Crystal structures of bis(cyanido)bis(N,N′-diethylthiourea-κS) mercury(II) and bis(cyanido)bis(N,N′-dipropylthiourea-κS) mercury(II)

Two mercury(II) complexes containing cyanide and, N,N′-diethylthiourea (detu) and N,N′-dipropylthiourea (dprtu) ligands, [(detu)₂Hg(CN)₂] (1) and [(dprtu)₂Hg(CN)₂] (2), respectively, have been prepared and characterized by X-ray crystallography. In the both complexes Hg atom lies on a 2-fold rotation axis, and is coordinated to the sulfur atoms of two thiourea ligands and to two cyanide carbon atoms. Both have a distorted tetrahedral environment with bond angles about the Hg atoms in the range of 93.41(4)°–146.75(19)°. In the crystal structures symmetry related molecules are linked via N-H-N hydrogen bonds resulting in the formation of a two-dimensional network in 1, while in 2 a double stranded one-dimensional chain is formed.     

Synthesis,Spectral, Thermal and Structural Study of Monoaquabis(Acetylsalicylato-κO)bis(Nicotinamide-κN)Copper(II)

Abstract  

The compound has been formed by mononuclear [Cu(C₉H₇O₄)₂(C₆H₆N₂O)₂(H₂O)] units in which the metal ion as well as the water ligand lies on a twofold symmetry axis, so that only one acetylsalicylate ligand and one nicotinamide ligand are independent. The distortion from ideal five-coordinate geometries can be described best by the degree of trigonality τ. For a regular square-pyramidal (SQP) geometry the trigonality parameter is 0 and for a trigonal–bipyramidal (TBP) structure it increases to 1. The copper coordination geometry is that of a square pyramid (τ = 0.23), with the N atoms from nicotinamide ligands and the bonded carboxylate O atoms from acetylsalicylate ligands defining the quasi-planar square base. The apical site is occupied by the aqua ligand, a bond which coincides with the twofold symmetry axis and is thus exactly perpendicular to the basal plane. The thermal decomposition takes place in four steps: removing of moisture, dehydration of aqua ligand, the elimination of the nicotinamide (na) ligand and the decomposition of acetyl-groups and oxidation of salicylate ion ligands. In complex, all ligands are coordinated to the metal ion as monodendate. The IR spectra of the intermediate products showed similar results.     

Synthesis and crystal structure of [{V3(μ-Cl)4(μ 3-Cl) (μ 3-OH)(thf)2(teeda)}2]·2(thf) (teeda = N,N,N′N′-tetraethylethane-1,2-diamine)

The title complex was prepared from the reaction of [V₂(-Cl)₃(thf)₃]₂[Zn₂Cl₆] with N,N,NN-tetraethylethane-1,2-diamine (teeda) in refluxing thf and its crystal structure exhibits two triangulo-[V₃(-Cl)₃(-Cl)( ₃-OH)(thf)₂(teeda)]⁺ cations bridged by two chlorides. The molecular structure (monoclinic, space group P2 ₁/n, Z = 2, a = 11.8005(7) Å, b = 18.7492(14) Å, c= 15.6253(9) Å, = 103.600(4) shows each vanadium site in a distorted octahedral geometry. V1 and V2 have two thf molecules bounded in cis configuration, and V3 completes the hexa-coordination with the diamine teeda. Main bond distances are 2.5149(12) Å for V(1)--Cl(1), 2.062(3) Å for V(1)- ₃-O(3), 2.5554(12) Å for V(1)- ₃-Cl(4), 2.140(3) Å for V(1)–O(1)(thf), 2.243(4) Å for V(3)–N(1)(teeda), and 3.0437(9) for V(1)···V(2).     

The structure of N,N′-bis(2-hydroxyphenyl)butanediamide

The structure of N,N-bis(2-hydroxyphenyl)butanediamide has been determined. The molecule consists of two 2-hydroxyphenyl moieties which are attached (at the 2 position) to the two nitrogens of the butanediamide. The compound C₁₆H₁₆N₂O₄ crystallizes in the monoclinic space group P2₁/c witha=5.576(1),b=4.8853(6),c=25.397(6) Å and =90.58(1)°.     

Crystal structure of [Yb(L(NO3)2(H2O)2](NO3), L = bromo-N,N,N′,N′-tetraethylmalonamide

[Yb(L(NO₃)₂(H₂O)₂](NO₃), L = bromo-N,N,N,N-tetraethylmalonamide crystallizes in the triclinic spacegroup P-1 with cell dimensions a = 9.030(9), b = 12.036(12), c = 12.392(13) Å, = 84.52(1), = 77.58(1), = 67.21(1)° , d_calc = 1.935 g cm^-3 for Z = 2. The ytterbium atom in the complex cation is nine-coordinate being bonded to two oxygen atoms from the malonamide ligand, two nitrate anions, and three water molecules.     

Co(II)(C7H7O2N)2(C12H12N2)2微晶粉体的水热合成及表征

本文以对氨基苯甲酸和联苯胺为配体,通过水热合成制备Co(II)的配合物,得到Co(II)(C7H7O2N)2(C12H12N2)2(C7H7O2N= p-aminobenzoic acid, p-abza, C12H12N2= Benzidine)深蓝色微晶颗粒.通过元素分析、IR等方法对配合物进行了表征,并通过TG分析对该配合物的热稳定性及热分解机理做了初步探讨.     

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.     

Hydrogen Bonding Patterns of Coordinated Ligands in Hybrid Materials: Crystal Structures of Hydronium Tetra(Thiocyanato-κN)-Zinc(II): Tris(2-Amino-4,6-Dimethylpyrimidinium) (2-amino-4,6-dimethylpyrimidine) Dinitrate and Bis(2-Amino-4,6-Dimethylpyrimidinium) Tetrachlorocobaltate(II) Monohydrate

Abstract  

Hydronium tetra(thiocyanato-κN)-zinc (II) tri (2-amino-4,6-dimethylpyrimidinium) 2-amino-4,6-dimethylpyrimidine dinitrate [H₃O⁺ Zn(NCS)₄ 3(C₆H₁₀N₃ ⁺) C₆H₉N₃ 2(NO₃)⁻] and bis(2-amino-4,6-dimethylpyrimidinium) tetrachlorocobaltate(II) monohydrate [2(C₆H₁₀N₃ ⁺)] CoCl₄ H₂O have been synthesized and characterized by X-ray diffraction analysis and spectroscopic studies. In compound 1, the coordination geometry around zinc is distorted tetrahedral, Zn being bonded to four N atoms from the thiocyanate anions. In compound 2, the anion [CoCl₄]²⁻ displays distortion from ideal tetrahedral geometry. The 2-amino-4,6-dimethylpyrimidine cations are not directly coordinated to zinc/cobalt, but are hydrogen bonded to the thiocyanate/chloride ions. In both the compounds the protonated nitrogen N1 and the 2-amino group are hydrogen bonded to the nitro group/chloride ions/water molecule through N–H···O and N–H···Cl hydrogen bonds to form R₂²(8) motifs. In both the compounds, the pyrimidine cations also form base pairs via a pair of N–H···N hydrogen bonds involving the amino group and the unprotonated ring N atom. The crystal structures are further stabilized by N–H···S, O–H···O, C–H···O and C–H···Cl hydrogen bonds.     

Crystal structure of calcium (Ornithinato-N (α), N (δ), N (δ )-triacetato)cobaltate(III) octahydrate Ca[Co(Orntra)]2 ⋅ 8H2O

The X-ray crystal structure of calcium (ornithinato-N _(α) N _(δ) N _{(δ )}-triacetato)cobaltate(III) octahydrate Ca[Co(Orntra)]₂ ? 8H₂O has been determined. The crystals are orthorhombic, a = 21.163(4) Å, b = 8.391(2) Å, c = 19.101(4) Å, V = 3391.9(9) ų, Z = 4, and space group Pca2₁. In the trinuclear linear molecule [Co(μ-Orntra)]₂Ca(H₂O)₅, two independent anions [Co(Orntra)]^? are joined with the Ca²⁺ cation by the bridging bonds through the terminal O atoms. In each [Co(Orntra)]^? anion, the Co atom occurs in the octahedral environment of two N atoms and four O atoms of the Orntra ligand and closes four five-membered and one seven-membered chelate rings. Two O atoms of two anions occupy axial vertices in a pentagonal bipyramid of the Ca²⁺ ion. Five O(H₂O) atoms are located in the equatorial plane. The asymmetric C atoms in the anions bound to the same Ca²⁺ cation have an identical absolute configuration. The crystal involves the molecules belonging to both configurations. The coordinated and outer-sphere H₂O molecules participate in an extended system of hydrogen bonds.     

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.     

Synthesis and structural characterization of a (N,N′-bis[2(S)-pyrrolidylmethyl]-propane-1,3-diamine) nickel (II) complex

The nickel(II) complex [Ni(C₄H₃NCH=N–(CH₂)₃–N=CHC₄H₃N)], (1) containing the symmetrical N₄ tetradentate Schiff base ligand, which is the 2:1 condensation product of pyrrole-2-carboxaldehyde and 1,3-diaminopropane respectively, was prepared. Structural investigation shows that it is monomeric, having space group P2₁/c, a = 7.989(7), b = 17.406(14), c = 9.193(5) Å, = 90, = 100.39(6), = 90, and Z = 4. The coordination geometry around the nickel atom is slightly distorted square planar and the conformation of the six-membered ring containing the metal,azomethine nitrogens and three carbon atoms of the connecting 1,3-diaminopropane is a symmetric boat.     

Reaction of trimethylaluminum and trimethylgallium with bifunctional amines: Syntheses and molecular structures of [Me2Al−N(CH2CH2)2−C−(OCH2)2]2 and [Me2Ga−N(Si(H)Me2)2]2

The crystalline products [Me₂Al–N(CH₂CH₂)₂–C–(OCH₂)₂]₂ (I) and [Me₂Ga–N(Si(H)Me₂)₂]₂ (II) were prepared from reactions of trimethylaluminum and trimethylgallium with 1,4-dioxa-8-azaspiro[4.5]-decane and 1,1,3,3-tetramethyldisilazane, respectively, in toluene. The organoaluminum dimer crystallizes in the monoclinic space groupP2₁/c with unit cell parametersa=8.970(2) ,b=9.683(2) ,c=12.833(3) , =103.18(2)°,V=1085.3(3) ³, andD _calcd=1.22 g cm^–3 forZ=2. Least-squares refinement based on 935 observed reflectionsI>3(I) in the range 3.5°<2<45.0° led to a finalR factor of 0.033 (R _w =0.041). The dimeric organosilazagallium crystallizes in the triclinic space group with unit cell parametersa=7.636(2) ,b=9.168(2) ,c=9.466(3), =72.81(2)°, =87.94(2)°, =69.90(2)°,V=593.0(3) ³, andD _calcd=1.30 g cm^–3 forZ=1. Least-squares refinement based on 1661 observed reflectionsI>3(I) in the range 3.5°<2<48.0° led to a finalR factor of 0.055 (R _w =0.070). Both compoundsI andII reside about a crystallographic center of symmetry and contain a planar M₂N₂ (M=Al forI, Ga forII) four-membered ring withI having an Al...Al contact of 2.801 .     

Crystal structure of 1,3-(N,N′-benzamide)-2-methyl-1-pentene

Crystals of the title compound are monoclinic (C20H22N2O2): space groupP2₁/n,a=11.800(3),b=13.820(2),c=11.004(3) Å,=92.74(3)°. The structure was solved by direct methods and refined by block-matrix least-squares procedure to giveR=0.078 andRw=0.076 for 1960 reflections above 3(I). The two amide groups are not coplanar with respect to their benzene rings. An intramolecular N-HO hydrogen bond was found in the molecules which are joined in chains by other strong N-HO hydrogen bonds.     

Structure of bis[α-(1,2,4-triazole-1-yl)-acetophenone] dichorozinc(II) complex [ZnCl2(C2H2N3CH2COPh)2]

The crystal and molecular structure of [ZnCl₂(N⁴-trzCH₂COPh)₂] (trz = 1,2,4-triazole) has been determined by X-ray crystallography. It crystallizes in the monoclinic system, space group C2/c, with lattice parameters a = 26.7892(4) Å, b = 4.9392(2) Å, c = 20.7872(1) Å, = 127.517 (1), and z = 4. The complex has C ₂ symmetry. The coordination geometry of each Zn atom is distorted tetrahedral formed by two Cl atoms and two tertiary N atoms of the -(1,2,4-triazole-1-yl)-acetophenone ligands. The two equivalent Zn–Cl and Zn–N bonds form bond angles around the Zn(II) atom in the range 101.4(1)–120.8(1). C–H O intermolecular interactions link the molecules in infinite chains in the [101] direction.     

Crystal structure of trans-W2(CO)6(PPh2H)2(μ2-PPh2)2

The molecular structure of trans-W²(CO)₆(PPh²H)²(₂-PPh²)² was determined by X-ray diffraction analysis. The two tungsten centers, bridged by two diphenylphosphido ligands, are separated by 3.0667(6) Å with W–P–W angles of 77.10(5) and 77.08(5). Average tungsten–phosphorus bond distances are 2.461(17) and 2.4576(21) Å for bridging and terminal phosphorus groups, respectively, with a range of 0.037 Å for the former and 0.001 Å for the latter. The complex crystallizes in the monoclinic space group P2₁/c with a = 19.282(4) Å, b = 12.158(2) Å, c = 21.294(9) Å, = 92.821(4), and Z = 4.     

孔道结构铁磷酸盐(C4H12N2)2[Fe6(HPO4)2(PO4)6(H2O)2]·H2O的水热合成及热变化过程研究

在与前人不同的条件下水热合成了孔道结构铁磷酸盐(C4H12N2)2[Fe6(HPO4)2(PO4)6(H2O)2]·H2O.用ICP、有机元素分析仪、TG-DTA、变温XRD、变温FT-IR等分析技术对其成份、物相和热变化过程进行了系统研究.结果表明,室温-330℃,化合物失去吸附水,有机模板哌嗪开始氧化脱氢;330-380℃,哌嗪环破坏,大部分有机模板和结晶水脱除,化合物结构骨架明显破坏;470℃化合物完全非晶化;650℃形成FePO4和Fe4(P2O7)3新物相.哌嗪起到平衡电荷和支撑结构的作用.哌嗪环破坏并脱除是导致结构破坏的根本原因.     

Synthesis,Crystal Structure,and Antibacterial Activity of Di-μ-chlorido-bis({2-[(4-methoxyphenyl)-iminomethyl]pyridine-κ2N,N'] Mercury(II)

Crystallography Reports - A coordination polymer [Hg(L)Cl2]n consisting of HgCl2 and Schiff base bidentate ligand (4-methoxyphenyl) pyridine-2yl methyleneamine (L) was prepared and structurally...     

Crystal Structures and Properties of Bis(2-Aminopyrimidine-N-)-Bis(Thiocyanato-N)Zinc(II) and Catena-[2-Aminopyrimidine-N- (μ-Thiocynanto-S,N)(Thiocyanato-S)Cadmium(II)]

Abstract  

Complexes [Zn(NCS)₂(2-AMP)₂] (2-AMP = 2-aminopyrimidine) 1 and [Cd(SCN)₂(2-AMP)₂]_n 2 are prepared and characterized by X-ray crystallographic methods. 1 crystallizes in the monoclinic, space group C2/c, with a = 13.5761(14), b = 8.3330(10), c = 13.5962(15) ?, β = 99.5450(10)°, V = 1516.8(3) ?³, Z = 4. In 1, the zinc atom is coordinated by four N atoms from two AMP and two NCS⁻. 2 crystallizes in the monoclinic, space group C2/c, with a = 9.7259(11), b = 19.332(2), c = 8.2149(9) ?, β = 99.817(2)°, V = 1522.0(3) ?³, Z = 4. Complex 2 is made up of 1D chains along a-axis. Each Cd is attached to four NCS⁻ bridges and two pendant 2-AMP ligands.     

Iodine Intercalation of Bi2Sr2Ca(n−1)CunOy(N=2,3) Superconductors by Using Reactants I2 or FeI2

Abstract

The change of superconductivity induced by intercalation is very interesting We have investigated on intercalation into Bi2212 single crystal and Bi2223 polycrystalline superconductors using FeI₂ or I₂ as reactant. The iodine intercalation by using FeI₂ as a reactant into Bi2223 phase is reported for first time as long as we know. In iodine intercalation into Bi2212 by using FeI₂ as reactant, the critical tem T_Conset in out-of-plane measurement has suddenly decreased on X=0.95. Similar changes of T_Conset with higher X have been observed independent of directions and reactants. T_Conset of I_xBi₂Sr₂CaCu₂O_y intercalated by FeI₂ is a little lower than one of I_xBi₂Sr₂CaCu₂O_y intercalated by I₂. This is likely due to the change of hall concentration induced by reduction of host In iodine intercalation into Bi2223, the smaller change of T_Conset with increasing amount of intercalant is likely due to the number of CuO₂ planes between ntercalant layers.     

配合物[Cu(C7H5N3O2)2·(H2O)2](NO3)2的合成、晶体结构及荧光性质

合成了标题化合物[Cu(C7H5N3O2)2·(H2O)2](NO3)2,并用元素分析、红外、紫外、X射线单晶衍射进行了表征.此外,还研究了配合物的荧光性质.结果表明,该晶体属三斜晶系,Pī空间群,a=0.72484(11) nm, b=0.81483(12) nm, c=0.92079(14) nm, α=69.425(2) o, β=78.031(2)o, γ=84.955(2) o, Z=1, F(000)=279, R1 = 0.0272, wR2 = 0.0715;在λex=370 nm的光激发下,配合物在739 nm出现特征荧光.