The Preparation, Characterization and X-ray Structural Analysis of Tetrakis[1-Methyl-3-(2-Propyl)-2(3H)-Imidazolethione]Cadmium(II) Hexafluorophosphate

Abstract  A new compound, [Cd(mipit)₄][PF₆]₂ has been synthesized and characterized via standard solid and solution state methods including single crystal X-ray crystallography (mipit = 1-methyl-3-(2-propyl)-2(3H)-imidazolethione). The title compound crystallizes in tetragonal space group I4 ₁ /a with a = 12.478(2) ?, b = 12.478(2) ?, c = 28.806(6) ?, and Z = 4. The complex is a high melting, colorless solid that has a distorted tetrahedral CdS₄ coordination geometry. Thermogravimetric analysis results for the title compound as well as for another potential CdS synthon and two potential CdSe synthons are reported. Graphical Abstract  The synthesis and characterization of the title compound, a new ionic homoleptic cadmium complex, tetrakis[1-methyl-3-(2-propyl)-2(3H)-imidazolethione]cadmium(II) hexafluorophosphate is reported. The results of a single crystal X-ray diffraction analysis reveal a distorted tetrahedral CdS₄ coordination sphere about the cadmium. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

1,3-Bis(4-Pyridinylcarbonyl)-2-Imidazolidinethione and Its First Cluster Complex: Synthesis,Crystal Structure and Luminescence Properties

Abstract  The first cluster complex of 1,3-bis(4-pyridinylcarbonyl)-2-imidazolidinethione (4-bpit) with CuI was prepared and characterized. Single crystal X-ray diffraction analysis established that the compound crystallizes in the monoclinic system, space group C2/m, with a = 15.601(3), b = 12.438(3), c = 12.570(3)?, β = 110.02(3), Z = 4, V = 2291.8(8)?³. This compound is also a coordination polymer with one-dimensional double-ribbon structure containing the adaptable rhomboid Cu₂I₂ cluster unit. The solution-state luminescence spectra showed that the high-energy emission may be associated with a ligand-to-ligand charge-transfer excited state. Graphical Abstract  The first cluster complex of 1,3-bis(4-pyridinylcarbonyl)-2-imidazolidinethione (4-bpit) with CuI was prepared and characterized. This compound is also a coordination polymer with one-dimensional double-ribbon structure containing the adaptable rhomboid Cu₂I₂ cluster unit. The solution-state luminescence spectra showed that the high-energy emission may be associated with a ligand-to-ligand charge-transfer excited state.     

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.     

X-ray Crystal Structure of Trans -UO2(N(SiMe3)2)2(THF)2: One in a Series of Uranyl(VI) Complexes Supported by Bis(trimethylsilyl)amido Ligands

Abstract The title compound trans-UO₂(N(SiMe₃)₂)₂(THF)₂ (1) was synthesized and characterized by X-ray crystallography. The complex crystallizes in the monoclinic space group C2/c (#15) with lattice parameters a = 16.0771(5) ?, b = 13.1196(4) ?, c = 16.9391(6) ?, β = 116.853(1)°, V = 3187.61(18) ?³, Z = 4, D _calc = 1.532 g cm^-3. The six-coordinate uranium(VI) center adopts an all-trans octahedral geometry consisting of mutually trans oxo groups, silylamido ligands, and neutral THF donors. Structural comparisons of this uranyl(VI) bis(amido) complex with a related tris(amido) derivative within the series are made based on symmetry, charge, and coordination number. Graphical Abstract The X-ray crystal structure of the title complex is reported, providing comparisons based on symmetry, charge, and coordination number with a related uranyl(VI) amido derivative within this series.      

Synthesis and Crystal Structure of 2,13-Bis(acetamido)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0<Superscript>1.18</Superscript>,0<Superscript>7.12</Superscript>]docosane Tetrachlorocobalt(II)dihydrate

Abstract The novel ionic compound [H₂bdtd][CoCl₄] · 2H₂O (1) was prepared by the reaction between CoCl₂ and 2,13-bis(acetamido)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^1.18,0^7.12]docosane (bdtd) in adjusted to pH 3.0 by 1.0 M HCl and structurally characterized. The crystals are monoclinic C2/c with a = 18.7777(9), b = 9.7356(4), c = 20.0884(9) ?, β = 109.6340(10)°, V = 3458.9(3) ?³, Z = 4. The dication H₂bdtd occupies a special position about an inversion center. The cobalt(II) atom in the anion is in a distorted tetrahedral environment with four chloride ligands. The crystal structure is stabilized by a variety of hydrogen-bonding contacts involving the dication, chloride anions and solvent water molecules. Cyclic voltammetry of [CoCl₄]²⁻ anion in 1 undergoes irreversible one-electron reduction to the Co^II/Co^I. Graphical abstract The crystal structure of the ionic compound [H₂bdtd][CoCl₄] · 2H₂O (1) consists of [H₂bdtd]²⁺ cation, [CoCl₄]²⁻ anion and water molecules joined together by ionic interaction and hydrogen bonds. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Synthesis and Structure of the Dimeric Copper(II) Complex Tetrakis[<Emphasis Type="Italic">N</Emphasis>-thiazol-2-yl-(4-methylphenyl)sulfonamidate]dicopper(II)

Abstract The coordination chemistry of the ligand N-thiazol-2-yl-toluenesulfonamidate towards the copper(II) ion has been investigated using an electrochemical synthesis method. The X-ray structure of this complex was elucidated and is discussed. The compound crystallised in the monoclinic crystal system, P2₁/c space group with a = 17.3888(9), b = 16.3003(9), c = 18.3679(9) ? and β = 114.3640(10)°. Four bidentate sulfathiazolato anions bridge two metal centers in a paddle-wheel fashion, with the nitrogen atoms as donors to give a dimeric species with a Cu···Cu distance of 2.7859(5) ?. Graphical Abstract The coordination chemistry of the ligand N-thiazol-2-yl-toluenesulfonamidate towards the copper(II) ion has been investigated using an electrochemical synthesis method. The X-ray structure of the product has been elucidated and is discussed. Sulfathiazolato anions act as bridging ligands to give a dimeric species with a Cu···Cu distance of 2.7859(5) ?.      

Synthesis and Crystal Structure of a Mixed-Ligand Cobalt(II) Complex with 2-Aminobenzimidazole

Abstract  The cobalt(II) complex, [Co(abz)₂(SCN)₂] 1, has been synthesized by the reaction of cobalt(II) nitrate with ammonium thiocyanate and abz ligands (abz = 2-aminobenzimidazole), and was fully structurally characterized by elemental analysis, IR spectra, X-ray diffraction and thermogravimetric experiments. It crystallizes in the triclinic P-1 space group with a = 8.6316(10), b = 9.3426(10), c = 13.254(2) ?, α = 95.793(2), β = 95.870(2), γ = 115.7380(10), V = 945.1(2) ?³, and Z = 2. The central cobalt(II) atom is four-coordinated to nitrogen donors from two neutral abz ligands and two isothiocyanate anions respectively, adopting a slightly distorted tetrahedral geometry. In addition, the intermolecular N–H···N and N–H···S hydrogen bonds interactions link the discrete mononuclear units into infinite three-dimensional networks. Index Abstract  The essence sentence of the paper: In the mixed-ligand mononuclear complex, [Co(abz)₂(SCN)₂], the four coordinated cobalt(II) atom exhibits a slightly distort tetrahedron, which is further assembled into 3D infinite network by intermolecular hydrogen interactions.      

Crystal Structures of (2-oxo-2H-Quinaxalin-1-yl)-acetic Acid and its Cobalt and Nickel Complexes and Their Comparison with (1,3-Dioxo-1,3-dihydro-isoindol-2-yl)-acetic Acid

Abstract The crystal structures of (2-oxo-2H-quinaxalin-1-yl)-acetic acid and its cobalt and nickel complexes are determined. The (2-oxo-2H-quinaxalin-1-yl)-acetic acid (1) crystallizes in orthorhombic, Pbca, a = 12.8571(11) ?, b = 9.4267(8) ?, c = 15.0095(13) ?, the cobalt complex of (2-oxo-2H-quinaxalin-1-yl)-acetic acid (2) crystallizes as dihydrate in triclinic, P-1 space group with a = 4.81150(10) ?, b = 11.8631(2) ?, c = 12.4867(3) ?, α = 71.7800(10)°, β = 79.2490(10)°, γ = 84.9020(10)° whereas the nickel complex of (2-oxo-2H-quinaxalin-1-yl)-acetic acid (3) crystallizes in monoclinic, P2₁/c space group with a = 14.9210(5) ?, b = 4.81730(10) ?, c = 15.7672(5) ?. and β = 99.823(2)°. The crystal structure of the ligand and the complexes are compared with structures of (1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid and its cobalt and nickel complexes. Index Abstract The crystal structures of (2-oxo-2H-quinaxalin-1-yl)-acetic acid and its nickel and cobalt complexes are compared with (1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid and its corresponding complexes with nickel(II) and cobalt(II).      

Synthesis and Structure of a CdI<Subscript>2</Subscript> Coordination Polymer with 1,4-Bis(benzimidazole-1-yl-methylene)benzene (bbmb)

Abstract  In this paper, solution reaction of cadmium iodide with organic multifunctional ligand 1,4-bis(benzimidazole-1-yl-methylene)benzene generated a 1D polymer [CdI₂ (bbmb). (DMF) (CH₃CN)]_n 1, and the crystal structure has been determined (C₂₇H₂₈CdI₂N₆O), Mr = 818.75, a  = 14.929(1) ?, b = 17.381(2) ?, c = 15.850(1) ?, β = 114.8190(10)°, space group C2/c, Z = 4, and V = 3733.3(6) ?³. In 1 the tetrahedral coordination of Cd(II) and the conformation of the bbmb ligand make it a wave-shaped structure.

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Graphical Abstract  Synthesis and structure of a CdI2 coordination polymer with 1,4-bis(benzimidazole-1-yl-methylene)benzene(bbmb) Xiucun Liu, Xiaoling Guo, Yunyin Niu, Qingli Wang, Qian Cui, Hongwei Hou, Xiaorui Lv, SeikWeng Ng Solution reaction of cadmium iodide with organic multifunctional ligand 1,4-bis(benzimidazole-1-yl-methylene)benzene (bbmb) generated a 1D polymer [CdI₂ (bbmb) (DMF)(CH₃CN)]_n, in which the tetrahedral coordination of Cd(II) and the conformation of bbmb ligand make it a wave-shaped structure.

     

Synthesis and Crystal Structure of One-Dimensional Carboxylate-Bridged Copper(II) Complex with 2-Pyridylmethylamino-3-butyric acid

Abstract The tridentate Schiff base carboxylate-containing ligand 2-pyridylmethylamino-3-butyric acid (Hpaba) reacts with copper(II) perchlorate to give the one-dimensional chain complex {[Cu(μ-paba)](ClO₄)·H₂O} _n (1). The coordination geometry of each copper(II) ion is best described as a square-plane with two nitrogen atoms and one carboxylate oxygen atom of the ligand, and one carboxylate oxygen atom belong to another ligand. It crystallizes in the monoclinic system P2₁/c with a = 12.717(2), b = 7.9163(15), c = 14.981(2) ?, β = 111.14(1)°, V = 1406.8(4) ?³, Z = 4. Cyclic voltammogram of 1 undergoes the reversible one-electron oxidation to the Cu(III) and the reversible one-electron reduction to the Cu(I) state. Graphical Abstract Crystal structure of 1 reveals a syn-anti carboxylate-bridged one dimensional chain complex in which the coordination environment around each copper(II) ion exhibits a distorted square plane.      

Synthesis, Crystal Structure of a New Co(II) Complex with Pyrazine-2,3,5,6-tetracarboxylic Acid

Abstract A new complex [Co(H₂pztc)(bpy)H₂O] (H₄pztc = pyrazine-2,3,5,6-tetracarboxylic acid, bpy = 2,2′-bipyridine) has been synthesized by hydrothermal reactions of Co(NO₃)₂ · 6H₂O with H₄pztc and bpy and characterized by IR and X-ray diffraction single crystal structure analysis. It belongs to monoclinic system, P2₁/c space group with a = 13.454(2) ?, b = 12.939(2) ?, c = 11.4993(19) ?, α = 90°, β = 111.640(3)°, γ = 90°. This complex is assembled into 3D supramolecular architecture by hydrogen bonds (O–H···O, C–H···O). Index Abstract A new complex of cobalt(II) with pyrazine-2,3,5,6-tetracarboxylic acid and 2,2′-bipyridine is assembled by intermolecular hydrogen bonds forming 2D layer and 3D supramolecular network.      

Synthesis and Crystal Structure of 4,6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde

Abstract The title compound, 3, 6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]- benzene-1,3-dicarbaldehyde was synthesized by Vilslmeier reaction from resveratrol (trans-3,4′,5-trihydroxystilbene). Its structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2₁/n with crystallographic parameters: a = 7.2950(15) ?, b = 14.781(3) ?, c = 12.202(2) ?, β = 96.57(3)°, μ = 0.108 mm⁻¹, V = 1307.1(5) ?, Z = 4, Dx = 1.445 g/cm³, F(000) = 592, T = 293(2) K, 2.17°≤ θ ≤ 26.00°. The X-ray results demonstrated that the Vilslmeier reaction of resveratrol with DMF, POCl₃ and CH₃CN yielded 4,6-dhydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde. Graphical Abstract In this article, a resveratrol derivative was prepared and structurally characterized by single crystal X-ray diffraction.      

Synthesis of <Emphasis Type="Italic">E</Emphasis> Isomer and Crystal Structures of <Emphasis Type="Italic">E</Emphasis> and <Emphasis Type="Italic">Z</Emphasis> Isomers of 3-(2,5-Dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile

Abstract Details of the synthesis of the E isomer of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile, and the X-ray crystal structures of both the E and Z isomers of this compound are presented. The E isomer crystallizes in the P2₁/c space group with cell parameters, a = 8.5659(17) ?, b = 16.399(3) ?, c = 11.224(2) ?, α = 90°, β = 95.27(3)°, γ = 90°and Z = 4. The Z isomer crystallizes in the Pca2₁ space group with cell parameters, a = 4.1223(8) ?, b = 19.113(4) ?, c = 19.453(4) ?, α = 90°, β = 90°, γ = 90° and Z = 4. Index Abstract Synthesis of E isomer and X-ray crystal structure determination of both E and Z isomers of 3-(2,5-dimethoxyphenyl)-2-(4-methoxyphenyl)acrylonitrile are presented.      

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 and Structure of a Copper Complex of a Macrocyclic Ligand with Dissimilar HN+N(Amino)O2 and N2(Imino)O2 Inners

Abstract The copper complex [Cu(C₂₃H₂₇Br₂N₄O₂)(H₂O)(NO₃)]₂ was synthesized and characterized by X-ray diffraction. The complex crystallizes in the triclinic system with space group P-1, lattice parameters: a = 13.2293(18) (?), b = 14.184(20) (?), c = 16.522(23) (?), α = 91.923(2)°, β = 111.777(2)°, γ = 111.259(2)°, V = 2632.0(6) ?³, Z = 4, D _c = 0.88 Mg m⁻³. In the title compound [Cu(C₂₃H₂₇Br₂N₄O₂)(H₂O)(NO₃)]₂, the coordination polyhedron of the Cu atom is a square-planar environment. The structure consists of mononuclear units in which the copper(II) ions are linked in the plane by N, N′ iminato and O, O′ phenoxo atoms. In addition the crystal lattice contains one water molecule per unit. Graphical Abstract Dissymmetric ligand was efficiently synthesized and used to prepfsare a copper(II) complex which was characterized by X-ray diffraction      

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        

Crystal Structure and Magnetic Properties of a Novel Octa-coordinated Manganese(II) Complex

Abstract  The self-assembly and structural characterization of the new manganese(II) [MnL ₂](ClO₄)₂(CH₃OH)_0.5 (1) complex has been achieved. The crystallographic data for the complex 1: Orthorhombic Pbca , a = 16.287(2) ?, b = 21.293(2)?, c = 32.718(3) ?, V = 11,347(2) ?³, Z = 8. The two polydentate ligands strand intertwined each other and around the manganese(II) ions forming a mononuclear complex. The Mn(II) ion is eight-coordinated with the eight donor nitrogen atoms of two ligands to form a distorted square antiprismatic coordination geometry. The magnetic properties investigation indicates that there is a weak antiferromagnetic exchange coupling between the Mn(II) ions of the complex. Index Abstract  An octa-coordinated Mn(II) complex which exhibits a distorted square antiprismatic coordination geometry has been achieved by using a bisbidentate Schiff-base ligand.      

Synthesis and Structure of Di-μ-oxo-bistripyrazolylborato Dioxo Vanadium (V) Complex with Lattice of Diacetonitrile

Abstract A novel oxovanadium complex was obtained by the reaction of VOSO₄ · 3H₂O with tripyrazolylborate sodium in MeOH. The complex (1) was characterized by element analysis, IR spectroscopy, ¹HNMR and its crystal for X-ray diffraction recrystallized from saturated CH₃CN solution. The compound crystallizes in the monoclinic, space group Pbca, with cell dimensions of a = 15.531(2) ?; b = 18.007(2) ?; c = 10.725(2) ?; V = 2,999.4(8) ?³ and D _calc = 1.533 g/cm³ for Z = 4. The structure was solved by direct methods and refined to an R-value of 0.0401. Structure analysis show that it is a di-μ-oxo-bistripyrazolylborato dioxo vanadium (V) complex with lattice of diacetonitrile. In addition, the electronic structure and the bonding characters of the complex were analyzed with ab initio calculations. Index Abstract 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 New Mo(V) Complex of Cyano Ligands

Abstract  A new complex, [H₃teta][Mo(CN)₈] · H₂O, (teta = 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetra-azacyocloteradeca-4,11-diene), has been synthesized and characterized by IR spectrum, element analysis and single crystal X-ray diffraction: monoclinic, space group P2(1)/c with a = 10.8553(8) ?, b = 12.4854(8) ?, c = 22.6348(15) ?, α = 90.00°, β = 97.3080(10)°, γ = 90.00°, Mr = 609.63, v = 3042.8(4), Z = 4. There are one [H₃teta]³⁺, one [Mo(CN)₈]³⁻ and one water molecule in the asymmetric unit. The complex is interconnected through hydrogen bond and formed into a 3D porous network. Graphical Abstract  A new complex, [H₃teta][Mo(CN)₈] · H₂O, has been synthesized and characterized by IR spectrum, element analysis and single crystal X-ray diffraction. And it shows a 3D porous network through hydrogen bonds.      

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.