Synthesis and Crystal Structure of a New Coordination Polymer from Cadmium and V-Shape Ligand Bis(imidazol-1-yl) methane

Abstract  The new coordination polymer, [Cd(BIM)₂(NO₃)₂]_n, has been prepared from the reaction of bis(imidazol-1-yl) methane (BIM) with Cd(NO₃)₂ in methanol and water. The compound were characterized by single crystal X-ray diffraction and IR spectroscopy, it crystallizes in the monoclinic space group C2/m with a = 14.400(3) ?, b = 9.3894(18) ?, c = 8.6926(17) ?, β = 123.499(2)°, V = 980.1(3) ?³, Z = 2. The Cd atoms are coordinated to four nitrogen atoms from four different BIM ligands and two nitrates to form a slightly distorted octahedral geometry. Further, the BIM ligands act as a bridged ligand to form 1D infinite cationic double chain with a 16-membered macrometallacyclic tetragonal box structure. Graphical Abstract   Synthesis and Crystal Structure of a New Coordination Polymer from Cadmium and V-Shape Ligand Bis(imidazol-1-yl) methane Chuan-Ming Jin*, Ling-Yan Wu, Zhen-Xing Zhong A new coordination polymer with 1D infinite cationic double chain with a 16-membered macrometallacyclic tetragonal box structure has been prepared from the reaction of bis(imidazol-1-yl) methane (BIM) and Cd(NO₃)₂.      

Synthesis and Structure of (Bis(1-propylbenzimidazol-2-yl)-trans-1,2-cyclohexane)copper(II) Dichloride and the Structure of a Novel, Unexpected By-Product

Abstract  

Two structures containing the novel ligand bis(1-propylbenzimidazol-2-yl)-trans-1,2-cyclohexane, L, are reported. The first structure, (bis(1-propylbenzimidazol-2-yl)-trans-1,2-cyclohexane)copper(II) dichloride, Cu(II)(L)Cl₂ 1, crystallized in the monoclinic space group P 2₁/n with a = 10.992(4) ?, b = 13.576(5) ?, c = 18.047(7) ?, β = 106.909(8) and V = 2576.7(16) ?³ and Z = 4. Complex 1 exhibits a D _2d-flattened tetrahedral Cu(II)N₂Cl₂ coordination geometry, for which the four-coordinate geometry index τ₄ of 0.59 lies almost midway between the ideal geometry values of zero (square-planar) and 1 (tetrahedral). The second and unexpected structure, (bis(1-hydro-3-propylbenzimidazol-1-ium)-trans-1,2-cyclohexane)(μ⁴-oxo-hexa-(μ²-chloro)-tetra(chloro-copper(II)) di(nitromethane) solvate, 2[H₂L]²⁺[Cu₄OCl₁₀]⁴⁻·(CH₃NO₂)₂, 2, consists of three dimensionally hydrogen bonded bis(benzimidazolium) dications and tetra-copper(II)-oxo-chloride tetra-anions, interspersed with nitromethane solvate molecules. A balanced equation for the formation of the byproduct suggests that it forms via an acid–base reaction in the presence of water in the reaction mixture. The complex crystallized in the triclinic space group P −1 with a = 13.696(3) ?, b = 13.819(3) ?, c = 16.797(4) ?, α = 89.480(4), β = 87.308(4)°, γ = 89.434(4) and V = 3175.3(12) ?³ and Z = 2. Ligand L contains two stereogenic centers, each of the same handedness, and, since the space groups determined for structures 1 and 2 are centrosymmetric, both structures are racemates.     

Condensation Reaction of 1,2,3,4-Tetrahydro-1,10-phenanthroline and Formaldehyde: Synthesis and Crystal Structures of Bis(1,2,3,4-tetrahydro-1,10-phenanthroline-6-yl)methane and Its p-Toluenesulfonate Salt

Crystallography Reports - A new heterocyclic compound, bis(1,2,3,4-tetrahydro-1,10-phenanthroline-6-yl) methane (1), was obtained by the condensation reaction of...     

Synthesis,Crystal Structure,and Characterization of 2-Phenyl-N-(pyrazin-2-yl)Acetamide

The title compound, 2-Phenyl-N-(pyrazin-2-yl)acetamide, C₁₂H₁₁N₃O, was prepared by the coupling reaction and the product was crystallized by using toluene and methanol mixture(1:1) The structure of the compound was confirmed by elemental analysis, FTIR, ¹H NMR, thermogravimetric analysis, differential thermal analysis, UV-Visible spectroscopy, and single-crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 2₁/c with the following unit-cell parameters: a = 8.1614(10), b = 14.9430(13), c = 9.3877(9) Å, β = 103.653(12)°, and Z = 4. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0465 for 1486 observed reflections. An intramolecular C&sbnd;H···O hydrogen bond generates an S(6) graph-set motif. In the crystal, molecules are linked by N&sbnd;H···O and C&sbnd;H···O hydrogen bonds, forming a two-dimensional network.     

Crystal and Molecular Structures of Tris(1-Methylimidazol-2-yl)Phosphine,Tris(4-Methylthiazol-2-yl)Phosphine and its Sulfide

Abstract  Two crystal structures of tris(azolyl)phosphines, PR₃ [R′ = 1-methylimidazol-2-yl (1) or R′′ = 4-methylthiazol-2-yl (2)], and the crystal structure of the sulfurisation product of 2, R′′₃PS (3), were determined. All compounds crystallise in polar space groups, 1 in the orthorhombic space group Pna2₁ with cell parameters a = 13.9779(15) ?, b = 9.2492(10) ? and c = 10.2439(11) ?; 2 in the trigonal space group, R3c, with a = 15.2383(10) ? and c = 10.5882(13) ? and 3 in the orthorhombic space group, Cmc2₁, with a = 13.466(3) ?, b = 9.308(2) ? and c = 12.207(3) ?. Graphical Abstract  This article presents two crystal structures of tris(azolyl)phosphines and one of a tris(thiazolyl)phosphine sulfide, a compound which show potential for wide application in coordination chemistry due to their multidentate nature.      

Synthesis, Crystal Structure and Cytotoxic Property of Bis(4-chlorobenzoato)bis[1-(2-aminoethyl)piperidine]disilver(I)

Abstract  

4-Chlorobenzoic acid reacts with silver oxide and 1-(2-aminoethyl)piperidine to give a dinuclear silver(I) complex, [Ag₂(C₇H₄ClO₂)₂(C₇H₁₆N₂)₂]. The complex was characterized by elemental analysis and X-ray diffraction. The complex crystallizes in the triclinic space group P−1 with unit cell dimensions a = 6.8550(10), b = 8.7370(10), c = 13.859(2) ?, α = 73.213(3), β = 87.945(3), γ = 77.050(3)°, V = 774.09(18) ?³, Z = 1, R ₁ = 0.0386, and wR ₂ = 0.0791. The dimeric Ag complex is located on an inversion center. The Ag atom in the complex is three-coordinated by two N atoms from two 1-(2-aminoethyl)piperidine ligands and by one O atom of a 4-chlorobenzoate ligand, forming a triangular coordination. In the crystal structure, the molecules are linked through intermolecular N–H···O hydrogen bonds, forming chains running along the a axis. The complex shows high cytotoxic property to both normal and carcinoma cells.     

Synthesis,Characterization and Crystal Structure of Bis(isothiocyanato)-bis(pyridine) Zinc(II) Crystal

Abstract  Bis(isothiocyanato)-bis(pyridine) zinc(II) crystal has been prepared at room temperature and characterized by elemental analysis, IR spectrum and X-ray single crystal determination. The complex crystallizes in monoclinic space group P2₁/m with unit cell parameters: a = 5.5786(3), b = 11.0587(5), c = 12.1616(6) ?, β = 96.776(3)°, V = 745.03(6) ?³, Z = 2, D _x  = 1.514 g cm⁻³. The X-ray structure determination has revealed that the crystal is centered-symmetrical and the crystallographic symmetry face runs the two isothiocyanate ligands and the Zn(II) cation. Index Abstract  The title compound, bis(isothiocyanato)-bis(pyridine) zinc(II), was synthesized by zinc compound, KSCN and C₅H₅N (pyridine) and its crystal structure was determined. Single crystal X-ray structure determination reveals that the crystal is centered-symmetrical, and the crystallographic symmetry face runs the two isothiocyanate ligands and the Zn(II) cation.      

Structures of Bis(1-ethylbenzimidazol-2-yl)alkyl Copper(II) Dichlorides: An Unusual Cocrystallization

Abstract  Two structures containing pseudo-tetrahedral Cu(II)N₂Cl₂ coordination complexes are reported. The first molecular structure (A) of the compound, 1,1′bis(1-ethylbenzimidazol-2-yl)propane copper(II) dichloride (triEtBBIM)Cu(II)Cl₂, 1, is reported. The complex crystallized in the triclinic space group P-1 with a = 8.616(3) ?, b = 9.302(3) ?, c = 14.314(4) ?, α = 85.613(6)°, β = 85.170(6)°, γ = 66.117(6)° and V = 1044.1(5) ?³ with Z = 2. The second structure (B) contains 1 and (3,3′bis(1-ethylbenzimidazol-2-yl)pentane) copper(II) dichloride (tetEtBBIM)Cu(II)Cl₂, 2, both of which, cocrystallize in an equal molar ratio with a nitromethane solvate molecule. The complex crystallized in the monoclinic space group P2₁/c with a = 18.876(4) ?, b = 14.975(3) ?, c = 18.344(4) ?, β = 116.75(3)°, and V = 4630.3(16) ?³ with Z = 4. The cocrystallization of such discrete complexes has been coined a chemical Janus. Graphical Abstract  The title complexes contain pseudo-tetrahedral Cu(II)N₂Cl₂ coordination. One of the structures is the result of an unusual cocrystallization, in which two different discrete Cu(II) molecules cocrystallize in an equimolar ratio with a nitromethane solvate molecule.      

链状钴配合物的水热合成、晶体结构及荧光性质

采用水热法合成得到了链状钴配合物[Co(4,4'-bipy)(H2O)4]n· 2nH2L· 4nH2O(H2L-＝2,5-二羟基苯磺酸离子,4,4'-bipy＝4,4'-联吡啶).采用X射线单晶衍射、元素分析、红外光谱、热重分析等对配合物进行了组成和结构表征.单晶衍射研究表明,配合物中钴离子与4,4'-bipy的氮原子配位和水分子的氧原子配位,形成扭曲的八面体配位构型. H2L-配体没有配位,只是平衡结构中的电荷.在结构单元中,[Co(4,4'-bipy)(H2O)4] +,H2L-和H2 O之间通过氢键相连.配合物的荧光发射峰与配体相比发生了红移,最大发射峰在411 nm.     

Synthesis,Crystal Structure and Fluorescent Study of Bis(2-(2-hydroxyphenyl)benzimidazolate)zinc with Ethanol Solvate

Abstract  The zinc(II) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Zn(2-(2-hydroxyphenyl)benzimidazolate)₂]·C₂H₅OH (1 · C₂H₅OH) has been synthesized and characterized by X-ray crystallography and photoluminescent analysis. The complex crystallizes in monoclinic space group P2₁/c with cell parameters a = 10.156(1) ?, b = 25.771(3) ?, c = 9.674(1) ?, α = 90°, β = 103.641(2)°, γ = 90°, Z = 4, V = 2460.4(4) ?³. The central Zn(II) is four-coordinate and has a tetrahedral geometry. The steady-state and time-resolved photoluminescent spectra for the title compound have also been studied. The emission property can be ascribed to ligand-centered charge-transfer transition (LCCT) with π → π* property. Index Abstract   A new co-crystal of Zn(II) complex of 2-(2-hydroxylphenyl)benzimidazole with ethanol solvate has been prepared, characterized by X-ray crystallography and fluorescent studies.      

Synthesis,Crystal Structures and Fluorescence Properties of Ni (II) and Cu (II) Complexes with 1-(Furan-2-ylmethylene)-4-phenylthiosemicarbazone

Abstract  

Two coordination complexes, NiL ₂ and CuL ₂ {L = bis[1-(furan-2-ylmethylene)-4-phenylthiosemicarbazone]}, were synthesized and determined by X-ray crystallography. Both crystallize in the Orthorhombic system, space group Pbcn, with lattice parameters: a = 11.935 (2) Å, b = 15.314(3) Å, c = 12.952(3) Å and Z = 4 for Ni (II); a = 20.850(4) Å, b = 15.049(3) Å, c = 7.5633(5) Å and Z = 4 for Cu (II). In both complexes, the central metal atom is coordinated in a distorted square-planar with two ligands through two S and N atoms, respectively. The EA, UV, IR and TG-DTG were studied and the possible structures of the complexes were speculated. Moreover, the fluorescence of the complexes were studied. The results reveal that copper complex can emit purple fluorescence in solvents.     

Synthesis,Characterization and Crystal Structure of Tetraphenylphosphonium Bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-Nickelate Acetone Solvate Crystal

Abstract  

A new crystal of tetraphenylphosphonium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)-nickelate acetone solvate (BPNI) has been prepared at room temperature and characterized by elemental analysis, UV–Vis–NIR absorption spectrum and X-ray single crystal determination. The complex crystallized in monoclinic space group P2/c with unit cell dimensions a = 24.5350 (6) ?, b = 7.3097 (2) ?, c = 23.1141 (6) ?, β = 115.585 (2)°, V = 3738.89 (17) ?³, Z = 4, D _x .= 1.5081 (1) g cm⁻³. The X-ray structure determination revealed that the crystal is centro-symmetrical and there are two halves of independent cations in the molecule.     

含(1E,2E)-N1,N2-双((8-丁氧基喹啉-2-)亚甲基)乙烷-1,2-二胺的双核银配合物的合成与晶体结构

基于(1E,2E)-N1,N2-双((8-丁氧基喹啉-2-)亚甲基)乙烷-1,2-二胺的双核银配合物被合成,用1H NMR,单晶衍射表征其结构.该配合物I是一个三斜晶体,空间群为P-1,其余参数是:a=13.489(5)?,b=13.550(5)?,和c=19.836(8)?,α=70.077(6)°,β=75.145(9)°,γ=82.430(6)°,V=3291(2)?3,Z=2,C60H68Ag2F12N8O5P2, Mr=1486.90,Dx=1.500 g/cm3,T=296(2)K.晶体结构显示8-羟基喹啉衍射物是一个四齿配体,链接两个银离子.在室温下,用乙腈作为溶剂,浓度为1×10 -6mol· L-1,8-羟基喹啉衍射物与配合物I有相似的荧光光谱.     

Crystal Structures of a Series of Bis{(2-Aminobenzoyl-)amino}alkanes

Abstract  The crystal structures of 1,2-bis-{(2-aminobenzoyl-)amino}ethane(1), 1,4-bis-{(2-aminobenzoyl-)amino}butane(2) and 2,2-dimethyl-1,3-bis-{(2-aminobenzoyl-)amino}-propane(3) have been determined by single crystal X-ray diffraction analysis. 1 and 2 are centrosymmetric molecules which lie on crystallographic centers of symmetry and adopt extended conformations. On the other hand, owing to the odd number of carbon atoms in the spacer unit, 3 does not show centrosymmetry, but crystallizes in a non-centrosymmetric space group and assumes a folded conformation. The crystal structures of 1, 2 and 3 are compared with the known structures of anthranilamide (7) and the N-alkyl anthranilamide derivative 8. Crystal data: 1 C₁₆H₁₈N₄O₂, monoclinic, space group P2₁/a, a = 9.5262(8) ?, b = 5.4200(5) ?, c = 15.3821(14) ?, β = 105.980(5)° and V = 763.52(12) ?³, for Z = 2. 2 C₁₈H₂₂N₄O₂, monoclinic, space group C2/c, a = 32.0710(17) ?, b = 5.4732(4) ?, c = 9.7326(5) ?, β = 102.570(4)° and V = 1667.42(17) ?³, for Z = 4. 3 C₁₉H₂₄N₄O₂, orthorhombic, space group Pca2₁, a = 16.7676(4) ?, b = 10.1847(2) ?, c = 10.5338(5) ?, and V = 1798.89(7) ?³, for Z = 4. Index Abstract  The crystal structures of 1,2-bis-{(2-aminobenzoyl-)amino}ethane(1), 1,4-bis-{(2-aminobenzoyl-)amino}butane(2) and 2,2-dimethyl-1,3-bis-{(2-aminobenzoyl-)amino}-propane(3) have been determined by single crystal X-ray diffraction analysis. 1 and 2 are centrosymmetric molecules which lie on crystallographic centers of symmetry and adopt extended conformations, whereas 3 does not show centrosymmetry, but crystallizes in a non-centrosymmetric space group and assumes a folded conformation.      

Synthesis,Characterization and Crystal Structure of the Bis(2,4-dinitrobenzoato)tetrabutyldistannoxane(IV) Dimer

Abstract The title compound, bis(2,4-dinitrobenzoato)tetrabutyldistannoxane(IV), was obtained from the reaction of di-n-butyltin(IV) oxide with 2,4-dinitrobenzoic acid. It crystallizes out as the usual dicarboxylatotetrabutyldistannoxane(IV) dimer. In the monoclinic system P2₁/c, a = 12.391(3) ?, b = 19.937(5) ?, c = 15.026(4) ?, α = γ = 90°, β = 102.857(2)°, V = 3618.95(16) ?³ and Z = 2. A crystal structure determination of the title compound reveals the presence of a centrosymmetric planar Sn₂O₂, with two different environments for tin atoms and two distinct carboxylate groups. Two of the carboxylate groups are bonded to the exocyclic tin atom in a bidentate bridging manner and the remaining two carboxylate groups are bonded to the tin atom in a monodentate manner. As a result, both the tin atoms moieties in the complex are five coordinate and exhibit trigonal bipyramid geometry. Index Abstract Synthesis, Characterization and Crystal Structure of the Bis(2,4-dinitrobenzoato)tetrabutyldistannoxane(IV) Dimer Yip Foo Win, Teoh Siang Guan, Lim Eng Khoon, Shea Lin Ng, Hoong Kun Fun A crystal structure determination of the title compound reveals the presence of a centrosymmetric planar Sn₂O₂, with two different environments for tin atoms and two distinct carboxylate groups.      

Mn(II) and Zn(II) Complexes Constructed by Bis(4-(1H-Imidazol-1-yl)phenyl)methanone and Salicylate: Syntheses and Crystal Structures

Crystallography Reports - Two complexes with V-shaped ligands, [(L1)2Mn(H2O)4](HSA)2] (1), {[(L1)2Zn(H2O)2](HSA)2}n (2) (L1 = bis(4-(1H-imidazol-1-yl)phenyl)methanone, H2SA = salicylic acid), have...     

Syntheses,Crystal Structures and Fluorescence Properties of Zn(II) Complexes with Pyrazolone Derivatives

Abstract   N-(1,3-Diphenyl-4-benzal-5-pyrazolone)-salicylidene hydrazone(H₂L ¹ ) and its zinc complex Zn(HL ¹ )₂ · 2CH₃OH (1) have been synthesized and characterized by elemental analyses, IR spectra, thermal analyses and single-crystal X-ray diffraction studies. The X-ray diffraction analyses of the complex Zn(HL ¹ )₂ · 2CH₃OH (1) and the known compound Zn₄(L ² )₄ (2) (H₂L ²  = N-(1,3-diphenyl-4-phenylethylene-5-pyrazolone)-salicylidene hydrazone) show that different acyl groups in position 4 of pyrazolones may lead to the different coordination mode of the ligands and distinctive structures of the same central metal Zn(II) complexes, of which 1 is a mononuclear complex while 2 is a tetranuclear complex. Meanwhile, two Zn(II) complexes have different thermal stabilities and fluorescence properties. Graphical Abstract