One-pot concomitant preparation of two copper(II) coordination polymers with different configurations of bridging bithiophene ligands

2020 ◽  
Vol 76 (1) ◽  
pp. 37-43
Author(s):  
Zhi-Qiang Shi ◽  
Ning-Ning Ji ◽  
Hai-Liang Hu
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Three Dimensional ◽  
Chain Structure ◽  
X Ray Diffraction ◽  
Compound I ◽  
One Pot ◽  
X Ray ◽  
Vis Spectroscopy

By employing the conjugated bithiophene ligand 5,5′-bis(1H-imidazol-1-yl)-2,2′-bithiophene (bibp), which can exhibit trans and cis conformations, two different CuII coordination polymers, namely, poly[[μ-5,5′-bis(1H-imidazol-1-yl)-2,2′-bithiophene-κ2 N:N′](μ2-4,4′-oxydibenzoato-κ2 O:O′)copper(II)], [Cu(C14H8O5)(C14H10N4S2)] n or [Cu(bibp)(oba)] n , (I), and catena-poly[μ-aqua-bis[μ-5,5′-bis(1H-imidazol-1-yl)-2,2′-bithiophene-κ2 N:N′]bis(μ3-4,4′-oxydibenzoato)-κ3 O:O′:O′′;κ4 O:O′,O′′:O′-dicopper(II)], [Cu2(C14H8O5)2(C14H10N4S2)(H2O)] n or [Cu2(bibp)(oba)2(H2O)] n , (II), have been prepared through one-pot concomitant crystallization and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis, powder X-ray diffraction (PXRD) and thermogravimetric (TG) analysis. Single-crystal X-ray diffraction indicates that the most interesting aspect of the structure is the existence of sole trans and cis conformations of the bibp ligand in a single net of (I) and (II), respectively. Compound (I) displays a threefold interpenetrating three-dimensional framework with a 4-connected {65.8} cds topology, whereas (II) features a one-dimensional chain structure. In the crystal of (II), the polymeric chains are further extended through C—H...O hydrogen bonds and C—H...π interactions into a three-dimensional supramolecular architecture. In addition, strong intramolecular O—H...O hydrogen bonds formed between the bridging water molecules and the carboxylate O atoms improve the stability of the framework of (II). Furthermore, solid-state UV–Vis spectroscopy experiments show that compounds (I) and (II) exhibit optical band gaps which are characteristic for optical semiconductors, with values of 2.70 and 2.26 eV, respectively.

Two new CdII MOFs of 1,4-bis(1H-benzimidazol-1-yl)butane and flexible dicarboxylate ligands: luminescence sensing towards Fe3+

2020 ◽  
Vol 76 (11) ◽  
pp. 1024-1033
Author(s):  
Fang-Hua Zhao ◽  
Shi-Yao Li ◽  
Wen-Yu Guo ◽  
Zi-Hao Zhao ◽  
Xiao-Wen Guo ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Layer Structure ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy

Two new CdII MOFs, namely, two-dimensional (2D) poly[[[μ2-1,4-bis(1H-benzimidazol-1-yl)butane](μ2-heptanedioato)cadmium(II)] tetrahydrate], {[Cd(C7H10O4)(C18H18N4)]·4H2O} n or {[Cd(Pim)(bbimb)]·4H2O} n (1), and 2D poly[diaqua[μ2-1,4-bis(1H-benzimidazol-1-yl)butane](μ4-decanedioato)(μ2-decanedioato)dicadmium(II)], [Cd2(C10H16O4)2(C18H18N4)(H2O)2] n or [Cd(Seb)(bbimb)0.5(H2O)] n (2), have been synthesized hydrothermally based on the 1,4-bis(1H-benzimidazol-1-yl)butane (bbimb) and pimelate (Pim2−, heptanedioate) or sebacate (Seb2−, decanedioate) ligands. Both MOFs were structurally characterized by single-crystal X-ray diffraction. In 1, the CdII centres are connected by bbimb and Pim2− ligands to generate a 2D sql layer structure with an octameric (H2O)8 water cluster. The 2D layers are further connected by O—H...O hydrogen bonds, resulting in a three-dimensional (3D) supramolecular structure. In 2, the CdII centres are coordinated by Seb2− ligands to form binuclear Cd2 units which are linked by bbimb and Seb2− ligands into a 2D hxl layer. The 2D layers are further connected by O—H...O hydrogen bonds, leading to an 8-connected 3D hex supramolecular network. IR and UV–Vis spectroscopy, thermogravimetric analysis and solid-state photoluminescence analysis were carried out on both MOFs. Luminescence sensing experiments reveal that both MOFs have good selective sensing towards Fe3+ in aqueous solution.

Synthesis and Characterization of the nido-Platinaborane 7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me

2011 ◽  
Vol 66 (4) ◽  
pp. 387-391
Author(s):  
Jinling Miao ◽  
Yong Nie ◽  
Haiyan Chen ◽  
Daqi Wang ◽  
Markus Enders ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Chain Structure ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ir And Nmr Spectroscopy

The reaction of closo-B10H102− with PtCl2(PPh3)2 in the presence of MeCOSH afforded the title platinaborane nido-7,7-(PPh3)2-7-PtB10H11-11-OC(O)Me (1), which has been characterized by IR and NMR spectroscopy, MS, elemental analysis, and single-crystal X-ray diffraction. In contrast to the known products having exo-polyhedral Pt-S-C-O-B ring(s) from the same reaction with Ph- COSH, compound 1 has a B-acetoxy group on the open PtB4 face of the nido-PtB10 cluster. The structure of 1 features both intramolecular/intermolecular C-H· · ·O hydrogen bonds and intramolecular C-H· · ·H-B dihydrogen bonds, which link the molecules into a 1-D chain structure.

Synthesis, crystal structures and magnetic characterisation of two 2p–3d metallic coordination polymers

2017 ◽  
Vol 41 (6) ◽  
pp. 365-369 ◽  
Author(s):  
Chongchong Xue ◽  
Jingwen Shi ◽  
Daopeng Zhang
Keyword(s):  
Magnetic Susceptibility ◽  
Coordination Polymers ◽  
Supramolecular Structure ◽  
Three Dimensional ◽  
Building Blocks ◽  
Chain Structure ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Dimensional Network

The coordination polymers {Mg[Fe(L)(CN)5]}n·0.5nH2O and {MgCu2(CH3COO)6}n [L = bis( N-imidazolyl)methane] have been synthesised. X-ray diffraction revealed that {Mg[Fe(L)(CN)5]}n·0.5nH2O has a one-dimensional neutral chain structure consisting of alternating [Mg(L)2(H2O)2)]2+ species and [Fe(L)(CN)5]2– building blocks, which can be further linked into a three-dimensional supramolecular structure by inter-chain p–p interactions. {MgCu2(CH3COO)6}n has a three-dimensional network with the [MgCu2(CH3COO)6] unit as neutral core extended by Mg–O bonds. Magnetic susceptibility studies on {MgCu2(CH3COO)6}n revealed antiferromagnetic interactions between adjacent Cu(II) ions.

Two novel alkaline earth coordination polymers constructed from cinnamic acid and 1,10-phenanthroline: synthesis and structural and thermal properties

2018 ◽  
Vol 74 (2) ◽  
pp. 240-247 ◽  
Author(s):  
Nassima Bendjellal ◽  
Chahrazed Trifa ◽  
Sofiane Bouacida ◽  
Chaouki Boudaren ◽  
Mhamed Boudraa ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Coordination Polymers ◽  
Crystal Engineering ◽  
Alkaline Earth ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
X Ray ◽  
Carboxylate Groups ◽  
A Chain

In coordination chemistry and crystal engineering, many factors influence the construction of coordination polymers and the final frameworks depend greatly on the organic ligands used. The diverse coordination modes of N-donor ligands have been employed to assemble metal–organic frameworks. Carboxylic acid ligands can deprotonate completely or partially when bonding to metal ions and can also act as donors or acceptors of hydrogen bonds; they are thus good candidates for the construction of supramolecular architectures. We synthesized under reflux or hydrothermal conditions two new alkaline earth(II) complexes, namely poly[(1,10-phenanthroline-κ2N,N′)bis(μ-3-phenylprop-2-enoato-κ3O,O′:O)calcium(II)], [Ca(C10H7O2)2(C10H8N2)]n, (1), and poly[(1,10-phenanthroline-κ2N,N′)(μ3-3-phenylprop-2-enoato-κ4O:O,O′:O′)(μ-3-phenylprop-2-enoato-κ3O,O′:O)barium(II)], [Ba(C10H7O2)2(C10H8N2)]n, (2), and characterized them by FT–IR and UV–Vis spectroscopies, thermogravimetric analysis (TGA) and single-crystal X-ray diffraction analysis, as well as by powder X-ray diffraction (PXRD) analysis. Complex (1) features a chain topology of type 2,4 C4, where the Ca atoms are connected by O and N atoms, forming a distorted bicapped trigonal prismatic geometry. Complex (2) displays chains of topology type 2,3,5 C4, where the Ba atom is nine-coordinated by seven O atoms of bridging/chelating carboxylate groups from two cinnamate ligands and by two N atoms from one phenanthroline ligand, forming a distorted tricapped prismatic arrangement. Weak C—H...O hydrogen bonds and π–π stacking interactions between phenanthroline ligands are responsible to the formation of a supramolecular three-dimensional network. The thermal decompositions of (1) and (2) in the temperature range 297–1173 K revealed that they both decompose in three steps and transform to the corresponding metal oxide.

Synthesis and structural characterization of two coordination polymers constructed by bis(4-(1H-imidazol-1-yl)phenyl)methanone and 5-(tert-butyl)isophthalate ligands

2019 ◽  
Vol 74 (3) ◽  
pp. 261-265 ◽  
Author(s):  
Gao-Feng Wang ◽  
Shu-Wen Sun ◽  
Wei-Bing Wang ◽  
Hong Sun ◽  
Shao-Fei Song
Keyword(s):  
Single Crystal ◽  
Coordination Polymers ◽  
Weak Interactions ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Elemental Analyses ◽  
Solvothermal Methods

AbstractTwo coordination polymers, {[Co(bipmo)(tbip)]·3H2O}n (1) and {[Cd(bipmo)(tbip)]·3H2O}n (2) (bipmo=bis(4-(1H-imidazol-1-yl)phenyl)methanone, H2tbip=5-tert-butylisophthalic acid), were synthesized by solvothermal methods and structurally characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. The results from single-crystal X-ray diffraction data indicate that the solid state structures of 1 and 2 consist of metal-aromatic carboxylate layers, which are pillared by weak interactions to generate a three-dimensional network. The topological structures of 1 and 2 are uninodal nets based on 3-connected nodes with the Schläfli symbol of {63}.

scholarly journals One-Pot Synthesis, X-ray Single Crystal and Molecular Insight of Enaminone-Based β-Morpholino-/N-Methylpiperazinyl-/Pyrrolidinylpropiophenone

Crystals ◽  
2020 ◽  
Vol 10 (4) ◽  
pp. 282
Author(s):  
Assem Barakat ◽  
Saied M. Soliman ◽  
Matti Haukka ◽  
Abdullah Mohammed Al-Majid ◽  
Mohammad Shahidul Islam ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Spectroscopic Properties ◽  
Secondary Amines ◽  
Dft Studies ◽  
X Ray Diffraction ◽  
One Pot ◽  
X Ray ◽  
One Pot Synthesis ◽  
Hirshfeld Analysis

One-pot synthesis of three enaminones, (E)-1-(4-chlorophenyl)-3-morpholinoprop-2-en-1-one 1, (E)-1-(4-chlorophenyl)-3-(4-methylpiperazin-1-yl)prop-2-en-1-one 2, and (E)-1-(4-chlorophenyl)-3-(pyrrolidin-1-yl)prop-2-en-1-one 3 were achieved. The synthetic protocol via three components reaction of p-chloroacetophenone with DMFDMA (N,N-dimethylformamid-dimethylacetal) and the corresponding secondary amines (morpholine/N-methylpiperazine/pyrrolidine) in dioxane under heating for 2.5–4 h at 102 °C yielded the requisite enaminones. This protocol has the advantage of no separation of intermediate, no need for column purification with quantitative yield for the target compounds. The chemical features of the β-enaminones 1–3 were assigned by NMR. β-Enaminones 1, and 2 were assigned by single crystal X-ray diffraction technique. The intermolecular interactions in the crystal structures were analyzed quantitatively using Hirshfeld analysis. The Cl…H and O…H hydrogen bonds are common in both compounds while the C-H…π and N…H contacts are more significant in 2 than 1. DFT studies were investigated to show the electronic and spectroscopic properties (NMR and UV-Vis) of the studied systems.

The Crystal Structure of Potassium Hydrogeniodate (V), KIO3•HIO3

1972 ◽  
Vol 50 (8) ◽  
pp. 1134-1143 ◽  
Author(s):  
G. Kemper ◽  
Aafje Vos ◽  
H. M. Rietveld
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Powder Diffraction ◽  
Qualitative Agreement ◽  
Three Dimensional ◽  
Neutron Powder Diffraction ◽  
X Ray Diffraction ◽  
Good Qualitative Agreement ◽  
X Ray

The crystal structure of KIO3•HIO3 has been determined by three-dimensional single crystal X-ray diffraction and by neutron powder diffraction. The crystallographic data are a = 7.025(2), b = 8.206(2), c = 21.839(5) Å, β = 97.98(2)°, space group P21/c, Z = 8 units KIO3•HIO3. The residual [Formula: see text] was 0.048 for 7516 independent X-ray reflections measured on a three-circle diffractometer with Zr-filtered Mo radiation. The results of the present study show good qualitative agreement with the structure recently determined by Chan and Einstein (7). The HIO3 and [Formula: see text] groups are pyramidal, the I—O(H) bonds vary from 1.898 to 1.939(4) Å and the I—O bonds from 1.786 to 1.827(4) Å, these lengths are not corrected for the effects of thermal motion. Strong O—I … O interactions and electrostatic attractions between K+ and Oδ− give slabs of thickness [Formula: see text] The slabs are connected by hydrogen bonds of 2.710 and 2.694 Å.

Syntheses, Structures and Photoluminescent Properties of the Two Novel Coordination Polymers [Cd(pydc)2(tu)]n and [Cd2(SO4)(nic)2(tu)1.5(H2O)2]n (pydc = Pyridine-2,3-dicarboxylate, nic = Nicotinate, tu = Thiourea)

2011 ◽  
Vol 66 (5) ◽  
pp. 459-464 ◽  
Author(s):  
Chao Xu ◽  
Sheng-Bo Liu ◽  
Taike Duan ◽  
Qun Chen ◽  
Qian-Feng Zhang
Keyword(s):  
Hydrogen Bonds ◽  
Coordination Polymers ◽  
Room Temperature ◽  
Three Dimensional ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
One Dimensional ◽  
X Ray ◽  
Dimensional Network

Two novel cadmium coordination polymers, [Cd(pydc)2(tu)]n (1) and [Cd2(SO4)(nic)2(tu)1.5 - (H2O)2]n (2) (pydc = pyridine-2,3-dicarboxylate, nic = nicotinate, tu = thiourea), have been synthesized under hydrothermal conditions and structurally characterized by X-ray diffraction analysis. 1 is a one-dimensional ladder coordination polymer in a two-dimensional network formed by hydrogen bonds. 2 consists of two kinds of Cd(II) centers in different coordination environments connected via nicotinate and sulfate to form a two-dimensional grid network integrated in a three-dimensional framework generated by hydrogen bonds. 2 shows intense fluorescent emission in the solid state at room temperature

A new CdII coordination polymer with a self-penetrating architecture induced by the molecular conformation of a rigid bithiophene ligand

2018 ◽  
Vol 74 (2) ◽  
pp. 218-223 ◽  
Author(s):  
Ning-Ning Ji ◽  
Zhi-Qiang Shi ◽  
Hai-Liang Hu
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
Coordination Polymers ◽  
Molecular Conformation ◽  
Topological Analysis ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Design And Synthesis ◽  
Mixed Ligands

The design and synthesis of coordination polymers with a self-penetrating architecture has attracted much interest not only due to their interesting structures but also due to their potential applications. 5,5′-Bis(pyridin-4-yl)-2,2′-bithiophene (bpbp), as a conjugated bithiophene ligand, can exhibit trans and cis conformations and this can lead to the construction of a self-penetrating architecture. In addition, the semi-rigid ancillary ligand 4,4′-oxybis(benzoic acid) (H2oba) can adopt different coordination modes, resulting in coordination polymers with high-dimensional skeletons. A new CdII coordination polymer based on mixed ligands, namely poly[diaquapentakis[μ-5,5′-bis(pyridin-4-yl)-2,2′-bithiophene-κ2 N:N′]bis(nitrato-κ2 O,O′)tetrakis(μ3-4,4′-oxydibenzoato)-κ10 O:O,O′:O′′,O′′′;κ6 O:O′:O′′-pentacadmium(II)], [Cd5(C14H14O5)4(NO3)2(C18H12N2S2)5(H2O)2] n , (I), has been synthesized under solvothermal conditions and characterized by single-crystal X-ray diffraction, IR spectroscopy and elemental analysis. Single-crystal X-ray diffraction indicates that there are three crystallographically independent CdII cations, three bpbp ligands, two deprotonated oba2− ligands, one nitrate ligand and one coordinated water molecule in the asymmetric unit. One CdII centre is seven-coordinated, exhibiting a distorted {CdN2O5} pentagonal bipyramidal geometry, while the other two Cd centres are both six-coordinated, showing slightly distorted {CdN2O4} octahedral geometries. The most interesting feature is the co-existence of trans and cis conformations in a single net, allowing structural interpenetration via self-threading and yet the expected self-penetrating structure was obtained. Topological analysis shows that the whole three-dimensional framework can be classified as a 3-nodal (4,6,6)-c net with Schläfli symbol {613.82}2{66}, which is a new topology. Furthermore, the luminescence properties of (I) were examined in the solid state at room temperature.

scholarly journals Crystal structures ofN-[(4-phenylthiazol-2-yl)carbamothioyl]benzamide andN-{[4-(4-bromophenyl)thiazol-2-yl]carbamothioyl}benzamide from synchrotron X-ray diffraction

2016 ◽  
Vol 72 (9) ◽  
pp. 1343-1347 ◽  
Author(s):  
Ekaterina S. Gantimurova ◽  
Alexander S. Bunev ◽  
Kristina Yu. Talina ◽  
Gennady I. Ostapenko ◽  
Pavel V. Dorovatovskii ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Dihedral Angles ◽  
Active Pharmaceutical Ingredients ◽  
X Ray Diffraction ◽  
Compound I ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Phenyl Rings ◽  
Compound Ii

The title compounds, C17H13N3OS2, (I), and C17H12BrN3OS2, (II), are potential active pharmaceutical ingredients. Compound (I) comprises two almost planar fragments. The first is the central (carbamothioyl)amide (r.m.s. deviation = 0.038 Å), and the second consists of the thiazole and two phenyl rings (r.m.s. deviation = 0.053 Å). The dihedral angle between these planes is 15.17 (5)°. Unlike (I), compound (II) comprises three almost planar fragments. The first is the centralN-(thiazol-2-ylcarbamothioyl)amide (r.m.s. deviation = 0.084 Å), and the two others comprise the bromophenyl and phenyl substituents, respectively. The dihedral angles between the central and two terminal planar fragments are 21.58 (7) and 17.90 (9)°, respectively. Both (I) and (II) feature an intramolecular N—H...O hydrogen bond, which closes anS(6) ring. In the crystal of (I), molecules form hydrogen-bonded layers parallel to (100) mediated by N—H...S and C—H...O hydrogen bonds. In the crystal of (II), molecules form a three-dimensional framework mediated by N—H...Br and C—H...O hydrogen bonds, as well as secondary S...Br [3.3507 (11) Å] and S...S [3.4343 (14) Å] interactions.

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