A simple synthetic route to the formation of tetracopper(I) 2-mercaptothiazoline compounds — The crystal structures of [Cu4(S-thiaz)4(PEt2Ph)2], [Cu4(S-thiaz)4(PEt3)2], [Cu4(S-thiaz)4]2, and [Cu4(S-thiaz)4]4

2006 ◽  
Vol 84 (2) ◽  
pp. 251-256 ◽  
Author(s):  
Olaf Fuhr ◽  
Lucia Fernandez-Recio ◽  
Dieter Fenske
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Copper Complexes ◽  
Synthetic Route ◽  
Reaction Conditions ◽  
One Dimensional ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Oligomeric Compounds

Reactions of copper(I) acetate with 2-mercaptothiazoline (HS-thiaz) in the presence of tertiary phosphines lead to the formation of tetranuclear sulphur-bridged copper complexes. Depending on the reaction conditions, isolated clusters ([Cu4(S-thiaz)4(PR3)2] (PR3 = PPh3 (1), PEt2Ph (2), PEt3 (3)), oligomeric compounds ([Cu4(S-thiaz)4]2 (4) and [Cu4(S-thiaz)4]4 (5)), or a one-dimensional polymer ([Cu4(S-thiaz)4]∞ (6)) are formed. The structures of the compounds 2–5 have been determined by single crystal X-ray analysis.Key words: copper, 2-mercaptothiazoline, single crystal X-ray analysis.

Comparative Structural Studies on Three-Coordinate Copper(I) Halide Complexes With Tertiary Phosphines. Crystal Structures of [(PPh2Mes)CuX]2 and [(PPhMes2)CuX]2 (Mes = Mesityl X = Cl, Br, I)

1992 ◽  
Vol 45 (7) ◽  
pp. 1155 ◽  
Author(s):  
GA Bowmaker ◽  
D Camp ◽  
RD Hart ◽  
PC Healy ◽  
BW Skelton ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Copper Atom ◽  
Structural Studies ◽  
Coordination Environment ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Structure Determinations ◽  
Halide Complexes ◽  
The Subject

The 1 : 1 complexes of the substituted triphenylphosphine ligands mesityldiphenylphosphine and dimesitylphenylphosphine with copper(1) chloride, bromide and iodide have been the subject of single-crystal X-ray structure determinations at 295 K. All six complexes crystallize as air-stable dimeric molecules, [(PPh2Mes)CuX]2 and [ (PPhMes2)CUX]2 with each copper atom in a distorted trigonal PCuX2. coordination environment. Crystals of [(PPh2Mes)CuCl]2 (1) are monoclinic, P21/n, a 9.961(3), b 18.687(6), c 11.009(7) Ǻ, β 114.63(4)°; R was 0.049 for 2450 'observed' reflections. [(PPh2Mes)CuBrI2 (2) is monoclinic, P21/n, a 9.939(2), b 18.832(6), c 11.238(6) Ǻ, β 115.36(3)°; R was 0.046 for 1803 'observed' reflections. [(PPh2Mes)CuI]2.4/3 C6H6 (3) is rhornbohedral, R3, a 36.877(8), c 9.047(5) A; R was 0.039 for 2537 'observed' reflections. Crystals of [(PPhMes2)CuCl]2.2MeCN (4) are triclinic, Pi, a 15.783(7), b 9.570(4), c 8.914(4) Ǻ, α 72.43(3), β 76.37(3), γ 74.03(3)°; R was 0.045 for 3341 'observed' reflections. [(PPhMes2)CuBr]2.3C6H6 (5) is monoclinic, C2/c, a 9.694(6), b 30.15(2), c 20.66(2) Ǻ, β 98.00(7)°; R was 0.047 for 2117 'observed' reflections. [(PPhMes2)CuI]2.2MeCN (6) is orthorhombic, PP1nb, a 11.694(8), b 14.77(1), c 29.76(3) Ǻ; R was 0.049 for 3447 'observed' reflections. Cu-P bond lengths are: 2.196(2) A (1); 2.198(3) Ǻ (2); 2.222(5) and 2.226(5) Ǻ (3); 2.202(1) Ǻ (4); 2.197(3) A (5); 2.201(4) and 2.264(5) Ǻ (6). The geometries of the LCuX2 and CuX2Cu units are compared with data reported for other monomeric and dimeric compounds for both phosphorus- and nitrogen-based ligands L.

Sn94– Zintl Ions as Reactive Precursor for Neat Solids: Syntheses and Crystal Structures of Rb4[SnTe4], KxCs4–x[SnTe4], and KxCs10–x[Sn4Te12]

2009 ◽  
Vol 64 (11-12) ◽  
pp. 1319-1324 ◽  
Author(s):  
Jian-Qiang Wang ◽  
Viktor Hlukhyy ◽  
Thomas F. Fässler
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Compound K ◽  
Reaction Conditions ◽  
Elemental Tellurium ◽  
X Ray ◽  
Zintl Ions ◽  
Tetrahedral Anion

The reactions of Zintl ions Sn94− formed in ethylenediamine solutions of K2Cs2Sn9 and Rb4Sn9 with elemental tellurium have been investigated. Addition of elemental tellurium to the filtrates of these solutions leads - depending on the reaction conditions - to four different products: Compounds K0.36(1)Cs3.64(1)[SnTe4] (1) and Rb4[SnTe4] (2) contain the tetrahedral anion [SnTe4]4−, and Cs4[Sn2Te7] (3) features the anion [Te2Sn(μ-Te)(μ-Te2)SnTe2]4−, whereas a novel Zintl anion [Sn4Te12]10− is present in compound K0.44(1)Cs9.56(1)[Sn4Te12] (4). Compounds 1, 2 and 4 have been structurally characterized by single-crystal X-ray diffraction

Solvothermal Syntheses and Crystal Structures of New One-dimensional Selenogallates [bappH2][Ga2Se4] (bapp = 1,4-Bis-(3-aminopropyl)piperazine) and [Mn(en)3][Ga2Se5] (en = Ethylenediamine)

2011 ◽  
Vol 66 (9) ◽  
pp. 877-881
Author(s):  
Chao Xu ◽  
Jing-Jing Zhang ◽  
Taike Duan ◽  
Qun Chen ◽  
Qian-Feng Zhang
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Solvothermal Syntheses ◽  
Polymeric Chains ◽  
Amine Complex ◽  
Solvothermal Conditions ◽  
Metal Amine

Two new selenogallates, [bappH2][Ga2Se4] (1) (bapp = 1,4-bis(3-aminopropyl)-piperazine) and [Mn(en)3][Ga2Se5] (2) (en = ethylenediamine), have been synthesized under solvothermal conditions and structurally characterized by single-crystal X-ray diffraction. Compounds 1 and 2 contain one-dimensional polymeric chains {[Ga2Se4]2−}∞ and {[Ga2Se5]2−}∞, respectively. The negative charges of the polymeric chains are balanced by a protonated 1,4-bis(3-aminopropyl)piperazine cation in 1 and by the metal-amine complex cations [Mn(en)3]2+ in 2. TGA analyses have shown that compound 2 is thermally more stable than compound 1.

Nitrato and Acetylacetonato Complexes of Copper(I)

1971 ◽  
Vol 49 (5) ◽  
pp. 761-766 ◽  
Author(s):  
W. A. Anderson ◽  
A. J. Carty ◽  
G. J. Palenik ◽  
G. Schreiber
Keyword(s):  
Single Crystal ◽  
Infrared Spectra ◽  
Heavy Atom ◽  
Monoclinic Space Group ◽  
Synthetic Route ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Heavy Atom Method ◽  
Nitrate Complexes

Copper(I) nitrate complexes of the types L2CuNO3, L3CuNO3, and L4CuNO3 (L = tertiary phosphine) have been synthesized by reduction of copper(II) nitrate with tertiary phosphines. Infrared spectra and single crystal X-ray measurements indicate the presence of bidentate nitrate in L2CuNO3, monodentate nitrate in L3CuNO3, and ionic nitrate in L4CuNO3.The single crystal X-ray structure of nitratobis (tricyclohexylphosphine)copper(I) is reported. CuO3N(PC18H33)2 crystallizes in the monoclinic space group C2/c with a = 18.18(1) Å, b = 9.240(6) Å, c = 22.41(2) Å, and β = 96.57(5)°. The structure was solved by the heavy atom method and refined with isotropic thermal parameters to an R of 0.14. The copper atom is tetrahedrally coordinated by two phosphorus atoms and two oxygen atoms of a bidentate nitrate group. The P—Cu—P angle (140(1)°) and Cu—P bond lengths (2.29(1) Å) are the largest reported for tetrahedral copper complexes.A facile synthetic route to acetylacetonatobis(phosphine)copper(I) complexes is also described.

scholarly journals A New Family of Homoleptic Copper Complexes of Curcuminoids: Synthesis, Characterization and Biological Properties

Molecules ◽  
2019 ◽  
Vol 24 (5) ◽  
pp. 910 ◽  
Author(s):  
William Meza-Morales ◽  
Juan Machado-Rodriguez ◽  
Yair Alvarez-Ricardo ◽  
Marco Obregón-Mendoza ◽  
Antonio Nieto-Camacho ◽  
...  
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Copper Complexes ◽  
Biological Properties ◽  
Planar Geometry ◽  
X Ray Diffraction ◽  
Paramagnetic Resonance ◽  
X Ray ◽  
New Family ◽  
Homoleptic Complex

We report herein the synthesis and crystal structures of five new homoleptic copper complexes of curcuminoids. The scarcity of reports of homoleptic complex structures of curcuminoids is attributed to the lack of crystallinity of such derivatives, and therefore, their characterization by single crystal X-ray diffraction is rare. The ligand design suppressing the phenolic interaction by esterification or etherification has afforded a significant increase in the number of known crystal structures of homoleptic metal complexes of curcuminoids revealing more favorable crystallinity. The crystal structures of the present new copper complexes show four-fold coordination with a square planar geometry. Two polymorphs were found for DiBncOC-Cu when crystallized from DMF. The characterization of these new complexes was carried out using infrared radiation (IR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR), and single crystal X-ray diffraction (SCXRD) and the antioxidant and cytotoxic activity of the obtained complexes was evaluated.

scholarly journals 6-Bromo-2’-(2-chlorobenzylidene)nicotinohydrazide and 6-Bromo-2’-(3-bromo-5-chloro-2-hydroxybenzylidene) nicotinohydrazide Methanol Solvate: Synthesis, Characterization, Crystal Structures and Antimicrobial Activities

2021 ◽  
Vol 68 (1) ◽  
pp. 65-71
Author(s):  
Hai-Yun Zhu
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Crystal Structures ◽  
Antibacterial Agents ◽  
Spectroscopic Method ◽  
Antimicrobial Activities ◽  
One Dimensional ◽  
X Ray ◽  
Axis Direction

Two newly synthesized nicotinohydrazones, 6-bromo-2’-(2-chlorobenzylidene)nicotinohydrazide (1) and 6-bromo-2’-(3-bromo-5-chloro-2-hydroxybenzylidene)nicotinohydrazide methanol solvate (2), have been obtained and structurally characterized by spectroscopic method and single crystal X-ray determination. The molecules in both compounds are in E configuration regarding to the azomethine groups. The molecules of compound 1 are linked via hydrogen bonds of N−H∙∙∙O, generating one dimensional chains running along the c-axis direction. The hydrazone molecules of compound 2 are linked by methanol molecules via hydrogen bonds of N−H∙∙∙O and O−H∙∙∙N, generating dimers. The in vitro antimicrobial activities of these compounds indicate that they are interesting antibacterial agents.

Anion influences on the structures of pyridyl-iminosulfonate copper(II) complexes and their reactivity in Chan–Lam couplings

2020 ◽  
Vol 98 (9) ◽  
pp. 502-510
Author(s):  
Valérie Hardouin Duparc ◽  
Alexandre Thouvenin ◽  
Frank Schaper
Keyword(s):  
Single Crystal ◽  
Coordination Polymers ◽  
Copper Complexes ◽  
Phenylboronic Acid ◽  
X Ray Diffraction ◽  
Copper Salts ◽  
One Dimensional ◽  
X Ray ◽  
Dimeric Complexes ◽  
Orthanilic Acid

Reaction of pyridylcarbaldehyde with taurine or orthanilic acid in the presence of copper salts provided copper complexes (PyC(H)N-CxHy-SO3)CuX with X = chloride, nitrate, acetate, or triflate and CxHy = o-C6H4 or C2H4. All complexes were characterized by single crystal X-ray diffraction and formed either mononuclear water adducts, dimeric complexes, or one-dimensional coordination polymers. Activities in the Chan–Lam coupling of aniline with phenylboronic acid varied by less than a factor of two between catalysts with various anions, supporting previous mechanistic claims that the anion does not participate in the formation of copper–boron intermediates. There is no difference in the performance of a catalyst with an alkyl backbone, indicating that sulfonate dissociation is not part of the catalytic cycle.

Crystal structures of (S)- and (R,S)-2,2′-bipyridine-3,3′-dicarboxylic acid 1,1′-dioxides and of their barium salts: absolute configuration and molecular distortion enforced by supramolecular self-assembly

1997 ◽  
Vol 212 (3) ◽  
Author(s):  
P. Vojtíšek ◽  
I. Císařová ◽  
J. Podlaha ◽  
Z. Žák ◽  
S. Böhm ◽  
...  
Keyword(s):  
Single Crystal ◽  
Dicarboxylic Acid ◽  
Crystal Structures ◽  
Absolute Configuration ◽  
Self Assembly ◽  
Barium Salt ◽  
X Ray Diffraction ◽  
X Ray

AbstractCrystal structures of the title compounds were determined by single crystal X-ray diffraction. Absolute configuration of the barium salt of (+)-(

Die Kristallstrukturen der isotypen Verbindungen Ba3[MoN4] und Ba3[WN4] / The Crystal Structures of the Isotypic Compounds Ba3[MoN4] and Ba3[WN4]

1991 ◽  
Vol 46 (5) ◽  
pp. 566-572 ◽  
Author(s):  
Axel Gudat ◽  
Peter Höhn ◽  
Rüdiger Kniep ◽  
Albrecht Rabenau
Keyword(s):  
Transition Metals ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ternary Compounds ◽  
The Third

The isotypic ternary compounds Ba3[MoN4] and Ba3[WN4] were prepared by reaction of the transition metals with barium (Ba3N2, resp.) under nitrogen. The crystal structures were determined by single crystal X-ray diffraction: Ba3[MoN4] (Ba3[WN4]): Pbca; Z = 8; a = 1083.9(3) pm (1091.8(3) pm), b = 1030.3(3) pm (1037.5(3) pm), c = 1202.9(3) pm (1209.2(4) pm). The structures contain isolated tetrahedral anions [MN4]6- (M = Mo, W) which are arranged in form of slightly distorted hexagonal layers and which are stacked along [010] with the sequence (···AB···). Two of the three Ba atoms are situated between, the third one is placed within the layers of [MN4]-groups. In this way the structures can be derived from the Na3As structure type.

Synthesis, IR spectrum, thermal behaviour and crystal structure of a novel one-dimensional cyano-bridged zinc(II)/nickel(II) complex

2005 ◽  
Vol 220 (1) ◽  
Author(s):  
Ahmet Karadag ◽  
Hümeyra Pasaoglu ◽  
Gökhan Kastas ◽  
Orhan Büyükgüngör
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Coordination Polymer ◽  
Single Crystal ◽  
Ir Spectrum ◽  
Polymeric Chain ◽  
X Ray Diffraction ◽  
Bimetallic Complex ◽  
One Dimensional ◽  
X Ray

AbstractThe cyano-bridged heteronuclear coordination polymer of zinc(II)/nickel(II) has been prepared by N-(2-hydroxyethyl)-ethylendiamine (hydet-en), alternatively named 2-(2-aminoethylamino)-ethanol and characterised by IR and thermal analysis. In the bimetallic complex, the decomposition of hydet-en ligands is seen to be endothermic whereas that of the cyano ligands is found to be exothermic. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The crystal structure of the zinc(II)-nickel(II) complex consists of a one-dimensional polymeric chain –Zn(hydet-en)

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