2-(1H-2-Benzimidazolyl)-6-(1-(arylimino)ethyl)pyridylnickel Complexes: Synthesis, Characterization, and Ethylene Oligomerization

2010 ◽  
Vol 63 (1) ◽  
pp. 109 ◽  
Author(s):  
Liwei Xiao ◽  
Min Zhang ◽  
Rong Gao ◽  
Xiaoping Cao ◽  
Wen-Hua Sun

A series of tridentate N,N,N-nickel complexes bearing 2-(1H-2-benzimidazolyl)-6-(1-(arylimino)ethyl)pyridines was synthesized and characterized by elemental and IR spectroscopic analysis. The molecular structures of representative complexes were determined by single-crystal diffraction, and these were found to have a six-coordinate distorted octahedral geometry around the Ni centre. On treatment with Et2AlCl, all nickel complexes exhibited good catalytic activities up to 106 g mol–1(Ni) h–1 for ethylene oligomerization with major dimerization. The steric and electronic effects on catalytic activities of metal complexes as well as the influence of various reaction parameters were carefully investigated.

2008 ◽  
Vol 61 (5) ◽  
pp. 397 ◽  
Author(s):  
Saliu A. Amolegbe ◽  
Maliha Asma ◽  
Min Zhang ◽  
Gang Li ◽  
Wen-Hua Sun

A series of chromium(iii) complexes ligated by N^N^N tridentate 2-quinoxalinyl-6-iminopyridine were synthesized and characterized by elemental analysis and infrared spectroscopy. Single-crystal X-ray diffraction analysis for the structure of complex C3 reveals a distorted octahedral geometry. When methylaluminoxane was employed as the co-catalyst, the chromium complexes showed high activities for ethylene oligomerization and polymerization. The distribution of oligomers obtained followed Schulz–Flory rules with high selectivity for α-olefins. Both steric and electronic effects of coordinated ligands affected the catalytic activities as well as the properties of the catalytic products. The parameters of the reaction conditions were also investigated to explore the optimum catalytic potentials of these complexes.


2018 ◽  
Vol 74 (8) ◽  
pp. 1049-1053
Author(s):  
Yue-Xin Guo ◽  
Hong-Cui Ma ◽  
Ren Bo ◽  
Ning Zhao ◽  
Li-Gang Zhao ◽  
...  

The molecular structures of tetraaqua[N,N′-bis(pyridin-4-yl)pyridine-2,6-dicarboxamide]sulfatomanganese(II) dihydrate, [Mn(SO4)(C17H13N5O2)(H2O)4]·2H2O or [Mn(H2 L 1)(SO4)(H2O)4]·2H2O, (I), and tetraaquabis[N,N′-bis(pyridin-4-yl)pyridine-2,6-dicarboxamide]cadmium(II) sulfate tetrahydrate, [Cd(C17H13N5O2)2(H2O)4]SO4·4H2O or [Cd(H2O)4(H2 L 1)2]·SO4·4H2O, (II), both contain a central metal atom in a distorted octahedral geometry coordinated equatorially by four oxygen atoms from water molecules. In (I), the axial positions are occupied by a nitrogen atom from H2 L 1 and an oxygen atom from the sulfate anion, whereas in (II), the axial positions contain two nitrogen atoms from two different H2 L 1 ligands and the sulfate anion acts as the charge-balancing ion. π–π stacking between pyridine rings and a network of hydrogen bonds involving the water molecules and the sulfate anions play a crucial role in the molecular self-assembly of the two structures.


1981 ◽  
Vol 59 (15) ◽  
pp. 2391-2401 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter

X-ray crystallographic studies of three transition metal complexes incorporating the novel anionic tridentate chelating ligand [Me2Ga(N2C5H7)OCH2CH2SR]− (R = Et or Ph) show that the ligand is facially coordinated in each case. Crystals of [dimethyl(3,5-dimethyl-1-pyrazolyl) (2-thioethoxyethoxy)gallato(N(2), O,S)]nitrosylnickel(I) are monoclinic, a = 8.8313(4), b = 7.2402(2), c = 26.539(1) Å, β = 94.390(3)°, Z = 4, space group P21/c, R = 0.040 and Rw = 0.050 for 2489 reflections. The Ni atom is in a distorted tetrahedral environment with bond angles about Ni ranging from 87.90(7) to 127.9(1)°. The nitrosyl coordination is slightly non-linear with Ni—N—O = 170.1(4)°. Important bond lengths (corrected for libration) are: Ni—S, 2.326(1), Ni—O, 2.019(2), Ni—N(pyrazolyl), 1.980(3), Ni—N(O), 1.633(3) and N—O, 1.156(4) Å. Crystals of [dimethyl(3,5-dimethyl-1-pyrazolyl) (2-thiophenoxyethoxy)gallato(N(2),O,S)]tricarbonylmanganese(I) are triclinic, a = 9.4911(5), b = 10.4323(6), c = 11.7618(7) Å, α = 86.17(1), β = 69.547(5), γ = 81.402(4)°, Z = 2, space group [Formula: see text]R = 0.029 and Rw = 0.035 for 2496 reflections. The Mn atom is coordinated to the fac-tridentate gallate ligand and to three carbonyl ligands resulting in a slightly distorted octahedral geometry. Important corrected bond lengths are: Mn—S, 2.397(1), Mn—O, 2.055(2), Mn—N, 2.082(3), and Mn—C, 1.794(4), 1.807(4), and 1.807(4) Å. Crystals of [dimethyl(3,5-dimethyl-1-pyrazolyl) (2-thioethoxyethoxy)gallato(N(2),O,S)](η3-cycloheptatrienyl)dicarbonylmolybdenum are monoclinic, a = 17.030(3), b = 19.097(2), c = 15.908(3) Å, β = 115.99(1)°, Z = 8, space group P21/n R =0.036 and Rw = 0.043 for 4477 reflections. The two crystallographically independent molecules differ primarily in the orientation of the S-ethyl moiety and each contains an η3-C7H7 ligand which occupies one coordination site of a distorted octahedron as a %-donating ligand. Important corrected bond distances are: Mo—S, 2.527(2) and 2.541(2), Mo—O, 2.241(5) and 2.237(4), Mo—N, 2.277(5) and 2.254(5), Mo—C(O), 1.940(7)–1.960(7), and Mo—C(C7H7), 2.198(6)−2.391(7) Å.


2019 ◽  
Vol 75 (12) ◽  
pp. 1613-1616
Author(s):  
Samundeeswari Mariappan Balasekaran ◽  
Frederic Poineau

Reports of quadrivalent transition-metal fluoride salts containing bulky organic cations are limited. In this context, we prepared the bis(tetraphenylarsonium) hexafluoridotechnetate(IV) dihydrate salt, (C24H20As)2[TcF6]·2H2O, by a cation metathesis reaction of (NH4)2[TcF6] in water. This is the first report of an arsonium salt of the hexafluoridotechnetate(IV) dianion. (AsPh4)2[TcF6]·2H2O crystallizes in the triclinic space group P\overline{1}. The [TcF6]2− anion adopts a slightly distorted octahedral geometry with an average Tc—F bond length of 1.933 Å. The cyclic voltammogram of (AsPh4)2[TcF6]·2H2O in CH3CN shows a one-electron reversible oxidation wave at 1.496 V.


2012 ◽  
Vol 68 (6) ◽  
pp. m824-m825 ◽  
Author(s):  
Ichraf Chérif ◽  
Jawher Abdelhak ◽  
Mohamed Faouzi Zid ◽  
Ahmed Driss

In the crystal structure of the title compound, (C5H6ClN2)[Cr(C2O4)2(H2O)2]·1.5H2O, the CrIII atom adopts a distorted octahedral geometry being coordinated by two O atoms of two cis water molecules and four O atoms from two chelating oxalate dianions. The cis-diaquadioxalatochromate(III) anions, 2-amino-5-chloropyridinium cations and uncoordinated water molecules are linked into a three-dimensional supramolecular array by O—H...O and N—H...O hydrogen-bonding interactions. One of the two independent lattice water molecules is situated on a twofold rotation axis.


2003 ◽  
Vol 58 (9) ◽  
pp. 916-921 ◽  
Author(s):  
Amitabha Datta ◽  
Samiran Mitra ◽  
Georgina Rosair

Two new bimetallic complexes [Zn(phen)3][Fe(CN)5(NO)] · 2 H2O · 0.25 MeOH, (1) and [(bipy)2(H2O)Zn(μ-NC)Fe(CN)4(NO)] · 0.5 H2O, (2), have been isolated (where phen = 1,10-phenanthroline and bipy = bipyridyl) and characterised by X-ray crystallography [as the 2 H2O · 0.25 CH3OH solvate for (1) and hemihydrate for (2)] infrared spectroscopy and thermogravimetric analysis. Substitution of phenanthroline for bipyridyl resulted in a cyano-bridged bimetallic species rather than two discrete mononuclear metal complexes. The bond angles of Fe-N-O were shown to be practically linear for both 1 [179.2(7)°] and 2 [178.3(3)°], and the Zn atoms have distorted octahedral geometry. The solvent molecules in both crystal lattices take part in forming hydrogen-bonded networks.


1974 ◽  
Vol 52 (16) ◽  
pp. 2923-2927 ◽  
Author(s):  
André L. Beauchamp ◽  
Bernard Saperas ◽  
Roland Rivest

The compound cis-Hg(SCN)2(Phen)2 belongs to the triclinic space group [Formula: see text] with a = 13.252(5), b = 11.077(4), c = 8.443(3) Å, α = 105.20(3), β = 83.25 (3), γ = 90.92(3)°, and Z = 2. The structure was solved by the heavy atom method and refined on 1718 independent reflections to an R factor of 0.069. The crystal contains discrete molecules, in which mercury is coordinated to four nitrogen atoms from two phenanthroline molecules and to two sulfur atoms from thiocyanate groups. These donor atoms define a distorted octahedral geometry around mercury. The Hg—N bond lengths are in the range 2.42(2)–2.52(2) Å, whereas the Hg—S bonds are equal to 2.622(8) and 2.582(8) Å. The molecules are packed in layers parallel to the (110) planes and the layers are held together by normal van der Waals interactions. Within the layers, the packing of the complex is characterized by parallel stacking of phenanthroline ligands at distances of ∼3.4 Å. The terminal nitrogen atoms of the thiocyanate groups are uncoordinated.


2012 ◽  
Vol 68 (8) ◽  
pp. m1055-m1055 ◽  
Author(s):  
M. Mobin Shaikh ◽  
Veenu Mishra ◽  
Priti Ram ◽  
Anil Birla

The structure of the centrosymmetric title complex, [Cu(C5H9O2)2(C6H7NO)2], has the CuIIatom on a centre of inversion. The CuIIatom is six-coordinate with a distorted octahedral geometry, defined by the N and O atoms of the chelating 2-(2-hydroxymethyl)pyridine ligands and two carboxylate O atoms from two monodentate pivalate ions. The crystal packing is stabilized by intermolecular C—H...O and intramolecular O—H...O hydrogen-bond interactions.


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