂O is apparently hydrogen bonded to two N atoms on different cations, and the methanol OH group to the chloride anion.     

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.     

Production of Complex Hydrosulphates in the K3H(SO4)2–Rb3H(SO4)2 Series: Part I

Crystallography Reports - The phase equilibria in the K3H(SO4)2–Rb3H(SO4)2–H2O cross section have been investigated under isothermal conditions at 25°C. The concentration limits of...     

Synthesis and crystal structure of 3-ammoniumphenyl sulfone selenate, 3-aminophenyl sulfone [C12H14N2O2S]SeO4 · [C12H12N2O2S]

The crystal structure of [C₁₂H₁₄N₂O₂S]SeO₄ · [C₁₂H₁₂N₂O₂S] was determined by X-ray diffraction on single crystal. Crystals are orthorhombic, space group Pbca, with cell parameters a = 11.545 (1), b = 8.143 (1), c = 55.783(1)Å, V = 5244.2 (8)ų and Z = 8. The structure can be described as organic layers built by [C₁₂H₁₄N₂O₂S]²⁺ cations and [C₁₂H₁₂N₂O₂S] molecules, parallel to ab plane, between which the inorganic groups SeO ₄ ^2? are inserted. In this atomic arrangement, H-bonds between the different species play an important role in the three-dimensional network cohesion.     

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.