Syntheses and Crystal Structure of a New Molecular Clip Based on Diethoxycarbonyl Glycoluril: C_(54)H_(38)N_8O_6·H_2O

A new glycoluril derivative 2 has been synthesized and characterized by singlecrystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 13.128(7), b = 13.245(7), c = 14.016(8) ?, α = 98.805(10), β = 102.036(9), γ = 101.470(10)°, V = 2287(2) ?3, Z = 2, C54H38N8O6·H2O, Mr = 912.94, F(000) = 952, T = 298(2) K, Dc = 1.326 g/cm3 and μ = 0.090 mm-1. Due to the intermolecular C–H...O interactions, two monomeric molecular clips dimerize as a dimeric building block in the crystalline state. Those building blocks form tape-like supramolecular polymers driven by intermolecular C–H...N interactions and water molecules which stabilized in the packing structure served as hydrogen-bonding donors.     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Novel Water Cluster [Mn(phen)_2·H_2O·Cl]·p-FBA·3H_2O

A novel water cluster [Mn(phen)2·H2O·Cl]·p-FBA·3H2O (p-FBA = p-fluorobenzoic acid and phen = 1,10-phenanthroline) was synthesized by the hydrothermal reaction of MnCl2 with p-FBA and phen at 150 ℃ and characterized by elemental analysis,IR spectra and TG. Its crystal structure was determined by X-ray single-crystal diffraction study. The crystal belongs to the triclinic system,space group P1,with a = 10.5768(1),b = 11.5960(1),c = 12.9916(2) ,α = 101.816(2),β = 95.397(2),γ = 103.052(2)o,V = 1502.8(3) 3,Z = 2,Dc = 1.463 g/cm3,R = 0.0399 and wR = 0.0997. The crystal structure shows that the manganese(Ⅱ ) ion is six-coordinated by four nitrogen atoms,one chloride ion and one oxygen atom forming a distorted octahedral coordination geometry. The structure includes three acyclically connected water molecules and one coordinated water molecule thus forming a (H2O)4 water cluster. This water pattern forms a cross-linked discrete ring. The steady (H2O)4 is further extended into a cage-like structure by the hydrogen-bonding interaction formed by dissociative aqua molecule and Cl-ligand. The dimer structure is further extended into a one-dimensional (1D) structure through C-H···O interaction. π···π Stacking interaction among adjacent phen aromatic rings further stabilizes the crystal structure.     

钴配合物[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4的合成与晶体结构研究

用硫酸钴、4,4'-联吡啶和2-磺酸基乙基膦酸合成了一个新颖的钴化合物:[Co_2(H_2O)_8(C_(10)H_8N_2)_2]·(HO_3PCH_2CH_2SO_3)(SO_4)(H_2O)_4,并对其进行了红外.元素分析、热重测试,通过单晶衍射仪测定了其晶体结构.结果表明,配合物属单斜晶系C2/c空间群,分子式为C_(22)H_(45)Co_2N_4O_(22)PS_2,分子量为930.57,晶胞参数为a=19.8456(18),b=11.2957(10),c=34.719(3)(A),β=106.095(3)°,晶胞体积为7477.9(12)(A)~3,Z=8,Dc=1.653 g/cm~3,F(000)=3856,μ=1.131 mm~(-1),最终残差因子R_1=0.0726,wR_2= 0.1719(相对于5612个I>2σ(I)的可观测衍射点).在这个化合物中,二齿配体4,4'-联吡啶把Co(II)桥连成[Co(4,4'-bipy)]~(2+)链.化合物中的[Co(4,4'-bipy)]~(2+)链有三个不同的朝向.2-磺酸基乙基膦酸没有参与配位而是做为一个有机模板剂填充在[Co(4,4'-bipy)]~(2+)链形成的空隙中.     

Synthesis and Characterization of a Manganese(Ⅱ) Coordination Compound with Two-dimensional Layer Structure: {[Mn_2(IP)_2(1,4-bdc)_2]·H_2O}n

A new complex {[Mn2(IP)2(1,4-bdc)2]·H2O}n(1)(IP = 1H-imidazo[4,5-f][1,10]-phenanthroline, 1,4-H2 bdc = 1,4-benzendicarboxylic acid), have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group Cc with a = 20.326(2), b = 24.249(2), c = 7.621(1), β = 108.546(6), V = 3561.2(7)3, Z = 4, Dc = 1.672 g/cm3, μ = 0.785 mm-1, F(000) = 1824, S = 1.067, the final R = 0.0299 and wR = 0.0752. Compound 1 possesses a 2D structural motif, in which two crystallographically independent 1,4-bdc dianions adopt the alternative mode of mixed bis(bidentate) and monodentate-bidentate coordination modes to bridge neighboring Mn(II) centers. And the 2D layers are linked up by hydrogen bonding and π···π stacking interactions to form a 3D network. The title compound has good thermal stability and exhibits photoluminescent emission maximum at 518 nm.     

Mo_8~ⅤW_2~ⅥO_(26)(C_5H_5N)_8·2H_2O: A Novel Mixed-valence Heterometal Polyoxometalate

A new mixed-valence heterometal cluster Mo8VW2VIO26(C5H5N)8·2H2O has been synthesized under solvothermal conditions and characterized by X-ray single-crystal diffraction, IR, UV-vis and XPS spectroscopy. The title compound crystallizes in the triclinic system, space group P1 with a = 11.708(3), b = 12.018(4), c = 13.316(4) , a = 112.184(4), β = 97.844(4), r = 110.043(3)o, V = 1551.9(8) 3 and Z = 1 at 293(2) K. The final full-matrix least-squares refinement converged to R = 0.0414 for 4460 observed unique reflections with I 2σ(I) and w R = 0.1290 for all data(5352) and S = 1.015. In addition, its thermal stability and fluorescent property have also been investigated.     

K_(4.5)Na_4(H_3O)_(3.5)[Ce(SiW_(11)O_(39))_2]·23H_2O的合成和晶体结构

合成了标题化合物K4.5Na4(H_3O)3.5 [Ce(SiW11O39)2]·23H_2O,用单晶X-ray 衍射方法测定了它的结构,该晶体属三斜晶系,空间群P,a=16.531(4) ,b=23.193(4),c=12.764 (2)?,α= 99.740(6),β = 91.90(1), γ = 94.84(1)°,V = 4801(2) ?3,Mr = 6180.91, Z=2,Dc = 4.276 g·cm－3,μ(MoKα)= 27.06 mm－1, F(000)= 5359, R = 0.0781 ,wR = 0.1838,I >2((I) 的可观察衍射点11936个。该分子是由2个α-SiW11O39结构单元通过1个铈离子联结起来,铈离子八配位,形成了1个畸变的十二面体结构,Ce-O键长2.39(2)～2.45(3) ?。在杂多化合物中,硅氧四面体的氧原子存在μ4-Oc和μ3-Oc的2种配位状态。     

新型过渡金属取代层状磷酸铝[C_4H_(11)N]_(0.77)[C_4H_(12)N]_(0.23)[C_3H_(12)N_2]_2[H_3O]_2·[Co_(0.23)Al_(5.77)P_8O_(32)]的共模板法合成及表征

采用共模板法以二乙胺和1,2-丙二胺为模板剂,合成了过渡金属取代的二维层状磷酸铝化合物[C4H11N]0.77[C4H1 2N]0.23[C3H12N2]2[Co0.2 3Al5.77P8O32][H3O]2(1).通过X射线衍射(XRD)、热重分析(TG)、元素分析(ICP-AES及CHN)、固体紫外-可见分析(Solid-UV-Vis)及扫描电子显微镜(SEM)等对化合物1进行了表征.该化合物属三斜晶系,P 1-空间群,晶胞参数a=0.95029(19)nm,b=1.2689(3)nm,c=1.2987(3)nm,α=118.70(3)°,β=97.64(3)°,γ=99.72(3)°,V=1.3117(5)nm3,Z=1.其无机骨架由铝(或钴)氧四面体(AlO4或CoO4)和磷氧四面体PO3(O)严格交替连接形成4,6,12-网层结构,无机层沿[001]方向堆砌成一维十二元环孔道.Co无序取代Al的位置,其Co/Al摩尔比约为1∶25.1.运用分子动力学模拟的方法,通过计算有机模板剂和无机骨架的相互作用,讨论了2种有机胺分子的共模板作用.     

Synthesis, Crystal Structure and Thermal Stability of the Coordination Polymer [Co（2-mpac）_2（py）·4H_2O）]_n

A new coordination polymer with the formula of [Co(2-mpac)2(py)·4H2O)]n (1, 2-mpac = 5-methyl-2-pyrazinecarboxylic acid, py = pyrazine) has been synthesized through hydrothermal synthesis and structurally characterized by X-ray single-crystal diffraction method. 1 exhibits a 3D supramolecular network. Crystal data: monoclinic, space group C2/m, a = 15.907(9), b = 7.104(3), c = 9.793(5), β = 95.232(8)o, V = 1102.0(10)3, Z = 2, S = 0.995, the final R = 0.0509, wR = 0.1626 for 1002 observed reflections with (I > 2σ(I)) and R = 0.0530, wR = 0.1667 for all data. In addition, elemental analysis, IR and thermalgravimetric analysis are presented.     

Synthesis and Crystal Structure of [Cu (C_8H_4O_2F_3S) (2, 2' -bipy) ]

1INTRODUCTIONCoppercomplexesarewidelyusedascatalystsinthedecompositionofdisubsti-tutedperoxides"'-Theelectronicstructureandbondingatthecatalystscanbeprof-itablypursuedbystudyingmodelcomplexes.Generally,theCu(I)complexesareob-tainedbyreactionofCu(l)saltswithligands.Wereporthereamethodofpreparingcopper(I)complexbythereactionofCupowderwith2-thenoyltrifluoroacetone,2,2'-bipyinmethanol.2EXPERIMENTALReactionwascarriedoutundernitrogenatmosphere.2,2-bipy(1mmol)wasaddedtoamixtureof2-thenoyl…     

Synthesis and Characterization of a Bismuth Incorporating Heptamolybdate： （NH4）4 [HMo7O24Bi（H2O）2CsH3N（CO2）2]·7H2O

A new one-dimensional molecule based on the linkage of [Mo7024] clusters and [BiL] （L = pyridine-2,6-dicarboxylic acid） assembles under ambient conditions. The title compound was characterized by X-ray powder diffraction, IR and UV spectra, thermogravimetric analysis, and single-crystal X-ray diffraction. Crystal data： C7H38BiMo7N5037, Mr = 1664.95, monoclinic, space group C2/c, a = 24.312（2）, b = 21.4869（18）, c = 18.5423（16） A, β = 111.6490（10）°, V = 9002.9（13） A3, Z = 8, μ = 5.883 mm-1, F（000） = 6304, GOF = 1.045, R = 0.0365 and wR = 0.1062.     

Synthesis and Crystal Structure of a Novel Compound:[Nd_3(OH)_7(O_2CC_6H_4SO_3)(H_2O)]_n·nH_2O with a Pillar-layered Structure

A novel Nd(Ⅲ) compound,[Nd3(OH)7(O2CC6H4SO3)(H2O)]n·nH2O 1,has been synthesized by the hydrothermal reaction of Nd2O3 and 3-sulfobenzoic acid monosodium salt. It was characterized by IR spectroscopy,elemental analysis,thermogravimetric analysis and single-crystal X-ray diffraction. It crystallizes in monoclinic,space group P21/c with a = 13.024(3),b = 10.961(2),c = 12.792(3) ,β = 91.271(3)°,V = 1825.6(7) 3,Z = 4,Mr = 787.97,Dc = 2.867 g/cm3,μ = 8.584 mm-1,F(000) = 1460,S = 1.035,R = 0.0442 and wR = 0.1166 (I 2σ(I)). In this compound,the cross-linkage of Nd atoms by bridging hydroxy groups results in a Nd-O inorganic 200 layer,and such layers are linked by the 3-O3S-C6H4-CO2 dianions into a pillar-layered structure. The lattice water molecules are located in the cavity.     

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

近些年来,合成和研究开发新型结构的有机鄄无机配合功能性材料日益成为人们关注的热点[1￣3]。金属杂多酸盐以其独特的分子结构及理化性质,已经成为构造新型分子功能材料的重要无机构筑块,作为电子受体的金属杂多酸盐可以与有机π电子给体如TTF、ET和有机金属茂合物结合,形成有机鄄无机复合物。该类化合物在光、电、磁、催化和超导领域有潜在的应用前景[4￣6],它们的结构不同,性质各异,其中一些具有超分子结构[7]。本研究通过水热合成法,合成了一种未见报道的Keggin结构硅钨酸盐超分子化合物｛[8鄄hydroxyquinolineH]44·+[SiW12O40]4·…     

Hydrothermal Synthesis and Structural Characterization of a Novel 3-D Open Framework Zinc Phosphate Microporous Compound(C_5N_2H_(14))·[Zn_3(OH_2)(PO_4)_2(HPO_4)]

One novel organically templated zincophophate(C5N2H14)·[Zn3(OH2)(PO4)2(HPO4)] has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction together with elemental analysis, infrared spectroscopy, thermogravimetric analysis, and powder X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/n, with a = 9.7904(11), b = 14.0287(14), c = 11.8651(13) , β = 104.690(3), V = 1576.4(3) 3, Z = 4, T = 296(2) K, Mr = 601.31 and Dc = 2.533 g/cm3. The compound consists of a macroanionic [Zn3(OH2)(PO4)2(HPO4)]2- framework and(C5N2H14)2+ cations, and its structure is built up from ZnO3(OH2), ZnO4, HPO4 and PO4 tetrahedral units that result in 4, 8 and 10-ring channels.     

Synthesis,Crystal Structure and Fluorescent and Thermal Stability Properties of the Zinc(Ⅱ) Complex [Zn(C_(15)H_(11)O_3)_2(C_(12)H_8N_2)_2]·5H_2O

A new complex has been synthesized with o-methylbenzoyl-benzoic acid(HL) and 1,10-phenanthroline(phen) in the mixture of water and ethanol. It crystallizes in monoclinic, space group C2/c with a = 13.6328(18), b = 17.7876(18), c = 19.998(2), β = 104.720(4)o, C54H48N4O11Zn, Mr = 994.33, V = 4690.2(9)3, Dc = 1.408 g/cm3, Z = 4, F(000) = 2072, μ(MoKα) = 0.59 mm-1, R = 0.0736 and wR = 0.2029. The crystal structure shows that the zinc ions are coordinated with two oxygen atoms from two HL molecules and four nitrogen atoms from two phen molecules, forming distorted octahedral coordination geometry. The fluorescent and thermal stability properties of the complex are studied. The result shows that it has one fluorescent emission band at around 412 nm. In addition, the complex is stable under 210 ℃.     

Hydrothermal Synthesis and Structure of One New Polyoxotungsate [Ni(trien)]_4[Ni_4(H_2O)_2(HPW_9O_(34))_2]·4H_2O

One new sandwich-type tetra-nickel substituted polyoxotungsate,[Ni(trien)]4-[Ni4(H2O)2(HPW9O34)2]·4H2O(1,trien=triethylenetetramine),has been hydrothermally synthesized and characterized by IR,elemental analysis,TGA,and single-crystal X-ray diffraction analysis.Crystal data for 1:triclinic,space group P with a=13.279(3),b=13.816(3),c=14.494(4),α=95.403(1),β=113.173(4),γ=93.809(3)o,V=2418.0(10)3,Z=1 and Dc=3.861 g/cm3.X-ray crystallographic study shows that compound 1 is a relatively rare inorganic-organic hybrid polyoxo tungstate constructed from sandwich Ni-substituted polyoxo-anions and nickel complexes.     

Hydrothermal Syntheses and Structural Characterizations of Two ML-Containing Polyoxomolybdates:[Cu~Ⅱ_2(HL)_3]_2[Mo_8O_(26)]·(H_2O)_4 and [Ni~Ⅱ(HL)_3]_2(Mo_8O_(26))·(H_2O)_3(HL=3-(2-Pyridyl)pyrazole)

Two new polyoxomolybdate compounds,namely CuII2(HL)3]2[Mo8O26]·(H2O)4(1) and [NiII(HL)3]2(Mo8O26)·(H2O)3(2)(HL = 3-(2-pyridyl)pyrazole),were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu(II) ions linked by three 3-(2-pyridyl)pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-(2-pyridyl)pyrazole ligands.Crystal data of 1:C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850(2),b = 18.510(4),c = 17.230(3) ,β = 100.57(3)°,V = 3401.6(12) 3,Z = 4,Dc = 2.324 g/cm3,F(000) = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775(Ⅰ 2σ(Ⅰ));Crystal data for 2:C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799(2),b = 14.7970(13),c = 23.141(2) ,β = 91.6180(10)°,V = 7119.0(11) 3,Z = 4,Dc = 2.077 g/cm3,F(000) = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696(Ⅰ 2σ(Ⅰ)).     

Synthesis,Crystal Structure and Biological Activity of 8-（（4-（（2,3-diaminopyridin-4-yl）oxy）-3-fluorophenyl）-amino）-2-（4-fluorophenyl）-3-methyl-2,7-naphthyridin-1（2H）-one

The new title compound 8-((4-((2,3-diaminopyridin-4-yl)-oxy)-3-fluorophenyl)-amino)-2-(4-fluorophenyl)-3-methyl-2,7-naphthyridin-1(2H)-one(C26H20F2N6O2, Mr = 486.48) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 15.365(3), b = 13.144(2), c = 11.863(2), β= 108.882(3)°, Z = 4, V = 2267.0(7)3, Dc = 1.425 g/cm3, F(000) = 1008, μ = 0.105 mm-1, MoKa radiation(λ = 0.71073), R = 0.0480 and wR = 0.1294 for 3197 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the region C(substituents of 8-amino group and 3-methyl group on the 2,7-naphthyridin-1(2H)-one ring) of compound 6 are effectively planar. Intramolecular and intermolecular hydrogen bonds together with π···π interations are found in the structure. In addition, compound 6 shows potent c-Met and c-Kit kinase inhibition activities.     

Synthesis and Crystal Structure of [2-Hydroxy- 5-（4-hydroxy-3-phenyliminomethylbenzyl）-benzylidene]-phenyl-amine

The title compound [2-hydroxy-5-（4-hydroxy-3-phenyliminomethyl-benzyl）-benzylidene]-phenyl-amine （C27H22N2O2, Mr = 406.47） was synthesized by 5,5′-methylene-bissalicylal- dehyde with aminobenezene, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 4.4026（6）, b = 1.501（13）, c = 0.95818（12） nm, β = 90.868（2）°, V= 4.2813（9） nm^3, Z= 8, Dc= 1.292 g/cm^3,μ = 0.010, F（000） = 1744, R = 0.0576 and wR = 0.1450 for 3766 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the molecule has a pair of intramolecular OH…N hydrogen bonds.     

A Novel Three-dimensional Extended Supramolecular Network Constructed from Octamolybdate Clusters and Morpholine Molecules： Nae（Hmorph）e[MosO26]·2H2O

A novel organic-inorganic hybrid, Na2(Hmorph)2[MosO26]·2H2O (1, Hmorph = morpholine), has been synthesized by convenient aqueous solution method and structurally characterized by single-crystal X-ray d...     

A New Bis-(As_3O_6) Capping 6-Molybdonickelate Complex:Preparation and Characterization of [Ni(en)_2(H_2O)]_2[(NiO_6)Mo_6O_(18)(As_3O_3)_2]·2H_2O

A new complex constructed from a unit with two As3O6 rings capping Anderson-type moieties,[Ni(en)2(H2O)2]2[(NiO6)Mo6O18(As3O3)2]·2H2O(1,en = ethylenediamine),has been hydrothermally synthesized and characterized by IR,single-crystal X-ray diffraction and thermogra-vimetric analysis.The compound crystallizes in triclinic,space group P1 with a = 9.1230(16),b = 11.8078(9),c = 12.2111(9) ,α = 114.5210(10),β = 98.0350(10),γ = 100.0320(10)o,Mr = 2029.80,C8H44As6Mo6N8Ni3O36,V = 1145.0(2) 3,Dc = 2.944 g/cm3,Z = 1,GOF = 0.997,μ = 7.203 mm-1,F(000) = 970,R = 0.0352 and wR = 0.1019.Compound 1 consists of an Anderson-type capped by a two-ring(As3O6) unit [(NiO6)Mo6O18(As3O3)2]4-,two six-coordinate [Ni(en)2(H2O)2]2+ cations and two water molecules.