Binuclear Copper(II) Complexes of Some Tetradentate Pyridyl Phthalazine Ligands. Structure, Electrochemistry and Magnetism - Crystal-Structure of Aqua-µ-[1,4-Di-(4',6'-Dimethylpyridin-2'-Ylamino)-Phthalazine-N1',µ-N2 ,µ-N3,N1'']-µ-Hydroxo-Dinitratodicopper(II) Nitrate

1986 ◽  
Vol 39 (7) ◽  
pp. 1007 ◽  
Author(s):  
SK Mandal ◽  
TC Woon ◽  
LK Thompson ◽  
MJ Newlands ◽  
EJ Gabe
Keyword(s):  
Variable Temperature ◽  
Magnetic Moments ◽  
Magnetic Data ◽  
Redox Potentials ◽  
Binuclear Copper ◽  
Triclinic Space Group ◽  
X Ray ◽  
One Step ◽  
Strong Exchange ◽  
Very High

The molecular structure of aqua-μ-[1,4-di(4′,6′-dimethylpyridin-2′- ylamino )phthalazine-N1′,μ-N2,μ-N3,N1′]-μ- hydroxo-dinitratodicopper (II) nitrate has been determined by single-crystal X-ray diffractometry . The compound is triclinic, space group Pī , with two molecules in the unit cell of dimensions a 7.8064(11), b 12.9137(14), c 14.8564(14), α 69.857(8), β 80.074(10), γ 83.659(11). The structure was refined by least-squares to a residual of 0.057 for 2806 reflections. The binuclear centre in the complex involves a five-coordinate and a tetragonally distorted six-coordinate copper atom, each with a coordinated, bidentate nitrate, a copper-copper separation of 3.156 Ǻ and a Cu-O(H)-Cu bridge angle of 113.7°. This complex, and other related systems, exhibit low room-temperature magnetic moments (< 1.2 BM), suggesting antiferromagnetically coupled binuclear copper centres , and in the case of the complex [Cu2( paps )(OH)Cl3].3H2O variable- temperature magnetic data indicate moderately strong exchange with -2J = 432 cm-1. Very high redox potentials are observed for these complexes [0.00-0.83 V (v. s.c.e .)] involving two-electron transfer in one step or two separate steps.

Binuclear copper(II) complexes of the tetradentate ligand 1,4-di(2′-pyridyl)aminophthalazine: some novel five-coordinate derivatives

1969 ◽  
Vol 47 (22) ◽  
pp. 4141-4152 ◽  
Author(s):  
L. K. Thompson ◽  
V. T. Chacko ◽  
J. A. Elvidge ◽  
A. B. P. Lever ◽  
R. V. Parish
Keyword(s):  
Room Temperature ◽  
Principal Series ◽  
Magnetic Data ◽  
Binuclear Copper ◽  
Neutral Form ◽  
Deprotonated Form ◽  
Copper Salts ◽  
X Ray ◽  
Anionic Ligand ◽  
Aromatic Carboxylate

Reaction of the title ligand (L) with copper salts leads to the formation of three principal series of compounds, LCu2X3(OH)•H2O (X = Cl, Br), LCu2(RCO2)3, and LCu2(RCO2)4, where RCO2 represents various aliphatic and aromatic carboxylate species. Magnetic data, electronic spectroscopic data both at room temperature and at −196 °C, infrared spectra, and microanalytical data are correlated to reveal that these complexes contain a binuclear copper-copper system in which the copper atoms are 5-coordinate and square pyramidal. Brief details are presented of an X-ray structural analysis of the chloride complex confirming the structure proposed.The ligand forms complexes both in its neutral form and in an anionic deprotonated form. The ultraviolet spectra of the complexes distinguish these modes of bonding. The electronic spectra are discussed in terms of the 5-coordinate square pyramidal copper chromophore deemed to be present. In the complex L2Cu, the copper atom has a trigonally distorted 6-coordinate environment with tridentate anionic ligand.

Crystal Structure and Spectroscopic Behaviour of a Binuclear Copper(II) Complex of Mefenamic Acid and Dimethylsulfoxide

1998 ◽  
Vol 53 (8) ◽  
pp. 871-874 ◽  
Author(s):  
G. Facchin ◽  
M. H. Torre ◽  
E. Kremer ◽  
O. E. Piro ◽  
E. J. Baran
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Mefenamic Acid ◽  
Electronic Spectra ◽  
Anthranilic Acid ◽  
Binuclear Copper ◽  
Triclinic Space Group ◽  
Spectroscopic Behaviour ◽  
Space Group ◽  
X Ray

Abstract The crystal structure of the binuclear Cu(II) complex [Cu(mef)2DMSO]2 (mef = deprotonated N-2,3-dimethylphenyl-anthranilic acid; DMSO = dimethylsulfoxide) has been determined by single-crystal X-ray diffractometry. It crystallizes in the triclinic space group P1̄ with Z = 1. IR and electronic spectra of the compound are also discussed briefly.

Synthesis, Crystal Structure and Magnetic Properties of a (μ-Hydroxo)(μ-Pyrazolato) Dicopper(II) Complex

2000 ◽  
Vol 55 (9) ◽  
pp. 796-802 ◽  
Author(s):  
H. Kara ◽  
Y. Elerman ◽  
K. Prout
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Variable Temperature ◽  
Powdered Sample ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Present Complex ◽  
Square Planar ◽  
Super Exchange Interaction

Preparation and magnetic properties of a 3,5-dimethylpyrazolate bridged binuclear copper(II) complex [Cu2(L)(3 ,5 -pyz)] (L = 1,3-Bis(2-Hydroxy-5-Chlorosalicylideneamino)propan- 2-ol) is reported. The crystal structure determined by X-ray diffraction methods. (C22H20N4O3CI2CU2), triclinic, space group P1̄, a = 9.622(3), b = 10.921(2), c = 11.420(3) Å, α = 100.73(2), β = 94.04(2), Υ = 108.08(2)°, V = 1110.2(5) Å3, Z = 2. Two copper(II) ions in a square-planar coordination are bridged via alkoxide oxygen and 3,5-dimethyl pyrozolate nitrogen atoms to form a dinuclear unit. The metal coordination sphere is four-coordinate, planar with an N2O2 donor set. The dihedral angle between the two coordination planes is 166.83°. There are significant intermolecular interactions between neighbouring binuclear entities. The shortest intermolecular Cu (1) ... Cu(1)i distance is 3.383(1) Å and the Cu(1) - O ( 1)i distance is 2.666(3) Å (i = 1 -x, -y, 1 - z). The variable-temperature magnetic susceptibility measurement for a powdered sample of the complex was carried out in the temperature range 5 - 350 K and analysed to obtain values of the parameter J in the exchange Hamiltonian ℋ = -2JScu Scu; 2J = -164 cm-1. The magnetic moment at 300 K is about 2.42 μB, and 0.22 μB at 5 K. The weak antiferromagnetism of the present complex is reasonably explained in terms of the orbital countercomplementary effect based on Hoffmann's theory for super-exchange interaction

Synthesis, crystal structure and magnetic properties of the complex [ReCl3(tppz)]·MeCN

RSC Advances ◽  
2015 ◽  
Vol 5 (123) ◽  
pp. 101616-101622 ◽  
Author(s):  
J. Palion-Gazda ◽  
I. Gryca ◽  
B. Machura ◽  
Francesc Lloret ◽  
Miguel Julve
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Variable Temperature ◽  
Donor Ligands ◽  
Magnetic Data ◽  
Nitrogen Donor Ligands ◽  
X Ray ◽  
Nitrogen Donor

The paper reports the synthesis, X-ray structure and a deep analysis of the variable-temperature magnetic data of the new complex [ReCl3(tppz)]·MeCN being a very scarce example of mononuclear Re(iii) complexes incorporating nitrogen donor ligands.

Copper(II) complexes of open-chain thioether ligands terminated by salicylaldimine functionality*This article has a companion paper in this issue (doi: 10.1139/v11-081).

2011 ◽  
Vol 89 (10) ◽  
pp. 1190-1201 ◽  
Author(s):  
C. Robert Lucas ◽  
John M.D. Byrne ◽  
Julie L. Collins ◽  
Louise N. Dawe ◽  
David O. Miller
Keyword(s):  
Magnetic Susceptibility ◽  
Single Crystal ◽  
Variable Temperature ◽  
Companion Paper ◽  
Structural Studies ◽  
Binuclear Copper ◽  
Open Chain ◽  
X Ray ◽  
Variable Temperature Magnetic Susceptibility ◽  
Coordination Spheres

From 1,11-bis(salicylaldimine)-3,6,9-trithiaundecane (H2L1), 1,11-bis(salicylaldimine)-6-oxa-3,9-dithiaundecane (H2L2), and 1,8-bis(salicylaldimine)-3,6-dithiaundecane (H2L3), syntheses for [Cu(L1)]2 (I), Cu(L2)·CH3OH (II), Cu(L3) (III), [Cu(HL3)][CH3COO] (IV), [Cu(HL1-sal)]Cl2 (V), Cu4(L1)2Br4(H2O)2·2H2O (VI) and Cu2(L2)Br2·xH2O (VII) are described. Single crystal X-ray structural studies for I, III and VII are reported. Variable temperature magnetic susceptibility studies of I, VI and VII are discussed. The examination of VII represents the first magneto-structural study of a binuclear copper(II) species with NSO3Br coordination spheres. This study examines perturbation by one or more of the donor atoms so that none of the known magnetostructural models predicts the copper–copper coupling.

scholarly journals The physico-chemical properties of 4-chlorophenoxyacetates of Mn(II), Co(II), Ni(II) and Cu(II)

2018 ◽  
Vol 33 (1) ◽  
pp. 07
Author(s):  
W. Ferenc ◽  
M. Bernat ◽  
J. Sarzynski ◽  
B. Paszkowska
Keyword(s):  
Magnetic Moments ◽  
Chemical Properties ◽  
Bidentate Ligands ◽  
X Ray Diffraction ◽  
Magnetic Studies ◽  
X Ray ◽  
Physico Chemical ◽  
One Step ◽  
Polycrystalline Solids ◽  
Ligand Fields

The complexes of 4-chlorophenoxyacetates of Mn(II), Co(II), Ni(II) and Cu(II) have been synthesized as polycrystalline solids, and characterized by elemental analysis, spectroscopy, magnetic studies and also by X-ray diffraction and thermogravimetric measurements. The analysed complexes have the following colours: pink for Co(II), green for Ni(II), blue for Cu(II) and a pale pink for Mn(II) compounds. The carboxylate group binds as monodentate and bidentate ligands. On heating to 1173K in air the complexes decompose in several steps. At first, they dehydrate in one step to anhydrous salts, that next decompose to the oxides of respective metals. Their magnetic moments were determined in the range of 76-303K. The results reveal them to be high-spin complexes of weak ligand fields.

scholarly journals Complexes of 4-chlorophenoxyacetates of Nd(III), Gd(III) and Ho(III)

2018 ◽  
Vol 35 (1) ◽  
pp. 67
Author(s):  
W. Ferenc ◽  
M. Bernat ◽  
J. Sarzyński ◽  
H. Głuchowska
Keyword(s):  
Thermal Decomposition ◽  
Magnetic Moments ◽  
X Ray Diffraction ◽  
Magnetic Studies ◽  
Bridging Ligands ◽  
X Ray ◽  
Gaseous Products ◽  
Carboxylate Groups ◽  
One Step ◽  
Ligand Fields

The complexes of 4-chlorophenoxyacetates of Nd(III), Gd(III) and Ho(III) have been synthesized as polycrystalline hydrated solids, and characterized by  elemental analysis, spectroscopy, magnetic studies and also by X-ray diffraction and thermogravimetric measurements. The analysed complexes have the following colours: violet for Nd(III), white for Gd(III) and cream for Ho(III) compounds. The carboxylate groups bind as bidentate chelating (Ho) or bridging ligands (Nd, Gd). On heating to 1173K in air the complexes decompose in  several steps. At first, they dehydrate in one step to form anhydrous salts, that next decompose to the oxides of respective metals. The gaseous products of their thermal decomposition in nitrogen were also determined and the magnetic susceptibilites were measured over the temperature range of 76-303K and the magnetic moments were calculated. The results show that 4-chlorophenoxyacetates of Nd(III), Gd(III) and Ho(III) are high-spin complexes with weak ligand fields. The solubility value in water at 293K for analysed  4-chlorophenoxyacetates is in the order of 10-4mol/dm3.

Negative hyperconjugation in hexachloro-3-cyclopentenylaminosulphenyl halides: Preparation and X-ray structure of C5Cl6NSBr and synthesis of C5Cl6NS+AsF6−

1991 ◽  
Vol 69 (6) ◽  
pp. 1022-1027 ◽  
Author(s):  
Allen Apblett ◽  
Tristram Chivers ◽  
James F. Fait ◽  
Rainer Vollmerhaus
Keyword(s):  
Crystal Structure ◽  
Key Words ◽  
Good Yield ◽  
Variable Temperature ◽  
Triclinic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Compound C ◽  
Negative Hyperconjugation ◽  
C Nmr

The reaction of hexachlorocyclopentadiene with (NSCl)3 at 65 °C in the absence of a solvent produced hexachloro-3-cyclopentenylidenaminosulfenyl chloride, C5Cl6NSCl, in good yield. The derivatives C5Cl6NSX(X = Br, I, C5Cl6N, NPr2i, Ph) were prepared by treatment of C5Cl6NSCl with Me3SiBr, Me3SiI, Ph3Sb, iPr2NH, and Ph2Hg, respectively. The crystal structure of C5Cl6NSBr was determined by X-ray crystallography. Crystals of C5Cl6NSBr are triclinic, space group [Formula: see text] with a = 9.626(2), b = 9.810(2), c = 13.736(2) Å, α = 79.68(1), β = 88.62(1), γ = 74.73(1)°, Z = 4, final R and Rw values were0.075 and 0.063, respectively, for 4850 unique observed reflections. The > C=NSBr moiety adopts a syn conformation and there are two different molecules of C5Cl6NSBr in the asymmetric units. The bond lengths are d(C=N) = 1.278(8) and 1.253(8), d(N—S) = 1.560(6) and 1.569(6), and d(S—Br) = 2.229(2) and2.235(2) Å. The bond angles at nitrogen are 146.7(4) and 148.6(4) and those at sulfur are 116.8(2) and 116.5(2)°. The unusual geometry of the < C=NSBr moiety is explained in terms of negative hyperconjugation (nN → σSBr*). A variable temperature 13C NMR of C5Cl6NSCl provides evidence for a fiuxional process (ΔG*298 = 68.1 ± 1.2 kJ mol−1) in solution. The dark purple compound C5Cl6NS+AsF6− was synthesized from the reaction of C5Cl6NSCl and AgAsF6 in SO2. Key words: hexachloro-3-cyclopentenylidenamino sulfides, crystal structure, hexachloro-3-cyclopentenylidenaminosulfenyl bromide.

Synthesis, characterization, and dynamic behaviour of pseudoferrocene complexes

1990 ◽  
Vol 68 (11) ◽  
pp. 1923-1931 ◽  
Author(s):  
Michael D. Clerk ◽  
Michael J. Zaworotko ◽  
Bozena Borecka ◽  
T. Stanley Cameron ◽  
Donald L. Hooper ◽  
...  
Keyword(s):  
Dynamic Behaviour ◽  
Variable Temperature ◽  
Grignard Reagents ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
H Nmr ◽  
Ring Rotation ◽  
Methyl Phenyl

Carbanion sources (organolithium and Grignard reagents) react with [(mesitylene)2Fe]2+ and [(mesitylene)(Ch)Fe]+ cations (Ch = cyclohexadienyl) to afford neutral Ch2Fe and ChCh′Fe ("pseudoferrocene") complexes, respectively. Addition of R− (R− = methyl, phenyl, benzyl, and t-butyl) occurs stereospecifically via exo addition at an unsubstituted carbon atom of the arene ring. The synthesis and characterization of these complexes is detailed and the structure of bis(η5-exo-6-phenyl-1,3,5-trimethylcyclohexadienyl)iron(II), 3b, has been determined by single crystal X-ray diffraction analysis. 3b crystallizes in the triclinic space group [Formula: see text], with a = 11.947(2), b = 12.784(1), c = 8.865(2), α = 108.59(1)°, β = 108.19(1)°, γ = 84.91(1)°, and Dcalcd 1.227 g cm−3 for Z = 2. Least-squares refinement gave a conventional R value of 0.0452 for 2080 independent observed reflections. The structure reveals that the complex adopts a gauche-eclipsed conformation. The variable temperature (vt) 1H NMR spectra of pseudoferrocenes are interpreted in terms of restricted ring rotation around the ligand—metal—ligand axis. Keywords: arene, cyclohexadienyl, pseudoferrocene, variable temperature NMR, X-ray diffraction.

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