Anionic pyrazolyl-bridged nickel nitrosyl complexes. Synthesis, structure, and reactivity

1979 ◽  
Vol 57 (23) ◽  
pp. 3099-3106 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Ion Pair ◽  
Sodium Ion ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Space Group ◽  
Nitrosyl Complexes ◽  
Pyrazolyl Group ◽  
The Mean ◽  
Distorted Tetrahedral Coordination ◽  
Molecular Unit

A series of anionic pyrazolyl-bridged nickel nitrosyl complexes, M+[(ON)Ni(μ-L2)(μ-X)Ni(NO)]− (where L = pyrazolyl, N2C3H3, or 3,5-dimethylpyrazolyl, N2C5H7; X = Cl, Br, I, or N2C5H7; and M = Na, (CH3)4N, or (C2H5)4N) is described. Crystallographic analyses have been carried out on two of these complexes. Crystals of [(C2H5)4N]+[(ON)Ni(μ-I)(μ- N2C5H7)2Ni(NO)]− are orthorhombic, a = 19.910(1), b = 14.0330(7), c = 9.3195(9) Å, Z = 4, space group Pn21a and crystals of [(C4H8O)2Na][(ON)Ni(μ-N2C5 H7)3Ni(NO)] are orthorhombic, a = 19.897(2), b = 19.529(3), c = 15.894(2) Å, Z = 8, space group Pbca. Both structures were solved by Patterson and Fourier syntheses and were refined by full-matrix least-squares procedures to R = 0.027 and 0.057 for 2572 and 2168 reflections with I ≥ 3σ(I) respectively. The structure of [(C2H5)4N]+[(ON)Ni(μ-I)(μ-N2C5H7)2Ni(NO)]− consists of discrete cations and binuclear anions which have approximate C2v symmetry. The nickel atoms have distorted tetrahedral coordination geometry. Important mean molecular dimensions (distances corrected for libration) are: Ni—I—Ni, 73.67(2)°, Ni—I, 2.765(3), Ni—NO, 1.649(5), Ni—N(pyrazolyl), 1.980(14) Å, and Ni—N—O, 172.5(18)°. The structure of [(C4H8O)2Na][(ON)Ni(μ-N2C5 H7)3Ni(NO)] consists of discrete ion-pair units in which the two NiNO moieties are bridged by three N2C5H7 ligands, two of which are coordinated to the sodium ion via a novel η2(N,N) π-interaction (mean Na—N = 2.61(3) Å). The sodium is also coordinated to two tetrahydrofuran oxygen atoms to give a distorted tetrahedral coordination geometry about the sodium (Na—O = 2.301(6) and 2.266(5) Å). Except for disordered tetrahydrofuran carbon atoms, the molecular unit has approximate C2v symmetry. The nickel atoms have distorted tetrahedral coordination geometry, the mean distances being Ni—NO, 1.591(6), Ni—N(pyrazolyl), 1.985(2) for the unique pyrazolyl group and 2.016(5) Å for the pyrazolyl nitrogen atoms coordinated to Na. The mean Ni—N—O angle is 176.9(11)°.

Thiophenophane–metal complexes. I. Preparation, X-ray structure, and cyclic voltammetry of 2,5,8-trithia[9](2,5)thiophenophane, L, and of its metalcomplexcation bis(2,5,8-trithia[9](2,5)thiophenophane-S2,S3]copper(I),[CuL2]+1

1988 ◽  
Vol 66 (6) ◽  
pp. 1506-1512 ◽  
Author(s):  
C. Robert Lucas ◽  
Liu Shuang ◽  
Michael J. Newlands ◽  
Jean-Pierre Charland ◽  
Eric J. Gabe
Keyword(s):  
Cyclic Voltammetry ◽  
Reference Electrode ◽  
Molecular Structures ◽  
Saturated Calomel Reference Electrode ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Space Group ◽  
X Ray ◽  
H Nmr ◽  
Distorted Tetrahedral Coordination

Preparation of the thiophenophane C10H14S4, (L), and syntheses of its copper(I) complex [CuL2]ClO4 or [CuL2]BF4 are described. The 13C and 1H nmr spectra of L and the ir spectra (4000–200 cm−1) of [CuL2]ClO4 and [CuL2]BF4 are reported. The molecular structures of L and [CuL2]ClO4 have been determined. For L: space group P21/a, a = 7.9347(2) Å, b = 18.7479(3) Å, c = 8.8596(2) Å, β = 108.446(2)°, Z = 4, Rf = 0.048, and Rw = 0.034. For [CuL2]ClO4: space group P21/c, a = 9.4363(1) Å, b = 18.2768(3) Å, c = 16.2157(3) Å, β = 96.520(2)°, Z = 4, Rf = 0.056, and Rw = 0.037. The Cu(I) complex has distorted tetrahedral coordination geometry; its perchlorate anion is non-coordinating and disordered. The Cu—S bond lengths lie in the range 2.301–2.392 Å and the S—Cu—S angles in the range 92.43—150.26°. Cyclic voltammetry of [CuL2]ClO4 (10−3 mol/L in dimethylsulfoxide, 0.1 mol/L Et4NClO4, glassy carbon working electrode, platinum counter electrode, aqueous saturated calomel reference electrode against which the ferrocenium/ferrocene potential under similar conditions was 400 mV) shows a quasi-reversible oxidation (E1/2 = 0.150 V, ΔEp = 170 mV at 50 mV/s). Thiophene's effect as a sub-unit in a small macrocycle upon properties of the latter is discussed.

scholarly journals [1,2-Bis(dicyclohexylphosphanyl)-1,2-dicarba-closo-dodecaborane-2κ2P,P′]di-μ-chlorido-1:2κ4Cl:Cl-dichlorido-1κ2Cl-dimercury(II)

2014 ◽  
Vol 70 (4) ◽  
pp. m140-m140
Author(s):  
Liguo Yang
Keyword(s):  
Metal Atom ◽  
Title Compound ◽  
Chelate Ring ◽  
The Other ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Axis Direction ◽  
Envelope Conformation ◽  
The Mean ◽  
Distorted Tetrahedral Coordination

The title compound, [Hg2Cl4(C26H54B10P2)], was synthesized by the reaction of 1,2-bis(dicyclohexylphosphanyl)-1,2-dicarba-closo-dodecaborane with HgCl2. Both HgIIatoms show a distorted tetrahedral coordination geometry, provided by the two bridging chloride anions and the P atoms of the diphosphanyl ligand for one metal atom, and by two bridging and two terminal chloride anions for the other. The five-membered HgP2C2chelate ring assumes an envelope conformation, with the HgIIatom displaced by 0.1650 (5) Å from the mean plane of the other four atoms (r.m.s. deviation = 0.002 Å). In the crystal, B—H...Cl interactions link the molecules, forming a supramolecular chain along thea-axis direction.

scholarly journals Tetrakis(dimethoxyboryl)methane

IUCrData ◽  
2016 ◽  
Vol 1 (8) ◽  
Author(s):  
Sumeng Liu ◽  
Gregory S. Girolami
Keyword(s):  
Title Compound ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Occupancy Factor ◽  
Bond Lengths ◽  
Methoxy Groups ◽  
Synthetic Intermediate ◽  
Distorted Tetrahedral Coordination

The title compound, tetrakis(dimethoxyboryl)methane (systematic name: octamethyl methanetetrayltetraboronate), C9H24B4O8or C[B(OMe)2]4, is a useful synthetic intermediate. Crystals of this compound at 102 K conform to the orthorhombic space groupPbcn. The molecules, which reside on sites of crystallographic twofold symmetry, have idealized -4 point symmetry like most other CX4molecules in which eachXgroup bears two non-H substituents at the 1-position. The central C atom has a slightly distorted tetrahedral coordination geometry, with C—B bond lengths of 1.5876 (16) and 1.5905 (16) Å. One of the methoxy groups is disordered over two sets of sites; the major component has an occupancy factor of 0.676 (8).

Bis(2,9-dimethyl-1,10-phenanthroline)copper(I) tetraphenylborate dichloromethane solvate

2007 ◽  
Vol 63 (3) ◽  
pp. m800-m802 ◽  
Author(s):  
William T. Eckenhoff ◽  
Tomislav Pintauer
Keyword(s):  
Bond Length ◽  
Dihedral Angle ◽  
Title Compound ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Π Stacking ◽  
Distorted Tetrahedral Coordination

In the title compound, [Cu(C14H12N2)2]C24H20B·CH2Cl2, CuI is chelated by two 2,9-dimethyl-1,10-phenanthroline (2,9-Me2phen) ligands, in a distorted tetrahedral coordination geometry. The average Cu—N bond length is 2.032 Å, and the interligand dihedral angle is 77.60 (6)°. The complexes form π–π stacking interactions between 2,9-Me2phen ligands, with a perpendicular interplanar separation of 3.652 (5) Å.

scholarly journals Bis[μ-1,3-bis(1H-imidazol-1-yl)propane-κ2N3:N3′]bis(dichloridozinc) dihydrate

2014 ◽  
Vol 70 (5) ◽  
pp. m184-m184
Author(s):  
Xiao-Juan Wang ◽  
Yun-Long Feng
Keyword(s):  
Zinc Complex ◽  
Complex Molecule ◽  
Dimensional Structure ◽  
Water Molecules ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Lattice Water ◽  
Bridging Ligand ◽  
Cl Atoms ◽  
Distorted Tetrahedral Coordination

The title hydrated complex, [Zn2Cl4(C9H12N4)2]·2H2O, is a discrete dinuclear zinc complex with 1,3-bis(1H-imidazol-1-yl)propane as the bridging ligand. The complex molecule lies about a crystallographic inversion centre. The ZnIIatom exhibits a distorted tetrahedral coordination geometry defined by two imidazole N atoms and two Cl atoms. O—H...Cl hydrogen bonding between the lattice water molecules and the terminal Cl atoms of the molecule lead to a two-dimensional structure extending parallel to (100).

One-dimensional CuIand AgIladder-like coordination polymers supported by 2-ethyl-1-(pyridin-3-ylmethyl)-1H-benzimidazole

2013 ◽  
Vol 69 (9) ◽  
pp. 1017-1021
Author(s):  
Liu-cheng Gui ◽  
Guang-ming Liang ◽  
Hua-hong Zou ◽  
Zhong Hou
Keyword(s):  
Hydrogen Bonds ◽  
Metal Ion ◽  
Three Dimensional ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Asymmetric Unit ◽  
Counter Anion ◽  
One Dimensional ◽  
Solvent Molecules ◽  
Distorted Tetrahedral Coordination

The title complexes, poly[[bis[μ2-2-ethyl-1-(pyridin-3-ylmethyl)-1H-benzimidazole-κ2N1:N3]copper(I)] tetrafluoroborate acetonitrile monosolvate], {[Cu(C15H15N3)2]BF4·CH3CN}n, (I), and poly[[bis[μ2-2-ethyl-1-(pyridin-3-ylmethyl)-1H-benzimidazole-κ2N1:N3]silver(I)] perchlorate methanol monosolvate], {[Ag(C15H15N3)2]ClO4·CH3OH}n, (II), are isostructural and exhibit one-dimensional ladder-like structures in which each asymmetric unit contains one metal ion (Cu+or Ag+), two 2-ethyl-1-(pyridin-3-ylmethyl)-1H-benzimidazole (bep) ligands, one counter-anion (tetrafluoroborate or perchlorate) and one interstitial molecule (acetonitrile or methanol). Each metal ion exhibits a distorted tetrahedral coordination geometry consisting of two pyridyl and two benzimidazole N atoms from four distinct ligands. Two metal ions are linked by two bep ligands to form a centrosymmetric 18-memberedM2(bep)2metallacycle, while adjacentM2(bep)2metallacycles are further interlinked by another two bep ligands resulting in a ladder-like array. In the extended structure, four adjacent ladder-like arrays are connected together through C—H...F, O—H...O and C—H...O hydrogen bonds between bep ligands, solvent molecules and counter-anions into a three-dimensional supramolecular structure.

Crystal and molecular structure of bis[methyltris(1-pyrazolyl)gallato]nickel(II)

1979 ◽  
Vol 57 (14) ◽  
pp. 1823-1825 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Nickel Atom ◽  
Exact Formula ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Gallium Atom ◽  
Full Matrix ◽  
Distorted Tetrahedral Coordination

Crystals of bis[methyltris(1-pyrazolyl)gallato]nickel(II) are rhombohedral, a = 9.6670(5), c = 23.893(1) Å, Z = 3, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.030 and Rw = 0.035 for 925 reflections with I ≥ 3σ (I). The crystal structure consists of well separated molecules of [MeGa-(N2C3H3)3]2Ni having exact [Formula: see text] (S6) symmetry and approximate D3d symmetry. The coordination geometry about the nickel atom is octahedral with Ni—N = 2.109(2) Å, N—Ni—N = 90.65(6) and 89.35(6)°. The gallium atom has distorted tetrahedral coordination geometry with Ga—N = 1.939(2), Ga—C = 1.940(4) Å, N—Ga—N = 99.55(6), and N—Ga—C = 118.16(5)°.

Redetermination of [bis(2-pyridyl)amine-N,N′]copper(II) diperchlorate

2000 ◽  
Vol 57 (1) ◽  
pp. m25-m27 ◽  
Author(s):  
Miao Du ◽  
Xian-He Bu ◽  
Lin-Hong Weng ◽  
Xue-Bing Leng ◽  
Ya-Mei Guo
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Coordination Sphere ◽  
Chain Structure ◽  
Title Complex ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
A Chain ◽  
Distorted Tetrahedral Coordination ◽  
Close Contacts

In the crystal structure of the title complex, [Cu(C10H9N3)2](ClO4)2, the CuIIcenter is four-coordinated by the nitrogen donors of the pyridine rings of the ligand, bis(2-pyridyl)amine. The crystal structure reveals that the CuN4coordination sphere has a distorted tetrahedral coordination geometry with a crystallographicC2axis through the CuIIcenter. The perchlorate anions link the complex cations to form a chain structure through C—H...O close contacts and N—H...O hydrogen bonds.

catena-Poly[silver(I)-μ-4-aminobenzenesulfonato-μ-2,3-diethylpyrazine]

2007 ◽  
Vol 63 (11) ◽  
pp. m2707-m2707 ◽  
Author(s):  
Hai-Yan Liu ◽  
Ji-Cheng Ma ◽  
Jin Yang
Keyword(s):  
Hydrogen Bonds ◽  
Title Compound ◽  
Coordination Geometry ◽  
Dimensional Chain ◽  
Tetrahedral Coordination ◽  
One Dimensional ◽  
Distorted Tetrahedral Coordination

In the title compound, [Ag(C6H6NO3S)(C8H8N2)], the AgI cation is four-coordinated by three N atoms from two different 2,3-diethylpyrazine ligands and one –NH2 group of a 4-aminobenzenesulfonate ligand, and one sulfonate O atom in a distorted tetrahedral coordination geometry. The AgI centers are doubly bridged by both types of ligands, forming a one-dimensional chain. N—H...O hydrogen bonds complete the structure.

scholarly journals Crystal structure of bis[μ-bis(diphenylphosphanyl)methane-κ2P:P′]-μ-chlorido-chlorido-1κCl-(1-phenylthiourea-2κS)disilver acetonitrile hemisolvate

2015 ◽  
Vol 71 (6) ◽  
pp. m133-m134 ◽  
Author(s):  
Arunpatcha Nimthong-Roldán ◽  
Janejira Ratthiwal ◽  
Yupa Wattanakanjana
Keyword(s):  
Hydrogen Bonds ◽  
Chloride Ion ◽  
Title Complex ◽  
Coordination Geometry ◽  
Supramolecular Architecture ◽  
Tetrahedral Coordination ◽  
Complex Molecules ◽  
Close Proximity ◽  
Crystal Complex ◽  
Distorted Tetrahedral Coordination

In the dinuclear title complex, [Ag2Cl2(C7H8N2S)(C25H22P2)2]·0.5CH3CN, each AgIion displays a distorted tetrahedral coordination geometry with two P atoms from two bis(diphenylphosphanyl)methane (dppm) ligands, one bridging chloride ion, one terminal chloride ion and one terminal S atom from theN,N′-phenylthiourea (ptu) ligand. The dppm ligands and the bridging chloride ion force the two Ag atoms into close proximity, with a short Ag...Ag separation of 3.2064 (2) Å. In the crystal, complex molecules are linked by N—H...Cl hydrogen bonds forming a dimer. The dimers are linkedviaweak C— H...Cl hydrogen bonds forming a two-dimensional supramolecular architecture in theyzplane. In addition, an intramolecular N—H...Cl hydrogen bond is observed.

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