Lewis-Base Adducts of Group 11 Metal(I) Complexes. XXXV. Complexes of the Asymmetric Bidentate Ligands (L) 2-Aminomethylpyridine and 2-Hydrazinopyridine With Copper(I) Halides: Syntheses and Structural Characterization of [CuL2]+X-, X = Cl, Br, I

1988 ◽  
Vol 41 (5) ◽  
pp. 623 ◽  
Author(s):  
PC Healy ◽  
JD Kildea ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Hydrogen Bonding ◽  
Structural Characterization ◽  
Lewis Base ◽  
Donor Group ◽  
Bidentate Ligands ◽  
Halide Anion ◽  
Nitrogen Bases ◽  
Ionic Complexes ◽  
Nitrogen Donor

The 1:2 adducts of the copper(I) halides (CuX ; X = Cl, Br, I) with the aliphatic/aromatic bidentate nitrogen bases 2-aminomethylpyridine, H2NCH2.C5H4N, and 2-hydrazinopyridine, H2N.NH.C5H4N, L, have been synthesized by recrystallization of stoichiometric copper(I) halide/base solutions from acetonitrile . In all cases, ionic complexes [CuL2]+ X- are obtained, copper being four-coordinated by a pair of bidentate ligands, and with widely varying distortions from ideal 2 symmetry. Cu-N (aromatic) in the 2-aminomethylpyridine adducts range from 1.979(8) to 2.037(5)Ǻ; while Cu-N(H2) are 2.102(9)-2.172(10)Ǻ, N( Ar )-Cu-N( Ar ) angles [130.7(2)-143.2(4)°] are larger than N(H2)-Cu-N(H2)[114.8(2)-116.3(4)°]. Comparable values for the 2-hydrazinopyridine complexes are 1.95(1)-2.036(5), 2.085(4)-2.214(7)Ǻ; 124.1(2)-140.8(4), 94.5(3)-128.0(3)°. In no case does the halide anion coordinate to the copper, displacing the aliphatic nitrogen donor group; rather it is stabilized in the crystal lattice by strong NH2…X hydrogen bonding.

Structural Characterization of Zinc and Iron (II/III) Complexes of a Porphyrin Bearing Two Built-in Nitrogen Bases. An Example of High-Spin Diaqua-Iron(III) Bromo Complex

2010 ◽  
Vol 49 (16) ◽  
pp. 7536-7544 ◽  
Author(s):  
Ismail Hijazi ◽  
Thierry Roisnel ◽  
Pascale Even-Hernandez ◽  
Florence Geneste ◽  
Olivier Cador ◽  
...  
Keyword(s):  
High Spin ◽  
Structural Characterization ◽  
Nitrogen Bases

Structural Characterization of a Cage Ligand Fragmentation Reaction

1994 ◽  
Vol 47 (1) ◽  
pp. 181 ◽  
Author(s):  
JM Harrowfield ◽  
AM Sargeson ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Room Temperature ◽  
Fragmentation Reaction ◽  
X Ray ◽  
Nitrogen Donor ◽  
Crystal Structural

The room temperature X-ray single-crystal structural characterization of a protonated copper(II) complex of a ligand artefact, L′, of L = N-Me6sar (described in an accompanying paper) is recorded, the new ligand L′ being generated formally by elimination of a CH2CH2 bridge between a pair of nitrogen donor atoms of L. The complex, [ ClCu (H2L′) (ClO4)3.2H2O, is orthorhombic, Pccn , a 22.528(7), b 10.544(3), c 13.748(6) Ǻ, Z = 4 formula units, R being 0.053 for 1133 independent 'observed' [I > 3σ(I)] reflections. The cation, containing five-coordinate square-pyramidal ClCuN4 copper, is disposed with the Cu- Cl bond [2.458(3)Ǻ] lying on a crystallographic 2 axis; Cu-N distances are 2.094(8) and 2.093(8)Ǻ.

Lewis-base adducts of Group 11 metal(I) compounds. 49. Structural characterization of hexameric and pentameric (triphenylphosphine)copper(I) hydrides

1989 ◽  
Vol 28 (7) ◽  
pp. 1300-1306 ◽  
Author(s):  
Candiera F. Albert ◽  
Peter C. Healy ◽  
John D. Kildea ◽  
Colin L. Raston ◽  
Brian W. Skelton ◽  
...  
Keyword(s):  
Structural Characterization ◽  
Lewis Base

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LI. Synthesis and Structural Characterization of Mononuclear Chloro-, Bromo- and Iodo-pyridinebis(triphenylphosphine)copper(I) Complexes

1989 ◽  
Vol 42 (6) ◽  
pp. 895 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Copper Atom ◽  
Lewis Base ◽  
X Ray

Complexes [ XCu ( py )(PPh3)2], X = Cl, Br, I, py = pyridine, have been synthesized and characterized by single-crystal X-ray structure determination. Chloride and iodide derivatives have similar cells [ isomorphous (?) but not isostructural ], triclinic, pi, a = 19.5 A, b = 10.5, c = 9.6 � , α ≈ 66, β ≈ 86, γ ≈ 83�, Z = 2; the bromide is monoclinic, Cc, a 13.568(9), b 15.760(12), c 16.545(8) � , β 95.65(5)�, Z = 4. Cl, Br, I structures were refined to residuals of 0.042, 0.055, 0.039 for 4288, 2241, 4808 'observed' reflections. In all cases, the copper atom is four-coordinate; for such an array, Cu-X lengths are unusually short [2.318(2), 2.459(2), 2.636(1) � (Cl, Br, I) and Cu-N unusually long (2.14(1) � ], while (Cu-P) increase from 2.264 to 2.288 � across the series. The dominant aspect of the complexes is thus that of XCu (PPh3)2 solvated by pyridine.

Structure and Dynamics of 9(10H)-Acridone and Its Hydrated Clusters. II. Structural Characterization of Hydrogen-Bonding Networks

2000 ◽  
Vol 104 (38) ◽  
pp. 8649-8659 ◽  
Author(s):  
Masaaki Mitsui ◽  
Yasuhiro Ohshima ◽  
Shun-ichi Ishiuchi ◽  
Makoto Sakai ◽  
Masaaki Fujii
Keyword(s):  
Hydrogen Bonding ◽  
Structural Characterization ◽  
Structure And Dynamics ◽  
Hydrogen Bonding Networks ◽  
Hydrated Clusters

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIII. Synthesis and Structural Characterization of Binuclear μ,μ'-Dichloro-, Dibromo and Diiodo-bis[(pyridine)(triphenylphosphine)copper(I)] Complexes, and Their Pyridine-4-carbonitrile Analogues

1989 ◽  
Vol 42 (6) ◽  
pp. 913 ◽  
Author(s):  
LM Engelhardt ◽  
PC Healy ◽  
JD Kildea ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Lewis Base ◽  
The Other ◽  
X Ray ◽  
Structure Determinations ◽  
M Phase ◽  
And Inversion ◽  
Iodide Single Crystal

Mixed base pyridine (py)/triphenylphosphine adducts of the copper(1) halides, CuX, have been synthesized for 1 : 1 : 1 stoichiometry for X = chloride and iodide; single-crystal X-ray structure determinations of these show them to be isomorphous and isostructural with that of the bromide recorded elsewhere, being �,�′- dihalo-bridged dimers , [(PPh3)( py )CuX2Cu( py )(PPh3)], monoclinic, C2/c, a ≈ 26.2, b ≈ 14.3, c ≈ 11 .2 � , β ≈ 95, Z = 4 dimers. The bromide has been isolated as a new monoclinic C 2/m polymorph, a 11 .279(8), b 14.268(6), c 13.858(4) �, β 109.33(6)�, Z=4 dimers, and details of its structure are also recorded. The structures of their pyridine-4-carbonitrile (pycn) analogues have also been determined and found to be also binuclear, with no cyano-copper interactions; these also are an isomorphous, isostructural series, monoclinic P21/n, a ≈ 15.4, b ≈ 8.1, c ≈ 17.9 � , β ≈ 101 �, Z = 2 dimers. In each series of dimers, one half of the dimer is crystallographically independent, the generators of the other half being twofold rotor (C2/c phase), mirror (C2/m phase) and inversion centre (P21/n phase) respectively.

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