scholarly journals Synthesis and Characterization of Nickel(II) Complexes of Nitrogen based Ligands of Type N,N,N′,N′-tetrakis(2-Pyridylmethyl)alkanediamine

2021 ◽  
Vol 33 (9) ◽  
pp. 2157-2161
Author(s):  
F.M. Nareetsile ◽  
R. Gontse ◽  
O.A. Oyetunji ◽  
V.C. Obuseng
Keyword(s):  
Crystal Structure Data ◽  
Octahedral Geometry ◽  
Methanol Solution ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Mononuclear Complexes ◽  
Ethanol Medium ◽  
Hexadentate Ligand

Hexadentate ligand of the type N,N,N′,N′-tetrakis(2-pyridylmethyl)alkanediamine (where alkane is butane (L1), hexane (L2) and octane (L3) reacted with Ni(ClO4)2·6H2O (stoichiometry 1:1) in alcoholic solutions yielding mononuclear complexes of the type [Ni(L)](ClO4)2·xH2O. The ligand L1 reacted with Ni(ClO4)2·6H2O in ethanol medium to give a violet powder of [Ni(L1)](ClO4)2·3H2O. The other mononuclear nickel(II) complexes using L2 and L3 were synthesized in methanol solution to give violet powders of [Ni(L2)](ClO4)2·2H2O and [Ni(L3)](ClO4)2·2H2O, respectively. All the three complexes were characterized by IR and elemental analysis. The X-ray crystallographic results for the purple crystals of [Ni(L1)](ClO4)2·3H2O shows the octahedral geometry on the Ni(II) ions together with the tetrahedral perchlorate anions separated from the [Ni(L1)]2+ cation. The crystal structure data show monoclinic space group P 21/c; a = 17.1748(10), b = 9.8273(6), c = 17.8146(10) Å; α = 90º, β = 95.0200(10)º, γ = 90º; V = 2995.2(3) Å3 , Z = 4.

Synthesis of ReItricarbonyl complexes with various sulfur- and oxygen-donating ligands: crystal structures of two ReIdinuclear structures bridged by S atoms

2018 ◽  
Vol 74 (10) ◽  
pp. 1116-1122
Author(s):  
Pheello I. Nkoe ◽  
Hendrik G. Visser ◽  
Chantel Swart ◽  
Alice Brink ◽  
Marietjie Schutte-Smith
Keyword(s):  
Hydrogen Bond ◽  
Intermolecular Hydrogen Bond ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Pyridine Ligand ◽  
X Ray ◽  
Hydrogen Bond Interactions ◽  
Mononuclear Complexes

The synthesis and characterization of two dinuclear complexes, namelyfac-hexacarbonyl-1κ3C,2κ3C-(pyridine-1κN)[μ-2,2′-sulfanediyldi(ethanethiolato)-1κ2S1,S3:2κ3S1,S2,S3]dirhenium(I), [Re2(C4H8S3)(C5H5N)(CO)6], (1), and tetraethylammoniumfac-tris(μ-2-methoxybenzenethiolato-κ2S:S)bis[tricarbonylrhenium(I)], (C8H20N)[Re2(C7H7OS)3(CO)6], (2), together with two mononuclear complexes, namely (2,2′-bithiophene-5-carboxylic acid-κ2S,S′)bromidotricarbonylrhenium(I), (3), and bromidotricarbonyl(methyl benzo[b]thiophene-2-carboxylate-κ2O,S)rhenium(I), (4), are reported. Crystals of (1) and (2) were characterized by X-ray diffraction. The crystal structure of (1) revealed two Re—S—Re bridges. The thioether S atom only bonds to one of the ReImetal centres, while the geometry of the second ReImetal centre is completed by a pyridine ligand. The structure of (2) is characterized by three S-atom bridges and an Re...Re nonbonding distance of 3.4879 (5) Å, which is shorter than the distance found for (1) [3.7996 (6)/3.7963 (6) Å], but still clearly a nonbonding distance. Complex (1) is stabilized by six intermolecular hydrogen-bond interactions and an O...O interaction, while (2) is stabilized by two intermolecular hydrogen-bond interactions and two O...π interactions.

Synthesis and Structure of cis-Dioxobis(pyrimidine-2-thiolato-N,S)molybdenum(VI)

1992 ◽  
Vol 45 (11) ◽  
pp. 1933 ◽  
Author(s):  
PR Traill ◽  
AG Wedd ◽  
ERT Tiekink
Keyword(s):  
Least Squares ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The characterization of two MoVI complexes, cis -[MoO2(2-pymS)2] and cis -[MoO2(2-pyS)2] (where 2-pymSH is pyrimidine-2-thiol and 2-pySH is pyridine-2-thiol), and their reaction with Ph3P are reported. The X-ray structure of cis -[MoO2(2-pymS)2] shows the molybdenum atom to exist in a distorted octahedral geometry defined by two mutually cis oxygen atoms and two chelating 2-pymS ligands so that the two sulfur atoms occupy approximate trans positions. Crystals of cis -[MoO2(2-pymS)2] are monoclinic, space group P 21/n, with unit cell dimensions: a 9.301(3), b 12.121(2), c 11.303(3) �, β 112.62(3)�, V 1176.3 �3, Z 4. The structure was refined by a full-matrix least-squares procedure to R 0.067 for 1858 reflections with I ≥ 2.5 (I).

Synthesis and characterization of mononuclear complexes containing 3-acetylamino-1,2,4-triazole (aat). X-ray structure of [Co(aat)2(H2O)2]Br2

1993 ◽  
Vol 209 (2) ◽  
pp. 219-223 ◽  
Author(s):  
Marina Biagini Cingi ◽  
Maurizio Lanfranchi ◽  
Anna Maria Manotti Lanfredi ◽  
Sacramento Ferrer ◽  
Jaap G. Haasnoot ◽  
...  
Keyword(s):  
Synthesis And Characterization ◽  
X Ray ◽  
Mononuclear Complexes

Synthesis and characterization of a macrocyclic copper complex containing the 14-membered 1,3,5,8,10,12-hexaazacyclotetradecane unit

2017 ◽  
Vol 72 (2) ◽  
pp. 115-118 ◽  
Author(s):  
Mohammad Hakimi ◽  
Zahra Mardani ◽  
Keyvan Moeini ◽  
Fabian Mohr
Keyword(s):  
Raman Spectroscopy ◽  
Elemental Analysis ◽  
Copper Complex ◽  
Copper Atom ◽  
Octahedral Geometry ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir

AbstractIn this work, a new macrocyclic copper complex, [Cu(ACE)(SCN)2]; ACE: 1,3,6,10,12,15-hexaazatricyclo[13.3.1.16,10]eicosane, was prepared and characterized by elemental analysis, FT-IR, Raman spectroscopy and single-crystal X-ray diffraction. X-ray analysis of [Cu(ACE)(SCN)2] reveals an elongated octahedral geometry around the copper atom in a centrosymmetric CuN6 environment.

scholarly journals Darstellung und Charakterisierung der μ3-Oxo-Cluster [Cp3Mo3(CO)4µ-Cl)(µ3-O)] und [Cp3Mo3(µ-CO)3(CO)3(µ3-O)]+ / Synthesis and Characterization of the µ3-Oxo Clusters [Cp3Mo3(CO)4μ-Cl)(μ3-O)] and [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+

1990 ◽  
Vol 45 (4) ◽  
pp. 508-514 ◽  
Author(s):  
B. Nuber ◽  
W. Schatz ◽  
M. L. Ziegler
Keyword(s):  
Structure Analysis ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

[CpMo(CO)3]2 (1) (Cp = cyclopentadienyl) reacts with InCl3 in diglyme to yield the oxo-cluster [Cp3Mo3(CO)4(μ-Cl)(μ3-O)] (2) and the cationic oxo-cluster [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+ as the salt [Cp3Mo3(μ-CO)3(CO)3(μ3-O)][CpMo(CO)3InCl3] (3). The compounds were characterized by elemental analysis, spectroscopic data and X-ray structure analysis. Compound 2 crystallizes in the orthorhombic space group P212121 with a = 1006.0(3), b = 1244.6(4) and c = 1600.8(5) pm, V = 2004.3 x 106 pm3, Z = 4. Compound 3 crystallizes in the monoclinic space group P 21/m with a = 874.4(8), b = 1407(1) and c = 1500(1) pm, β = 92.95(6) , V = 1843 × 106 pm3, Z = 2.

Synthesis and Characterization of the Nickel(II) Complex of a Macrocyclic Schiff Base Ligand with a Single Pendant Coordinating Hydroxyl Arm

2003 ◽  
Vol 56 (12) ◽  
pp. 1255 ◽  
Author(s):  
Ali Akbar Khandar ◽  
Seyed Abolfazl Hosseini-Yazdi
Keyword(s):  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Macrocyclic Schiff Base ◽  
Template Reaction ◽  
Pentadentate Ligand

The synthesis and characterization of a nickel(II) complex of the ligand 8,9,18,19-tetrahydro-7H,17H-dibenzo[f,o][1,5,9,13]dioxadiazacyclohexadecin-18-ol (L) is described. Complex [NiL(NO3)]NO3 was prepared by facile template reaction of the appropriate dialdehyde 2-(3-(2-formylphenoxy)-2-hydroxypropoxy)benzaldehyde (1) and 1,3-diaminopropane in the presence of nickel nitrate. X-Ray crystallography indicated that the compound was a six-coordinate complex that contained a pentadentate ligand and an NO3− anion trans to the alcoholic donor. The blue complex contains nickel(II) in a distorted octahedral environment of N2O4 donors, and crystallizes in the monoclinic space group C2/c with a 26.921(10), b 9.075(2), c 21.193(7) Å, β 122.12(2)°, and Z 8. From spectro-scopic and conductivity studies of the complex it has been found that six-coordinate [NiL(NO3)]+ cations and NO3− anions are formed in solution.

A convenient and selective route to a trans-difunctionalized macrocyclic hexadentate N4O2 ligand

2001 ◽  
Vol 79 (7) ◽  
pp. 1105-1109 ◽  
Author(s):  
Hongyan Luo ◽  
Robin D Rogers ◽  
Martin W Brechbiel
Keyword(s):  
Functional Groups ◽  
Metal Ion ◽  
Condensation Reaction ◽  
Synthesis And Characterization ◽  
Tetraaza Macrocycle ◽  
X Ray ◽  
Hexadentate Ligand

The synthesis and characterization of a novel difunctionalized tetraaza macrocycle, 1,8-bis(2-hydroxybenzyl)-1,4,8,11-tetraazacyclotetradecane (abbreviated H2bcyclamb), is described. The diprotic hexadentate ligand N4O2 was conveniently synthesized in two steps by the cyclic condensation reaction of 1,4,8,11-tetraazacyclotetradecane (abbreviated cyclam) and salicylaldehyde, followed by NaBH4 reduction of the cyclic hexahydropyrimidine condensate. The difunctionalization was selective and is the first procedure of trans-difunctionalization of a tetraazamacrocycle, without generating mono-, tri-, or tetra-functionalized products, with only 1,8-difunctionalized product being isolated, and with the convenience of the functionalization occurring as a result of deprotection. The trans-arrangement of the two functional groups in H2bcyclamb was verified by X-ray crystallographic studies of the copper(II) complex [Cu(H2bcyclamb)](OAc)2·2H2O. The crystal is monoclinic, P21/c, with a = 10.0931(2), b = 13.8820(1), c = 10.8752(1) Å, β = 106.332(1)°, V = 1462.26(3) Å3. The structure of [Cu(H2bcyclamb)](OAc)2·2H2O also shows the metal ion in an elongated octahedral geometry.Key words: 1,8-difunctionalized, cyclam, copper(II) complex.

scholarly journals Synthesis and X-Ray Crystal Structure of (1E)-1-(4-Chlorophenyl)-N-hydroxy-3-(1H-imidazol-1-yl)propan-1-imine

2013 ◽  
Vol 2013 ◽  
pp. 1-4 ◽  
Author(s):  
Mohamed I. Attia ◽  
Hazem A. Ghabbour ◽  
Maha S. Almutairi ◽  
Soraya W. Ghoneim ◽  
Hatem A. Abdel-Aziz ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Antifungal Agents ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonding Interactions

Synthesis and characterization of (1E)-1-(4-chlorophenyl)-N-hydroxy-3-(1H-imidazol-1-yl)propan-1-imine (4) are reported. X-ray crystal structure of the title oxime4confirmed its assigned (E)-configuration. The compound crystallizes in the monoclinic space groupP21/cwitha=13.4292(3) Å,b=8.8343(2) Å,c=11.1797(3) Å,α=90°,β=108.873(2)°,γ=90°,V=1255.03(5) Å3, andZ=4. The molecules are packed in crystal structure by weak intermolecularO–H⋯Nhydrogen bonding interactions. Compound4is a useful intermediate for the synthesis of new imidazole-containing antifungal agents.

Synthesis and structure of 3,5-dimethylpyrazolyl iron and cobalt dinitrosyl dimers

1979 ◽  
Vol 57 (23) ◽  
pp. 3119-3125 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Cobalt Complex ◽  
Cobalt Complexes ◽  
Iron Complex ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Boat Conformation ◽  
Coordination Geometry ◽  
X Ray ◽  
Metal Atoms

The synthesis and characterization of two 3,5-dimethylpyrazolyl metal dinitrosyl dimers [(N2C5H7)M(NO)2]2 (where M = Fe or Co) are described and their X-ray crystal structures detailed. Both complexes crystallize in the monoclinic space group C2/c, a = 23.848(2), 23.722(4), b = 10.7775(7), 10.6888(6), c = 14.764(1), 14.712(2) Å, β = 117.366(6), 117.094(7)°, Z = 8 (for the iron and cobalt complexes respectively). The structure of the iron complex was solved by Patterson and Fourier syntheses. The cobalt complex is isomorphous with the iron analog. Both structures were refined by full-matrix least-squares procedures to R = 0.028 and 0.035 for 4251 and 3376 reflections with I ≥ 3σ(I) respectively. Both complexes adopt a boat conformation for the central M—(N—N)2—M ring and display significantly non-linear M—N—O groups. The coordination geometry about the metal atoms is distorted tetrahedral. Important molecular dimensions (distances corrected for libration) are: mean Fe—N(pyrazolyl), 2.009(5), mean Fe—NO, 1.696(2) Å, Fe—N—O, 158.5(3)–168.2(2)°, mean Co—N(pyrazolyl), 1.992(7), Co—NO, 1.646(3)–1.680(3) Å, and Co—N—O, 161.6(3)–173.5(3)°. The iron complex is paramagnetic with formally "17-electron" iron atoms. Both structures are compared with similar four-coordinate metal dinitrosyl compounds.

Synthesis, Crystal Structure and Electrochemistry of μ-Acetatodi-μ-hydroxo-bis[(1,4,7-triazacyclononane)ruthenium(III)]-tris-iodide. Characterization of Some Ru(II)—Ru(III) Mixed Valence Species

1984 ◽  
Vol 39 (10) ◽  
pp. 1335-1343 ◽  
Author(s):  
Karl Wieghardt ◽  
Willy Herrmann ◽  
Martin Koppen ◽  
Ibrahim Jibril ◽  
Gottfried Hüttner
Keyword(s):  
Mixed Valence ◽  
Bond Distance ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
X Ray ◽  
Mononuclear Complexes ◽  
Second Wave

A series of mononuclear complexes of ruthenium containing the cyclic triamine ligand 1,4,7-triazacyclononane ([9]aneN3 = L; C6H15N3) have been prepared: [RuIIL (dmso)2Cl]Cl (dmso = dimethyl sulfoxide), [RuIIILX3] (X = C1- , Br-), [RuL2](PF6)2, [RuL(C2O4)I]. Hydrolyses of RuLCl3 under a variety of reaction conditions afford dinuclear species:[RuIII2L2(μ-OH)2(μ-CH3CO2)]I3·H2O , [RuIII2L2(μ-OH)2Cl2](PF6)2, and the mixed-valence species [Ru2L2(μ-Cl)3](PF6)2. The complex [Ru2L2(μ-OH)2(μ-CH3CO2)]I3-H2O has been characterized by a single-crystal X-ray diffraction study. The compound crystallizes in the monoclinic space group P21/c with a = 14.70(1) Å , b = 19.00(1) Å , c = 9.714(7) Å , β = 99.62(7)°, and V = 2674 Å3, dcalcd = 2.37 g cm-3 for Z = 4, and mol wt 952.3. The structure was solved by direct methods using 2519 unique reflections with I > 2σ(I). Final residuals were R1 = 0.0615 and R2 = 0.075. The structure consists of μ-hydroxo- and μ-acetato- bridged dinuclear cations and iodide anions. The observed diamagnetism and a short Ru-Ru bond distance of 2.572(3) Å are indicative of a Ru-Ru single bond. The electrochemical properties of [Ru2L2(μ-OH)2(μ-CH3CO2)]3+ and [Ru2L2(μ-Cl)3]2+ have been investigated by cyclic voltammetry, and by coulometry. Two one-electron redox processes have been identified for both complexes the first of which exhibits a reversible wave, whereas the second wave at more negative potentials is irreversible. The blue mixed valence species [Ru2L2(μ-OH)2(μ-CH3CO2)]2+ has been characterized in solution.

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