Interlayer-type Crystal Structure of N-（1-Adamantyl） urea

1 INTRODUCTION In the context of supramolecular chemistry, mo- lecules are joined together by intermolecular interac- tions to form a supramolecule whose physical pro- perties largely depend on the orientation and packing of molecules in the crystal structures[1]. The adaman- tane is a kind of cage alkane with high symmetry and stable framework. Its derivatives are extensively applied in the fields of medicine, macromolecular materials, aviation and so on due to the unique structures and …     

Synthesis and Crystal Structure of Dibromo [1,1′- bis(diphenylphosphino)ferrocene]cadmium(II)

1 INTRODUCTION The transition metal complexes containing ferrocene ligand arouse the interest of chemists because of their novel structures and special properties[1]. The ferrocene derivatives have been used in electrochemistry, in nonlinear optics, and as molecular ferromagnets. Some complexes of 1,1′-bis(diphenylphosphino)ferrocene (dppf) have been synthesized, and many of their crystal structures have been reported by far[2~5]. Here we report the synthesis and crystal structure of a …     

Synthesis, Crystal Structure and Magnetic Properties of a New 3D Cobalt Vanadate

A new cobalt vanadate compound 1 [Co^Ⅱ(H2O)2V2^VO6] has been hydrothermally synthesized and characterized by the elemental analyses and the single crystal X-ray diffraction analysis. Compound 1 crystallizes in the orthorhombic system, space group Pinna, with a=0.55646, b=1.06900, c=1.18452 nm, and Z=4. The magnetic susceptibility of the cobalt vanadate has been measured and indicates possible antiferromagnetic coupling between adjacent cobalt (Ⅱ) (0.5432—0.5697 nm) through bond or space.     

The Crystal Structure of Isosteviol

The title compound was prepared and its crystal structure was determined using X-ray crystallographic method. The crystal is orthorhombic, space group is P212121 with a= 1. 1114(2) nm, b=1.7677(3) nm, c=1.8312(3) nm; Z=8. The geometric structure and conformation of the title compound obtained by MMX molecular mechanics calculation are in agreement with those obtained from X-ray determination.     

Synthesis and Crystal Structure of O-Ethyl-N-（2,3,4-tri-O-acetyl-β-D-xylopyranosyl）-thiocarbamate

The crystal and molecular structures of O-ethyl-N-(2,3,4-tri-O-acetyl-p-D-xylopyranosyl)-thiocarbamate were determined by X-ray crystallography. It crystallizes in the orthorhombic system with space group P2(1)2(1)2(1), lattice parameters a=0.90636(18) nm, b=0.94716(19) nm, c=2.1855(4) nm, V=1. 8762 (7) nm3, and Z=4. All the substituents are in equatorial positions. There are four intramolecular interactions, each forming a five-membered ring. The molecules are linked by interactions to form three-dimensional framework. Atoms O6 and O8 show positional disorder.     

Preparation and Structure of A Novel Ethanolamine-occluding Aluminoarsenate

An aluminoarsenate, Al2As2O3.EAN, denoted as AlAsO4-1 was synthesized from EAN(EAN= ethanolamine), pyroarsenic acid and aluminium-iso-propylate systems. The crystal structure of AlAsO4-1 was determined by single crystal X-ray diffraction method. The compound crystallizes in orthorhombic space group Pcab with the unit cell constants:0 = 8.781(3), 6=10.261(3), c=20. 433(11) A .V = 1840.9 A3, 2=8. The final R and Rw factors are 0. 0401 and 0. 0344, respectively. The framework of AlAsO4-1 contains two types of Al atoms. It is interesting that in the asymmetric unit one of two Al atoms is strictly 4-coordinated and the other is 6-coordinated. The three-dimensional framework is built of two-dimensional nets which consist of 4-membered rings and 8-membered rings. The biggest open channel in the framework runs along [100], in which EAN template is located. Arsenic atoms can function as a component element for construction of three-dimensional net with topological novelty.     

Investigation on photochromism of 1,2-bis(1,4-dimethyl-2-phenyl)perfluorocyclopentene

The photochromic diarylethene, 1,2-bis(1,4-dimethyl-2-phenyl)perfluorocyclopentene has been synthesized and its single crystal can be obtained in hexane at -4℃. The structure of diphenylperluorocyclopentene bearing C2/c space group and monoclinic crystal system is very different from that of dithienylperfluorocyclopentene derivatives bearing Pī space group and triclinic crystal system by X-ray crystallographic analysis. The compound undergoes the phototchromic reaction in solution but no optical activity in single crystal. In addition, its optimum conformation in solvent is also discussed.     

Synthesis and Crystal Structure of Binuclear Copper （Ⅱ） Complex Containing （Dimethylaminomethyl）ferrocene

1 INTRODUCTION Transition metal complexes with ferrocene are of considerable interest in the past fifty years because of their novel structures and special properties[1, 2]. The chemistry of ferrocene and its derivatives has become richer and richer in the last decade. Many complexes containing ferrocenyl have been synthesized and characterized[3～5]. Recently we have reported the synthesis and crystal structure of dibromo[1,1?bis(diphenylphosphino)- ferrocene]cadmium (Ⅱ)[6]. Herein we…     

Highly stable Eu-coordination polymer exhibiting the highest quantum yield

Lanthanide luminescent materials with high quantum yield and thermal stability are of key importance for their practical application. Here we report crystal structures and luminescent properties of [Eu(pfbz)₂(phen)Cl](1) and [Tb(pfbz)2(phen)Cl](2)(pfbz = Pentafluorobenzoate). Single-crystal analysis reveals that both 1 and 2 crystallize in a polar space group of Cmc21.Investigation on their luminescent properties indicates that the solid-state quantum yields of 1 and 2 are 97.7% and 9...     

Preparation and Crystal Structure of Sodium Hydrogen Epoxysuccinate

1 INTRODUCTION In recent years, sodium hydrogen epoxysuccinatehas gained special attention as a raw material of po-lyepoxysuccinic acid (PESA)[1～3]. We have synthes-ized sodium hydrogen epoxysuccinate by the reac-tion of H2O2 and maleic anhydride in water ca-talyzed by tungstate and obtained its single crystal[1].Its structure was determined by X-ray Nonius CAD4diffractometer. Up to now some crystal structures oforganic carboxyl sodium have been determined[4～6].In this paper we …     

Stereoselective Synthesis of Sulfonyl-substituted trans-2,3-Dihydrofuran Derivatives via Reaction of Arsonium Ylides with α,β-Unsaturated Ketones

Trans-2,3-dihydrofuran derivatives 3 or 4 substituted with a sulfonyl group were prepared with high chemoselectivity and good yields by [1＋4]-addition reaction of α,β-unsaturated ketones 1 with arsonium bromide 2 in CH2Cl2 in the presence of potassium carbonate at room temperature.The structures of the products were characterized by IR,MS,^1H NMR,elemental analysis and single crystal X-ray diffraction analysis.A mechanism for the formation of products was also proposed.     

Crystallization and Preliminary Crystallographic Analysis of β- Trichosanthin, an Isoform of Trichosanthin from the Root Tuber of Trichosanthe kirilowii

β-Trichosanthin,a type 1 ribosome-inactivating protein (RIP) isolated from the root tuber of Trichosanthe kirilowii Maxim,is an isoform of trichosanthin. Here we report its crystal-lization in two crystal forms using the hanging-drop vapor-diffusion method. The form A and form B crystals belong to the orthorhombic space group P212121 and monoclinic space group P21,respectively. X-ray data have been collected to 1.6 and 1.2 resolution for form A and form B crystals,respectively,using a synchrotron source.     

Synthesis and Crystal Structure of [Ni(II)(L)(py)_3]·(py)

1 INTRODUCTION Schiff bases and their metal complexes are useful reagents in organic synthesis[1], and they have exhi- bited some biological activities as anticancer and antitumor drugs[2]. The crystal structures and physi- cal and chemical properties of many Schiff bases and their transition metals complexes have been re- ported[3~5]. Further interest in the coordination che- mistry of nickel(II) arises from the role of these complexes in several catalytic reactions, such as electrocat…     

Synthesis and Structure Study of Molybdenum Complex Mo[o-NHCOCH_3-m-NO_2C_6H_3COOH]_2_O2Cl_2·PhCl

The crystal and molecular structures of molybdenum complex, Mo [ o- NHCOCH3- m-NO2C6H3COOH]2O2Cl2.PhCl are reported. The crystal belongs to space group Cc of monoclinic system with unit cell parameters:α= 11. 214 (3) A .b= 19. 544 (4 ) A . c = 14. 091 (6) A .β=94.06(3)°,V'=3080.3 A3 and Z=4. The structure was refined to R=0. 061.The coordination number for the Mo atom Is six. The coordination polyhedron formed by four O atoms and two Cl atoms around the Mo atom is a distorted octahedron. Four O atoms and one Mo atom construct a plane. Two benzyl planes in coordinate groups and the benzyl plane of solvent are almost parallel. The quantum-chemical calculations were carried out. There are hydrogen bonds in the Complex. The EHMO calculations and the existence of hydrogen bonds prove that the O atoms are stronger coordinated atoms in the carbonyls than in the carboxyls.     

Conformation of α,α,α′-Trisubstituted Cyclododecanone

Ten α,α,α′-trisubstituted cyclododecanones were synthesized and characterized by elemental analyses, infrared, 1^H NMR and 13^C NMR spectra, and X-ray diffraction. NMR data could not give conformational information clearly, but some of their ring skeleton conformations of cyclododecanone moiety were showed to remain the unchanged [3333]-2-one conformation with little distortion, while the others were changed to the [3324]-2-one conformation in their crystal structures. These are consistent with the results of molecular mechanics calculation with Sybyl 6.9 software and Tripos force field, and semi-empirical quantum calculation with AM 1 method in Gaussian 98 software. Two geminal substituting groups are located at α-corner carbon atom, and the third group is at α-side-exo carbon atom in both conformations. Both [3333]-2-one and [3324]-2-one conformations are present in a dynamic equilibrium in the solution, but only one preferred conformation exists in the crystal solid.     

Synthesis and Crystal Structure of a 3-D Hydrogen-bonded Supramolecular Decavanadate Compound [Habo]_6[V_(10)O_(28)]·2C_3H_7OH·2H_2O

1 INTRODUCTION The chemistry of polyoxometalates has been at- tracting much attention due to the richness in their structures, electron and proton storage abilities, ther- mal stability and applications in catalysis, medicine and surface sciences[1～3]. In recent years, the mixed- valence as well as full oxidized vanadium polyoxo- anions have been crystallized with a variety of orga- nic molecules as counteranions[4～8]. However, the guiding principles of the crystal structures of poly- o…     

Characterization and Crystal Structure of a New Holmium(III) Complex with the Macrocyclic Ligand Derived from 2,6-Diformyl-4-methylphenol and Diethylenetriamine

The title compound (13,27-dimethyl-3,6,9,17,20,23-hexaazatricyclo-[23.3.1.111,15]- triaconta-1(29),2,9,11,13,15(30),16,23,25,27-decaene-29,30-diol-N3,N6,N9,O29,O30)-bis(nitrato-O,O′)- holmium(III) nitrate hydrate has been prepared and characterized by elemental analysis, infrared spectra, and electrospray mass spectra. Its crystal and molecular structures were determined by X-ray diffraction methods. The crystal crystallizes in the monoclinic system, space group C2/c with a = 23.737(12), b = 14.237(7), c = 19.801(10) , β = 91.36(1)o, Mr = 831.57, V = 6690(6) 3, Z = 8, Dc = 1.651 g/cm3, F(000) = 3344, R = 0.0482 and wR = 0.0923. The holmium ion is located in one of the compartments of the macrocyclic ligand and presents a distorted tricapped trigonal prismatic coordination geometry. The macrocycle is coordinated with two oxygen and three nitrogen atoms. Two nitrates are chelated in the opposite positions of the macrocycle, and the third one is ionic.     

Characterization and Crystal Structure of a New Holmium（Ⅲ） Complex with the Macrocyclic Ligand Derived from 2,6-Diformyl-4-methylphenol and Diethylenetriamine

The title compound （13,27-dimethyl-3,6,9,17,20,23-hexaazatricyclo-[23.3.1.1^11.15]- triaconta-l（29）,2,9,11,13,15（30）,16,23,25,27-decaene-29,30-diol-N^3,N^6,N^9,O^29,O^30）-bis（nitrato-O,O＇）- holmium（m） nitrate hydrate has been prepared and characterized by elemental analysis, infrared spectra, and electrospray mass spectra. Its crystal and molecular structures were determined by X-ray diffraction methods. The crystal crystallizes in the monoclinic system, space group C2/c with a = 23.737（12）, b = 14.237（7）, c = 19.801（10） A, β = 91.36（1）^o, Mr = 831.57, V = 6690（6） A^3, Z = 8, Dc = 1.651 g/cm^3, F（000） = 3344, R = 0.0482 and wR = 0.0923. The holmium ion is located in one of the compartments of the macrocyclic ligand and presents a distorted tricapped trigonal prismatic coordination geometry. The macrocycle is coordinated with two oxygen and three nitrogen atoms. Two nitrates are chelated in the opposite positions of the macrocycle, and the third one is ionic.     

Syntheses and Crystal Structures of Lanthanide Complexes of New 15-Membered Macrocyclic Ligands with Three Pendant Acetato Groups

Two new 15-memhored fimctionalized macrocycles, dioxo-polyazacydoalkanes with three pendant acetato groups, have been synthesized by the condensation reaction of DTPA dianhy-dride (DTPA = diethylenetrlamlnepentaacetic acid ) with 1,2-di-amlnopropane, ( 15-DTPA-1, 2-pn), or 1, 2-diaminocydohex-ane, (15-DTPA-1,2-cy). Their lanthanide complexes [ Ln ( 15-DTPA-1,2-pn)(H2O)]2[Ln= Eu (1), Gd (2)] and [Ln(15-DTPA-1,2-cy)(H2O)]2[Ln= Eu (3), Gd (4)] were also pre-pared. Single crystal X-ray diffraction analyses of complexes 2 and 4 show that they have dimeric structures in solid state;each metal ion is nine-coordinated in a distorted tricapped-trig-onal prism. In complex 4, the coexistence of two diastereoiso-meric molecules in the crystal lattice was observed.     

X-ray Structure of Bis（salicylidene）-p-diaminobenzene

IntroductionThe interactions between molecules involvingaromatic ring systems are of interest because oftheir effects on the structures and aggregation ofimportant biomolecules,on template efficiency in avariety of organic reactions,and on the solid statestructures of a variety oforganic molecules[1] .Con-sistent are the analysis results of more than 2 0 0phenylalanine- phenylalanine interactions in thecrystal structures of various proteins,which leadsto the following conclusions.( 1 ) Direct …