[Co(dmg)2Cl2]3·[Co(dmg)2Cl(OH)]·[Co(dmg)(phen)]·(H2O)4的合成和晶体结构

本文合成了一个复杂的单核配合物 [Co(H2dmg)2Cl2]3·[Co(H2dmg)2Cl(OH)]·[Co(Hdmg)(phen)]·(H2O)4 (H2dmg＝dimethylglyoxime, phen＝1,10-Phenanthroline).通过X射线衍射技术获得其单晶结构.在单晶结构中,每五个单核钴(II)的配位结构形成一个重复单元,是一个较为复杂的单晶.其空间群为P-1,晶胞参数为a＝1.3738nm;b＝1.4396nm;c＝1.8656nm.本文中我们将讨论该化合物的分子结构及相关光谱性质.     

The crystal structure of UO2Cl2(OH2)(MeCN)2·2MeCN

The crystal structure of UO₂Cl₂(OH₂)(MeCN)₂·2MeCN has been determined at 123 K. The crystal is orthorhombic, space group Pnma, witha=14.891(8),b=6.733(6),c=15.931(9) Å, andD _calc=2.18 g cm^–3 forZ=4. The finalR value for 951 unique observed [F ₀5(F ₀)] reflections is 0.064. The U atom is seven-coordinate, pentagonal bipyramidal. The two axial positions are occupied by the uranyl oxygen atoms. Within the equatorial plane lie two acetonitrile groups, two chlorine atoms and a water molecule, the latter positioned between the two chlorine atoms. All of the atoms except the uranyl oxygen atoms lie in crystallographic mirror planes. The water molecule is hydrogen bonded to the two uncoordinated solvent molecules. Several close contacts between the solvent methyl groups and chlorine atoms suggest weak C-H acidic interactions of the type C-HCl.     

Molecular structure of [trans-FeCl2(imidazole)4]Cl·THF·H2O

The structure of [trans-FeCl₂(imidazole)₄]Cl has been determined as the THF/H₂O solvate. The Fe-Cl and Fe-N distances in the cation are shorter than analogous trans-FeCl₂(L)₄ compounds, concomitant with the decreased ionic radius of Fe³⁺ versus Fe²⁺. Crystal data: orthorhombic, Pnma, a = 8.456(2), b = 20.991(4), c = 13.288(3) Å, V = 2358.6(8), andZ = 4.     

A hydrogen-bonded dichloromethane-perchlorate-water channel in the crystal structure ofcis-[Ru(bpy)2{PPh-(o-tolyl)2}Cl+][ClO4 −]·CH2Cl2·H2O

The complexcis-[Ru(bpy)₂{PPh(o-tolyl)₂}Cl⁺][ClO₄ ^–] crystallized from a solution in dichloromethane as the dichloromethane-water solvate. The structure was refined toR=4.5% for those 2433 reflections with |F _o|>6(|F _o|). The octahedral Ru(II) cation is associated with metal-ligand distances as follows: Ru–Cl=2.434(3)Å, Ru-PPh(o-tol)₂=2.382(2)Å, and Ru–N=2.037(7)–2.088(7)Å. The structure is stabilized by a hydrogen-bonded CH₂Cl₂...ClO₄ ^–...H₂O channel which incorporates adventitious water of crystallization.     

The synthesis and crystal structure of [La(OH2)5(phen)2]Cl3·4H2O·phen

[La(OH₂)₅(phen)₂]Cl₃·4H₂O·phen is centric, Pnna, witha=19.946(7),b=16.458(5),c=12.207(4)Å andD _calc=1.57 g cm^–3 forZ=4. The La(III) ion resides on a crystallographic twofold axis and is coordinated to four nitrogen atoms (from two phen molecules) and five water molecules resulting in a distorted tricapped trigonal prismatic geometry. An uncoordinated phen molecule, two chloride anions, and four uncoordinated water molecules are hydrogen bonded to the coordinated water molecules. The coordinated and uncoordinated phen molecules -stack diagonally through the unit cell.     

Crystal structure of [WBr2(CO)(PPh2Cy)2(η2-MeC2Me)]·CH2Cl2 (Cy = cyclohexyl)

[WBr₂(Co)(PPh₂Cy)₂(²-MeC₂Me)]·CH₂Cl₂ (Cy = cyclohexyl) crystallizes in the monoclinic space group, P2₁/n, with a = 10.606(12), b = 23.11(3), c = 18.19(2) Å, = 106.070(10) D_calc = 1.610g cm^–3 for Z = 4. The tungsten coordination geometry can best be considered as a distorted octahedron, with the but-2-yne ligand occupying one coordination site, which has a trans-Br(2) group. The equatorial plane is made up of trans-PPh₂Cy groups, with the bromo and carbonyl ligands occupying the other two sites.     

Structure of (meso-5,10,15,20-tetraphenylporphyrinato) dichlorophosphorus(V) chloride, [P(tpp)Cl2]+Cl−

The title compound [P(tpp)Cl₂]⁺Cl^– crystallizes in the space group P2₁/n witha=10.701(2),b=24.860(2),c=14.799(2), =94.24(2)°,Z=4. The phosphorus atom has an octahedral coordination geometry formed by the four nitrogen atoms (Np) of the porphyrinato group and the two chloride ions. The average phosphorus-chloride distance is 2.150(1) Å, with phosphorus situated 0.006 Å below the porphyrin ring.     

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.     

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 chloro[1-hydroxyethane-1,1-diphosphonato(3−)]ditin(II) monohydrate Sn2(HL)Cl · H2O

The synthesis and X-ray structure analysis of Sn₂(HL)Cl · H₂O, where HL ^3? is the anion of 1-hydroxyethane-1,1-diphosphonic acid, are reported. The coordination polyhedra of two independent tin(II) atoms are the Sn(1)O₂Cl and Sn(2)O₃ trigonal pyramids, in which one of the vertices is occupied by a lone electron pair (Sn-O, 2.144–2.218 Å and Sn-Cl, 2.573 Å). The pyramids are complemented by weaker Sn?O and Sn?Cl contacts to form severely distorted (3 + 3) octahedra. The SnO₂Cl and SnO₃ pyramids are linked by the HL ^3? bridging ligands into the [Sn₂(HL)Cl]₆ cyclic molecules, which, in turn, are joined by additional Sn?O, Sn?Cl, O(H₂O)?O(L), and O(H₂O)?Cl contacts with each other and with crystallization water molecules into a three-dimensional framework.     

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.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Synthesis and crystal structure of [WI(CO)(cis-dppen) η2-MeC2Me)2]I·CH2Cl2 {cis-dppen = bis(diphenylphosphino)ethene}

The complex [WI(CO)(cis-dppen)(²-MeC₂Me)₂]I·CH₂Cl₂(1) is prepared as a by-product from the reaction of equimolar quantities of [WI₂(CO)(NCMe)(²-MeC₂Me)₂] and cisdppen {dppen = bis(diphenylphosphino)ethene}. Complex 1, [WI(CO)(cis-dppen)(²-MeC₂Me)₂]I·CH₂Cl₂ crystallizes in the triclinic space group with a = 11.189(13), b = 12.331(14), c = 15.395(17) Å, = 83.61(1), = 86.06(1), = 64.48(1)°, U = 1904 ų, and Z = 2. The metal environment in the cation can best be considered as a distorted octahedron with the two but-2-yne groups taking up individual sites trans to phosphorus atoms of the dppen ligand. The coordination sphere is completed by mutually trans-carbonyl and iodide groups.     

Magneto-structural characterization of Cu4(prz)2(L)2Cl4 ·CH3CH2OH (LH=1,1-di-2-pyridyl-1-ethoxi methanol,przH=pyrazole)

The title compound, Cu₂C₁₇H₁₆O_2.5Cl₂, is a copper(II) complex, in which each dimeric unit has two copper atoms bridged by a pyrazolato ligand, a di(2-pyridyl)]methane ligand, and an oxygen atom from the modified methylene group that links the two pyridine rings (O-C-O-CH₂CH₃). The complex crystallizes in the monoclinic groupP2₁/n,a=7.7330(1),b=19.589(6),c=13.123(2)Å,=95.020(0)°,V=1980.3(7)ų,Z=4,F _w=514.3,D _Do =1.725 g cm^–3(MoK)=0.71073 Å,F(000)=1032,=2.44 mm^–1, R=0.044 for 2209 observed reflections,Rw=0.047,s=0.086. Each dimer is linked to the next unit by long chlorine bonds (Cu(2)-Cl(1)=2.846(2)Å). These tetrameric units form zigzagged chains through copperchlorine bonds of 3.380(2)Å. The copper(II) complex presents antiferromagnetic behavior withT _m=161 K.     

Crystal structure ofcis-[Ru(bpy)2{PPh2(o-tol)}Cl][ClO4]·1.5(CH2Cl2), a structure containing both ordered and disordered dichloromethane molecules of crystallization

The complexcis-[Ru(bpy)₂ {PPh₂(o-tol)}Cl][ClO₄] crystallizes from dichloromethane as the sesqui-dichloromethane solvate. The complex crystallizes in the monoclinic space group P2₁/n with Z=4. The structure was refined toR=5.50% for those 2552 independent reflections with |F ₀|>6(|F ₀|) The octahedral Ru(II) cation is associated with the following bond lengths: Ru-PPh₂(o-tol)=2.360(3)Å. Ru–Cl=2.433(2)Å and Ru–N(bpy)=2.041(8)–2.095(8)Å. Both the perchlorate anion and the dichloromethane molecules of solvation exhibit large amplitudes of vibration. One dichloromethane molecule lies in a general position, the other lies about an inversion center and suffers from disorder.     

配合物[Cu2(C6H2Cl2OC=N-C3H6COO)2(H2O)2]·3H2O合成与晶体结构

本文以苏氨酸,3,5-二溴水杨醛以及醋酸铜为原料合成了新型配合物[Cu2(C6H2Cl2OC=N-C3H6COO)2(H2O)2]·3H2O,并对其晶体结构经元素分析,红外光谱及X射线单晶衍射表征.结果表明:该晶体属单斜晶体结构,晶胞参数分别为:a=0.6985(2) nm, b=1.0789(2) nm, c=1.9639(3) nm, β=92.182(3) °, Mr=797.34, V=1.4789(6) nm3 , Z=2, Dc=1.790 g/cm3, μ(MoKa) =1.867 mm-1, F(000)=808, R=0.0321, wR= 0.0566.Cu(II)与一个N原子,两个O原子以及一个水分子构成三齿链状席夫碱.不对称单元结构包含两个配合物分子及三个由氢键链接的水分子.     

Crystal and molecular structure of bis(o-phenylenethiourea)selenium(II)chloride dihydrate,C14H12N4S2Cl2Se·2H2O

The synthesis and crystal structure ofbis(o-phenylenethiourea)selenium(II)-chloride dihydrate, Se(C₇H₆N₂S)₂Cl₂·2H₂O are reported. The compound crystallizes in the monoclinic space group, P2₁/n, with four molecules per unit cell, the dimensions of which area=10.243(3),b=13.341(4),c=14.273(4) Å,=93.00(3)°,U=1947.76 ų. The structure was solved by direct methods and refined by full-matrix least-squares toR=0.039 andR _w =0.040 for 3314 unique reflections. Selenium displays two strong coordinations arising from the two sulfurs, Se-S(1)=2.191(1), Se-S(2)=2.206(1) Å, and S(1)-Se-S(2)=101.0(1)°, and four secondary interactions involving three chlorines and one sulfur. The complex occurs as a dimer with two sets of very weakly interacting bridging pairs S(2), S(2)^a; and Cl(2), Cl(2)^a, where a denotes the inversion related atom. Lattice stabilization is ensured by the extensive network of hydrogen bonds involving chlorines, water oxygens, and nitrogens of phenylenethiourea ligands.     

ZnCl2·2NH4Cl结晶过程及其热分解行为

使用氯化锌(ZnCl2)和氯化铵(NH4Cl)制备了氯化锌铵(AZC,Ⅱ型,ZnCl2·2NH4Cl)晶体.采用X射线粉末衍射(XRD)技术研究了ZnCl2与NH4Cl摩尔比对晶体类型的影响.用热重分析(TC-DTG)手段研究了样品的热分解行为和非等温动力学特征.TG曲线结果表明AZC(Ⅱ)热分解由失NH4CI和ZnCl2热挥发两个步骤完成,TG和DTG曲线表明失NH4Cl包括4个微观过程.非等温分解动力学研究表明,失NH4Cl和znCl2热挥发两大步的表观活化能(E)分别为91.25 kJ·mol-1和104.76 kJ·mol-1,指前因子(A)分别为105.94s-1和104.51s-1.研究表明AZC(Ⅱ)晶体据具有良好热稳定性.晶体生长实验结果表明:合成(非提纯过的)AZC(Ⅱ)晶体可以用作制备ZnSe晶体的输运剂.     

X-ray diffraction studies oncis-[Ru(bpy)2(PMe3)Cl+][ClO4 −] andcis-[Ru(bpy)2{PMe2(o-tol)}Cl+][ClO4 −]; two ordered structures in thecis-bis(bipyridyl)chloro(phosphine)-ruthenium(II) series

The complexcis-[Ru(bpy)₂(PMe₃)Cl⁺][ClO₄ ^?] crystallizes in space group P2₁/c andcis-[Ru(bpy)₂{PMe₂(o-tol)]Cl⁺][ClO₄ ^?] crystallizes in space group $P\bar 1$ ; each is present as a racemate and neither structure suffers from disorder. The Ru?PMe₂(o-tol) bond length of 2.324(2)Å is slightly longer than the simple Ru?PMe₃ bond length of 2.310(2) Å.     

Crystal structure and low-temperature emission of [(dmp)Cu(μ-S2butphos)2Cu(dmp)][BF4]2·6CH2Cl2 (dmp=2,9-dimethyl-1,10-phenanthroline; S2butphos=1,4-bis(diphenylphosphinesulfido)butane)

The synthesis and crystal structure of a bimetallic luminescent Cu(I) complex containing 1,4-bis(diphenylphosphinesulfido)butane and the -diimine 2,9-dimethyl-1,10-phenanthroline (dmp) is described. The coordination geometry about the Cu(I) center is pseudo-tetrahedral. Interplanar interactions between phenyl groups on the phosphine sulfide ligands and the phenanthroline exist which are indicative ofintramolecular -stacking, leading to compressed S–Cu–S bond angles. The complex displays emission from a single metal-centered charge-transfer state at 77 K in a 41 ethanol/methanol (v/v) glass. This is in contrast to the triphenylphosphine complex, which exhibits dual luminescence from a charge-transfer and an intraligand state at 77 K. Crystal data: triclinic, ,a=13.619(4) Å,b=13.673(2) Å,c=15.384(2) Å, =75.08(1)°, =80.35(2)°, =80.67(2)°.