Synthesis and Crystal Structure of (CH_2)_3(3,5-Me_2Pz)_2. [PhBr_2Sn(CH_2)SnBr_2Ph].2HBr.H_2O (Pz=pyrazole)

1 INTRODUCTION The coordination chemistry of tin or organotin toward poly(pyrazol-1-yl)borate ligands has been extensively investigated in recent years owing to the antitumor activity of some related organotin derivatives containing N-donor ligands. A number of organotin(Ⅳ) complexes containing poly(pyrazol- 1-yl)borate ligands have been synthesized and characterized[1~3], some of which have also shown interesting structural characteristics and reactivities[4~6]. Recently, poly(pyrazol…     

Synthesis and Crystal Structure of (CH2)3(3, 5-Me2Pz)2·[PhBr2Sn(CH2)SnBr2Ph]·2HBr·2H2O (Pz = pyrazole)

The reaction of bis(dibromophenylstannyl)methane with 1, 3-bis(3, 5-dimethyl- pyrazol-1-yl)propane in a 1:1 or 1:2 ratio yields only 1:1 adduct which partly hydrolyzes to the title complex (C26H38Br6N4O2Sn2, Mr = 1155.42) during crystal growing. The title complex is of triclinic, space group P ī with a = 10.886(1), b = 12.508(1), c = 13.879(1) ?, α = 85.762(2), β = 85.159(2), γ = 84.020(2)°, V = 1868.8(4) ?3, Z = 2, Dc = 2.046 g/cm3, λ(MoKα) = 0.71073 ?, μ = 7.778 mm-1, F(000) = 1088, R = 0.0488 and wR = 0.1157 for 7560 observed reflections with I ≥ 2σ(I). The crystal structure analysis indicates that there is no direct interaction between the ligand and bis(dibromophenylstannyl)methane, and two tin atoms are bridged by two bromide atoms from the partial hydrolysis of this adduct.     

First structural characterization of guanidine, HN=C(NH(2))(2)

Structural information about the free base guanidine in the solid state could be obtained for the first time by determining the crystal structures of the 1:1 as well as the 2:1 co-crystals consisting of neutral guanidine and 2-amino-4,6-dimethyl-1,3,5-triazine using single crystal X-ray diffraction.     

新型离子型有机锡化合物{[Ph~2Sn]~2[2,6-Py(CO~2)]~3H~2O}^2^-.[HNEt~3]^+~2的合成、表征、性质及晶体结构

利用三苯基氯化锡和2,6-吡啶二甲酸在三乙胺存在下以1:1摩尔比反应,合成了离子型有机锡化合物{[Ph~2Sn]~2[2,6-Py(CO~2)]~3H~2O}^2^-[HNEt~3]^+~2。通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征。用X射线单晶衍射测定了该化合物的晶体结构。化合物为单斜晶系,空间群P2~1/n,a=1.7073(7)nm,b=1.7447(7)nm,c=2.5333(10)nm,β=109.694(7)°,Z=4,V=6.824(5)nm^3,D~c=1.282g/cm^3,μ=0.793mm^-^1,F(000)=2696,R~1=0.0563,WR~2=0.1539。化合物中两个锡原子呈七配位畸变五角双锥构型。生物活性测试结果表明,该化合物具有较强的体外抗肿瘤活性。     

新磷酸铝分子筛CFAP-2的合成与鉴定

新AlPO₄结晶分子筛相CFAP-2合成于TMEDA(N,N,N′,N′-四甲基乙基二胺)-P₂O₅-A1₂O₅-H₂O系统,反应物摩尔组成的范围是:TMEDA:P₂O₅:Al₂O₃:H₂O=(1-1.1):1:1:50,晶体形貌,X射线粉末衍射分析,热分析及红外光谱的研究表明:CFAP-2与A1PO₄-21的晶体结构不同,在350℃时,CFAP-2的原粉相转变为具有三维骨架孔结构的较稳定的结晶相。     

配合物[Sm(o-MOBA)3(phen)·H2O]2·4H2O的合成与晶体结构

The title complex [Sm(o-MOBA)₃(phen)·H₂O]₂·4H₂O has been synthesized by the reaction of SmCl₃·6H₂O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm³⁺ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.     

Formal [(2+2)+2] and [(2+2)+(2+2)] nonconjugated dienediyne cascade cycloadditions

[reaction: see text] Fluoranthene 2 and heptacycle 3 are easily accessible from the reaction of diyne 1 and norbornadiene (NBD) in the presence of the rhodium catalyst. The unusual [(2+2)+(2+2)] adduct 3 was confirmed by the X-ray crystal structure analysis.     

Synthesis and Crystal Structure of 1-Methylsulfinyl-1-methylthio-2-cyano-2-phenylethylene

1　ＩＮＴＲＯＤＵＣＴＩＯＮＤｉｔｈｉｏａｃｅｔａｌｓ[1 3]ｈａｖｅｄｅｍｏｎｓｔｒａｔｅｄｔｈｅｉｒｐｏｔｅｎｔｉａｌｆｏｒｔｈｅｓｙｎｔｈｅｓｉｓｏｆｈｅｔｅｒｏｃｙ ｃｌｅｓ,ｔｈｅｒｅｆｏｒｅ ,ｔｈｅｉｒｓｙｎｔｈｅｓｉｓａｎｄｒｅａｃｔｉｏｎｓｈａｖｅａｔｔｒａｃｔｅｄｍｕｃｈａｔｔｅｎｔｉｏｎ ,ｂｕｔｖｅｒｙｌｉｔｔｌｅｈａｓｂｅｅｎｒｅｐｏｒｔｅｄａｂｏｕｔｔｈｅｏｘｉｄａｔｉｏｎｏｆｄｉｔｈｉｏａｃｅｔａｌｓ[4].Ａｃｃｏｒｄｉｎｇｔｏｔｈｅｐｒｅｖｉ ｏｕｓｒｅｐｏｒｔ,ｔｈｅｏｘｉｄ…     

二聚体有机锡配合物{[n-Bu2Sn(O2CCH2CS2NC4H8)]2O}2的合成，表征及晶体结构(英)

The title compound, {[n-Bu₂Sn(O₂CCH₂CS₂NC₄H₈)]₂O}₂, has been synthesized by the reaction of (tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in 1∶1 molar ratio. The complex has been characterized by elemental analysis, IR and NMR. The crystal structure of it has been determined by X-ray single crystal diffraction. And the results showed that the crystal belongs to triclinic system with space group P1 and some crystal parameters: a=1.220 2(9) nm, b=1.315 8(10) nm, c=1.380 4(10) nm, α=111.215(9)°， β=99.357(9)°， γ=96.075(10)°, V=2.006(2) nm³, Z=1, F(000)=908, μ=1.489 mm^-1, D_c=1.474 g·cm^-3, R₁=0.037 5, wR₂=0.0839. The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron. Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only. CCDC: 220513.     

{[Cu2Br3]n[Cu(H-Leof)2]·2H2O}(Leof是左氟沙星)

C om m ent Levofloxacin (S-(-)9-fluoro-2,3-dihydro-3-m ethyl- 10-(4-m ethyl-1-piperazinyl)-7-oxo-7H -pyrido[1,2,3-de]- 1,4-benzoxaxin-6-carboxilic acid)(Leof),is a synthetic fluorinated quinolone derivative, having activity a- gainstboth Gram ( )and Gram …     

4-(2-羟基苯基)-亚胺基-戊-2-酮的晶体结构和谱学性质研究

通过邻氨基苯酚与乙酰丙酮反应,合成Schiff碱4-(2-羟基苯基)-亚胺基-戊-2-酮,获其单晶,测定晶体结构,用UV-Vis,IR,^HNMR谱对其进行了表征。其晶体属正交晶系,空间群P2~12~12~1,晶胞参数:a=0.8840(10)nm,b=1.05250(10)nm,c=1.12260(10)nm。V=1.0450(2)nm^3,Z=4,结构偏离因子R=0.0320,ωR=0.0669,吻合因子S=0.949存在较强的分子间氢键,O(1)与相邻分子的O(2)之间的平均距离为0.2640nm。晶体结构分析和谱学性质研究表明,化合物存在亚胺烯醇式和烯胺酮式两种异构平衡。     

An EPR and optical absorption study of VO2+ ions in sodium hydrogen oxalate monohydrate (NaHC2O4.H2O) single crystals

Electron paramagnetic resonance of VO(2+) doped sodium hydrogen oxalate monohydrate (NaHC(2)O(4).H(2)O) single crystals and powders are examined at room temperature. Single crystal rotations in each of the three mutually orthogonal crystalline planes namely ac*, b*c* and ab* indicate four different VO(2+) complexes with intensity ratios of 4:2:1:1. It is found from the EPR analysis that the Na(+) ions are replaced with the substitutional magnetically inequivalent VO(2+) ions. The powder spectrum also clearly indicates four different VO(2+) complexes, confirming the single crystal analysis. Crystalline field around the VO(2+) ion is nearly axial. The optical absorption spectrum show two bands centered at 15408 and 12453 cm(-1). Spin Hamiltonian parameters and molecular orbital coefficients are calculated from the EPR and optical data, and results are discussed.     

2-(2-苯并咪唑基)-4,4,5,5-四甲基-3-氧化咪唑啉-1-氧基自由基的合成、晶体结构与量化计算

报道了2-(2-苯并咪唑基)-4, 4, 5, 5-四甲基-3-氧化咪唑啉-1-氧基自由基(NITBzImH)的合成和晶体结构.晶体属正交晶系Pbca空间群.a=0.87446(4), b=1.55600(8), c=2.01139(1) nm,α=β=γ=90°,Z=8,V=2.7368(2) nm³, R=0.0478,ωR=0.1101;并用密度泛函(DFT)计算了该自由基的自旋密度分布.     

新型鼓状有机锡氧杂环羧酸簇合物[PhCH2Sn(O)(O2CC4H4N)]6·2CH2Cl2的合成和晶体结构

利用三苄基氧化锡与2-吡咯甲酸反应，合成六聚体-苄基锡氧2-吡咯甲酸酯簇 合物．通过元素分析、红外光谱、核磁共振氢谱和X射线单晶衍射对其结构进行了 表征．X射线单晶衍射测试结果表明：化合物为三斜晶系，空间群P1^-，α＝1． 2644(3)nm，b＝1．7416(4)nm，c＝1．9285(4)nm，α＝90．021(4)°，β＝94． 585(4)°，γ＝90．021(4)°，Z＝2，V＝4．2330(16)nm^3，Dc＝1．715g／cm^3 ，μ＝1．936mm^-1，F(000)＝2136，R＝0．0527，wR＝0．0708．该化合物为鼓型 簇状结构，锡原子为畸变的八面体构型．     

Thermochemische Untersuchungen im System V/Nb/O. II Zum chemischen Transportverhalten im Bereich V2O5/Nb2O5/VO2/NbO2

Thermochemical Investigations in the System V/Nb/O. II. Chemical Transport in the Region V₂O₅/Nb₂O₅/VO₂/NbO₂ Transport experiments were used to support the phase relationships of the V₂O₅/Nb₂O₅/VO₂/NbO₂ system, which were established by annealing experiments of powder mixtures. The phase relations were studied in the NbO₂-rich region of the system by means of X-ray and ESMA methods. The NbO₂-rich section is characterized by the following two phase and three phase regions: Two phase region: V₃Nb₉O₂₉/rutile mixed crystal V_1?xNb_xO₂ Two phase region: BI-mixed crystal/V_xNb_1?xO₂ Three phase region: V₃Nb₉O₂₉/solubility limit LG1 (V_1?xNb_xO₂)/BI-mixed crystal Three phase region: solubility limit LG1 (V_1?xNb_xO₂)/BI-mixed crystal/solubility limit LG2 (V_xNb_1?xO₂). The composition of the solubility limits LG1 and LG2 was ascertained by means of ESMA-investigation: LG1: 57.5 ± 5 mol% NbO₂/43.5 ± 5 mol% VO₂ LG2: 22.5 ± 5 mol% NbO₂/78.5 ± 5 mol% VO_2?     

Mononuclear (Pd, Pt), heterodinuclear (PdAg, PtAg), and tetranuclear (Pd2Ag2, Pt2Ag2) 1,1-ethylenedithiolato complexes

lp;&-5q;1 The reactions of [Tl2[S2C=C[C(O)Me]2]]n with [MCl2L2] (1:1) or with [MCl2(NCPh)2] and PPh3 (1:1:2) give complexes [M[eta2-S2C=C[C(O)Me]2]L2] [M = Pt, L2 = 1,5-cyclooctadiene (cod) (1); L2 = bpy, M = Pd (2a), Pt (2b), L = PPh3, M = Pd (3a), Pt (3b)] whereas with MCl2 and QCl (2:1:2) anionic derivatives Q2[M[eta2-S2C=C[C(O)Me]2]2] [M = Pd, Q = NMe4 (4a), Ph3P=N=PPh3 (PPN) (4a'), M = Pt, Q = NMe4 (4b)] are produced. Complexes 1 and 3 react with AgClO4 (1:1) to give tetranuclear complexes [[ML2]2Ag2[mu2,eta2-(S,S')-[S2C=C[C(O)Me]2]2]](ClO4)2 [L = PPh3, M = Pd (5a), Pt (5b), L2 = cod, M = Pt (5b')], while the reactions of 3 with AgClO4 and PPh3 (1:1:2) give dinuclear [[M(PPh3)2][Ag(PPh3)2][mu2,eta2-(S,S')-S2C=C[C(O)Me]2]]]ClO4 [M = Pd (6a), Pt (6b)]. The crystal structures of 3a, 3b, 4a, and two crystal forms of 5b have been determined. The two crystal forms of 5b display two [Pt(PPh3)2][mu2,eta2-(S,S')-[S2C=C[C(O)Me]2]2] moieties bridging two Ag(I) centers.     

[(enH)2(enH2)Sn2Se6]的合成、结构及性能研究

采用溶剂热法,以K2Se:SnCl2·2H2O∶Se∶en=1∶1∶4∶48的摩尔比,在150 ℃下反应5d,生成黄色透明柱状晶体[(enH2)2Sn2Se6·en]。该晶体属于三斜晶系 ,空间群为Pl^-,晶胞参数,a=0.8659(2)nm,b=1.1055(2)nm,c=0.66360(10)nm, a=104.44(3)°,β=110.93(3)°,γ=79.74(3)°,V=0.57198(19)nm^3,Z=1.[ (enH2)Sn2Se6]晶体由质子化的乙二胺正离子（enH)^+,(enH2)^2+和二聚硒代锡根 负离子（Sn2Se6)^4-堆积而成。在AxSn2Se6系列化合物,正离子A的大小对晶体结 构的类型产生重要的影响。研究表明,此晶体具有1.76eV的能隙（Eg）,是个半导 体,对太阳辐射具有选择吸收特性,在温度低于180℃时是稳定的。     

Crystal Structure of a Silver Phosphate-Tellurate: Te(OH)6 · 2Ag2HPO4

Crystal structure of a new silver phosphate-tellurate: Te(OH)₆ · 2Ag₂HPO₄ has been solved using 2534 X-ray reflections with a final R value: 0.048. This salt is monoclinic, P2₁/n with a bimolecular unit cell:a = 5.950(3), b = 20.52(1), c = 5.829(3) Å, β = 119.89(5°). As in the already described phosphate-tellurates the main feature of this crystal structures is the coexistence in the same crystal of two different types of anions: TeO₆ octahedra and PO₄ tetrahedra.     

{Cu[H_2NC(CH_2OH)_3]_2}{Pic}_2·H_2O的合成与晶体结构

三羟甲基氨基甲烷与苦味酸(Pic)铜在乙醇水混合液中反应,制得少见的不对称氢键连接的超分子化合物{Cu[H2NC(CH2OH)3]2}{Pic}2?H2O。晶体属三斜晶系,空间群为P ,晶胞参数为a = 6.894(1),b = 8.219(1),c = 13.543(3) ? ?= 79.290(1),?= 8 3.36(2), ?= 84.590(1)埃轿狢20H30CuN8O22,V = 746.9(2) 3,Z = 1,Dc = 1.774 g/cm3,F(000) = 411,?= 0.844 mm-1,R = 0.0334,Rw = 0.0863。在配合物的结构单元中, Cu2+位于对称中心,分别与2个四齿配体(三羟甲基氨基甲烷)中的2个OH,1个NH2,三齿配位,呈笼状螯合。而另一个OH,因配体和中心离子构型的限制,不参与配位。     

有机锡配合物{[(n-C8H17)2Sn(O2CCH2CS2NC4H8O)]2O}2的合成，表征及晶体结构

The title complex {[(n-C₈H₁₇)₂Sn(O₂CCH₂CS₂NC₄H₈O)]₂O}₂ has been synthesized by the reaction of (morpholinylthiocarbamoylthio)acetic acid with the di-n-octyltin oxide in 1∶1 molar ratio. The complex was characterized by elemental analysis, IR and ¹H NMR. The crystal and molecular structure of complex was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system with space group P1 and unit cell dimensions: a=1.201 5(9) nm, b=1.481 8(11) nm, c=1.894 1(14) nm, α=72.485(10)°, β=88.586(10)°, γ=66.893(9)°, and Z=1, μ=1.034 mm^-1, V=2.941(4) nm³, D_c=1.295 g·cm^-3, F(000)=1 196, R₁=0.058 8, wR₂=0.155 8. The complex is a centrosymmetric structure with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom. The endo-cyclic tin atoms and the exo-cyclic tin atom are all five-coordinate and have coordination geometry of distorted trigonal bipyramid with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are monodentate and connecting to each of exo-cyclic tin atoms by using one oxygen atom, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom. CCDC: 277048.