Synthesis and Crystal Structure of Tri—（2—mercaptopyridine N—oxide）bis（dimethyl sulfoxide） Dysprosium（Ⅲ）

A range of rare earth metal complexes of 2-mercaptopyridine N-oxide (Hmpo) have been synthesized, and studied by elemental analysis and IR spectroscopic technique. Crystal structure of Dy(mpo)3(DMSO)2 (DMSO = dimethyl sulfoxide) has been determined. The complex crystallizes in the triclinic system, space group Pī with lattice parameters: a = 9.602(3), b = 9.803(3), c = 15.498(5)A, α= 89.51(1), β= 85.73(1), γ= 62.99(1)°, Dc = 1.787 g/cm3, C19H24N3O5S5Dy, Mr = 697.21, Z = 2, F(000) = 690, μ = 3.321mm-1, the final R = 0.0237 and wR = 0.0587 for 4116 reflections with I>σ2(I). The coordination number of dysprosium Ⅲ is eight, and its coordination geometry is a somewhat distorted square antiprism with O(3), O(4), O(5), S(3) and O(1), O(2), S(1), S(2) at the tetragonal bases (dihedral angle between their mean planes is 2.9(1)0). Around the Dy atom, three five-membered ring planes (Dy, O, N, C, S) make the dihedral angles of 74.42, 11.31 and 83.72, respectively.     

3-甲基-5-氰基-6-氨基-1-苯基-4-(3,4-二甲氧基苯基)-1,4-二氢吡喃[2,3-c]吡唑的合成和晶体结构

标题化合物C22H20N4O3 3是由2-氰基-3-(3,4-二甲氧基苯基)丙烯腈1和3-甲基-1-苯基-2-吡唑-5-酮2在KF-Al2O3催化下在N,N-二甲基甲酰胺(DMF)溶剂中反应而得。结构通过单晶X-射线衍射分析确定,其晶体属于三斜晶系,空间群Pī,a = 9.450(3),b = 10.876(2), c = 11.435(2) ,a = 115.51(1), b = 102.82(1),g = 98.47(2), Mr = 388.42, V = 994.1(3) 3,Dc = 1.298 g/cm3, Z = 2, m (MoKa) = 0.089 mm-1, F(000) = 408。晶体结构用直接法解出,使用全矩阵最小二乘法对原子参数进行修正,最后的偏离因子R = 0.0420,wR = 0.1070。单晶X-射线衍射分析表明平面Ⅰ与平面Ⅱ、平面Ⅲ、平面Ⅳ的夹角分别为102.31、29.24和1.43。平面Ⅱ与平面Ⅲ和平面Ⅳ的夹角分别为73.50和100.91,平面Ⅲ和平面Ⅳ的夹角为27.81, 另外晶体中还存在分子间氢键。     

Synthesis and Structure of 6-(4- Fluorobenzylamino)-3-methylthio-1,5- diphenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one

1 INTRODUCTION It was reported that the pyrazolopyrimidinone derivatives play a very important role in the bio- chemistry of living cell. Many potential drugs[1～3] and agrochemicals[4, 5] have been modeled on the compound, and the study on derivatives …     

Synthesis and Structural Characterization of a Novel 2D Supramolecular Complex {[Dy_2Zn(dinic)_4(H_2O)_8]·H_2O}n (H_2dinic = 2,5-Pyridinedicaboxylic Acid)

1INTRODUCTION Studies on the syntheses,structures,and proper-ties of lanthanide-transition metal complexes are currently of great interest not only due to their beha-viors as good models to investigate the nature of magnetic exchange interactions between3d and4f metal ions in magnetic materials but also to the fascinating coordination properties of Ln(III)[1～6].Although some infinite lanthanide(III)-transition metal compounds have been obtained by the con-ventional self-assembly reacti…     

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.     

CRYSTAL STRUCTURE OF THE METHYL 4—（N—（1—OXYPROPYL）—N—PHENYLAMINO]—1—[2—（2—THIENYL）ETHYL]—4—PIPERIDINECARBOXYLATE（R31826）HYDROCHLORIDE

<正> C22H28N2O3S.HCl, Mr = 436.9, triclinic,P1;a=8.557(3),b= 10.299(2),c= 13.894(2)A;α= 99.25(1),β=86.64(2),γ= 107.68(2)°;V= 1151.2(3)A3,Z= 2, DC = 1.27g/cm3,R=0.064. The torsion angle C(14)-C(1)-N(2)-0(19) in the title compound is 137.5 being much larger than that (106°) in R30730. The dihedral angle between mean planes of the thiophene ring and piperidine ring is about 83 .     

Synthesis and Crystal Structure of 1-（Trifluoromethyl）-1-（propioloyl）-（E）-3-oxo-（2-thienyl）-（2-naphthylamine）

1INTRODUCTIONTheSchiffbasesderivedfromb-diketonesandaliphaticamineshavebeenshowntoexistastheketo-amines.However,ifsubstituentseitherattheketooraminogrouparearomatic,itmaybeexpectedtheenoliminewillbethefavoredtautomericform[1].Recently,someSchiffbasesderivedfromTTA(4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione)andPMBPhavebeenstudiedbyWang[2]andYu[3]etal.Inordertostudytherelationshipbetweenthestructuresandperformancesofthesecompounds,thetitlecom-poundwillbereportedherein.2EXPERIMENT…     

Synthesis and Crystal Structure of a New Mononuclear Copper（Ⅱ） Complex with 4,4′,6,6′-Tetrabromo-2,2′- [ethylenedioxybis（nitrilomethylidyne）]diphenol

A new mononuclear Cu（II） complex, [Cu（L）] （H2L = 4,4′,6,6v-tetrabromo-2,2′- [ethylenedioxybis（nitrilomethylidyne）]diphenol）, has been synthesized and structurally characterized. X-ray crystal structure of the complex reveals that the Cu（Ⅱ） ion is four-coordinated by two oxygen atoms and two nitrogen atoms from L2- unit. Crystallographic data： monoclinic, space group P21/n with a = 14.076（2）, b = 6.9801（14）, c = 19.858 （2） A, β= 107.613（2）°, C16n10Br4CuN2O4, Mr = 677.44, V = 1859.6（5） A3, Dc = 2.420 g/cm3,μ = 9.796 mm^-1, F（000） = 1284, Z = 4, the final R = 0.0516 and wR = 0.0938 for 1879 observed reflections with I 〉 2σ（/）. The dihedral angel between the two coordination planes of Cu（1）-N（2）--O（4） and Cu（1 ）-N（ 1 ）-O（3）） is 30.08（6）°.     

Synthesis and Crystal Structure of 1-(1''''- t- Butyl-5''''-methyl-4-pyrazolyl-carbonyl)- 3,5-dimethyl-1H-yl-pyrazole

1 INTRODUCTION Pyrazole and its derivatives represent one of the most active classes of compounds possessing a wide spectrum of biological activities. During the past years considerable evidence has been accumulated to demonstrate the efficacy of pyra- …     

SYNTHESIS AND CRYSTAL STRUCTURE OF DINUCLEAR IRON CARBONYL DERIVATIVE (μ-SC_6H_5) (μ-P (SC_6H_5)_2) Fe_2 (CO)_5 (P-(SC_6H_5)_3)

<正> The reaction of Fe3(CO)12 with P(SPh)3 yields the tile compound. C41H30Fe2O5P2S6, Mr = 968. 65, monoclinic, space group, P21/n, a = 14. 449(9), b = 18. 046(11), c=16.871(10)(?), β=98. 76°, V = 4348(?)3, Z = 4, Dc=1. 480g/ cm3, λ(MoKα) = 0. 71073(?) The structure was determined by direct methods and difference Fourier syntheses and refined by full-matrix least-squares procedure to R = 0.084, Rw = 0.144 for 4059 reflections. Fe(1)-Fe(2) = 2. 576(6), Fe(2)-P(2) = 2.194(9)(?). The dihedral angle between the Fe(l)SFe(2) and Fe(1)PFe(2) planes is 81. 9°. The other one (dihedral angle between SFe(1)P and SFe(2)P planes) is 75. 2°.     

Crystal Structure of N-(O-Ethylphenylthionophos-phonyl) N'-(O-p-iodinephenylphenylthionophos-phonyl)thiosemicarbazide

1mThODUCT'ONSomecomPOundsofN--thionophosphonylandN,N'--his(thionophosphonyl)thiOSemicarbazideshaveattractedmuchattentionandbeenextensivelystudiedinrecentyears"~'i.ThiskindofcomPOundsareknowntohaveobviousantibacterialandantifungalactivitiest3}.TherearetwochiralphosphoratomsinthecomPOundsofN,N'--his(thionophosphonyl)thiosemicarbazide.Inordertostudyfurthertherelationshipbetweenthestructureandbiologicalactivities,hereinwerePOrtthecrystalstructureofakindofN,N'--his(thionophosphonyl)thiose…     

Synthesis and Structural Characterization of a Salt{[Co(Phen)3][Mo2S2(μ-S)2(edt)2]}2·(DMSO)2·(Et2O)(Phen = 1,10-Phenanthroline,edt = Ethane-1,2-dithiolate)

Reaction of [Et4N]2[Mo2S2(μ-S)2(edt)2] with CoCl2(6H2O and Phen in MeCN followed by recrystallization in DMSO/Et2O gave rise to dark-red block crystals of {[Co(Phen)3]- [Mo2S2(μ-S)2(edt)2]}2·(DMSO)2·(Et2O) 1 (C88H86Co2Mo4N12O3S18). 1 crystallizes in the monoclinic system, space group P21/c with a = 24.631(4), b = 16.117(3), c = 24.791(4) (A), β = 92.835°, V = 9829.3(3) (A)3, Z = 4, Mr = 2438.57, Dc = 1.648 g/cm3, F(000) = 4928, μ = 12.61 cm-1, R = 0.0936 and wR = 0.1682 for 12998 observed reflections with I > 2.0σ(I). In the structure of 1, the Co atom of the [Co(Phen)3]2+ dication is octahedrally coordinated by three Phen ligands. The Mo atom of the [Mo2S2(μ-S)2(edt)2]2- dianion is coordinated by two μ-S, one terminal S and two S atoms from edt, forming a distorted square pyramidal geometry. The mean Co-N and Mo…Mo bond distances are 2.139 and 2.872 (A), respectively.     

Crystal and Molecular Structure ofN—（Pyridin—2—yl—carbonyl）—2—ethoxycarbonyl—benzene sulfonamide

1 INTRODUCTION The sulfonylurea herbicides have been well known for their exceptional low dosage, good crop selectivity and low mammalian toxicity. They can block the biosynthesis of branched amino acids by inhibiting ALS enzyme in plants so as to inhibit weeds. Levitt G. divided the structure of sulfonylurea into three parts: (1) aryl group, (2) bridge and (3) heterocycle[1]. Later Ort et al. modified the bridge by omitting moiety NH in the bridge, synthesized N-(substituted pyrimid…     

Synthesis and Crystal Structure of Co(DMSO)2(H2O)2(SCN)2 with One-dimensional Hydrogen-bonded Structure (DMSO = Dimethylsulfoxide)

1 INTRODUCTION The development of supramolecular complexes has recently attracted considerable attention due to the fundamental interest in self-assembly processes of transition-metal complexes, supramolecular che- mistry and crystal engineering[1]. The ultimate goal is to gain control in order to direct their function[2]. Self-assembly through coordination and nonco- valent interactions such as hydrogen bonds, aromatic π···π stacking, steric repulsion and Van der Waals forces leads …     

Synthesis and Crystal Structure of 1,2-Bis(1-phenyl-3-methylthio- 4-iminopyrazolo[3,4-d]pyrimidin-5-yl) ethane

1 INTRODUCTION As purine analogs, pyrzolo[3,4-d]pyrimidines have anti-tumor[1], antibacterial[2] and anti-leukemic activities[3,4]. Few of these, however, have been studied for pesticidal activity. It is reported that some substituted pyrzolo[3,4-d]pyrimidines have good fungicidal activity[5~7]. These prompted us to study pyrazolo[3,4-d]pyrimidines analogs further. It is shown that two possible products can be formed in the reaction of ethyl N-pyrazolylformimidate with alkylamines as sh…     

Synthesis and Crystal Structure of cis-Bis(3-hydroxy2-ethyl-4-pyranonato)dioxomolybdenum(Ⅵ)

1 INTRODUCTION 3-Hydroxy-2-methyl-4-pyranone (maltol) and 3-hydroxy-2-ethyl-4-pyranone (ethylmaltol) are nontoxic compounds that have been applied to bio- inorganic chemistry over several decades[1, 2]. Their iron(III) complexes are relevant to the control of iron levels in the human body. Such complexes have been assessed for the amelioration of anaemia[3] and their respective ligands have been tested for the removal of excess burdens of iron in diseases such as siderosis, haemochroma…     

Synthesis and Crystal structure of [（Praseodymium）2（3,5—Binitro benzoyloxy）6（Dimethyl Sulfoxide）4]Complex

1 INTRODUCTION The polynuclear lanthanide complexes are specially interested and widely applied in the researches on light, electricity and magnetism[1～4], and the studies of the synthesis of polynuclear lanthanide complexes and its applications tend to be growing rapidly nowadays. Herein a report on the synthesis process and crystal structure of the title complex is presented. The crystal structure showed it is a non-electrolyte complex with one- dimensional chain. OCCOOPrOOCPr…     

Synthesis and Crystal Structure of 2[1-（1,1-Dimethylethyl）-5-methyl-1-H-pyrazol-4-ylcarbonyl]-N-phenyldrazinecarbothioamide

1INTRODUCTIONThiosemicarbazidespossessingNC=Sgroupareanessentialstructurefeatureresponsibleforvariousbiocidalproperties[1～7].Moreover,theyaretheconvenientandkeyintermediatesforthesyn-thesisofheterocycliccompoundssuchas1,3,4-thiadiazoles,1,2,4-triazoleand…     

Synthesis and Structure of 5-Amino-6-(4-fluorophenylamino)-3-methylthio-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one

The title compound (C18H15FN6OS) has been synthesized and its crystal structure was determined by X-ray analysis. The crystal belongs to monoclinic system, space group P21/n with a = 13.983(10), b = 7.337(5), c = 16.702(12) (A), α = 90, β = 98.277(12), γ = 90°, V = 1696(2)(A)3, Z = 4, Dc= 1.498 g/cm3, Mr = 382.42,μ = 0.224 mm-1, F(000) = 792, the final R = 0.0362 and wR = 0.0878 for 2579 observed reflections with I ＞ 2σ(Ⅰ). In the title compound, the atoms of C(1),C(2), C(3), C(4), C(5), N(1), N(2), N(3), N(4), N(5), N(6), O(1) and S(1) form a fully delocalized system with the average deviation of 0.0307(A). There exists a part of electron delocalization over the planes of Ⅰ (pyrazolo[3,4-d]pyrimidin-4-one moiety), Ⅱ (phenyl moiety) and Ⅲ (p-fluorophenylamine moiety). In the molecule, intermolecular hydrogen bonds between N(6)-H(6)…O(1)and C( 15)-H( 15)…O( 1 ) are observed.     

CRYSTAL AND MOLECULAR STRUCTURE OF BENZO-15-CROWN-5 POTASSIUM TETRACHLOROAURATE K(C_(14)H_(20)O_5)_2-AuCl_4

<正> The crystal and molecular structure of the title compound K(C14 H20O5)2AuCl4 has been determined by X-ray diffraction method.The crystallographic data are as follows;Mr=914.51,triclinic,space group P1,a=10.988(2),b=13.472(4),c=13.696(2)A,α=77.72(1),β=79.02(2),γ=64.92(2)°,V=1782.6(4)A3,Z=2,Dc=1.704 g.cm-3,μ=45.858 cm-1,F(000)=454,R=0.019,Rw=0.018 for 5697 observed reflections with I≥3σ(I).X-ray structure determination shows that benzo-15-crown-5(B15C5)forms a 2:1 complex with KAu-C14 in which K+is sandwiched between two crown rings.The dihedral angle between these two ether oxygen planes is 11.9°.The anion AuCl4-has a planar square configuration which is bound with the complex cation K(B15C5)2+by electrostatic force to form an ion-pair.