Synthesis and crystal structure of new supramolecular adducts of [PtCl6]2− with cucurbit [7] uril: [(H3O)2 (PtCl6)]3 (C42H42N28O14)2·H2O

A novel supramolecular adduct [(H₃O)₂ (PtCl₆)]₃ (C₄₂H₄₂N₂₈O₁₄)₂·H₂O (1) was synthesized by mixing [PtCl₆]²⁻ and cucurbit [7] uril in solution of hydrochloric acid. The crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to orthorhombic system and space group F dd2 with cell dimensions:a=4. 705 33 (5) nm,b=7. 153 80 (6) nm,c=1. 894 61 (2) nm,Z=16,V=63, 7744 (11) nm³,D _c =1.534 g/cm³, μ=3. 007 mm⁻¹,F(000)=29 120,R ₁=0.070 7,wR ₂=0. 169 2. In crystal, the cucurb [7] uril molecules from two zig-zag chains. Foundation item: Supported by the National Natural Science Foundation of China (20172040) Biography: Yan kun (1977-), female, Master, research direction: macrocyclic chemistry.     

Preparation,crystal structure and quantum chemical investigation of [Li(NTO) (H2O)]

[Li(NTO)(H₂O)₂] was prepared by mixing the aqueous solution of 3-nitro-1,2,4-triazol-5-one (NTO) and lithium hydroxide. The crystal structure of [Li(NTO)(H₂O)₂] was determined by single crystal diffraction analysis. The crystal is monoclinic, space group P2₁/n with crystal parameters of a = 0.742 0(2) nm, b = 0.344 9(1) nm,c = 2.490 6(3) nm, β= 94.89(1)°, Z = 4,D _c , = 1.799 g cm⁻³,V = 0.635 nm³, μ = 1.591 cm⁻¹, F(000) = 392. The finalR is 0.051. The MNDO MO calculation shows that the coordinate bonds of title compound possess certain extent of covalent character. O₂ atom of NTO anion is bonded to Li atom; the nitro group will be lost first when NTO is decomposed.     

Hydrothermal synthesis and crystal structure of copper （Ⅱ） coordination polymer composed of helix-like chains： [Cu（NIeH）（bpy）]

Hydrothermal reactions of Cu （Ⅱ） acetate, 2,2＇-bipyridyl （bpy） with 5-nitroisophthalic acid （H2NIPH） resulted in a new coordination polymer [Cu（NIPH）（bpy）] 1. Single crystal X-ray diffraction experiment indicates that 1 possesses a single helixlike chains, of which Cu atoms are coordinated by NIPH ligands and bpy ligands. Compound 1 crystallizes in the space group P2（ 1）/c, a = 0.955（19） nm, b = 1.259（3） nm, c = 1.3737（3） nm, ,6= 95.13（3）°, V= 1.6455（6） nm^3 and Z = 4. The TGA analysis shows that 1 has no remarkable weight loss up to 284℃, as a result of its high thermal stability. Magnetic measurements indicate an antiferromagnetic behavior of compound 1.     

[Ag(C_5H_6N_2)_2]·(C_7H_5O_2Cl)·2H_2O的合成和结构

合成出标题配合[Ag(C5H6N2)]·(C7H5O2Cl)·2H2O．配合物经X射线单晶结构分析结果表明,属三斜晶系, 空间群为P-1,a=0．736 8(4),b=0．955 3(6),c=1．5 56 6(9)nm,α=73．301(10),β=76．591(11),γ=75．961(10), V=1．024(10)nm3,Z=2,最终偏差因子R[I>2(I)]a,R1=0．076 6,wR2=0．145 4．     

Synthesis, crystal structure and properties of binuclear manganese complex [(bipy)2Mn2(μ-O)(μ-Ac)2(H2O)2](ClO4)2

Binuclear manganese complex [(bipy)₂Mn₂(μ-O)(μ-Ac)₂(H₂O)₂](ClO₄)₂ was synthesized by the reaction of MnAc₃ · 2H₂O with 2,2′-bipyridine in the HAc-NaAc buffer (pH = 4.0). X-ray diffraction result for the single crystal shows that the crystal is monoclinic, space group C₂/C, with a = 3.408 2(7),b = 0.864 4(2),c = 2.174 9(4) nm, β= 105.2∘, V=6.186(2) nm³, Z= 8. There are two very strong peaks of UV-Vis spectrum in the range of 400–600 nm, which are similar to those of Mn catalase and Mn ribonuleotide reductase extracted from organisms. Cyclic voltammogram shows that the complex in CH₃CN undergoes quasi-reversible one-electron reduction and oxidation at E_1/2=1.15V.     

Synthesis and Characterization of Polyamide-Containing 2, 6- （Substituded） pyridine Derivatives

0 IntroductionPayrriodminaetiics hoenteer oofc ythcleics m .os tC oambupnoduanndts a cnodn tbaeisntin kgno twhnepyridine ring are widely distributedin nature,principally asenzymes and alkaloids . Pyridine enzymes have been foundintissues of all plants and ani mals examined thus far ,andare derivedfromeither nicotinic acid or Vitamin B6[1].Pyr-idine derivatives are also the building block of many phar-maceuticals with a wide range of functionalities that includeantitubercular compounds ,antivi…     

Synthesis,Structure and Antitumor Activities of [Ni（dien）2][Ni（CN）4] Complex

Ni(II)-dien complex was prepared and characterized by X-ray diffraction. The crystal belongs to triclinic system, space group P-1, with crystallographic parametersa=0.888 13(18) nm,b=0.890 10(18) nm,c=1. 591 8(3) nm, α=77.71(3)°, β=89.12(3)°, γ=61.24(3)°,Z=2. The two dien molecules coordinate to the central Ni atom, the six nitrogen atoms form a distorted octahedron. Preliminary pharmacological tests showed this complex had antitumor activity against HepG₂ and HL-60 cell linesin vitro. Foundation item, Supported by the National Natural Science Foundation of China (29972034) Biography: Li Tao (1976-), male, Ph. D candidate, research direction: ophthalmology and chemicalbiology.     

Synthesis, structure and ethylene polymerization behavior of titanium complexes [C3H6（N = CH-Ar-O）2]TiCl2

Early transition metal catalysts containing twophenoxy-imine ligands, called FI catalysts which havevery high potential to become a new generation of olefinpolymerization catalysts, are new-type catalysts whichhave attracted much attention in recent years[1—3]. Many ofthem display activities comparable to those of the metal-locene catalysts and, in some cases, behave as living po-lymerization catalysts of α-olefins. Brookhart and Gibsonet al.[4,5] recently reported separately series of Schi…     

Preparation by a rheological phase reaction method and thermal decomposition reaction mechanism of nickelous salicylate tetrahydrate

0　IntroductionInrecentyears,studiesonBinghamfluid ,suchasElec trorheologicalfluid ,areactivelypursued[1 6] .Rheologicaltechniqueshavebeenplayinganimportantroleinsyntheticchem istry .Therheologicalphasereactionmethodisthe processofpreparingcompoundsormaterialsfromasolid liquidrheologicalmixture.Thatis,thesolidreactantsarefullymixedinapropermolarratio ,andmadeupbyaproperamountofwaterorothersolventstoaBinghambodyinwhichthesolidparticlesandliquidsubstanceareuniformlydistributed ,sothattheprodu…     

New crystal structure of molecular complex 1-piperidine carboxylate-piperidinium-H<Subscript>2</Subscript>O studied by X-ray single crystal diffraction

Piperidine absorbs CO2 and H2O in air to form a molecular complex： piperidium-l-piperidinecarboxylate-H2O. The structure of the complex was characterized by X-ray single crystal diffraction. The crystal structure was determined to be triclinic, space group P1^-with a=0.648 6（8） nm, b=0.809 200） nm, c= 1.357 1（16） nm, a=96.96706）°, β =102.506（15）°,γ=104.202 05）°, Z=2. The complex is stabilized via five hydrogen bonds between the three components, N-O electrostatic interaction and O-O interaction （electron transfer） betweenl-piperidinecarboxylate and H2O. Due to electron transference of carbamate ion, the oxygen atom in water molecule is strongly negatively charged and the O-H bond is considerably shorter than that of the free molecule of water. The formation of the molecular complex is a reversible process and will decompose upon heating. The mechanism of formation and stabilization is further investigated herein.     

Syntheses and lyotropic liquid crystal properties of a series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30

A series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30, Na16[As4W30M4(H2O)2O112]·XH2O (M = Zn,Cu,Co,Ni,Mn and Cd), have been synthesized for the first time and structurally characterized by elemental analysis, IR and 183W NMR spectra. The crystal structure of Na16[As4W30Cu4(H2O)2O112]·63H2O was determined to be a triclinic system, of P1 symmetry, a = 1.2721(3) nm, b = 2.451 6(5) nm, c = 2.6450(5) nm, α= 89.90(3)°,β= 77.32(3)°, γ= 89.96(3)°, 2=2. Using tetrahepty lammonium bromide as a phase transfer reagent, [As4W30Cu4(H2O)2O112]16- was transferred from aqueous solution to organic phase (benzene), and the heteropolyanion lost the coordination water molecules to form the coordination-unsaturated ion. After lactic acid was added to the benzene solution, the coordination-saturation was recovered. By esterification reaction between lactic acid and cholesterin, the latter was attached to the heteropolyanion indirectly. Therefore, a new type of lyotropic liquid crystal was obtained, which was characterized by a polarimicroscope, DSC and variable temperature wide-angle X-ray diffraction.     

Synthesis and properties of a Pr（Ⅲ） complex with 2-acetylbenzimidazoledehyde-glycine Schiff-base ligand

Abstract The 2-acetyl-benzimidazoledehyde-glycine Schiff-base ligand and the corresponding Pr（Ⅲ） complex Pr2L3（NO3）3· 2CH3OH （L=C11H10N3O2） were synthesized in methanol and characterized by a series of methods, including chemical analysis, elemental analysis, TOF-MS, ^1H NMR, UV-, IR-, Raman spectra, thermal analysis, and the three-dimension fluorescence excitation and emission spectra. The Pr（Ⅲ） complex exhibits extraordinary water-solubility and the Pr（Ⅲ） hydroxide appears at pH≥13. The complex also possesses specific fluorescent properties. Thus, at the excitation wavelengths 200.0-280.0 and 260-350 nm the fluorescence bands were observed at 290.0 and 400.0 nm, respectively.     

β-Ｄ-吡喃葡萄糖叠氮化物的合成及晶体结构

合成了β-Ｄ-O四乙酰基糖基叠氮化合物， 并得到单晶， 经X射线衍射方法解析， 其晶系属于单斜晶系，P2₁空间群， 其中a=0.759　6(6) nm,b=1.518　4(13) nm，c=1.641　2(14) nm，V=1.893　0(3) nm³，α=90.00°，β=90.045(1)°，γ=90.00° ，Z=2. 在晶体结构中， 六元糖环采取经典⁴C₁椅式构象， 糖环上所有 的取代基均以平伏键存在， 其中叠氮基不是以直线型结构存在， 呈现一定的弯曲现象.     

新型配位聚合物[Nd_2(ad)_3(H_2O)_2]_n·n(4,4’-bpy)的水热合成及晶体结构

以NdCl3·xH2O,ad(己二酸)和4,4’_bpy为原料,在水热合成反应条件下,合成了配位聚合物[Nd2(ad)3(H2O)2]n·n(4,4’_bpy),利用元素分析、红外光谱、X射线单晶衍射和荧光分析对其进行了表征.该配位聚合物属正交晶系,Pbcn空间群,晶胞参数为a=2.2012(6)nm,b=0.7778(2)nm,c=1.9724(5)nm,α=β=γ=90°,V=3.3770(15)nm3,Z=4,d=1.796g/cm3,μ=3.108mm-1,F(000)=1800,R1=0.0430,R2=0.0560.通过己二酸配体羧基氧原子桥联Nd3+形成三维网状结构,4,4’_bpy通过H键的连接存在于孔道中.     

Inorganic-organic hybrids constructed of bis（undecatungstogerma- nate）lanthanates polyoxoanions and oxalate-bridged dinuclear copper complexes and their magnetic properties

A series of inorganic-organic hybrids K₂Na _m H_9−m [{Ln(GeW₁₁O₃₉)₂}{Cu₂(bpy)₂(μ-ox)}]·nH₂O (bpy = 2,2-bipyridine and ox = oxalate; Ln = La, Nd, Sm, Eu, Gd; n = 19, 17, 22, 20, 19; m = 4, 4, 4, 9, 2) were isolated after reacting in a potassium acetate buffer. X-ray structural analyses show that compounds 1–5 are isomorphic and consist of [Ln(GeW₁₁O₃₉)₂]¹³⁻ polyoxoanion building blocks and oxalate-bridged dinuclear copper metalorganic complex with a 1D chain structure. The 1D chain further connects into the 3D framework by π-π interactions with neighboring bpy groups. The magnetic susceptibility data indicate that antiferromagnetic coupling between the neighboring Cu²⁺ ions in the structure and the rare earth ions affects magnetic property of the structure.     

Determination of crystal structure of omphacite

The chemical formula of omphacite was expressed with (MⅡ MⅠ ) (Si, AI)2O6. Cations that occupied the MⅡ site were large cations such as Ca or Na, and (Na/(Na+Ca)) ratio ranged from 0.2 to 0.8; the 6-coordinated MⅠ site accommodated cations such as Mg, Fe2+, Al, Fe3+ ,and(AI/(AI+Fe3+)) ratio was more than 0.5. Omphacite space groups reported were C2/ c, P2, P2/n, P2/c, cell parameters are α0 = 0.9600-0.9630 nm,b0 = 0.8750-0.8830 nm,c0 = 0.5230-0.5290 nm,β = 106°40′-107°10'. The sample was picked up from the eclogites in Zhucheng County, Shangdong Province. The intensity data were collected with the RIGAKU RASA Ⅱ -S four-circle single crystal diffractometer.The correct structure model was obtained by using the Patterson method and Fourier synthesis, SHELX-76 program, structure refinement with 905 independent diffraction points (| F0 |> 3σ |F0 |). After the structure parameter refinement, the R-factor reduced to 0.0515. The crystal structure analysis indicates that omphacite has a new space group-Pn space group.     

Syntheses, characterization, crystal structure and magnetic properties of copper(Ⅱ)α, β-unsaturated carboxylate complexes with trimethyl phosphate

Two ternary complexes Cu2A4[OP(OCH₃)₃]₂ (A represents CH₂== CH—COO- and CH₂== C(CH₃)—COO-) have been synthesized, and elemental analyses, IR, ESR, electronic reflectance spectra and magnetic studies were carried out. The single crystal X-ray diffraction shows that Cu₂[CH₂== C(CH₃)—COO]₄[OP(OCH₃)₃]₂ is triclinic, with space group P1, a = 1.05128(13), b = 1.7559(5), c = 1.94479(3) nm, α = 91.263(14)°, β = 102.559(6)°, γ = 106.339(13)°, Z = 4 and R = 0.0668. Two copper(Ⅱ) atoms are bridged by four a -methacrylate groups, and each copper(Ⅱ) atom is coordinated with a trimethyl phosphate molecule in the axial position, forming a distorted square pyramidal configuration. The symmetric center is between the two copper(Ⅱ) atoms, and the Cu-Cu bond distance is 0.26098(6) nm. The Cu-Cu distance and magnetic studies suggest that there exist antiferromagnetic interactions between the two copper(Ⅱ) atoms.     

[Cu(C_7H_5O_2)_2]·(C_4H_5N_2)的合成与晶体结构

报道了标题化合物的合成及晶体结构 .经 X射线单晶结构分析结果表明 ,该配合物 [Cu(C7H5O2 ) 2 ]·(C4 H5N3)属三斜晶系 ,空间群为 Pī,晶胞参数 a=0 .72 73(11) nm ,b=0 .9182 (14 ) nm,c=1.384 (2 ) nm,α=10 8.96 (2 )°,γ=94 .0 6 (2 )°,γ=96 .80 (2 )°,U=0 .86 2 (2 ) nm3,Z=2 ,F(0 0 0 ) =4 10 ,Dc=1.5 4 4 mg/ m3.最终偏差因子 R[I≥ 2 σ(I) ]a:R1 =0 .0 787,w R2 =0 .16 5 9     

［Ni(phen) 3］2［Ni(PO4)2(H2PO4)6(OH)6(MoO2)12］的合成和晶体结构

利用中温水热技术合成一种新型还原型钼磷酸盐： ［Ni(phen) ₃］₂［Ni(PO₄)₂(H₂PO₄)6(OH)₆(MoO₂)₁₂］(phen: 邻菲啰啉), 并通过单晶X射线衍射技术测定了该化合物的晶体结构.该化合物属于三斜晶系, P1空间群, 晶胞参数: a=1.404 2(3) nm, b=1.405 0(3) nm, c=1.408 2(3) nm, α=74.53(3)°, β=74.72(3)°,γ=74.81(3)°, V=2.527 6(9) nm3, Z=1, R1=0.076 2, wR2=0.168 6.     

[Gd2(BDC)3(H2O)2]n和[Ho2(BDC)3(H2O)2]n的合成和结构

用1,3-间苯二甲酸(BDC)和Ln2O3(Ln=Gd,Ho),通过水热法,加入少量3,5-二甲基吡啶,合成了具有二维结构的配位聚合物[Ln2(BDC)3(H2O)2]n.通过X射线单晶衍射的方法得到两种化合物的晶体数据.[Gd2(BDC)3(H2O)2]n的晶体数据C24H16O14Gd2,M=842.9,单斜晶系,空间群P21/n,a=1.341 nm,b=1.446 nm,c=1.343 nm,β=104.17°,V=2.528 nm3,Z=4,Mo-Kα,μ=5.264 cm-1,Dc=2.12 g·cm-3.[Ho2(BDC)3(H2O)2]n的晶体数据C24H16O14Ho2,M=860.2,单斜晶系,空间群P21/c,a=1.059 nm,b=1.420 nm,c=1.710 nm,β=97.90°,V=2.548 nm3,Z=4,Mo-Kα,μ=5.264 cm-1,Dc=2.12 g·cm-3.这两种化合物有相似的二维结构.Ln离子通过三种不同的BDC配体方式互相连接,组成了复杂的二维隧道,同时配位水分子在隧道中.