Dawson结构α-H_6P_2W_(18)O_(62)·3(CH_3)_2NH·H_2O的合成、表征和晶体结构(英文)

由二甲胺与H6P2W18O62·nH2O合成了电荷转移化合物α H6P2W18O62·3(CH3)2NH·H2O.单晶结构解析结果表明晶体属单斜晶系,空间群为P21／c,晶胞参数:a=1.2964(3)nm,b=1.3621(3)nm,c=4.1559(8)nm,β=90.02(3)°,V=7.338(3)nm3,Z=4.标题化合物具有可逆光色性.热分析表明,化合物阴离子在430.5℃左右分解.     

超分子化合物[M(4,4''''-bipy)2(H2O)4]·(4,4''''-bipy)2·(3,5-diaba)2·8H2O](M=Co,Ni,Cd)的合成及晶体结构

合成了3个超分子化合物[M(4,4'-bipy)2(H2O)4]·(4,4'-bipy)2·(3,5-diaba)2·8H2O(M=Co(1),Ni(2),Cd(3);4,4'-bipy=4,4'-联吡啶;3,5-diaba=3,5-二氨基苯甲酸阴离子),用红外光谱、元素分析及X-射线单晶衍射进行了表征。3个化合物的晶体都属于单斜晶系,空间群为P2/c。晶体学参数:化合物1:a=0.9389(2)nm,b=0.7751(1)nm,c=3.9284(6)nm,β=90.14(2)°,V=2.85880(69)nm3,Z=4,Dc=1.397g·cm-3,F(000)=1266,μ=0.380mm-1,R1=0.0349,wR2=0.0829;化合物2:a=0.9383(2)nm,b=0.7753(1)nm,c=3.9218(6)nm,β=90.09(1)°,V=2.85280(68)nm3,Z=2,Dc=1.399g·cm-3,F(000)=1268,μ=0.420mm-1,R1=0.0366,wR2=0.0805;化合物3:a=0.94091(13)nm,b=0.77885(11)nm,c=3.9712(5)nm,β=90.10°,V=2.9102(7)nm3,Z=2,Dc=1.433g·cm-3,F(000)=1308,μ=0.454mm-1,R1=0.0468,wR2=0.0964。3,5-diaba未参与配位,在配位阳离子[M(4,4'-bipy)2(H2O)4]2 中,金属离子M髤与来自2个4,4'-bipy的2个氮原子和4个水分子的氧原子配位,呈八面体的几何构型。分子中还存在未配位的4,4'-bipy。通过配位阳离子、游离4,4'-bipy及未配位的3,5-diaba间的丰富氢键,构建成具有三维结构的超分子化合物。     

新型磷酸钒孔道结构化合物(H3NCH2CH2NH3)3- [ (VO)4(PO4)2 (HPO4)4]的水热 合成及结构表征

以有机分子乙二胺作为模板剂合成了新型磷酸钒孔道化合物(H3NCH2CH2NH3)3^-[(VO)4(PO4)2(HPO4)4,并通过X射线单晶衍射实验进行了结构表征,晶体学数据为：C2/c,a=1.8505(9)nm,b=0.7089(4)nm,c=2.3304(10)nm,β=96.43(3)°,V-3.038(3)nm^3,Z=8,R=0.067,Rw^b=0.1635,该化合物具有非常独特和规整的二维孔道骨架结构,进一步的晶体化学研究表明该化合物为一新的VPO物相。     

新型磷酸钒孔道结构化合物(H3NCH2CH2NH3)3- [ (VO)4(PO4)2 (HPO4)4]的水热 合成及结构表征

以有机分子乙二胺作为模板剂合成了新型磷酸钒孔道化合物(H3NCH2CH2NH3)3^-[(VO)4(PO4)2(HPO4)4,并通过X射线单晶衍射实验进行了结构表征,晶体学数据为：C2/c,a=1.8505(9)nm,b=0.7089(4)nm,c=2.3304(10)nm,β=96.43(3)°,V-3.038(3)nm^3,Z=8,R=0.067,Rw^b=0.1635,该化合物具有非常独特和规整的二维孔道骨架结构,进一步的晶体化学研究表明该化合物为一新的VPO物相。     

一个新的三维配位聚合物Na[Cu_2(malonate)_2]·(ClO_4)·(H_2O)_2的合成与表征(英文)

通过Cu(ClO4)2和丙二酸在水溶液中的自组装合成了一个新的3D配位聚合物:Na[Cu2(malonate)2]·(ClO4)·(H2O)2。X鄄射线结构分析表明该化合物晶体属于正交晶系Pnma空间群(a=1.2565(3),b=1.05943(2),c=1.07556(14)nm,V=1.4317(4)nm3,Z=4)。该聚合物的空间堆积在沿b轴和c轴方向分别形成大小为0.98nm×0.83nm和0.40nm×0.40nm的方形孔洞,在沿a轴方向形成大小为0.85nm×0.40nm的砖墙形孔洞。磁性测试结果表明该化合物显示出铁磁性。导电性能测试实验表明它是一个半导体,经拟合得到其活化能为0.80eV。     

{Cd(dmt)_2(Hchdc)_2(H_2O)_2}_n配合物的合成与表征

通过水热合成的方法,以1,4-环己烷二羧酸、2,4-二氨基-6-甲基三嗪和CdCl_2·2.5H_2O为原料合成了一种单核的化合物{Cd(dmt)_2(Hchdc)_2(H_2O)_2}_n(dmt=2,4-diamino-6-methyl-triazine,H2chdc=1,4-cyclohexanedicarboxylic acid),并进行了IR和X射线单晶衍射(常温)的分析.结果表明,该化合物属于P2/c空间群,单斜晶系,晶胞参数:a=1.330 26(11)nm,b=0.541 47(4)nm,c=2.415 54(16)nm,β=115.751(3)°,V=1.567 1(2)nm~3,Z=2,Dc=1.570g/cm~3,F(000)=764,R1=0.035 2,wR2=0.092 7.该化合物中,中心金属离子Cd(II)与氧相连形成六配位构型,并通过4种不同的氢键作用最终形成了三维的堆积结构.     

一维链状超分子化合物[Cu(dafo)_2(H_2O)_2](OPA)_2的合成和晶体结构

用4,5-二氮芴-9-酮(dafo)、邻苯二甲酸和硝酸铜合成了二价铜的一维链状超 分子化合物[Cu(dafo)_2(H_2O)_2]-(OPA)_2(OPA=邻苯二甲酸一价阴离子),其结构 通过单晶X射线衍射法确定。该化合物是单斜晶系,空间群为P2(1)/c。晶胞参数： a = 0.71093(16)nm, b = 1.5724(4)nm, c = 1.5357(3)nm, α=90.000(5) °, β =102.220(4) °,γ=90.000(5) °, V = 1.6778(6)nm~3, Z = 2, F(000) = 814, M_r = 794.17, D_c = 1.527 g/cm~3, μ = 0.727 mm~(-1), R_1 = 0.0406, wR_2 = 0.0930.单晶结构分析表明该化合物具有一维链状结构,该结构是通过氢 键这种弱相互作用形成的。     

[Nd(ONO2)6][Cu(Im)(Phen)2]2(OH)·4H2O的合成、晶体结构及磁性质

用Nd(NO3)3·6H2O、Im(C3H4N2)、Phen(C12H8N2)和Cu(NO3)2·3H2O为原料,两步反应合成了标题化合物.该化合物晶体属P1空间群,晶胞参数a=1.012 6(2) nm,b=1.179 2(2)nm,c=1.398 5 nm,α=111.32(3)°,β=93.17(3)°,γ=90.33(3)°,Z=1,R=0.043.测定了化合物的UV-Vis-NIR及IR光谱和变温磁化率,发现标题化合物在低温下具有反铁磁性质.     

两个具stp三维拓扑构型的稀土配位聚合物{[Ln_2(pda)_3(H_2O)_2]·2H_2O}_n(Ln=Nd,La)

本文利用水热合成方法,将稀土氧化物与邻苯二乙酸(H2pda)反应得到了2个新颖的稀土配位聚合物{[Ln2(pda)3(H2O)2]·2H2O}n(Ln=Nd(1),La(2))。测定了它们的晶体结构,并进行了X-射线单晶衍射、红外光谱、荧光光谱和热重分析等性质的表征。晶体结构测定表明这2个化合物为异质同晶化合物。属单斜晶系,C2/c空间群。晶体学参数分别为配合物1:a=2.629 06(18)nm,b=1.611 72(11)nm,c=0.783 27(5)nm,β=93.173(5)°,V=3.313 9(4)nm3,Z=4,F(000)=1 840,μ=3.173 mm-1,Dc=1.878 g·cm-3,R1=0.022 6,wR2=0.060 9;配合物2:a=2.627 1(14)nm,b=1.614 9(8)nm,c=0.796 6(4)nm,β=92.850(9)°,V=3.375(3)nm3,Z=4,F(000)=1 816,μ=2.570 mm-1,Dc=1.823 g·cm-3,R1=0.0466,wR2=0.1416。化合物中邻苯二乙酸配体连接相邻的稀土金属离子,形成复杂的具有stp拓朴构型的三维网络结构。     

K_2CdSnS_4的溶剂热合成与晶体结构(英文)

利用溶剂热法合成了层状硫代锡(Ⅲ)酸镉(Ⅱ)化合物K2CdSnS4。单晶X-射线衍射分析结果表明,化合物属单斜晶系,C2/c空间群,a=1.102 1(5)nm,b=1.103 0(5)nm,c=1.515 1(10)nm,α=90°,β=100.416(12)°,γ=90°,V=1.811 4(17)nm3,Z=8,Dc=3.209 g·cm-3,Mr=437.60,μ=6.853 mm-1,F(000)=1 600,λ=0.071 073 nm,R=0.104 2,wR=0.200 8。该化合物由类金刚烷[Cd2Sn2S10]8-结构单元互相连接形成层状结构。紫外-可见漫反射光谱研究表明,化合物为半导体,带隙为2.2 eV。     

Ni(II), Pd(II), Cu(II) And Zn(II) complexes with N-(2-Pyridyl)Carbonylaniline (L), Syntheses and X-Ray Crystal structures of [Cu(L)2(H2O)2](No3)2, [Cu(L)2(H2O)2](Clo4)2 and [Zn(L)2(H2O)2](Clo4)2

Reaction of the N-(2-pyridyl)carbonylaniline ligand (L) with Cu(NO₃)₂, Cu(ClO₄)₂, Zn(ClO₄)₂, Ni(NO₃)₂ and PdCl₂ gives complexes with stoichiometry [Cu(L)₂(H₂O)₂](NO₃)₂, [Cu(L)₂(H₂O)₂](ClO₄)₂, [Zn(L)₂(H₂O)₂] (ClO₄)_2, [Ni(L)₂(H₂O)Cl](NO₃) and PdLCl₂. The new complexes were characterized by elemental analyses and infrared spectra. The crystal structures of [Cu(L)₂(H₂O)₂](NO₃)₂, [Cu(L)₂(H₂O)₂](ClO₄)₂, and [Zn(L)₂(H₂O)₂](ClO₄)₂ were determined by X-ray crystallography. The cation complexes [M(L)₂(H₂O)₂] contain copper(II) and zinc(II) with distorted octahedral geometry with two N-(2-pyridyl)carbonylaniline (L) ligands occupying the equatorial sites. The hexa-coordinated metal atoms are bonded to two pyridinic nitrogens, two carbonyl oxygens and two water molecules occupying the axial sites. Both the coordinated water molecules and uncoordinated amide NH groups of the N-(2-pyridyl)carbonylaniline (L) ligands are involved in hydrogen bonding, resulting in infinite hydrogen-bonded chains running in one and two-dimensions.     

Syntheses,characterizations and crystal structures of two new complexes, [Co2(CH2 =C(CH3)CO2)4(phen)2(H2O)2] and [Pb2(CH2 =C(CH3)CO2)4(phen)2]

Two new complexes, [Co₂(CH₂=C(CH₃)CO₂)₄(phen)₂(H₂O)₂] (1) and [Pb₂(CH₂=C(CH₃)CO₂)₄(phen)₂] (phen = 1,10-phenanthroline) (2), have been synthesized and structurally characterized by single crystal X-ray diffraction methods. There are two cocrystallized conformers of [Co(CH₂=C(CH₃)CO₂)₂(phen)(H₂O)] in the asymmetric unit of 1 with the Co atoms displaying similar coordination modes. In the asymmetric unit of 2, there exist two crystallographically independent [Pb(CH₂=C(CH₃)CO₂)₂(phen)] molecules with the Pb atoms showing completely different coordination geometries. Weak intermolecular interactions such as hydrogen bonding and π–π stacking are responsible for the supramolecular assembly and stabilization of the crystal structures of 1 and 2. The complexes are characterized by elemental analysis, IR spectra, and UV–Vis spectra. The fluorescent properties of 2 are also discussed.     

N(B(NMe2)2)(Si(NMe2)3)(Ti(NMe2)3), [N(Si(NMe2)3)(Ti(NMe2)2)]2 und N(SiMe3)(Si(NMe2)3)(Ti(NMe2)3) — Synthese und Charakterisierung neuer molekularer Einkomponentenvorläufer für nitridische und carbonitridische Keramiken

N(B(NMe₂)₂)(Si(NMe₂)₃) (Ti(NMe₂)₃), [N(Si(NMe₂)₃)(Ti(NMe₂)₂)]₂ und N(SiMe₃)(Si(NMe₂)₃)(Ti(NMe₂)₃) — Synthesis and Characterization of New Molecular Single-source Precursors for Nitride and Carbonitride Ceramics Synthesis and spectroscopic data of the title compounds are reported. [N(Si(NMe₂)₃)(Ti(NMe₂)₂)]₂ crystallizes in the space group P1 , a = 8.406(7), b = 10.673(8), c = 10.872(6) Å, α = 68.45(4)°, β = 71.72(4)°, γ = 78.11(7)°, 2 877 diffractometer data (F_o ? 2σF_o), R = 0.051. The compound is characterized by a planar four-membered Ti₂N₂-ring with exocyclic tris(dimethylamino)silyl substituents attached to the nitrogen atoms of the ring.     

Syntheses and Crystal Structures of [Ni(L)_2(NCS)_2] and [Co(L)_2(NCS)_2](L=Azobis(2-pyridine)

1 INTRODUCTION The synthesis of new organic-inorganic hybrid compounds is a relatively new research area that has developed rapidly in the last several years[1]. Bische- late ligand[2, 3], such as azobis(2-pyridine), is a novel tetradentate ligand expect…     

Crystal structures of cobalt(II) complexes with N-(2-hydroxyethyl)iminodiacetic and N,N-bis(2-carbamoylethyl)aminoacetic acids: Co(Heida)·2H2O and Co(Bcegly)(ClO4)·2H2O

The cobalt atom in the structures studied is situated in the center of an octahedron involving donor atoms N and 3O organic ligands Heida or Bcegly (ions of hydroxyethyliminodiacetate or bis(carbamoylethyl)aminoacetate, respectively), water molecule oxygen atom, and a carboxylic atom of the neighboring ligand in the trans-position to the N atom, so that each (II) ion is linked with two organic anions. This results in a formation of infinite chains — uncharged [Co(Heida)(H₂O)]_n or cationic {[Co(Bcegly)(H₂O)]⁺}_n. In both cases, a molecule of crystallization water is present, and in the second case, the charge of the chains is compensated by perchlorate ions. Aminoacetic cycle of the Heida ligand is approximately coplanar to another such cycle, while a similar cycle of the Bcegly ligand is in the plane of one of six-membered aminopropionamide cycles.     

[Bi2Cl10(H2-Norf)4(H2O)8](H-Norf是诺氟沙星)

CommentDuringinvestigationsonvariousmetalcomplexeswithH鄄Norf[1,2],complexationwithBiwasinvestigated.Fig.1showsthestructureofthefirstBi髥complexcontainingtheantibacterialdrugNorfloxacin○,[Bi2Cl10(H2鄄Norf)4(H2O)8].Thisisanioniccompoundcompris鄄ingfour[H2     

两种新型salen金属络合物WO2(salen)和MoO2-(salen)的合成

新合成了两种过渡金属salen络合物WO2(salen)和MoO2(salen).通过和已经有的文献比较,发现这两种络合物的分子结构是少见的β-cis构型.     

配合物Cu(phen)2 (dca)2的合成及晶体结构

合成了配合物Cu(phen)2 (dca)2(phen=C12H8N2为1,10-邻菲啰啉,dca-为二氰基氨基阴离子),用IR对其结构进行了初步表征,并测定了配合物的晶体结构.该晶体属单斜晶系,空间群为P21/c;晶胞参数a=0.8869(2)nm,b=1.4691(2)nm,c=1.9298(2)nm,β=100.90(1)°;V=2.4691(8)nm3,Z=4,F(000)=1132.00,Dc=1.496g/cm3,R=0.051,RW=0.068.中心铜(Ⅱ)离子分别与两个phen中的四个N原子和两个dca-的两个N原子配位,形成六配位的变形八面体结构.     

Synthesis and Crystal Structure of 4-Chloro-N- （2-（2-nitrophenyl）acetoxy）-N-（m-tolyl）benzamide

The new title compound 4-chloro-N-(2-(2-nitrophenyl)acetoxy)-N-(m-tolyl)benzamide(C22H17ClN2O5, Mr = 424.82) has been synthesized via the reaction of 4-chloro-N-hydroxy-N-(m-tolyl)benzamide with 2-(2-nitrophenyl)acetyl chloride. The structure of the product was confirmed by 1H NMR, 13 C NMR, IR, HRMS(ESI) and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a = 13.0269(10), b = 6.7251(6), c = 23.9313(16) , β = 99.931(6)o, V = 2065.1(3) 3, Z = 4, Dc = 1.366 g/cm3, F(000) = 880, μ = 0.221 mm-1, the final R = 0.0600 and wR = 0.1754 for 1981 observed reflections(I 2σ(I)). X-ray analysis indicates that the chloro-phenyl ring(C(10)~C(15)) and the methyl-substituted benzene ring(C(16)~C(21)) are not coplanar with the nitro-substituted benzene ring(C(1)~C(6)), with the dihedral angle to be 70.78° and 63.72°, respectively. Hydrogen bonds C(2)–H(2)···O(2) and C(7)–H(7B)···O(5) are observed.     

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…