scholarly journals Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal Characterization

Molecules ◽  
2019 ◽  
Vol 24 (22) ◽  
pp. 4059
Author(s):  
Iñigo PerezF ◽  
Edurne S. Larrea ◽  
Begoña Bazán ◽  
Gotzone Barandika ◽  
M. Karmele Urtiaga ◽  
...  
Keyword(s):  
Coordination Polymers ◽  
Three Dimensional ◽  
Thermal Characterization ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Space Group ◽  
Ionothermal Synthesis ◽  
3D Network ◽  
Pure Phase

Ionothermal synthesis is a little used method for the preparation of coordination polymers. By this method, two cadmium compounds were synthesized, 1, with formula Cd3(ox)F2(Ina)2 (Ina = isonicotinate) and 2, Cd(NO3)2(4,4′-Bpy) (4,4′-Bpy = 4,4′-Bipyridine). The modification of the reaction conditions has allowed to obtain 2 as a pure phase. The structure of both compounds was determined by a single-crystal X-ray diffraction. Compound 1 is isostructural to the previously reported Cd2Zn(ox)(OH)2(Ina)2. It crystallizes in the monoclinic space group P21/n and present a three-dimensional (3D) network, built-up from [Cd3(ox)F2]n2n+ layers, linked by isonicotinate ligands. Crystals of 2 are formed by twins of two components which are rotated ca. 180° to each other. This compound crystallizes in the triclinic P-1 space group and its structure can be describe as a two-dimensional (2D) 4 connected ‘sql’ net. The layers are composed by [Cd(NO3)2]n chains linked through 4,4′-Bpy ligands, and are pillared along the [011] direction. The thermal decomposition of 2 was studied by thermogravimetric and thermodiffractiometric techniques. The compound decomposes gradually starting from 160 °C, and due to heating, the structure suffers slight reversible changes in the bond distances and angles.

Synthesis, Structures and Properties of Two New Three-Dimensional Ce(III) Coordination Polymers with 2,2'-Bipyridine-4,4'-Dicarboxylic Acid

2013 ◽  
Vol 750-752 ◽  
pp. 1708-1711
Author(s):  
Rui Ping Zheng ◽  
Hui Yuan Chen ◽  
Jun Jie He ◽  
He Ping Zeng
Keyword(s):  
Dicarboxylic Acid ◽  
Coordination Polymers ◽  
Three Dimensional ◽  
Luminescent Properties ◽  
Dimethyl Formamide ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solvothermal Condition ◽  
Structures And Properties

Two new Ce(III) coordination polymers formulated as Ce(bpdc)(Hbpdc)(DMF)2 (1) and [Ce2(bpdc)3(DMF)2(H2O)4]·2DMF (2) (H2bpdc = 2,2'-bipyridine-4,4'-dicarboxylic acid, DMF = N,N-Dimethyl formamide) have been synthesized under solvothermal condition and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 2.2520(2), b = 1.17787(12), c = 1.16128(11) nm, α = 90, β = 95.5600(10), γ = 90°, V = 3.0658(5) nm3, Z = 4, Mr = 771.70, Dc = 1.672×10-9 g/cm3. Compound 2 crystallizes in triclinic, space group Pwith a = 1.00610(10), b = 1.17219(11), c = 1.36891(14) nm, α = 66.9340(10), β = 87.182(2), γ = 76.2570(10) °, V = 1.4411(2) nm3, Z = 1, Mr = 1371.25, Dc = 1.580×10-9 g/cm3. Both compounds exhibit 3D Ce(III)–organic frameworks. Furthermore, thermal stability and luminescent properties were also investigated. CCDC:(1)913670, (2)909563.

Two- and three-dimensional coordination polymers based on zinc(II) and furan-2,5-dicarboxylic acid: structure variation due to metal-to-linker ratio

2018 ◽  
Vol 74 (12) ◽  
pp. 1719-1724 ◽  
Author(s):  
Yimin Mao ◽  
Peter Y. Zavalij
Keyword(s):  
Dicarboxylic Acid ◽  
Coordination Polymers ◽  
Three Dimensional ◽  
Molar Ratio ◽  
Monoclinic Space Group ◽  
Structure Variation ◽  
Space Group ◽  
Hydrogen Bonding Pattern ◽  
Solvent Molecules ◽  
A Chain

Two ZnII-based coordination polymers (CPs) were synthesized by the hydrothermal method, using Zn(NO3)2·6H2O and furan-2,5-dicarboxylic acid (FDCA) in dimethylformamide (DMF) solvent, at 95 °C. Poly[tetrakis(dimethylazanium) [tetrakis(μ2-furan-2,5-dicarboxylato-κ2 O 2:O 5)dizinc(II)]], {(C2H8N)4[Zn2(C6H2O5)4]} n or {[DMA]4[ZnII 2(FDC)4]} n (DMA = dimethylazanium and FDC = furan-2,5-dicarboxylate), (1), was obtained with a 1:1 molar ratio of ZnII and FDCA. It crystallized in the monoclinic space group C2/c. Coordinated by ZnII ions, FDC2− ligands form 21 double-stranded helices propagating along the b axis. The helices are interconnected and extend laterally in the a direction, forming a two-dimensional (2D) sheet-like network. The 2D sheets are stacked along the c direction without interconnections. DMA cations are cocrystallized in (1) and are hydrogen bonded with carboxylate O atoms of the FDC2− ligands. The hydrogen-bonding pattern consists of R 2 2(4) and R 2 2(10) motifs alternating in a chain. Poly[bis(dimethylazanium) [bis(μ4-furan-2,5-dicarboxylato-κO 2:κO 2′:κO 5:κO 5)bis(μ3-furan-2,5-dicarboxylato-κO 2:κO 2′:κO 5)dizinc(II)] dimethylformamide 3.08-solvate], {(C2H8N)2[Zn2(C6H2O5)4]·3.08C3H7NO} n or {[DMA]2[ZnII 3(FDC)4]·3.08DMF} n , (2), was obtained with a 1:2 molar ratio of ZnII and FDCA. It crystallized in the monoclinic space group P21/c, forming a three-dimensional network. The pores are filled with DMA cations and DMF solvent molecules.

Two CoII coordination polymers of biphenyl-2,2′,5,5′-tetracarboxylic acid with flexible N-donor ligands: syntheses, structures and magnetic properties

2019 ◽  
Vol 75 (8) ◽  
pp. 1073-1083 ◽  
Author(s):  
Feng Su ◽  
Cheng-Yong Zhou ◽  
Lin-Tao Wu ◽  
Xi Wu ◽  
Jing Su ◽  
...  
Keyword(s):  
Coordination Polymers ◽  
Three Dimensional ◽  
Donor Ligands ◽  
Tetracarboxylic Acid ◽  
X Ray Diffraction ◽  
Magnetic Studies ◽  
Orbital Contribution ◽  
X Ray ◽  
3D Network ◽  
Methyl Benzene

Two CoII-based coordination polymers, namely poly[(μ4-biphenyl-2,2′,5,5′-tetracarboxylato){μ2-1,3-bis[(1H-imidazol-1-yl)methyl]benzene}dicobalt(II)], [Co2(C16H6O8)(C14H14N4)2] n or [Co2(o,m-bpta)(1,3-bimb)2] n (I), and poly[[aqua(μ4-biphenyl-2,2′,5,5′-tetracarboxylato){1,4-bis[(1H-imidazol-1-yl)methyl]benzene}dicobalt(II)] dihydrate], {[Co2(C16H6O8)(C14H14N4)2(H2O)2]·4H2O} n or {[Co2(o,m-bpta)(1,4-bimb)2(H2O)2]·4H2O} n (II), were synthesized from a mixture of biphenyl-2,2′,5,5′-tetracarboxylic acid, i.e. [H4(o,m-bpta)], CoCl2·6H2O and N-donor ligands under solvothermal conditions. The complexes were characterized by IR spectroscopy, elemental analysis, single-crystal X-ray diffraction and powder X-ray diffraction analysis. The bridging (o,m-bpta)4− ligands combine with CoII ions in different μ4-coordination modes, leading to the formation of one-dimensional chains. The central CoII atoms display tetrahedral [CoN2O2] and octahedral [CoN2O4] geometries in I and II, respectively. The bis[(1H-imidazol-1-yl)methyl]benzene (bimb) ligands adopt trans or cis conformations to connect CoII ions, thus forming two three-dimensional (3D) networks. Complex I shows a (2,4)-connected 3D network with left- and right-handed helical chains constructed by (o,m-bpta)4− ligands. Complex II is a (4,4)-connected 3D novel network with ribbon-like chains formed by (o,m-bpta)4− linkers. Magnetic studies indicate an orbital contribution to the magnetic moment of I and II due to the longer Co...Co distances. An attempt has been made to fit the χM T results to the magnetic formulae for mononuclear CoII complexes, the fitting indicating the presence of weak antiferromagnetic interactions between the CoII ions.

Dinuclear cobalt and nickel complexes of a mercaptoacetic acid substituted 1,2,4-triazole ligand: syntheses, structures and urease inhibitory studies

2019 ◽  
Vol 75 (12) ◽  
pp. 1658-1665 ◽  
Author(s):  
Zi-Yi Fang ◽  
Li Zhang ◽  
Jian-Ping Ma ◽  
Long Zhao ◽  
Shi-Ling Wang ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Mercaptoacetic Acid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
Hydrogen Bond Interactions ◽  
Triazole Ligand ◽  
Coordination Ability ◽  
Urease Inhibitory ◽  
Cobalt And Nickel

Because of its versatile coordination modes and strong coordination ability, the mercaptoacetic acid substituted 1,2,4-triazole 2-{[5-(pyridin-2-yl)-4H-1,2,4-triazol-3-yl]sulfanyl}acetic acid (H2L) was synthesized and characterized. Treatment of H2L with cobalt and nickel acetate afforded the dinuclear complexes {μ-3-[(carboxylatomethyl)sulfanyl]-5-(pyridin-2-yl)-4H-1,2,4-triazol-4-ido-κ2 N 1,N 5:N 2,O}bis[aqua(methanol-κO)cobalt(II)] methanol disolvate, [Co2(C9H6N4O2S)2(CH3OH)2(H2O)2]·2CH3OH (1), and {μ-3-[(carboxylatomethyl)sulfanyl]-5-(pyridin-2-yl)-4H-1,2,4-triazol-4-ido-κ2 N 1,N 5:N 2,O}bis[diaquanickel(II)] methanol disolvate dihydrate, [Ni2(C9H6N4O2S)2(H2O)4]·2CH3OH·2H2O (2), respectively. Complex 1 crystallized in the monoclinic space group P21/c, while 2 crystallized in the tetragonal space group I41/a. Single-crystal X-ray diffraction studies revealed that H2L is doubly deprotonated and acts as a tetradentate bridging ligand in complexes 1 and 2. For both of the obtained complexes, extensive hydrogen-bond interactions contribute to the formation of their three-dimensional supermolecular structures. Hirshfeld surface analysis was used to illustrate the intermolecular interactions. Additionally, the urease inhibitory activities of 1, 2 and H2L were investigated against jack bean urease, where the two complexes revealed strong urease inhibition activities.

THE CRYSTAL STRUCTURE OF K2TeBr6

1964 ◽  
Vol 42 (12) ◽  
pp. 2758-2767 ◽  
Author(s):  
I. D. Brown
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Least Squares ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Cubic Form ◽  
Efficient Packing

Crystals of K2TeBr6 are monoclinic, space group [Formula: see text] with a = 7.521, b = 7.574, and c = 10.730 Å; β = 89° 40′. Atomic positions have been found by three dimensional X-ray diffraction analysis (least squares R = 0.12). The crystals possess a K2PtCl6 structure which is distorted to allow a more efficient packing of the comparatively large anions than is possible with the undistorted cubic form. The stereochemistry of the octahedral TeBr6− ion (Te—Br = 2.71 Å) is discussed.

scholarly journals Two New Supramolecular Assemblies Obtained by Reaction Between Saccharin and Long-chain Diamines

2009 ◽  
Vol 64 (9) ◽  
pp. 1041-1045
Author(s):  
Eduardo E Castellano ◽  
Oscar E. Piro ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Three Dimensional ◽  
Supramolecular Assembly ◽  
Monoclinic Space Group ◽  
Ionic Crystals ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Anions And Cations ◽  
Bonding Characteristics

The crystal structures of heptamethylenediammonium bis(saccharinate) monohydrate, [H3N - (CH2)7 -NH3](sac)2・H2O (1) and octamethylenediammonium bis(saccharinate) hemihydrate, [H3N- (CH2)8-NH3](sac)2・0.5H2O (2), were determined by single-crystal X-ray diffraction methods. Compound 1 crystallizes in the triclinic space group P1̄ with 2 molecules per unit cell, and 2 in the monoclinic space group P21/a with Z = 4. The saccharinate moiety is planar in both compounds presenting bonding characteristics comparable to those found in other saccharinate salts. The ionic crystals are further stabilized by an extensive H-bonding network, which links the anions and cations into an infinite three-dimensional supramolecular assembly. The FTIR spectra of the adducts are briefly discussed in comparison with those of the constituent molecules.

A comparison of the molecular structures of Dicyclohexyl(N-phenylthiocarbamoyl)-phosphine and Diphenyl(N-phenylthiocarbamoy1)phosphine as determined by X-ray crystallography

1984 ◽  
Vol 37 (10) ◽  
pp. 1991 ◽  
Author(s):  
SW Cowan ◽  
BF Hoskins ◽  
ERT Tiekink
Keyword(s):  
Three Dimensional ◽  
Unit Cell ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Conformational Effects

The crystal and molecular structures of the title compounds, (C6H11)2PC(S)N(H)C6H5(1) and (C6H5)2PC(S)N(H)C6H5(2) have been determined by single-crystal three-dimensional X-ray diffraction techniques. Crystals of (1) are monoclinic, space group P21/c, with eight molecules in the unit cell of dimensions a 20.541(4), b 17.784(2), c 10.2564(9) � and β 94.54(1)�; (2) crystallizes in the triclinic space group P1 with two molecules in the unit cell which has the dimensions a 9.242(2), b 9.994(3), c 10.373(3) �, α 68.56(2), β 71.21(2) and γ 86.00(2)�. Both structures were refined by a least-squares procedure, applying anisotropic thermal parameters to all non-hydrogen atoms, with the use of 3119 and 2971 statistically significant reflections for (1) and (2) respectively; final R 0.055 for (1) and R 0.061 (Rw 0.062) for (2). The N, C(l), S moieties of both (1) and (2) display features consistent with the delocalization of π-electrons. There are notable differences in some of the bond angles between (I) and (2) which have been attributed to conformational effects arising from variations in steric pressures; this may account for the observed differences in reactivity between the two compounds.

Crystal structure of 9-Oxofluorene-4-carboxylic acid

1981 ◽  
Vol 34 (5) ◽  
pp. 1143 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
GF Katekar
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
A Cell

The crystal structure of 9-oxofluorene-4-carboxylic acid has been determined by direct methods using three-dimensional X-ray diffraction data, and refined to R0·068 for 1323 'observed' reflections. Crystals are monoclinic, space group P21/c with 24 in a cell of dimensions a 3·843(3), b 7·986(5), c 3269(2) �, β 96·64(4)�. The molecules form centrosymmetric hydrogen-bonded cyclic dimers [O···O 2·642(3) �] with the plane of the carboxylic acid making an angle of 26·5� with that of the 9-oxofluorene group. Stacks of molecules form down the a axis with 3.843 �. separation.

A5Fe3O6] (A = Rb, Cs), Cs[FeO2] und Cs8[Fe2O7]: Neue Oxoferrate der schweren Alkalimetalle / A5Fe3O6] (A = Rb, Cs), Cs[FeO2] and Cs8[Fe2O7]: New Oxoferrates of the Heavy Alkaline Metals

2004 ◽  
Vol 59 (7) ◽  
pp. 771-781 ◽  
Author(s):  
Gero Frisch ◽  
Caroline Röhr
Keyword(s):  
Mixed Valence ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Alkaline Metals ◽  
Space Group ◽  
X Ray ◽  
Mixed Valence Compounds ◽  
The Ideal

The title compounds were synthesized at a temperature of 775 K via reaction of Fe2O3 with elemental cesium and rubidium alone or in combination with their hyperoxides AO2 where required by stoichiometry. The structures of the dark-red crystals have been determined by single crystal x-ray diffraction (Cs[FeO2]: cubic, space group Fd3m, a = 839.2(2) pm, Z = 8, R1 = 0.0547 and A5[Fe3O6] (A = Cs: orthorhombic, space group P212121, a = 861.8(2), b = 870.7(2), c = 1658.7(3) pm, Z = 4, R1 = 0.0617 and A = Rb: tetragonal, space group I4̅2d, a = 862.01(8), c= 1504.7(2) pm, Z =4, R1= 0.0334). These three compounds contain three-dimensional networks [FeO2], in the case of the ideal stuffed cristobalite composed of corner-sharing tetrahedra [FeO4/2], in the case of the new mixed valence compounds A5[Fe3O6] formed by corner-sharing of tetrahedra [FeIIIO4/2] and triangles [FeIIOO2/2] in a 1:2 ratio. The crystal structure of the cation rich compound Cs8[Fe2O7] (monoclinic, space group P21/c, a = 722.32(12), b = 1789.0(3), c = 733.88(12) pm, β =118.976(3)°, Z = 4, R1=0.0287) exhibits di-ferrate anions [Fe2O7]6− composed of two cornersharing [FeIIIO4] tetrahedra with a linear Fe-O-Fe bridge.

Wrap-around Encapsulated Cs(dibenzo-24-crown-8)+ Cations form Linear Coordination Polymers with Dicyanoargentate Anions Ag(CN)2-

1999 ◽  
Vol 54 (9) ◽  
pp. 1129-1132 ◽  
Author(s):  
Julia A. Rusanova ◽  
Philip J. Squattrito ◽  
Vera V. Ponomareva ◽  
Konstantin V. Domasevitch ◽  
Volodimir N. Kokozay
Keyword(s):  
Crown Ether ◽  
Coordination Polymers ◽  
Metal Cation ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Polymeric Structure ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Linear Coordination

The new macrocyclic dicyanoargentate complex Cs(dibenzo-24-crown-8)[Ag(CN)2] has been prepared and studied by means of X-ray diffraction (monoclinic, space group P21/a, with a = 12.730(3), b = 15.443(3), c = 15.323(3) Å, V = 3005(1) Å3, Z = 4, R1 = 0.041; wR2 = 0.048 for 5488 unique reflections with I > 3σ(I)). The lattice consists of complex Cs(db- 24-crown-8)+ cations (as an example of the “wrap-around” structure) and [Ag(CN)2]- anions forming a one-dimensional polymeric structure. The caesium atoms are coordinated with 8 oxygen atoms of the macrocycle and two nitrogen atoms of the dicyanoargentate groups, bonding to the cation on both sides of the crown-ether. It is the first structure of a dibenzo-24-crown-8 complex with a large metal cation such as Cs+.

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