The IR Spectra Analysis and Crystal Structure of V_3(μ_3-O)(μ_2-O_2CEt)_6(O)_2(THF)·2CHCl_3

The title compound (C_ 24H_ 40Cl_6O_ 16V_3, M_r = 950.08) was synthesized from the reaction of VCl_3 and NaO_2CEt in CHCl_3 and THF. The crystal structure has been determined by X-ray single-crystal diffraction analysis. It crystallizes in monoclinic space group C2/c with a = 12.5768(4), b= 16.5601(4), c = 19.3574(7) , β = 99.879(1)°, V = 3971.3(2)3, D_c = 1.589 g/cm3, μ= 1.157 mm -1, F(000)=1932, Z=4, R = 0.055, wR = 0.1539 (I2σ(I)). This compound has an unusual coplanar V_3O core with a C_2 axis passing through O(1), V(1), O(10): one V-μ_3O is short (1.628 ), the other two are longer (2.381 ). It was characterized by IR, 1H NMR, and EPR spectra. It was unstable and the decomposition process of this compound was studied using IR spectroscopy.

Synthesis and Crystal Structure of[(CH_3)_4N]_4,H_2[ZnW_(11)SnO_(39)]·9H_2O

The complex [(CH_3)_4N]_4,H_2[ZnW_(11)SnO_(39)]·9H_2O Crystallizes in themonoclinic space group P21/m with cell dimensions: a=13. 164(3) A, b=21. 502(4)A, c=13. 234(3) A, a=90, β=91. 70(3), r=90, V=3744. 3(13) A3, Z=4,Mr= 3307. 15, Dc= 2. 933 g/cm3, A (MoKa ) = 0. 71073 A, u=175. 45 cm-1,F(000) = 2956, T= 293K, R=0. 0801 for 8401 observed reflections. The anion in thetitle compound is of a-typekeggin structure.

Synthesis, Characterization and Crystal Structure of (Z)-1-[2-(Triarylstannyl)vinyl]-1-indanols and Their Arylha-lostannyl Derivatives

Z)-1-[2-(Tri-o-tolylstannyl)vinyl]-1-indanol (1) and (Z)-1-[2-(tri-p-tolylstannyl)vinyl]-1-indanol (2) were syn-thesized by the addition reaction of 1-ethynylindanol with tri-o-tolyltin and tri-p-tolyltin hydride. The aryl groups in compound 1 and 2 were substituted by Br2 or I2 to yield monohalide derivatives (36). The compounds 16 were characterized by elemental analysis, 1H NMR and FT-IR spectroscopy. The crystal structures of 1, 2 and 4 have been determined by single crystal X-ray diffraction analysis. The Sn atom in 1 and 2 exhibits a tetrahedral geometry distorted towards trigonal bipyramid due to a weak intramolecular interaction between Sn and the hydroxyl O atoms [0.2839(4) nm and 0.2744(5) nm], while the Sn atom in 4 adopts a trigonal bipyramidal geometry with a significant O→Sn(1) interaction [0.2552(5) nm].

Crystal Structure and Property Research on Compounds Co(Ⅱ) and Zn(Ⅱ) with 3-Methylbenzoic Acid

Two compounds with 3-methylbenzoic acid（HL） [Co（L）2（4,4＇-bipy）]n 1 and [Zn2（L）4（4,4＇-bipy）]n 2（L = 3-methylbenzoic acid） have been hydrothermally synthesized directly and characterized by single-crystal X-ray diffraction analysis,elemental analyses,IR spectra and ultraviolet-visible diffuse reflection integral spectra（UV-Vis DRIS）.The two compounds are both one-dimensional infinite chains.The structural difference is that 1 is a double-chain structure and 2 is only a single chain one.At the same time,the carboxylate groups adopt different modes in the two compounds,relatively.Additionally,in order to explore the structural characteristic,two-dimen-sional IR spectra are investigated for 1 and 2.Photo-luminescent property of 2 is also researched in detail.

The Structure of Insoluble Pectinates and Alginates of Polyvalent Metals Based on IR Spectra Data

Using the method of IR spectroscopy it was ascertained that in pectinates and alginates of polyvalent metals the coordination bonds between cations Pb2+, Cu2+, Zn2+, Cr3+, Mn2+, Fe2+, Co2+, Ni2+ and the oxygen atoms of carboxyl and hydroxyl groups, pyranose cycle and glycosidic linkage of polyuronides, the water molecules are formed. It was also ascertained that Cu2+ cations form asymmetrical structures with carboxyl groups of polyuronides (monodentate ligands) and cations of other metals—symmetrical structures with carboxyl groups of polyuronides (bidentate ligands).

Crystal and Molecular Structure, and Spectral Characteristics of Sodium 3,5-Bis(Hydroxyimino)-1-Methyl-2,4,6-Trioxocyclohexanide

Sodium 3,5-bis(hydroxyimino)-1-methyl-2,4,6-trioxocyclohexanide C7H5N2NaO5 (I) has been isolated as the only product of the reaction of nitrosation of methylphloroglucinol. The structure of the titled compound has been determined from single crystal X-ray diffraction data. The hydrated C7H5N2NaO52.5H2O crystallizes in the monoclinic space group C2/c, with a(?) 16.408(3);b(?) 12.446(3);c(?) 13.716(3);(o) 126.34(3). The planar organic anion exists in a triketo-dihydroxyimino form with the C–O and C–N distances from 1.220(2) to 1.271(2)?? and from 1.292(2) to 1.293?? respectively. In the IR spectrum of I, the sharp absorption band occurred at 1681 cm-1 due to C=O stretching indicating the strong H-interactions. The correlations of theoretical (DFT-B3LYP/aug-cc-pVDZ) and experimental UV-vis absorption spectra in neutral and alkaline ethanolic solutions showed the existence of hydroxyimino-nitroso tautomerism while ionization of I.

Crystal and Molecular Structure of 4-Benzoyl-1,5-diphenyl-1H-pyrazole-3-carbonitrile

The crystal structure of potential active 4-benzoyl-1,5-diphenyl-1H*-pyrazole-3-carbonitrile (C23H15N3O) (I) has been determined from single crystal X-ray diffraction data. Also IR, Uv-vis and NMR spectral data were determined. The title compound crystallizes in the monoclinic space group P* 21/c, with a* = 9.3167(2), b* = 20.6677(3), c* = 10.6143(3) ?, β* = 112.665(3)°, V* = 1886.00(8) ?3, Dcalc* = 1.23g cm-3, Z* = 4. In the structure, intermolecular H*-bonds lead to the formation of a centrosymmetric dimmer of the molecule. Furthermore, the compound has a wide transmission window (300 to 1100 nm) with a transparency of nearly 100% and the UV cut-off wavelength occurs at 242 nm.

A dinuclear molybdenum cluster containing i-mnt ligand: synthesis and crystal structure of [Mo_2S_4(i-mnt)_2] (Et_4N)_2

A dinuclear molybdenum(V) cluster compound (Et4N)2[Mo2S4(i-mnt)2] (i-mnt=l,l-dicyanoethylene-2,2-dithiol, (S2C=C(CN)2]2-) has been prepared by the ligand substitution reaction of Mo2S4(iso-pr2dtp)2 (iso-pr2dtp=S2P(OC3H7)2-) with K2(i-mnt) in the presence of Bt4NI. This cluster was characterized by inrrared spectrum, UV-Vis spectrum and single crystal structure analy-sis. The cluster anion [Mo2S4(i-mnt)2]2- possesses C, symmetry with a crystallographic mirror plane through two bridging S atoms. By the S....S supramolecular interactions between two adjacent cluster anions the [Mo2S4(i-mnt)2]2- anions are linked to form infinite chains along the b axis. Crystal data: monoclinic, space group C2/m, a=1.8748(6), b=1.5360(4), c=1.4322(5) nm, ,β=112.02(2)°, V=3.823(4) nm3, Z=4, Dc=1.50 g/cm3. The final R=0.038 and .RW=0.053 for 3015 observed unique reflections.

Synthesis and Structure of K_3Na_3〔MnMo_9O_(32)〕·6H_2O

The title compound was synthesized from the manganese(Ⅶ ), titanium(Ⅲ ) and molybdate. It was crystallized as K3Na3[MnMo9O32,). 6H2O in the rhombohedral space group R32(155 # ), with a=b= 15. 521 (4), c= 12. 417 (6) A γ=120. 00 (1 )°. V= 2590. 1 (1 ) A 3, Z= 3, M.= 1778. 08, Dc= 3. 396g/cm3, λ(MoKa)=0. 71073A, μ= 42. 5 cm-1, F(000) ~ 2754 and the structure was determined by Xray diffraction methods, refined to a residual of 0. 048 for 1137 independent observablereflections with I≥3σ(I). There are Potassium, sodium canons, [MnMo9O32]6- anion, and crystalline water molecules in the complex. The anion may be constructedfrom a hypothetical MnIVMo6 Anderson species by removing three alternate MoO6, octehedra and placing three MoO6, octahedra above and below the MnMo3 unit, thus the resulting structure has D3 symmetry.

Synthesis and Structure of K_6H_7〔Dy(SiMo_6W_5O_(39))_2〕·10H_2O

K6H7 [Dy(SiMo6W5O39)2] 10H2O, Mr= 4878. 5, is triclinic, sapcegroup P1 with a= 22. 697(5) A; b= 12. 835(4) A; c= 18. 216(6) A; a= 90. 56(2); β= 98. 24(2); γ= 90. 51 (2)°；V= 5251 (2) A3； Z= 2, Dc= 3.08 g/cm3; F(000) = 4321; S = 1. 550, μ= 183.65 cm-1. Refinement resulted in a final R of0.091, based on 7816 with I>3δ independent renections. The structure contains discrete [Dy (SiW5Mo6O39) 2] 13 - anions. The orientations fo the W and Mo atoms are random in the crystal. The MO6 octahedron and SiO4 tetrahedron are somewhat distorted.

Synthesis and Structure of K_6PMo_7V_2W_3O_(40)(H_2O)_(16)

The reddish--brown prismatic crystal of the title compoundK6PMo7V2W3O40., (H2O)16,, (Mr.= 2518. 8) crystallizes in tetragonal system, space groupP4n2(# 118), with a= 14. 083(1), b= 14. 083(2), c= 12. 572(3) A, V=2493. 6(l)A3 D.= 2. 72 g/cm'3 Z= 2.λ(MoKa) = 0. 71073 A, μ= 108. 9 cm-l, F(000) 1840, final R= 0. 038 and Rw= 0. 050 for 1388 observed reflections with I>3. 0σ(I).. The title compound contains heteropolyanion [(Mo7W3,V2)PO40]6- linked together byK+ ions and water molecules. The heteropolyanion has the well--known Keggin structure. The 12 metal atoms in the cage of the anion comprise seven Mo, three W and twoV atoms in a random distribution. The M--M (M= 7/12 Mo+ l/4W + l/6 V) average distance in the anion is 3. 535 A. The P--M distance is 3. 537A. The P--O distance is 1. 54 A, and the M--O distances are from 1. 64 to 2. 42A for O atoms coordinated to one, two and three M atoms respectively. Potassium ions are coordinated byeight O atoms from the anion and water molecules.

Structure of Potassium of Undecatungstomononickelosilicate

The compound K4[α-SiNiW11O38]·10H2O,Mr=3053.86,crystallizes in the orthorhombic, space group Pnn2 with cell dimensions a=14.203（8）,b=14.214（6）,c=12.460（3）,V=2515（2）,Z=2,Dc=4.03 g/cm￣3,λ（MoKα）=0.71069,μ=273.1 cm（-1）,F（000）=2672.The structure was solved by direct methods.The least-square refinement based on 1190 observed reflections[I】 6σ（I）] converged to a final R=0.076.The anion in the title compound is of α type Keggin structure,although the octahedron MO6 is greatly distorted. Atoms Ni and W are statistically distributed in the crystal.

Studies on the Structure and IR Spectra of Aquacobalt(Ⅱ)-undecatungstosilicate and Aquanickel(Ⅱ)-undecatungstosilicate

Some heteropolyacids and their salts display unique activities and selectivities in both homophase and heterophase catalytic reactionst, and have attracted more and more attention. The following four tungstosilicates have recently been synthesized, in which

超分子化合物{[Mn_2(pda)(phen)_4(H_2O)_2]·2H_2O·2ClO_4^-}的构筑及表征

利用间苯二乙酸、1,10-邻菲啰啉和高氯酸锰在水热条件下反应制备了一种新型超分子配合物{[Mn2(pda)(phen)4(H2O)2]·2H2O.2ClO4-}(H2pda=间苯二乙酸,phen=1,10-邻菲啰啉).通过X单晶衍射测定了晶体结构,并用元素分析、红外光谱等技术对其进行了表征.配合物属3斜晶系,空间群为P-1,a=1.129 0(2)nm,b=1.705 0(2)nm,c=1.734 5(1)nm;α=110.559(1)°,β=107.588(9)°,γ=93.102(12)°;Z=1,R1=0.071 0,wR2=0.202 9.晶体结构分析表明2个锰在1个间苯二己酸的连接下形成了一个双核结构,再在船型六元环氢键和π…π堆积共同作用下,双核结构单元被连成2维网络结构.毗邻的2维结构之间又通过氢键的支撑,拓展为3维网状超分子体系.

Keggin型P-Mo-V杂多酸的合成

Three PMoV heteropoly acids(HPAs)with different number of V atoms were synthesized and characterized by ICPAES,TG,IR and XRD.The IR spectra indicated that they are Keggin structure.Compared the IR spectrum of PMo HPA with those of PMoV HPAs,it was found that the characteristic absorption peak values(CAPV)of all of the PMoV HPAS were redshifted.

[Zn(DMF)_6]H_2SiW_(12)O_(40)·(CH_3)_2NH的合成,晶体结构及性质

The title compound H2SiW12O40·(CH3)2NH was synthesized in mixed solvent of aqueous and acetonitrile, and its crystal structure had been determined using single crystal X ray diffraction. The crystal belongs to monoclinic, space group C2/m, a=2.0654(4)nm, b=1.3306(3)nm, c=1.3194(3)nm, β=119.59(3)°, V=3.1531(11)nm3, Dc=3.606Mg·m-3, Z=2, R=0.0462, Rw=0.0836. The title compound comprises of a 2+ unit, a polyanion and a free (CH3)2NH molecule. The ESR spectrum of the title compound shows that charge transfer between organic groups and polyanion takes place under irradiation of the sunlight in solid state. The TG study of the title compound shows that it had four stages of the weight loss, and the increase of the decomposition temperature for the polyanion shows that the stability of the polyanion was enhanced due to the influence of Zn2+ ion. CCDC:175866.

超分子化合物｛[8-hydroxyquinolineH]_4^(4+)·[SiW_(12)O_(40)]^(4-)·2H_2O｝的水热合成、晶体结构及热稳定性

A supermolecular compound, {8-hydroxyquinolineH44+·SiW12O404-·2H2O} was synthesized by hydrothermal reaction with silico-tungstic acid and 8-hydroxyquinoline. The crystal of the compound belongs to monoclinic system, space group P21/n, with a=1.282 6(6) nm, b=2.292 7(4) nm, c=2.092 0(6) nm, β=95.495(2)°, Z=4, V=6.124 1(7) nm3, Dc=3.791 g·cm-3, μ=22.568 mm-1, F(000)=6 200, R1=0.029 3, wR2=0.069 3, GOF=1.079. Su-permolecular compound is composed of one SiW12O404- with Keggin structure, four protonated cations of 8-hydroxyquinoline, two hydrones. Thermal analysis results showed that the anionic skeleton construction of heteropoly acid in compound decomposed approximately at 349.0 ℃. CCDC: 622142.

Schiff碱与锰(Ⅲ)的单核和双核配合物的合成与结构

本文报道合成了以水杨醛及邻香草醛缩丙醇胺 Ｓｃｈｉｆｆ 碱与锰（ Ⅲ） 的六个新型配合物，其中［ Ｍｎ２（ｓａｌｐａ）２ （ Ｐｈ Ｃ Ｏ Ｏ）２ ］·２ Ｃ Ｈ２ Ｃｌ２ ，［ Ｍｎ２ （ｖａｎｐａ）２ （ Ｐｈ Ｃ Ｏ Ｏ）２ ］·２ Ｃ Ｈ Ｃｌ３ ，［ Ｍｎ２ （ｖａｎｐａ）２ （ Ｃｌ Ｃ Ｈ２ Ｃ Ｏ Ｏ）２ ］（ Ｈ２ｖａｎｐａ 为邻香草醛缩丙醇胺； Ｈ２ｓａｌｐａ 为水杨醛缩丙醇胺） 三个为双核，［ Ｍｎ（ Ｈｓａｌｐａ）２（ Ｈ２ Ｏ） Ｃｌ］ ，［ Ｍｎ（ Ｈｖａｎｐａ）２（ Ｈ２ Ｏ） Ｂｒ］ 和［ Ｍｎ（ Ｈｓａｌｐａ）２（ Ｎ Ｃ Ｓ）］ 三个为单核。并对配合物的合成进行了讨论，同时对配合物的红外光谱进行了归属。对配合物［ Ｍｎ２（ｖａｎｐａ）２（ Ｐｈ Ｃ Ｏ Ｏ）２］·２ Ｃ Ｈ Ｃｌ３ 进行了单晶结构测定，其锰与锰间的距离为２ ．８４８ 〓，对配合物的磁距也进行了测定。

新型笼状钼磷超分子化合物的水热合成与晶体结构

用水热法首次合成了含有２ 种有机胺的新型笼状钼磷超分子化合物〔ＮＨ３（ＣＨ２）６ＮＨ３〕７〔ＮＨ３（ＣＨ２）２ＮＨ３〕２（Ｈ３Ｏ）６〔Ｐ２ Ｍｏ５Ｏ２３〕４·１１Ｈ２Ｏ，并通过元素分析、红外和Ｘ－ 射线单晶衍射法进行了结构表征．晶体属三斜晶系，空间群ｐ１杂多阴离子中的每个〔Ｐ２Ｍｏ５Ｏ２３〕６－ 是由５ 个ＭｏＯ６ 八面体和两个ＰＯ４ 四面体键合而成，其中Ｍｏ，Ｐ原子成一个畸变五角双锥构型．

稀土配合物[Pr(1,3-pda)_(0.5)(nbca)_2(H2O)_2]的合成及结构研究

在水热条件下合成了一个新颖的Pr(Ⅲ)配合物[Pr(pda)0.5(nbca)2(H2O)2](pda=间苯二乙酸,nbca=5-硝基[1,1'-联苯]3-羧酸),并利用元素分析、X-单晶衍射、红外光谱、热重分析等对其进行表征.结果表明,该配合物属于单斜晶系,空间群为C12/c1,a=2.726 38(13)nm,b=1.010 66(5)nm,c=2.143 87(10)nm,β=94.258(1)°,V=5.891 0(5)nm3,Z=8.晶体结构分析表明:在该配合物中Pr3+离子是1个8配位的配合离子,2个配体作为间隔物将稀土金属离子Pr3+链接形成[-Pr-pda-Pr-nbca-]n Z字形链,由5-硝基[1,1'-联苯]3-羧酸羧基的桥连支撑将1维链拓展为2维(6,6)波浪网面.