Synthesis and Crystal Structure of 2,2-Dimethyl-4-[1H-（ 1,2,4-triazolyl）]-4- [ 1H-benzotriazolyl]-3- butanone[t-BuCOCH（C2H2N3）（C6H4N3）]

1 INTRODUCTION Triazole nuclei appear frequently in the structures of various natural products and biologically active compounds, notably thiamine (vitamin B), peni- cillins, antibiotics such as micrococcin[1], and many metabolic products of fungi and p…     

Synthesis and Crystal Structure of 9-Amino-7-（2-chlorophenyl）-6H-benzo[c]thiochromene-8,8,10（7H）-tricarbonitrile DMF Solvate

The title compound 9-amino-7-(2-chlorophenyl)-6H-benzo[c]thiochromene-8,8,10(7H)-tricarbonitrile DMF solvate(C25H20ClN5OS,Mr = 473.97) was synthesized and crystallized.The crystal belongs to triclinic,space group P1 with a = 7.6393(2),b = 10.5212(3),c = 15.0573(4) ,α = 86.797(1),β = 79.445(1),γ = 75.379(1)°,Z = 2,V = 1151.16(5) 3,Dc = 1.367 g.cm-3,μ(MoKα) = 0.285 mm-1,F(000) = 492,R = 0.0389 and wR = 0.1005 for 3455 observed reflections(I > 2σ(I)).X-ray analysis reveals that the new six-numbered ring(C(1)-C(6)) forms a skew boat conformation.The molecule links a molecule of DMF via the N(1)-H(1A)...O(1) hydrogen bond,while another hydrogen bond C(23)-H(23A)...N(2) links adjacent molecules,forming dimmers along the a axis.     

Preparation and structural properties of 7,8-dioxa[6]helicenes and 7a,14c-dihydro-7,8-dioxa[6]helicenes.

The potentially chiral 7,8-dioxa[6]helicenes 1-1c have been prepared by oxidation of their precursors the 7a,14c-dihydro-7,8-dioxa[6]helicenes 3. The crystal structure determination of 3b cis-7a,14c-dihydro-3,12-dibromo-7,8-dioxa[6]helicene unambiguously confirms the cis configuration of the 7a,-14c hydrogens in compounds 3 as previously implied from NMR measurements and also shows that 3b crystallizes in a chiral conformation in the solid state. Selective deuteration of the sterically crowded 1,14 positions of 7,8-dioxa[6]helicene 1 influenced the crystal structure. The deuterium labeled compound D2-1 exhibits a disordered structure, whereas 1 had been found to crystallize in a complex structure which can be described as an analogous partly ordered modulated superstructure. When dehydrogenation of compound 3 to obtain compound 1 was attempted, harsh synthetic conditions gave the unexpected halogenated compounds 5-chloro-7,8-dioxa[6]helicene 1c and cis-7a,14c-dibromo-7,8-dioxa[6]helicene 3c. Compounds 1d and 3b were identified by solving their crystal structure.     

Synthesis and Crystal Structure of 1-（4-Fluorophenyl）-2-hexylthiobenzo[4,5]-furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H）-one

The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854(3) ,b = 17.2678(4) ,c = 18.1828(5) ,β = 99.364(2) °,V = 4332.58(18) 3,Z = 4,Dc = 1.338,F(000) =1824,μ = 0.185 mm-1,MoKa radiation(λ = 0.71073) ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I > 2σ(I) . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5(1H) -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.     

[Co(enMe)_3]_2[As_8V_(14)O_(42)(H_2O)]·10H_2O的水热合成、性质和晶体结构

合成了一种新的砷-钒-氧簇合物[Co(enMe)3]2[As8V14O42(H2O)]10H2O(enMe为1,2-丙二胺),用元素分析、IR和TGA-DTA等进行了表征,并用X射线衍射法测定了晶体结构。结果表明,该晶体属单斜晶系,C2/c空间群,晶胞参数a=28.990(7),b=15.540(6),c=22.77(1),b=131.24(4),Mr=2744.68,V=7714(7)3,Z=4,F(000)=5232,m(MoKa)=7.239mm-1,Dc=2.363g/cm3,R=0.069,Rw=0.073。结构测定表明,结构中簇阴离子[As8V14O42(H2O)]4-与配位阳离子[Co(enMe)3]2+之间靠静电作用相结合,同时通过氢键构成无限的三维骨架结构。     

Synthesis and Crystal Structure of 8-(2,3-Dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo [f] cyclohepta [c] quinoline

The title compound 8-(2,3-dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo[f]-cyclohepta[c]quinoline(C26H25NO2,Mr=383.47) was synthesized and characterized by IR,1H NMR,13C NMR and elemental analysis.The crystal belongs to triclinic,space group P1 with a= 8.1490(16),b=9.2550(19),c=14.373(3) ,α=86.96(3),β=89.66(3),γ=70.32(3)°,Z=2,V=1019.2(4) 3,Dc=1.250 g·cm-3,μ(MoKα)=0.078 mm-1,F(000)=408,the final R=0.0555 and wR=0.1240 for 2228 observed reflections(Ⅰ > 2σ(Ⅰ)).X-ray analysis reveals that the seven-numbered ring is slightly similar to a six-numbered ring,forming the chair-like conformation.The four rings(Ⅰ,Ⅱ,Ⅲ and Ⅳ) in the benzo[f]cyclohepta[c]quinoline moiety form a screw structure.     

Synthesis and Crystal Structure of a 3-D Hydrogen-bonded Supramolecular Decavanadate Compound [Habo]6[V10O28]·2C3H7OH·2H2O

A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·solvents and its crystal structure was reported as follows: monoclinic, space group P21/n, a =11.419(9), b = 16.811(16), c = 15.521(12) (A), β= 102.98(2)°, V= 2903(4) (A)3, Z = 4, C15H46N3O19V5,Mr = 827.25, Dc = 1.893 g/cm3, λ(MoKα) = 0.71073 A,μ = 1.636 mm-1, F(000) = 1696, the final R =0.0696 and wR = 0.1361 for 4641 observed reflections with I ＞ 2σ(I). The compound is based on decavanadate clusters [V 1oO28]6-. The hydrogen bonding interactions among Habo+ cations, solvents and decavanadate clusters extend 1 into a three-dimensional supramolecular architecture.     

Synthesis and Crystal Structure of 3-Phenyi- 6-（4-methylphenyi）-1,2,4-triazolo[4,3-b]-1,2,4-triazine

1 INTRODUCTION The fused heterocycles bearing 1,2,4-triazine have attracted considerable attention in recent years owing to their biological and pharmaceutical activi- ties[1～3]. The 1,2,4-triazine core is a versatile synthe- tic platform to access a wide range of condensed heterocyclic ring systems via inter- and intramolecu- lar Diels-Alder reaction with a vast array of dieno- philes[4～6]. IBD (iodobenzene diacetate) is commer- cially available and used as benign non-metallic oxidant…     

Crystal Structure and Biological Activities of (R)-N''-[2-(4-Methoxy-6-chloro)-pyrimidinyl]-N-[3-methyl-2-(4-chlorophenyl)butyryl]-urea

The title compound (R)-N'-[2-(4-methoxy-6-chloro)-pyrimidyl]-N-[3-methyl-2-(4-chlorophenyl)butyryl]-urea has been synthesized, and its crystal structure and biological behaviors were studied. Crystallographic data: C17H18Cl2N4O3, Mr = 397.25, monoclinic, space group P21/c, a = 12.331 (2), b = 14.025(3), c = 23.085(5) (A), β = 99.607(4)°, Z = 8, V = 3936.2(13) (A)3, Dc = 1.341 g/cm3, F(000) = 1648, R = 0.0718, wR = 0.1585 and μ(MoKα) = 0.353 mm-1. The preliminary biological tests showed that the title compound has definite insecticidal and fungicidal activities.     

Synthesis and Crystal Structure of 2-(Diphenylphosphine oxide)-3-(diphenylphosphine oxide ethynyl) spiro [bicyclo[2.2.1]hepta-2,5-diene-7,1''''-cyclopropane]

1 INTRODUCTION Organic phosphine compounds always attract great interest for their unique properties and extensive uses in biochemistry, pesticide chemistry and synthetic organic chemistry. In the last two decades, much attention has been paid to phosphorus-containing olefin and acetylenic compounds for their applications in transition metal chemistry, asymmetric catalysis and photorearrang- ement [1~7 ]. Previously, we have reported the crystal structure of a novel host compound which …     

Synthesis and Structure of 2-Isobutyl-6-(2'''',4''''-dichlorophenyl)imidazo[2,1-b]-1,3,4-thiadiazole

1INTRODUCTIONThethiadiazoleandimidazolecompoundsareextensivelystudiedduetotheirspectrumbioacti-vities[1～4].Amongthem,theimidazo[2,1-b]-1,3,4-thiadiazolederivativesarepharmaceuticallyimpor-tantbecauseoftheirimmunostimulant[5],antifugal[6],antimicrobial[7]…     

Synthesis and Crystal Structure of 2-(4''-Methylphenoxy)-5,8,9-trimethyl-3-phenyl Thieno[3'',2'':5,6]pyrido[4,3-d]pyrimidin-4-(3H)-one Hydrochloride

The title compound 2-(4′-methylphenoxy)-5,8,9-trimethyl-3-phenyl thieno[3′,2′:5,6]pyrido[4,3-d]pyrimidin-4(3H)-one hydrochloride (C26H23Cl4N3O2S, Mr = 583.33) has been deter- mined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 14.8442(11), b = 11.5131(8), c = 17.2010(13) (A), β = 113.7250(10)o, V = 2691.3(3) (A)3, Z = 4, Dc = 1.440 g/cm3, S = 1.094, μ = 0.547 mm-1, F(000) = 1200, the final R = 0.0571 and wR = 0.1458. X-ray analysis reveals that the title compound combines with a molecule of dichloromethane by an intramolecular hydrogen bond. The thienopyridine ring is almost coplanar, and the dihedral angle between the thiophene plane and the pyridine plane is 0.6o.     

Synthesis and Crystal Structure of 2-Ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3（2H）-one

The crystal structure of the title compound 2-ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3(2H)-one(C15H15ClN2O4,Mr = 322.74) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of orthorhombic,space group Pccn with a = 16.7246(10),b = 19.6626(12),c = 9.3013(6) ,V = 3058.7(3) 3,Z = 8,Dc = 1.402 g/cm3,μ = 0.269 mm-1,F(000) = 1344,the final R = 0.0506 and wR = 0.1464 for 2568 reflections with I 2σ(I).In addition,disordered C(14) and C(15) atoms exist in the crystal structure.     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Mo(V) Phosphate [Zn(Mo~v_6P_4O_(31)H_(10))_2(C_4H_(14)N_3)_2]·2C_4H_(13)N_3·8H_2O

1 INTRODUCTION Hydrothermal synthesis of Mo(V) phosphates has allowed various structures, all characterized by the presence of identical clusters with the composition Mo12MP8X62 (X = O, OH) to be stabilized[1～6]. Many Mo(V) phosphates with such clusters have been iso- lated to date. The first compound was discovered by Haushalter and Lai[1] for M = Na with the formula (PPh4)2[(H3O)2NaMo6P4O24(OH)7]?5H2O. Recently, a second type of structure has been observed for M = Na (Na8(…     

The First Example of a Supramolecular Structure Containing [2-（1H-Pyrazol-3-yl）-pyridine] Complex and both α- and β-Octamolybdates

The title compound, [Ni（C8N3H7）3]4[Mo8O26]2·6H2O 1, has been synthesized from the reaction of 2-（1H-pyrazol-3-yl）-pyridine （L） with （NH4）2MoO4·2H2O and NiCl2·6H2O. Elemental analysis, IR, UV spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure of the compound. Crystal data： C96H96Mo16N36Ni4O58, Mr = 4451.97, monoclinic system, space group P21/n, a = 20.846（5）, b = 14.825（5）, c = 23.122（5） A ,β= 91.594（5）°, V = 7143（3）A^3, Z = 2, F（000） = 4344, Dc = 2.070 g/cm^3,μ = 1.968 mm^-1, R = 0.0452 and wR = 0.1056 for 17102 independent reflections （Rint = 0.0442） and 11074 observed reflections （I 〉 2σ（I））. Structural analysis indicates that two kinds of octamolybdates （[α-Mo8026]^4- and [β-Mo8026]^4-） co-exist in the compound. This is the first example of a supramolecular structure containing L complex as well as both α- and β-octamolybdate clusters.     

Synthesis and Crystal Structure of a Cyano- bridged Bimetallic Complex[La(DMSO)_3(H_2O)_3- Cr(CN)_6]·H_2O (DMSO = Dimethylsulfoxide) with One-dimensional Chain Molecular Structure

1 INTRODUCTION Over the last decade, there has been continuous interest in cyanide-bridged lanthanide-transition me- tal complexes due to their extensive applications in preparing rare earth orthoferrites[1], chemical sensor materials[2], fluorescent ma…     

Synthesis and Crystal Structure of [Mn(DPMT)2Cl2(H20)2]

The title compound [Mn(DPMT)2Cl2(H2O)2] (DPMT = 1 -[[2-(2,4-dichlorophenyl)-1,3-dioxolan-2-yl]methyl]-1H-1,2,4-triazole) was synthesized by the reaction of MnCl2-4H2O and DPMT in ethanol solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2/c with a=23.913(4), b=7.8883(13), c=8.6291(14) (A),β=95.816(3)°,V=1619.4(5)(A)3,Z=2,C24H26Cl6MnN6O6 Mr=762.15, Dc=1.563 g/cm3, μ=0.950 mm'1, S=1.045, F(000)=774, R=0.0462 and wR=0.0981. The molecular structure is a centrosymmetric conformation, and two ligands are symmetrically located on both sides of the Mn atom. The manganese atom is surrounded by two nitrogen atoms from ligands, two chlorine atoms and two oxygen atoms from water molecules to form a slightly distorted octahedral geometry.     

Synthesis, Crystal Structure and Luminescent Property of a Novel 1-D Cadmium(II) Complex: [Cd_2(C_8H_3NO_6)_2(H_2O)_4]_n·2nH_2O

A novel one-dimensional chain-like coordination polymer constructed from 3-nitro- benzene-1,2-dicarboxylic acid, [Cd2(C8H3NO6)2(H2O)4]n·2nH2O, has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to monoclinic, space group P21/c with a = 6.1252(8), b = 20.706(3), c = 8.8067(11) , β = 95.608(2)°, V = 1111.6(2) 3, Mr = 751.12, Dc = 2.244 g/cm3, F(000) = 736, μ = 2.011 mm-1, Z = 2, the final R = 0.0262 and wR = 0.0692 for 2338 observed reflections with I > 2σ(I). The structure of the title compound presents a 1-D chain-like structure constructed by dimer units, [Cd2(C8H3NO6)2(H2O)4]n, through two carboxylate oxygen atoms. The fluorescence of the title compound has been also discussed in this paper.     

Synthesis and Crystal Structure of a Complex Bimetallic Salt [Ni(trans_[14]diene)] [Ni (mnt)_2]

1INTRoDUCTIONMacrocycliccoordinationcomPOundshavebeenwidelyinvestigatedinthepastdecadesbecauseoftheirrelationshiptocomplexesofbiologicalsignificancesuchasthePorphyrinsandcorrins(lJ.Structuresofmanymacrocycliccompoundshavebeenre-ported,especiallythecompoundscontainingN4macrocyclicligands"'.However,toourknowledge,onlyafewcrystalstructuresofcomplexbimetallicsaltscontainingmacrocyclicligandshavebeendeterminedbyX-raydiffractionmethod.Inthispa-per,werePortthesynthesisandstructureofthetit1ecom…     

Synthesis and Crystal Structure of a Novel One-dimensional Coordination Polymer [ （C14H18N2）（Pb2i6）]n

1 INTRODUCTION The organic-inorganic hybrid material is a new type of composite between organic and inorganic polymers, and has captured the imaginations of che- mists due to its potential applications in electric con- ductivity, magnetism, ion exchange…