Enamine Configuration of 5-Methyl-2-phenyl-4-[（Z）-3-tolylamino-phenylmethylene]pyrazol-3（2H）-one

1 INTRODUCTION In contrast to the old-line academic and practical studies of 1-phenyl-3-methyl-4-benzoyl-5-pyrazo- lone (PMBP) on the metal coordination chemistry[1], the complexes of β-ketoamines derivated from PMBP received little attention due to its complicated com- plexation. However, in recent years, there has a sudden growth of this area as a result of its timely interest in biological activities[2]. Recently, a series of β-ketoamines[3] containing PMBP have been prepared fro…     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound[Et4N]2[Mo2(CO)8(SC6H4-CH3-p)2]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅｔｈｉｏｌａｔｅｌｉｇａｎｄｗａｓｉｎｔｒｏｄｕｃｅｄｉｎｔｏｍｏｌｙｂｄｅｎｕｍｃａｒｂｏｎｙｌｃｏｍｐｏｕｎｄｉｎ1 984 [1],ｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｎｌｏｗ ｖａｌｅｎｃｅＭｏ -ＳＲｃｏｍｐｏｕｎｄｓｈａｓｒｅｃｅｉｖｅｄａｔｔｅｎｔｉｏｎｆｏｒｔｈｉｓｋｉｎｄｏｆｌｏｗ ｖａｌｅｎｃｅｃｏｍｐｏｕｎｄｓｐｏｓｓｅｓｓｃｅｒｔａｉｎａｄｖａｎｔａｇｅｏｎｃｏｍｐｏｕｎｄｓｙｎ ｔｈｅｓｉｓ,ｍｏｌｅｃｕｌｅｓｔｒｕｃｔｕｒｅａｎｄｐｈｙｓｉｃａｌａ…     

Synthesis and Crystal Structure of 5-Methoxy- butyrolacto[3,4-b]-1-N-cyclohexylaziridine

1 INTRODUCTION The study of aziridine derivatives has been an ac-tive area in organic chemistry due to their interestingreactive properties and special structures[1～3]. Aziri-dine compounds contain unique nitrogen skeleton ofthree-membered heterocycle, which is widely presentin many natural products. They have been used toobtain a variety of biologically important moleculessuch as amino acids, amino alcohols, alkaloids, andβ-lactam antibiotics[2～4]. Although the synthetic routesto azir…     

Structure of Ethanol Coordinated 1,8,15,22-Tetra-（2′,2′,4′-trimethyl-3′-pentoxy）phthalocyaninatocobalt

Crystal structure of ethanol coordinated 1,8,15,22-tetra(2′,2′,4′-trimethyl-3-pentoxy) phthalocyaninatocobalt (C64H80N8O4Co·2C2H5OH, Mr = 1176.43) was determined by X-ray diffrac- tion methods. The crystal is of monoclinic, space group P21/c with a = 16.4294(4), b = 8.0560(2), c = 24.3654(7)(A。), β = 98.3680(8)°, Z = 2, V = 3190.6(1) (A。)3, Dc = 1.225 g/cm3, F(000) = 1262, μ(MoKα) = 0.326 mm-1, the final R = 0.0865 and wR = 0.2737 for 4787 observed reflections with I ≥ 2σ(I). The bulky branched alkyloxy substituents lead to a one structural isomer and space the phthalocyanine molecules where two ethanol molecules coordinate to the cobalt atom from two sides of each molecule.     

Synthesis and Structural Characterization of a New Cadmium(Ⅱ) Complex with a Double Betaine

A new flexible double betaine L (L =1,4-bis(pyridinio-4-carboxylato-N-methyl)and its crystal structure was determined by single-crystal X-ray diffraction analysis.Crystallo13.7854(3), b = 14.2820(3), c = 14.9188(4)(。A), β = 116.418(1)°, V = 2630.5(1)(。A)3, Z = 4, Dc = 1.704g/cm3, μ(MoKα) = 0.911 mm-1, F(000) = 1368, the final R = 0.0315 and wR = 0.0768 for 3637observed reflections with I ＞ 2σ(I).In complex 1, L acts as a monodentate ligand to link a Cd(Ⅱ) ion in a novel coordination mode of double betaines.The mononuclear [Cd(H2O)4L(NO3)] units are connected through intermolecular hydrogen bonds and π-π stacking reactions to generate a 3D network.     

Synthesis and Crystal Structure of 4-Phenyl-5-(1′- t-butyl-5′-methyl-4′-pyrazolyl)-1,2,4-triazol-3-thione

The crystal structure of 4-phenyl-5-(1′-t-butyl-5′-methyl-4′-pyrazolyl)-1,2,4-triazol- 3-thione 5 (C16H19N5S, Mr = 313.42) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 6.680(2), b = 27.44(1), c = 9.388(4)(A。), β = 106.738(6)°, V = 1648(1)(A。)3, Z = 4, Dc = 1.263 g/cm3, μ= 0.200 mm-1, F(000) = 664, R = 0.0608 and wR = 0.1176. The results confirmed that 5 can be assigned to the thione tautomeric form.     

Synthesis and Crystal Structure of[Ni(C5H2N2O4)(2, 2'-bipy)(H2O)2]·2H2O

The crystal structure of [Ni(C5H2N2O4)(2, 2?-bipy)(H2O)2]·2H2O 1 has been determined by X-ray diffraction. Crystal data: triclinic system, space group P ī with a = 7.9424(3), b = 9.9417(3), c = 12.1867(3) (A。）, α = 84.771(1), β = 77.375(2), γ = 68.993(2)°, C15H18N4O8Ni, Mr = 440.7, V = 876.16(5) (A。）3, Z = 2, Dc = 1.672 g/cm3, F(000) = 456, ((MoK() = 1.162 mm-1, the final R = 0.0464 and wR = 0.1055 for 3026 observed reflections with I > 2((I). In the title compound, the nickel ion is coordinated by a nitrogen atom and an oxygen atom from the orotate ligand, two nitrogen atoms from 2, 2'-bipy and two oxygen atoms from the coordinated water molecules in a distorted octahedral geometry. The presence of intermolecular hydrogen bonding and (-( stacking interaction of aromatic rings from 2, 2'-bipy results in a 3D structure.     

Synthesis and Crystal Structure of 2-Benzylamino-6-methyl-3-cyano-8- phenyl-5H-bispyrazolo[3,4-d,3'''',2''''-b]pyrimidine

1 INTRODUCTION The pyrazolopyrimidines have attracted conside- rable attention due to their versatile physiological activities, and a number of them exhibit excellent fungicidal[1], antiphlogistic[2～4] and antiumor[5] acti- vities. However, our interest in pyrazolo- pyrimidine stems is their applications as bactericide[6]. Herein we report the synthesis and structure of a tricyclic ring system bispyrazolo[3,4-d, 3?,2?-b]pyrimidine 1. 2 EXPERIMENTAL The 1H NMR spectra (CDCl3) were …     

Crystal Structure of Hydrochlorate of 1,1''''-Bis[(4-pyridylamino)carbonyl]ferrocene

1 INTRODUCTION Recently, there is great current interest in the possibility of using organometallic complexes as ligands to construct mixed-metal suprastructures[1], and ferrocenyl compounds containing mono-or poly- pyridyl fragments have also attracted much attention due to their strong coordinate abilities. For example, Grepioni and coworkers have described the design, synthesis and structure characterizations of several complexes [Fe(η5-C5H4-1-C5H4N)2](AgI)22 /(CuII)24 / (ZnII)24…     

Synthesis and Characterization of {2-Formyl-6-[1-(2,4,6-trimethylphenyl)]-4- chlorophenoxy}_2Ni and Its Ethylene Oligomerization

1 INTRODUCTION Late-transition metal complexes as catalysts for ethylene oligomerization and polymerization have become an intense research subject[1]. Nickel com- plexes are in hot point due to the significant achieve- ments of academic research[2, 3] and industrial appli- cations[4, 5]. The nickel complexes with bidentate [P,O] ligands were industrialized as the SHOP pro- cess for α-olefins[4]. It is supposed that late transition metal complexes have a strong propensity of under- goi…     

Synthesis and Crystal Structure of Potassium triaqua（ethyleneamin—N,N,N‘,N’—tetraacetate）gadolinium（Ⅲ）pentahydrate

1 INTRODUCTION The chemistry of lanthanide (Ⅲ) complexes has a considerable history. The stereochemistry of the lanthanide (Ⅲ) complexes with ethyleneamine- N, N, N, N-tetraacetate (Edta) has been investigated[1~10]. Up to now, many Ln-Edta complexes with the chemical formulae of M[Ln(Edta)(H2O)m]nH2O (M = Na+, K+, Cs+, NH4+, Guanium; m = 2, 3; n = 0, 1, 3, 5) have been reported and suggested that the coordination modes and crystal systems for the Ln-Edta complexes depend on …     

Synthesis and Crystal Structure of Pd（ptac—C,N）（acac—O,O）

1INTRODUCTIONTherehasbeenconsiderableattentionfocusedonthestudyofpalladiumcomplexinorganicsynthesis,catalyticprocesses,chemicalreactivity,spectroscopyandstructuralanalysisandfunctionalmaterials[1].Manypalladacycleshavebeenappliedinthepreparationofliquid-crystallinecomplexes[2],andsomeofthemshowantitumoractivity.Theincreasingimportanceofsuchcyclo-organometalliccomplexleadsustoinvestigatethecyclicPdcomplexeswithenhancedchemicalandthermalstability,fromwhichdetailedspectroscopicandstructuralc…     

Syntheses and Structural Characterizations of [Co~Ⅲ(TPA)(N_3)_2]·(ClO_4) and [Cu~Ⅱ(TPA)(N_3)]·(ClO_4) (TPA=Tris(2-pyridylmethyl)amine)

1 INTRODUCTION As a versatile ligand, N3- has been attracted great interest for several decades. In addition to mono- dentate coordination through a single N-donor, the azide group is not only an efficient antiferromag- netic coupler in the 1,3-fashion…     

Synthesis and Crystal Structure of [SmN（CH2COO）3（H2O）2].H2O

1　ＩＮＴＲＯＤＵＣＴＩＯＮＲａｒｅＥａｒｔｈ (ＲＥ)ｅｌｅｍｅｎｔｓａｒｅａｐｐｌｉｅｄｉｎａｇｒｉｃｕｌｔｕｒｅａｎｄｍｅｄｉｃｉｎｅ .Ｔｈｅｒｆｏｒｅ,ｂｅｔｔｅｒｕｎｄｅｒｓｔａｎｄｉｎｇｏｆｔｈｅｂｏｎｄｉｎｇｏｆＲＥｉｏｎｓｉｎｔｈｅｃｏｍｐｌｅｘｅｓｗｉｔｈａｍｉｎｏａｃｉｄｓｉｓｎｅｃｅｓｓａｒｙ .ＴｈｅｃｒｙｓｔａｌｓｔｒｕｃｔｕｒｅｏｆＲＥｃｏｍｐｌｅｘｅｓｗｉｔｈｔｈｅｓｉｍｐｌｅｓｔａｍｉｎｏａｃｉｄｇｌｙｃｉｎｅｗｅｒｅｓｔｕｄｉｅｄｂｅｆｏｒｅ[1- 4].Ｔｏｒｅｓｅａｒｃｈ…     

Synthesis and Crystal Structure of a New Chain Coordination Polymer [Cu（inio）2（H2O）]∞ （Inio = Isonicotinic Acid N-Oxide）

1 INTRODUCTION With deep studies on the complex biology system and syntheses of new functional complexes, people have paid more and more attention to the polynuclear complexes. In the construction of one to three dimensional frameworks, multi-dentate ligands are usually used to bridge the metal centers to form polymeric structures[1, 2]. The isonicotinic acid N-oxide can function as a good mono-dentate ligand[3～8] through one oxygen atom from the group of -NO or carboxyl, and the dep…     

Synthesis, Crystal Structure and Optical Properties of a New Nd(Ⅲ) Nitronyl Nitroxide Complex [Nd(NIT2Py)2(NO3)3]

A new Nd(Ⅲ) nitronyl nitroxide complex [Nd(NIT2Py)2(NO3)3] (NIT2Py = 2-(2'-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been synthesized and structurally characterized by X-ray diffraction.It crystallizes in monoclinic, space group P21/n with a = 12.396(4), b =11.134(4), c = 23.360(7)(。A), β = 98.178(6)°, V= 3191.2(18)(。A)3, C24H32NgNdO13, Mr = 798.83, Dc =1.663 g/cm3, μ(MoKα) = 1.704 mm-1, F(000) = 1612, Z = 4, the final R = 0.0425 and wR = 0.0957for 6532 independentreflections with Rint = 0.0642 and 4552 observed reflections (I ＞ 2σ(I)).The complex exists as discrete mononuclear molecules and the neodymium(Ⅲ) ion is ten-coordinated with three bidentate nitrate anions and two radical ligands (NIT2Py) via bidentate chelating mode.The optical properties of the complex are discussed.     

Synthesis and Structure of Barium Complex Containing 2,2,6,6-Tetramethyl-3,5-heptanedionate and 1,10-Phenanthroline Ligands

1　ＩＮＴＲＯＤＵＣＴＩＯＮＭｅｔａｌ ｏｒｇａｎｉｃｃｈｅｍｉｃａｌｄｅｐｏｓｉｔｉｏｎ(ＭＯＣＶＤ)ｉｓａｎａｐｐｅａｌｉｎｇｔｅｃｈｎｉｑｕｅｆｏｒｅｌｅｃ ｔｒｏｎｉｃａｐｐｌｉｃａｔｉｏｎｓ.ＡｓｏｎｅｏｆｔｈｅＭＯＣＶＤｓｏｕｒｃｅｍａｔｅｒｉａｌｓｆｏｒＹＢＣＯｓｕｐｅｒｃｏｎｄｕｃｔｏｒｆｉｌｍｓ,ｂｉｓ( 2 ,2 ,6,6 ｔｅｔｒａｍｅｔｈｙｌ 3,5 ｈｅｐｔａｎｅｄｉｏｎａｔｅ)ｂａｒｉｕｍｈａｓｂｅｅｎｅｘｔｅｎｓｉｖｅｌｙｕｓｅｄｉｎｔｈｅｐａｓｔ[1～ 3].Ｔｈｅｌａｒｇｅｓｉｚｅｏｆｔｈｅ…     

Synthesis and Structure Characterization of Aqua-（μ2-carbonato-O,O′）-（2,2′-bipyridyl）-copper（Ⅱ） Dihydrate

Under hydrothermal conditions the reaction of cis-aconitic acid with Cu2(OH)2CO3 and bipy (bipy = 2,2'-bipy) in H2O/DMF (3:2) afforded a neutral mononuclear compound [Cu- (bipy)((2-CO3)(H2O)](2H2O, which has been structurally characterized by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic, space group Pī with a = 8.3950(5), b = 8.7974(5), c = 9.4496(3)（A。）, α = 98.270(3), β = 93.014(3), γ = 100.068(3)°, V = 677.83(6) （A。）3, Dc = 1.635 g/cm3, Z = 2, C11H14CuN2O6, Mr = 333.78, μ = 1.637 mm－1, λ(MoKα) = 0.71073 （A。）, F(000) = 342, the final R = 0.0616 and wR = 0.1273 for 1621 observed reflections with I > 2σ(I). The structure of the complex contains a distorted square pyramidal core with a bipy, a carbonate anion and a water molecule coordinating to a CuⅡ atom. The dihedral angle between the two planes composed of N(1)N(2)Cu(1) and O(1)O(3)Cu(1) is 21.73(8)°. The intermolecular hydrogen bonds (O…O) are observed in the crystal structure.     

Synthesis and Crystal Structure of Potassium Triethylenetetraaminehexaacetatodi [Oxo-vanadium(Ⅳ)] Hexahydrate, K_2[V_2O_2(ttha)]·6(H_2O)

1 INTRODUCTION Interest in vanadium in the physiology and biochemistry has promoted enormously in recent years. Vanadium is known to exist in alternative nitrogenase metalloenzyme systems fixing nitrogen. It is also found to participate in biological processes exhibiting mitogenic behavior and enzyme inhi- bition[1]. Up to date, several crystal structures have been reported about vanadium with carboxylic or polycarboxylic acid[2, 3]. However, very few struc- tures of vanadium complexes …     

Hydrocarbon-Soluble Mercuracarborands: Syntheses, Halide Complexes, and Supramolecular Chemistry

The syntheses of macrocyclic species composed of carborane derivatives joined via their carbon vertices by electrophilic mercury atoms are described. The reaction of closo-1,2-Li(2)[C(2)B(10)H(10)(-)(x)()R(x)()] with HgI(2) gives Li(2)[(1,2-C(2)B(10)H(10)(-)(x)()R(x)()Hg)(4)I(2)] [R = Et, x = 2 (5.I(2)Li(2)); R = Me, x = 2 (6.I(2)Li(2)); R = Me, x = 4 (7.I(2)Li(2))]. 6.I(2)(K.[18]dibenzocrown-6)(2) crystallizes in the monoclinic space group C2/m [a = 28.99(2) ?, b = 18.19(1) ?, c = 13.61(1) ?, beta = 113.74(2) degrees, V = 6568 ?(3), Z = 4, R = 0.060, R(w) = 0.070]; 7.I(2)(NBu(4))(2) crystallizes in the monoclinic space group P2(1)/c [a = 12.77(1) ?, b = 21.12(2) ?, c = 20.96(2) ?, beta = 97.87(2) degrees, V = 5600 ?(3), Z = 2, R = 0.072, R(w) = 0.082]. The precursor to 7, closo-8,9,10,12-Me(4)-1,2-C(2)B(10)H(8) (4), is made in a single step by reaction of closo-1,2-C(2)B(10)H(12) with MeI in trifluoromethanesulfonic acid. The free hosts 5, 6, and 7 are obtained by reaction of the iodide complexes with stoichiometric quantities of AgOAc. A (199)Hg NMR study indicates that sequential removal of iodide from 5.I(2)Li(2) and 6.I(2)Li(2) with aliquots of AgOAc solution leads to formation of two intermediate host-guest complexes in solution, presumed to be 5(6)ILi and 5(2)(6)(2).ILi. Crystals grown from a solution of 6.I(2)Li(2) to which 1 equiv of AgOAc solution had been added proved to be an unusual stack structure with the formula 6(3).I(4)Li(4) [tetragonal, I4/m, a = 21.589(2) ?, c = 21.666(2) ?, V = 10098 ?(3), Z = 2, R = 0.058, R(w) = 0.084]. Addition of 2 equiv of NBu(4)Br ion to 5 or 6 gives 5.Br(2)(NBu(4))(2) and 6.Br(2)(NBu(4))(2), respectively, while addition of 1 equiv of KBr to 6 forms 6.BrK. 5.Br(2)(NBu(4))(2) crystallizes in the triclinic space group P&onemacr;, [a = 10.433(1) ?, b = 13.013(1) ?, c = 15.867(2) ?, alpha = 91.638(2) degrees, beta = 97.186(3) degrees, gamma = 114.202(2) degrees, V = 1492 ?(3), Z = 1, R = 0.078, R(w) = 0.104]. The hosts 5 and 6 form 1:1 supramolecular adducts with the polyhedral anions B(10)I(10)(2)(-) and B(12)I(12)(2)(-) in solution.