Synthesis, Crystal Structures and Fluorescence Property of Bis(benzimidazol-2-yl)methane Dichloride

Abstract  

The title compound, a salt of C₁₅H₁₃N₄ ²⁺2Cl⁻, was synthesized and determined by X-ray crystallography. It crystallizes in the orthorhombic system, space group Pbcn, with lattice parameters a = 9.973(2) ?, b = 9.5012(19) ?, c = 15.574(3) ?, V = 1475.8(5) ?³, Z = 4, C₁₅H₁₃Cl₂N₄, Mr = 320.19, Dc = 1.441 g/cm³. In the crystal structure, the Cl⁻ anion interact with the same benzimidzaole through two kinds of hydrogen bonds forming a 1D hydrogen-bonded chain, two 1D hydrogen-bonded chain cross with each other and form 2D layer structure. The EA, UV, IR and TG-DTG were studied and the possible structures of the title compound were speculated. Moreover, the fluorescence of the title compound was studied. The results reveal that it can emit purple fluorescence in DMF solvent.     

Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane

Abstract The title complex [Co₂(bte)₃(NCS)₄(H₂O)₂] _n (bte = 1,2-bis(triazol-1-yl)ethane) has been prepared. Single-crystal X-ray analysis reveals that the complex crystallizes in space group P ī with a = 7.7962(2), b = 8.3407(4), c = 14.7735(5) ?, α = 86.835(2), β = 76.2031(9), γ = 80.583(3)°. The crystal consists of two discrete complexes, [Co(bte)(NCS)₂(H₂O)₂] and [Co(bte)₂(NCS)₂]. The structure of [Co(bte)(NCS)₂(H₂O)₂] consists of neutral chain containing Co(II) bridged by bte molecules. The six-co-ordination of Co²⁺ is achieved by means of two trans NCS⁻ ions and water molecules. The structure of [Co(bte)₂(NCS)₂] demonstrates a one-dimensional neutral chain through bte-bridge, in which the Co(II) atom is in a distorted octahedral environment formed by four nitrogen atoms of the triazoles and two nitrogen atoms from two trans thiocyanato liagnds. Index abstract Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane This paper reports the synthesis and crystal structure of complex [Co₂(bte)₃(NCS)₄(H₂O)₂]_n (bte = 1,2-bis(triazol-1-yl)ethane), which consists two different neutral chains containing Co(II) bridged by bte molecules.      

Synthesis and Crystal Structure of a New Cobalt(II) Complex: Bis(pyridine)bis(4,4,4-trifluoro-1-(6-methoxynaphthalen-2-yl)butane-1,3-dione) Cobalt(II)

Abstract  

A new Co(II) complex 2 with ligand 4,4,4-trifluoro-1-(6-methoxynaphthalen-2-yl) butane-1,3-dione 1 and pyridine are prepared and crystallized from an acetone solution. The obtained red and transparent crystal conforms to the empirical formula of Co(C₁₅H₁₀O₃F₃)₂·(C₅H₅N)₂. It crystallizes in monoclinic, space group C2/c with a = 23.3152(14), b = 12.0225(7), c = 15.3950(10) ?, β = 124.1360(10)°, V = 3571.8(4) ?³, Z = 4, C₄₀H₃₀CoF₆N₂O₆, Mr = 807.59, F(000) = 1652, Dc = 1.502 g/cm³, μ = 0.564 mm⁻¹, the final R = 0.0466 and wR = 0.1043 for 3901 observed reflections with I > 2σ(I). X-ray structural analysis revealed that the Co(II) atom is coordinated by two oxygen atoms of 1,3-dione ligands 1 and two nitrogen atoms of pyridines, forming a distorted octahedron coordination geometry.     

Synthesis,Crystal Structure,and Luminescent Properties of a Cadmium(II) Coordination Polymer Constructed by Bis(4-(1H-Imidazol-1-yl)phenyl) Methanone and 1,4-Benzenedicarboxylate Ligands

Crystallography Reports - A coordination polymer with the V-shaped ligands, {Cd2(bipmo)2(bdc)2?H2O}n (1), (where bipmo is bis(4-(1H-imidazol-1-yl)phenyl)methanone; H2bdc is...     

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.      

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.      

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.      

Synthesis and Crystal Structure of a One-Dimensional Chain Cadmium Coordination Polymer Bridged Through 1,2-bis(imidazol-1-yl)ethane

Abstract The cadmium(II) complex [Cd(phba)₂(bim)(H₂O)₂]_n (1) (phba = 4-hydroxybenzoate, bim = 1,2-bis(imidazol-1-yl)ethane) has been synthesized and structurally characterized by X-ray diffraction analysis. It crystallizes in the monoclinic space group C2/c, a = 23.820(4) ?, b = 9.5331(14) ?, c = 11.1086(19) ?, β = 111.519(4)°, V = 2346.7(7) ?³, Z = 4. The coordination geometry of Cd(II) atom is distorted octahedral; it is coordinated by two nitrogen atoms from the imidazole rings of two symmetry-related bim molecules, and four oxygen atoms from two symmetry-related phba anions and two water molecules. The Cd(II) atoms are bridged by bim molecules to form a one-dimensional chain. Graphical abstract Synthesis and crystal structure of a one-dimensional chain cadmium coordination polymer bridged through 1,2-bis(imidazol-1-yl)ethane Yuping Zhang, Liyan Wang, Shouwu Wang, Baolong Li, Yong Zhang The cadmium(II) complex [Cd(phba)2(bim)(H2O)2]n (1) has been synthesized and structurally characterized by X-ray diffraction analysis. The coordination geometry of Cd(II) atom is distorted octahedral; it is coordinated by two nitrogen atoms from the imidazole rings of two symmetry-related bim ligands, and four oxygen atoms from two symmetry-related phba anions and two water molecules. The Cd(II) atoms are bridged by bim ligands to form a one-dimensional chain.     

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.     

Synthesis and Characterization of Bis(methyl-2-pyridylmethylidenedrazinecarbodithioate)manganese(II)

Abstract  Brown crystals of title compound, bis(methyl-2-pyridylmethylidene-drazinecarbodithioate)manganese(II), was formed by reaction of methyl-2-pyridylmethylidenehydrazinecarbodithioate(HNNS) with manganese perchlorate at 323 K temperature and recrystallized from ethanol at room temperature, crystallizing in the monoclinic system, space group P2(1)/n, with a = 11.631(2), b = 14.010(3), c = 13.128(3) ?, β = 105.791(11)°; V = 2058.6(7)  ?³, D _c  = 1.533 g/cm³, Z = 4, C₁₆H₁₆N₆MnS₄, M _r  = 475.53, μ(M₀ K _α ) = 1.060 mm⁻¹, F (000) = 972. The structure was refined to R = 0.0441, wR = 0.1196 for 3,682 (I > 2σ(I)) reflections and S = 1.110. In title complex the coordination geometry about manganese is distorted octahedral and the two ligands in the mer configuration (S and tertiary N atom cis to each other and the iminic N atoms trans). Furthermore, the neutral molecule units Mn^II(NNS)₂ are connected by hydrogen bonds C–H···N and C–H···S and form a three dimensional ordered network structure. Graphical Abstract  The title compound, Mn(NNS)₂, exists as discrete molecules in which the central MnII atom is coordinated by two S atoms and four N atoms from two ligands NNS- molecules in a mer-octahedral configuration. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis and Crystal Structure of a Cobalt Coordination Polymer Based on Bis(4-(1H-imidazol-1-YL)phenyl)methanone and trans-1,2-Cyclohexanedicarboxylate

Crystallography Reports - A cobalt coordination polymer with V-shaped ligands, {[L1Co(trans-CHDCA)] · 2H2O}n (L1 = bis(4-(1H-imidazol-1-yl)phenyl)methanone, trans-H2CHDCA =...     

Synthesis of 1,2-dimethoxy-1,2-di(pyridin-2-yl)-1,2-ethanediol: Crystal and molecular structure determination

The compound, 2-hydroxy-[1,2-di(pyridin-2-yl)]ethane-1-one, 1, was isolated from the reaction of 2-pyridinecarboxaldehyde and 2-pyridinemethanol at 140°C without catalyst or solvent and characterized by¹H-NMR and IR spectral data. The compound 1 was treated with ethyl acetate to produce the 1,2-di(pyridin-2-yl)ethane-1,2-dione, 2. When 2 was dissolved in an excess of CH₃OH, crystals of 1,2-dimethoxy-1,2-di(pyridin-2-yl)-1,2-ethanediol, 3, were obtained. The molecular and crystal structure of 3 was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system belonging to the P2₁/n space group with a = 6.867(2) ?, b=9.546(4) ?, c=10.522(5) ?, α=90°, β=98.48(4)°, γ=90°. The asymmetric unit comprises two molecules of 3. Although the di-hemiketal was obtained in crystal form, it was found to be unstable, because its IR spectrum changed after a short time, indicating that it had been converted back to the original diketone, 2. The IR showed signals at 1713, and 1690 due to νC =O assigned to di-ketone group.     

Synthesis,Molecular Structure and Quantum Chemical Studies of N-(2-Fluorophenyl)-1-(5-Nitrothiophen-2-yl)methanimine

Crystallography Reports - N-(2-Fluorophenyl)-1-(5-nitrothiophen-2-yl)methanimine has been synthesized and characterized by single-crystal X-ray determination. Molecular geometry from X-ray...     

Crystal and molecular structure of Bis(N-[pyrid-2-yl]-1-imino-2-carbethoxy-3-oxo-butan-2-ido)-palladium (II)

The crystal and molecular structure of the title compound has been determined by X-ray diffraction techniques. It crystallizes in the orthorhombic space group Pbca with 4 formula units C₂₄H₂₆N₄O₆Pd in the unit cell. The lattice constants are a = 17.259, b = 19.070, and c = 7.480 Å. The structure was solved by the heavy atom technique and refined by least-squares calculations to the conventional R = 0.057. The coordination sphere of palladium as well as the molecular geometry of the ligands are discussed in the paper.     

Synthesis and molecular structure of propylene-bis(benzoylacetoneiminato)copper(II), [Cu(ba)2-1,2-pd]

The title compound C₂₃H₂₄N₂CuO₂ (4 in Scheme 1) was prepared and characterized by IR, UV, and GC measurements. The structure was solved by direct methods, and full-matrix least-squares refinement of structural parameters led to a conventionalR factor of 0.049 for 1879 reflections. The copper(II) atoms are in a nontetrahedrally distorted planar coordination. A disorder of the five-membered chelate ring has been observed: two alternative positions,A andB for C20, C21 and C22 were found and refined with constrained C-N and C-C bond length. In bothA andB rings, connected by pseudosymmetry plane, the ethylene bridge shows the gauche conformation, with the methyl group in the axial position. The geometry of the molecule is discussed.     

Crystal structures of copper(II) nitrate,copper(II) chloride,and copper(II) perchlorate complexes with 2-formylpyridine semicarbazone

Compounds dinitrato(2-formylpyridinesemicarbazone)copper (I), dichloro(2-formylpyridinesemicarbazone) copper hemihydrate (II), and bis(2-formylpyridinesemicarbazone)copper(2+) perchlorate hydrate (III) are synthesized and their crystal structures are determined. In compounds I–III, the neutral 2-formylpyridine semicarbazone molecule (L) is tridentately attached to the copper atom via the N,N,O set of donor atoms. In compounds I and II, the Cu: L ratio is equal to 1: 1, whereas, in III, it is 1: 2. In complex I, the coordination sphere of the copper atom includes two nitrate ions with different structural functions in addition to the L ligand. The structure is built as a one-dimensional polymer in which the NO₃ bidentate group fulfills a bridging function. The coordination polyhedron of the copper(2+) atom can be considered a distorted tetragonal bipyramid (4 + 1 + 1). Compound II has an ionic structure in which the main element is the [CuLCl₂ · Cu(H₂O)LCl]⁺ dimer. In the dimer, the copper atoms are linked via one of the μ₂-bridging chlorine atoms. The coordination polyhedra of the central atoms of the Cu(H₂)LCl and CuLCl₂ complex fragments are tetragonal bipyramid and tetragonal pyramid, respectively. In compound III, the copper atom is octahedrally surrounded by two L ligands in the mer configuration.     

Structural Properties of S-alkylated Dithiolene Chelates (I). Crystal and Molecular Structures of Bis(S-ethyl-ethene-1,2- dithiolato)palladium (II) and Bis(S-ethyl-ethene-1,2-dithiolato) platinum (II)

Bis(S-ethyl-ethene-1,2-dithiolato)palladium(II), Pd(S₂C₄H₇)₂, is monoclinic, P 2₁/n, with a = 7.598(1) Å, b = 10.445(2) Å, c = 8.031(1) Å, β = 95.3(1)° and Z = 2. The structure was determined by 893 independent reflections and refined by the block-diagonal leastsquares method to R = 0.12. The chelate molecule is nearly planar and the palladiumsulfur distances are 2.278(6) Å and 2.403(6) Å. Bis(S-ethyl-ethene-1,2-dithiolato)platinum(II), Pt(S₂C₄H₇)₂, is monoclinic, P 2₁/a, with a 13.114(2) Å, b = 12.873(2) Å, c = 7.446(2) Å, β = 96.1(1)° and Z = 4. The structure was solved from 2040 independent reflections. The compound is not isomorphic with the isomeric palladium complex. In the unit cell there exist two symmetry independent molecules. The platinum-sulfur distance is 2.280 (6) Å.