Mononuclear and Trinuclear Palladium(II) Complexes of Single- and Three-Ring Benzyl- or Xylyl-Substituted Cyclam Derivatives

2005 ◽  
Vol 58 (5) ◽  
pp. 339 ◽  
Author(s):  
Ying Dong ◽  
Leonard F. Lindoy ◽  
Peter Turner
Keyword(s):  
Crystal Structures ◽  
Complex Cation ◽  
Palladium Complexes ◽  
X Ray ◽  
Square Planar ◽  
Single Ring ◽  
Palladium Ion ◽  
Selection Of

A selection of 1 : 1 (palladium/ligand) complexes of cyclam derivatives incorporating from one to three N-benzyl groups has been synthesized. Related 3 : 1 species of two symmetrically branched, tri-cyclam species incorporating 1,3,5-‘tribenzyl’ or phloroglucinol cores are also reported. The X-ray crystal structures of the palladium complexes of two isomeric forms of the N,N′-dibenzylated (single-ring) macrocycle have been determined. In each complex the palladium ion occupies the N4-plane of the respective macrocycles in a square planar arrangement, with each complex cation adopting a stable trans-III configuration.

Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX42- (X = Cl, Br, I)/Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX42- Ions (X = Cl, Br, I)

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

Abstract The compounds [(C6H5)4As]2 TeCl4 (1), [(C2H5)4 N]2 TeBr4 · CH3CN (2), and [(C2H5)4N]2TeI4 (3) were prepared by the reaction of Te, X2 , and excess (C2H5)4NX (X = Br, I) in acetonitrile solution or by heating of [(C6H5)4 As]2TeCl6 , Te, and (C6H5)4 ASCl for several hours in the same solvent.The structures of 1-3 were determined from single crystal X-ray data.1 crystallizes in the monoclinic space group P21/n with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, β = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, I4/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te -CI, Te -Br, and Te-I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively.

Crystal structures of hexa(N-methylurea)cobalt(II) sulfate and thiosulfate

1980 ◽  
Vol 33 (2) ◽  
pp. 425 ◽  
Author(s):  
BN Figgis ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Complex Cation ◽  
X Ray Diffraction ◽  
Threefold Axis ◽  
X Ray

The crystal structures of the title compounds, [Co(C2H6N2O)6](SO4)(1) and[Co(C2H6N2O)6](S2O3) (2), have been determined at 295 K by X-ray diffraction using diffractometer data and refined by least squares to residuals of 0.042 (1), 0.043 (2) [875 and 926 reflections with I > (3σ(I)]. Crystals are trigonal, R 3c, a 1.4890(1) nm, α 43.34(1)° (1); a 1.4760(3) nm, α 44.53(1)° (2), Z 2. The compounds are isostructural; the complex cation has 3 symmetry, Co-O, 209.6(2) (1), 209.9(2) pm (2); the geometry of the ligand is well defined and precise, but the anions, located at sites of symmetry 32, are disordered. ��� The cobalt environment is distorted from Oh symmetry, being compressed along the threefold axis.

Palladium Complexes with Bidentate P,N Ligands: Synthesis, Characterization and Application in Ethene Oligomerization

2002 ◽  
Vol 57 (7) ◽  
pp. 803-809 ◽  
Author(s):  
Gabi Müller ◽  
Martti Klinga ◽  
Peter Osswald ◽  
Markku Leskelä ◽  
Bernhard Rieger
Keyword(s):  
Single Crystal ◽  
Phosphorus Atom ◽  
Palladium Complexes ◽  
Metal Center ◽  
Coordination Geometry ◽  
Trans Position ◽  
Pyridine Ligand ◽  
X Ray ◽  
Square Planar ◽  
In Trans

Palladium complexes of two different P,N ligands (a phosphane-pyridine and a phosphane-imine ligand) were synthesized and characterized. Single crystal X-ray structure analyses of the palladium diiodide compounds revealed a square-planar coordination geometry at the metal center with a longer Pd-I bond in trans-position to the phosphorus atom. The chloro-methyl palladium species of the phosphane-pyridine ligand was applied for the oligomerization of ethene using a borate salt as cocatalyst.

Oxidative coupling of cycloalkanones with 3-(pyridin-2-yl)-1,2,4-triazinone coordinated to Pd(II)

2018 ◽  
Vol 73 (8) ◽  
pp. 583-587
Author(s):  
Mustafa M. El-Abadelah ◽  
Firas F. Awwadi ◽  
Hamdallah A. Hodali ◽  
Rasha S. Rawajfeh ◽  
Monther S. Zreid ◽  
...  
Keyword(s):  
Single Crystal ◽  
Spectral Data ◽  
Oxidative Coupling ◽  
Coupling Reaction ◽  
X Ray ◽  
X Ray Crystallography ◽  
Square Planar ◽  
Pd Complexes ◽  
Palladium Ion

AbstractDichloro[3-(pyridin-2-yl)-1,2,4-triazinone]Pd(II) undergoes oxidative C–C coupling reaction with cyclopentanone and cyclohexanone at 110°C to yield the respective Pd complexes, chloro[1-(4-chlorophenyl)-5-(2-hydroxycyclopent-1-enyl)-3-(pyridin-2-yl)-1,2,4-triazin-6(1H)-one]palladium(II) (3) and chloro[1-(4-chlorophenyl)-5-(2-hydroxycyclohex-1-enyl)-3-(pyridin-2-yl)-1,2,4-triazin-6(1H)-one]palladium(II) (4). The structures of both complexes are supported by spectral data and confirmed by single-crystal X-ray crystallography. The molecules 3 and 4 stack to form tunnel structures, whilst the geometry around the palladium ion is square planar.

Octahedral Complexes of a Mixed N,N,O-Donor Ligand N-trans-(2'-hydroxycyclohexyl)-2-aminomethylpyridine

2004 ◽  
Vol 57 (5) ◽  
pp. 483 ◽  
Author(s):  
Mark J. Robertson ◽  
Geoffrey A. Lawrance ◽  
Marcel Maeder ◽  
Peter Turner
Keyword(s):  
Complex Cation ◽  
Monoclinic Space Group ◽  
Cyclohexene Oxide ◽  
Donor Ligand ◽  
X Ray ◽  
Single Isomer ◽  
Square Planar ◽  
Bonding Interaction ◽  
Distorted Octahedral ◽  
Jahn Teller

The unsymmetric mixed-donor Nam,Npy,O-ligand N-trans-(2'-hydroxycyclohexyl)-2-aminomethylpyridine (pyca, 1) was readily prepared by reaction of an epoxide (cyclohexene oxide) with (2-aminomethyl)pyridine. The ligand forms octahedral bis-tridentate complexes, exemplified with isolation of copper(II), nickel(II), zinc(II), and cobalt(III) compounds; in addition, a square-planar palladium(II) complex with the ligand behaving as bidentate was prepared. The bis-tridentate octahedral complexes may exist in six geometric isomeric forms, and molecular mechanics analysis was employed to predict the most stable isomer for copper(II), nickel(II), and cobalt(III) complexes. For the copper(II) and cobalt(III) complexes, the predictions match the X-ray crystal structures of the single isomer isolated in each case. Both the copper(II) complex [Cu . 12](ClO4)2 and the cobalt(III) complex [Co . 1 . (1–H)](ClO4)2 crystallized in the monoclinic space group P21/n (no. 14), with a 9.8400(13), b 15.434(2), c 10.0180(13) Å, and β 109.004(2)°, and a 14.162, b 18.583, c 21.596 Å, and β 100.04°, respectively. Both complexes adopt distorted octahedral structures. The copper(II) complex exists as the all-trans-fac isomer with Jahn–Teller elongation of the Cu–O bond [2.3795(19) Å] compared to Cu–Npy [2.040(2) Å] and Cu–Nam [2.024(2) Å] distances. The cobalt(III) complex appears as the cis,cis,trans(Npy) fac isomer, but deprotonation of one of the two alcohol groups leads to all six M–L distances differing: for each of two similar independent complex cations, Co–O [e.g. 1.9123(16), 1.9459(16) Å], Co–Nam [e.g. 1.949(2), 1.968(2) Å], and Co–Npy [e.g. 1.938(2), 1.940(2) Å] vary, with particularly the deprotonated alcohol bond significantly shorter than the protonated bond, despite a strong hydrogen bonding interaction with the protonated alcohol in the partner complex cation in the unit cell.

Crystal structures of (RS)-Di-μ-chloro-tetrakis(ethane-1,2-diamine)nickel(II) dichloride and diperchlorate

1978 ◽  
Vol 31 (2) ◽  
pp. 285 ◽  
Author(s):  
GA Bottomley ◽  
LG Glossop ◽  
CL Raston ◽  
AH White ◽  
AC Willis
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Complex Cation ◽  
Dimeric Complex ◽  
X Ray Diffraction ◽  
X Ray ◽  
Coordination Sites

The crystal structures of [(en)2NiCl2Ni(en)2] Cl2 (1) and [(en)2NiCl2Ni(en)2] (ClO4)2 (2) have been redetermined from single- crystal X-ray diffraction data at 295(1) K and refined by least squares to residuals of 0.073 and 0.052 respectively for 1345 and 1605 'observed' reflections respectively. Crystals of (1) are monoclinic, P21/n, a 14.053(4), b 11.309(3), c 6.326(1) Ǻ, β 94.22(2)�, Z 2. Crystals of (2) are monoclinic, P21/n, a 8.885(12), 6 19.707(20), c 7.120(8) Ǻ, β 108.99(4)�, Z 2. In both (1) and (2), a dimeric complex cation is observed, a pair of cis coordination sites about the nickel in each case being occupied by the bridging chlorines; the latter are asymmetric (Ni-Cl, 2.461(3), 2.551(3)(1); 2.461(3), 2.512(3) Ǻ (2)).

Crystal structures of trans-Dichloro- and Dibromo-bis(2,6-dimethylpyridine)copper(II)

1977 ◽  
Vol 30 (9) ◽  
pp. 1947 ◽  
Author(s):  
JA Campbell ◽  
CL Raston ◽  
JN Varghese ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Compound A ◽  
Full Matrix ◽  
X Ray ◽  
Square Planar

The crystal structures of the title compounds have been determined at 295(1) K by X-ray diffraction and refined by full-matrix least squares to residuals of 0.045 and 0.067 for 1224 and 1955 ?observed? reflections respectively. The compounds are isomorphous (triclinic, Pī, Z 1). Dichloro compound: a 8.068(2), b 8.024(2), c 7.646(2) Ǻ, α 93.84(2), β 113.44(2), γ 117.11(2)�. Dibromo compound: a 7.999(2), b 7.921(2), c 7.849(2) Ǻ, α 94.37(2), β 112.85(2), γ 115.99(2)�. The copper atoms are square-planar coordinated with two halide and two base ligands coordinated necessarily trans by virtue of the siting of the molecule on a centre of symmetry. Cu-X, Cu-N are 2.264(2), 2.011(3) (dichloro); 2.425(1), 1.997(4) Ǻ (dibromo). The plane of the lutidine is almost normal to the CuN2X2 plane.

Coordination of 6-Methyl-2,2'-bipyridine. Structure of Bivalent Copper and Palladium Complexes

1991 ◽  
Vol 44 (2) ◽  
pp. 219 ◽  
Author(s):  
D Onggo ◽  
DC Craig ◽  
AD Rae ◽  
HA Goodwin
Keyword(s):  
Palladium Complexes ◽  
Partial Hydrolysis ◽  
Monoclinic Space Group ◽  
Coordination Environment ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Square Planar ◽  
Bivalent Copper ◽  
Hydrolysis Of

Bis ( ligand ) complexes of 6-methyl-2,2′-bipyridine (L) with copper(II) and palladium(II) have been prepared, and their structures have been determined by single-crystal X-ray diffractometry . In the formation of the complex fromcopper(II) tetrafluoroborate and L, partial hydrolysis of a coordinated fluoroborate ion to the hydroxytrifluoroborate ion occurs. The stereochemistry about copper in [CuL2OHBF3][BF4] is essentially trigonal bipyramidal with an axial compression. The nitrogens of the methyl-substituted pyridine rings coordinate in the axial sites. In [PdL2Cl][BF4] the coordination environment about palladium is square planar and one of the 6-methylbipyridine molecules functions as a unidentate group, the nitrogen of the methyl-substituted pyridine ring being uncoordinated. The average metal-nitrogen distance is 2.032 Ǻ in the copper complex and 2.042 Ǻ in the palladium complex. [CuL2OHBF3][BF4] is monoclinic, space group P21/c, Z = 4, a 9.005(2), b 17.868(2), c 15.298(3) Ǻ, β 104.13(1)°. [PdL2Cl][BF4] is monoclinic, space group P21/c, Z = 4, a 9.606(5), b 14.748(2), c 16.311(8)Ǻ, β 96.13(2)°.

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