Syntheses and Characterization of Two New Mixed-Ligand Bismuth(III) Complexes, Crystal Structure of [Bi(phen)2(NO3)(NCS)2(MeOH)]

2005 ◽  
Vol 60 (4) ◽  
pp. 389-392 ◽  
Author(s):  
Ali Morsali

Complexes [Bi(phen)2(NO3)(NCS)2(MeOH)] and [Bi(phen)2(NO3)2(NCS)] have been synthesized and characterized by their IR spectra and elemental analyses. The structure of the [Bi(phen)2(NO3)(NCS)2(MeOH)] complex has been confirmed by X-ray crystallography. The Bi atoms are unsymmetrically eight-coordinated, N6O2. The arrangement of the ligands does not show a gap in the coordination geometry around the Bi(III) ion, indicating that its lone pair of electrons is not active. The thiocyanate ligands are coordinated to the bismuth atom via the nitrogen atom. There is π-π stacking interactions between the parallel aromatic rings belonging to adjacent chains

2004 ◽  
Vol 59 (10) ◽  
pp. 1109-1113 ◽  
Author(s):  
Ali Reza Mahjoub ◽  
Ali Morsali ◽  
Ramin Ebrahim Nejad

AbstractThe 1:2 and 1:1 mixed-ligand mercury(II) complexes with 2,2’-bipyridine (bpy) containing two different anions, Hg(bpy)n(SCN)X (X= CH3COO−, NO3− and ClO4−), have been synthesized and characterized by elemental analysis, and IR, 1H and 13C NMR spectroscopy. The structure of [Hg(bpy)2(SCN)]NO3 was confirmed by X-ray crystallography. The complex is monomeric and the Hg atom has an unsymmetrical five-coordinate geometry, with four nitrogen atoms of two bpy ligands and one sulfur atom of the thiocyanate ligand as donor atoms. This is in contrast to lead(II) complexes, [Pb(phen)2(NO3)(NCS)], [Pb(phen)(O2CCH3)(NCS)] where the thiocyanate ligands are coordinated to the lead atom via the nitrogen atom. There is a π −π stacking interaction between the parallel aromatic rings.


2018 ◽  
Vol 73 (12) ◽  
pp. 999-1003 ◽  
Author(s):  
Mohammad Hakimi ◽  
Homeyra Rezaei ◽  
Keyvan Moeini ◽  
Heidar Raissi ◽  
Vaclav Eigner ◽  
...  

AbstractA new cyclotriphosphazene, 2,2,4,4,6,6-hexakis (o-tolylamono)-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinine (MPAP), was prepared using microwave irradiation and identified by elemental analysis, FT-IR, Raman, 31P NMR spectroscopy, and single-crystal X-ray diffraction. In the crystal, in addition to hydrogen bonds, the network is further stabilized by inter- and intramolecular π–π stacking interactions between aromatic rings.


1991 ◽  
Vol 46 (5) ◽  
pp. 687-692 ◽  
Author(s):  
Mohamed A. S. Goher ◽  
Franz A. Mautner

Two 1:1 mixed ligand complexes of copper(II) azide with substituted quinoline and pyridine, namely catena di-μ(1,1)-azido-(4-methylquinoline)copper(II) (1) and catena di-μ(1,3)-azido-[di-μ(1,1)-azido-bis(2-methylpyridine)dicopper(II)] (2) have been prepared and characterized by X-ray crystallography.Crystal data: 1, C10H9N7Cu, space group P21/c, a = 577.8(2), b = 2202.3(5), c = 919.9(2) pm, β = 93.92(2)°, Ζ = 4, and R = 0.035 for 1293 observed MoKa data; 2, C6H7N7Cu, space group P21/a, a = 823.7(2), b = 1303.8(4), c = 895.3(3) pm, β = 112.23(2)°, Ζ = 4, and R = 0.022 for 2133 observed ΜοΚα diffractometer data. In the structure of 1, the Cu(II) has a strongly distorted trigonal bypyramidal coordination, where both azido groups function as μ(1,1) bridging ligands resulting in a columnar structure along the a axis. The polymeric complex 2 has a less distorted square pyramidal structure; one half of the azide groups act as μ(1,1) bridging ligands to form centrosymmetric dimers. These dimeric units are further connected by the remaining μ(1,3) bridging azido groups to form layers within the ab-plane. Infrared and electronic spectral data are also presented and discussed.


1999 ◽  
Vol 77 (7) ◽  
pp. 1262-1273 ◽  
Author(s):  
John E Drake ◽  
Layla N Khasrou ◽  
Anil G Mislankar ◽  
Raju Ratnani

Mixed ligand derivatives of Me2TeLL'2, where L = N,N-dialkyl dithiocarbamate or O,O-alkylene dithiophosphate and L' = O-alkyl dithiocarbonate, have been synthesized and characterized by elemental analysis, 1H, 13C, 31P, and 125Te NMR spectroscopy and infrared and Raman spectroscopy, and X-ray crystallography. Me2Te[S2CNMe2][S2COEt], 8: P[Formula: see text] (no. 2), with cell parameters a = 10.073(3) Å, b = 10.139(2) Å, c = 9.108(2) Å, α = 92.36(2)°, β = 115.55(2)°, γ = 111.19(2)°, V = 760.7(4) Å3, Z = 2, R = 0.0343, Rw = 0.0296. Me2Te[S2CNEt2][S2COMe], 9: P21/c (no. 14) with cell parameters a = 9.881(4) Å, b = 17.671(3) Å, c = 10.149(4) Å, β = 113.65(3)°, V = 1623.3(10) Å3, Z = 4, R = 0.0567, Rw = 0.0514. The immediate environment about tellurium in both molecules is essentially that of a saw-horse structure in which the lone pair is apparently stereochemically active and occupying an equatorial position in a distorted trigonal bipyramid. The S-Te-S angles in the two molecules are 166.87(6)° and 162.0(1)° for 8 and 9, respectively. In both molecules, the Te—S bonds to the dithiocarbamate groups are slightly shorter than those to dithiocarbonates. The dithiocarbamate groups are oriented to give secondary interactions involving the apparently terminal sulfur atoms resulting in Te—S distances of 3.205(2) and 3.277(4) Å, respectively, in 8 and 9. However, only in 9 is there a similar Te—S distance of 3.346(5) Å involving the S2COMe group because in 8, the OEt group of S2COEt, rather than the terminal S atom, is oriented toward Te. Key words: structure, tellurium, methyl, dithiocarbamates, dithiocarbonates, dithiophosphates.


2009 ◽  
Vol 62 (5) ◽  
pp. 475 ◽  
Author(s):  
Gemma Aragay ◽  
Josefina Pons ◽  
Jordi García-Antón ◽  
Ángeles Mendoza ◽  
Guillermo Mendoza-Díaz ◽  
...  

In this paper, the synthesis of two new N,N′,N-ligands, bis[2-(3,5-diphenyl-1-pyrazolyl)ethyl]amine (L1) and bis[2-(3,5-diphenyl-1-pyrazolyl)ethyl]ethylamine (L2) is reported. These ligands form complexes with the formula [PdCl(N,N′,N)]Cl when reacting with [PdCl2(CH3CN)2] in a 1:1 metal-to-ligand molar ratio. Treatment of these ligands with [PdCl2(CH3CN)2] in a 1:1 metal-to-ligand molar ratio in the presence of AgBF4 or NaBF4 gave [PdCl(N,N′,N)](BF4) complexes. These PdII complexes were characterized by elemental analyses, conductivity measurements, mass spectrometry, and IR, 1H, and 13C{1H} NMR spectroscopies. The X-ray structure of the complex [PdCl(L2)](BF4) has been determined. The metal atom is coordinated by two azine nitrogen atoms and one amine nitrogen atom of the aminopyrazole ligand. The distorted square planar coordination is completed by one chlorine atom. In this complex, intermolecular π–π stacking interactions are present.


2004 ◽  
Vol 59 (9) ◽  
pp. 1039-1044 ◽  
Author(s):  
Ali Morsali

Lead(II) complexes with 2,2':6',2''-terpyridine (tpy) and 2,4,6-tris(2-pyridyl)-1,3,5-triazine (trz) ligands, [Pb(tpy)(CH3COO)2] and [Pb(trz)(CH3COO)2], have been synthesized and characterized by IR, CHN elemental analysis and 207Pb NMR. The structure of Pb(tpy)(CH3COO)2 was confirmed by single crystal X-ray data. The complex is monomeric and the Pb atom has an unsymmetrical seven-coordinate geometry, being coordinated by three nitrogen atoms of the 2,2’:6’,2”-terpyridine ligand and four oxygen atoms of the CH3COO− ligands. The arrangement of the ligands in the two complexes exhibits a coordination gap around the Pb(II) ion, occupied possibly by a stereoactive lone pair on lead(II). The coordination around lead atoms is hemidirected. The parallel aromatic rings in Pb(tpy)(CH3COO)2 show π − π stacking.


2005 ◽  
Vol 60 (3) ◽  
pp. 300-304 ◽  
Author(s):  
Ali Morsali ◽  
Ali R. Mahjoub ◽  
Mohammad J. Soltanian ◽  
Parisa E. Pour

Lead(II) complexes with 2,2′-bipyridine (bpy) containing two different anions, [Pb(bpy)(CH3- COO)X] (X = I-, NO3-, and ClO4-), have been synthesized and characterized by CHN elemental analysis, IR-, 1H NMR- and 13C NMR spectroscopy. The structure of [Pb(bpy)(ClO4)(CH3COO)]n was confirmed by X-ray crystallography. The complex is a one-dimensional polymer as a result of perchlorate ligand bridging. The Pb atom has an unsymmetrical eight-coordinate geometry. The arrangement of the bpy, acetate and nitrate ligands leaves a coordination gap at the Pb(II) ion, occupied probably by a stereo-active lone pair of electrons. There is a π- π stacking interaction between the parallel aromatic rings that may be formed by influence lone pair activity


2005 ◽  
Vol 60 (4) ◽  
pp. 403-407 ◽  
Author(s):  
Veysel T. Yilmaz ◽  
Serkan Guney ◽  
William T. A. Harrison

The reactions of N-(2-aminoethyl)piperazine (aeppz) with tetraaqua-bis(saccharinato)zinc(II) and -cadmium(II) in ethanol solution yield the new complexes trans-[Zn(sac)2(aeppz)2] (1), and trans- [Cd(sac)2(aeppz)2] (2) (sac = saccharinate), respectively. The complexes were characterized by elemental analyses, IR spectroscopy and X-ray crystallography. Both complexes 1 and 2 are mononuclear of Ci symmetry. The zinc(II) and cadmium(II) ions are coordinated by two neutral aeppz ligands and two sac anions in an elongated distorted octahedral environment. The aeppz ligand acts as a bidentate N, N’ donor through the central heterocyclic N atom and the N atom of the aminoethyl group, while the sac ligand is O-coordinated via the carbonyl O atom. The packing of the molecules in the crystals in both complexes is consolidated by arene π −π stacking interactions between the sac rings and by intermolecular hydrogen bonds involving the amine groups of aeppz and the sulfonyl oxygen atoms of the sac ligands


Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.


2012 ◽  
Vol 13 (8) ◽  
pp. 10537-10552 ◽  
Author(s):  
Vincent J. B. Ruigrok ◽  
Mark Levisson ◽  
Johan Hekelaar ◽  
Hauke Smidt ◽  
Bauke W. Dijkstra ◽  
...  

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