Synthesis, Characterization and Crystal Structures of Monomeric and Imidazolate-Bridged Polymeric Copper(II) Complexes of 5-Methyl-1,5,9-triazanonane

2000 ◽  
Vol 53 (10) ◽  
pp. 883 ◽  
Author(s):  
Hai-Liang Zhu ◽  
Xiao-Lan Yu ◽  
Xiao-Ming Chen
Keyword(s):  
Oxygen Atom ◽  
Variable Temperature ◽  
Magnetic Measurement ◽  
Orthorhombic Space Group ◽  
Apical Position ◽  
Space Group ◽  
Pyramidal Geometry ◽  
Trigonal Bipyramidal ◽  
Square Pyramidal Geometry ◽  
Distorted Trigonal Bipyramidal

Two complexes [Cu(mtan)(H2O)(ClO4)](ClO4) (Im = imidazolate) (1) and [Cu(mtan)(Im)]n (ClO4)2n (mtan = 5-methyl-1,5,9-triazanonane) (2) have been prepared and characterized. Single-crystal X-ray analysis reveals that (1) crystallizes in the orthorhombic space group Pbcm, with a 8.906(5), b 12.255(6), c 14.821(4) Å and V 1618(1) Å3, and complex (2) crystallizes in the orthorhombic space group Pca21, with a 11.125(7), b 9.149(6), c 15.180(7) Å and 1545(1) Å3. The copper(II) atom in complex (1) is in a distorted square-pyramidal geometry, being coordinated by three nitrogen atoms from an mtan ligand and one oxygen atom from an aqua ligand at the basal plane and one perchlorate oxygen atom at the apical position. The structure of complex (2) features polymeric cationic chains composed of [Cu(mtan)(Im)]+ repeating units and discrete perchlorate anions. The Cu(1) atom in each unit has a severely distorted trigonal-bipyramidal geometry, being coordinated by three nitrogen atoms from one mtan ligand and two nitrogen atoms from two Im groups. The structural units are linked by -Im groups to give one-dimensional chains. The variable-temperature magnetic measurement on the powder sample of (2) reveals intrachain, medium antiferromagnetic interaction with g = 2.240 and J = –36.45 cm–1 through the -Im bridges.

Different ZnIIcation coordination geometries in di-μ-acetato-bis{2-chloro-6-[(pyridine-2-ylmethylimino)methyl]phenol}dizinc(II) chloroform monosolvate

2013 ◽  
Vol 69 (11) ◽  
pp. 1348-1350 ◽  
Author(s):  
Young-Inn Kim ◽  
Jin Young Lee ◽  
Young-Kwang Song ◽  
Sung Kwon Kang
Keyword(s):  
Quantum Yield ◽  
Title Compound ◽  
The Other ◽  
Bidentate Coordination ◽  
Strong Emission ◽  
Pyramidal Geometry ◽  
Trigonal Bipyramidal ◽  
Coordinate Geometry ◽  
Square Pyramidal Geometry ◽  
Distorted Trigonal Bipyramidal

In the title compound, di-μ-acetato-κ2O:O;κ2O:O′-bis[(6-chloro-2-{(E)-[(pyridin-2-yl)methylimino]methyl}phenolato-κ3N,N′,O)zinc(II)], [Zn2(C13H10ClN2O)2(C2H3O2)2]·CHCl3, the ZnIIcation adopts a five-coordinate geometry and is coordinated by two N atoms and one O atom of a tridentate 6-chloro-2-{(E)-[(pyridin-2-yl)methylimino]methyl}phenolate ligand and two O atoms of two bridging acetate groups, but their coordination geometries differ. One ZnIIcation adopts a distorted trigonal bipyramidal geometry and the other a square-pyramidal geometry. The two acetate ligands bridge two ZnIIcations with mono- and bidentate coordination modes. The title compound exhibits a strong emission at 460 nm upon excitation at 325 nm with a quantum yield of 23.1%.

Die Kristallstrukturen von (η5-C5Me5)MoMe4 und (η5-C5Me5)WMe4 / The Crystal Structures of (η5-C5Me5)MoMe4 and (η5-C5Me5)WMe4

1995 ◽  
Vol 50 (8) ◽  
pp. 1207-1209 ◽  
Author(s):  
Katrin Köhler ◽  
Alexander Steiner ◽  
Herbert W. Roesky
Keyword(s):  
Crystal Structures ◽  
Lattice Parameters ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Pyramidal Geometry ◽  
Square Pyramidal Geometry

The crystal structures of (η5-C5Me5)MoMe4 1 and (η5-C5Me5)WMe4 2 are reported. 1 and 2 crystallize in the orthorhombic space group Pbcm with the lattice parameters a = 681.4(2) pm, b = 1538.6(6) pm, c = 1402.4(6) pm with 4 units per cell (1), and a = 684.99(6) pm, b = 1547.3(2) pm, c = 1405.5(2) pm with 4 units per cell (2). Both compounds are monomeric and have a square-pyramidal geometry.

Five-coordinated halogenomercurate(II) complexes: crystal structures of bis(L-tryptophanium) trichloromercurate(II) and bis(D,L-homocysteine thiolactonium) tetrabromomercurate(II)

1981 ◽  
Vol 59 (1) ◽  
pp. 138-143 ◽  
Author(s):  
Langford Book ◽  
Arthur J. Carty ◽  
Chung Chieh
Keyword(s):  
Crystal Structures ◽  
Chloride Ions ◽  
Strong Hydrogen Bond ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Experimental Conditions ◽  
Space Group ◽  
Trigonal Bipyramidal ◽  
Unit Form ◽  
Distorted Trigonal Bipyramidal

Reactions of L-tryptophan and D,L-homocysteine with mercury(II) halides in acidic ethanol/water solutions result in the formation of bis(L-tryptophanium) trichloromercurate(II) (TPTC) and bis(D,L-homocysteine thiolactonium) tetrabromomercurate(II) (HTTB) respectively. Their crystal structures consist of halide-bridged polymeric chains of quasi HgX3− units. The coordination geometry around Hg(II) in both anions is distorted trigonal bipyramidal. There are no chemical bonds between the amino acid cations and the mercury(II) ions. TPTC is monoclinic, space group P21, with a = 16.688(5), b = 5.626(1), c = 14.022(5) Å, β = 108.17(3)°. The structure was solved and refined from 2433 independent counter measured reflections to an R factor of 0.062. The two independent tryptophan molecules per asymmetric unit form a single cation via a strong hydrogen bond between the carboxylate groups. Thus the compound can be represented by MHgCl3 where M is the cation. One of the three Cl− ions is strongly bonded to one Hg(II) ion and weakly bonded to two other Hg(II) ions. In addition to the three short Hg—Cl distances of 2.403(3), 2.376(4), and 2.614(4) Å, there are two long Hg—Cl bonds of 2.833(4) and 2.888(4) Å to each Hg(II), from the weakly bridged chloride ions. HTTB is orthorhombic, space group Pnma with a = 8.068(3), b = 24.985(7), and c = 8.828(3) Å. The structure was refined to an R value of 0.066 for 819 observed reflections (I ≥ 3σ(I)), however, inclusion of unobserved reflections did not change the parameters. The homocysteine free base used in the reaction was lactonised under the experimental conditions to a thiolactonium ion. There are three relatively short Hg—Br interactions (2.566(3) twice, 2.662(4) Å) within the distorted trigonal bipyramidal stereochemistry of each mercury atom and two longer Hg—Br bonds (2.917(6) and 3.087(5) Å). The polymeric, anion chains arrange in layers on the mirror planes (y = ±1/4) with these layers sandwiched by two layers of cations.

scholarly journals The Crystal Structure of TlBrI2(4-methylpyridine-N-oxide)2

1988 ◽  
Vol 43 (1) ◽  
pp. 132-133 ◽  
Author(s):  
W. Hiller ◽  
A. Castiñeiras ◽  
M. E. García- Fernandez ◽  
M. R. Bermejo ◽  
J. Bravo ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Bromine Atom ◽  
Unit Cell ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Thallium Atom ◽  
Trigonal Bipyramidal Geometry ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal ◽  
Methyl Pyridine

Abstract The unit cell of TlBrI2 (4-methylpyridine-N-oxide) 2 is orthorhombic, space group Pnna. with a = 1126.9(3),b = 919.8(2),c = 1210.4(3) pm.and Z = 4. The structure consists of discrete TlBrI2 (4-methyl-pyridine-N-oxide)2 molecules which have a distorted trigonal-bipyramidal geometry. The thallium atom is coordinated to two iodine atoms and a bromine atom in equatorial positions, and by two 4-methyl-pyridine-N-oxide ligands in the axial positions.

Conformational polymorphism in a cobalt(II) dithiocarbamate complex

2020 ◽  
Vol 76 (9) ◽  
pp. 921-926
Author(s):  
Jetnipat Songkerdthong ◽  
Phimphaka Harding ◽  
David J. Harding
Keyword(s):  
Slow Evaporation ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pyramidal Geometry ◽  
Dithiocarbamate Ligand ◽  
Coordinate Geometry ◽  
Square Pyramidal Geometry

Two conformational polymorphs of (N,N-dibutyldithiocarbamato-κ2 S,S′)[tris(3,5-diphenylpyrazol-1-yl-κN 2)hydroborato]cobalt(II), [Co(C45H34BN6)(C9H18NS2)] or [TpPh2Co(S2CNBu2)], 1, are accessible by recrystallization from dichloromethane–methanol to give orthorhombic polymorph 1a, while slow evaporation from acetonitrile produces triclinic polymorph 1b. The two polymorphs have been characterized by IR spectroscopy and single-crystal X-ray crystallography at 150 K. Polymorphs 1a and 1b crystallize in the orthorhombic space group Pbca and the triclinic space group P-1, respectively. The polymorphs have a trans (1a) and cis (1b) orientation of the butyl groups with respect to the S2CN plane of the dithiocarbamate ligand, which results in an intermediate five-coordinate geometry for 1a and a square-pyramidal geometry for 1b. Hirshfeld surface analysis reveals minor differences between the two polymorphs, with 1a exhibiting stronger C—H...S interactions and 1b favouring C—H...π interactions.

scholarly journals Eisen- und Cobaltkomplexe mit Schwefelliganden: Darstellung und Kristallstrukturen von [Me4N][FeCl{S2P(OMe)2}2], [Me4N][CoCl{S2P(OMe)2}2], [Et4N][FeCl{S2P(p-C6H4Me)2}2], [Et4N]2[FeCl{ S2PS(OMe) } 2] und [Fe { S2P(OMe)2 }3] / Iron and Cobalt Complexes with Sulfur-Containing Ligands: Preparation and Crystal Structures of [Me4N][FeCl{S2P(OMe)2}2],[Me4N][CoCl{S2P(OMe)2}2], [Et4N][FeCl{S2P(p-C6H4Me)2}2], [Et4N]2[FeCl{S2PS(OMe)}2] and [Fe{S2P(OMe)2}3]

1990 ◽  
Vol 45 (2) ◽  
pp. 245-257 ◽  
Author(s):  
Kristin Kirschbaum ◽  
Uta Bönnighausen ◽  
Ewald Gesing ◽  
Klaus Greiwe ◽  
Ulrich Kuhlmann ◽  
...  
Keyword(s):  
Reaction System ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Metal Centers ◽  
Space Group ◽  
Trigonal Bipyramidal ◽  
Mononuclear Complexes ◽  
Sulfur Containing ◽  
Distorted Trigonal Bipyramidal

The reaction systems MCl2/K{S2P(OMe)2} (M = Fe(II), Co(II)), FeCl2/Na{S2S2P(p-C6H4Me)2}, and FeCl3/K2{S2PS(OMe)} in methanol afford the mononuclear complexes [FeCl{S2P(OMe)2}2]-, [CoCl{S2P(OMe)2}2]-, [FeCl{S2P(p-C6H4Me)2}2]-, and [FeCl{S2PS(OMe)}2]2-, which were isolated as salts [Me4N][FeCl{S2P(OMe)2}2] (1), [Me4N][CoCl{S2P(OMe)2}2] (2), [Et4N][FeCl{S2P(p-C6H4Me)2}2] (3) and [Et4N]2[FeCl{S2PS(OMe)}2] (4), respectively. Crystals of [Me4N][MCl{S2P(OMe)2}2] are triclinic, space group P 1 (Z = 2): Fe(II), a = 7.165(3), b = 8.628(3), c = 16.526(6)Å, α = 83.98(3), β = 85.32(3), γ = 89.80(3)°; Co(II), a = 7.164(2), b = 8.612(2), c = 16.504(4)Å, α = 84.59(2), β = 84.63(2), γ = 89.41(2)°. The structures of 1 and 2 were refined to R (Rw) = 0.034 (0.043) and 0.028 (0.032), respectively. Compound 3 is monoclinic, space group C2/c, Z = 4 with a = 23.831(5), b = 10.536(3), c = 17.133(4)Å, β = 114.43(3)°. Its structure was refined to R (Rw) = 0.046 (0.052). 4 crystallizes in the orthorhombic space group Pccn with a = 13.310(2), b = 12.982(2), c = 18.968(3) Å, and Z = 4. The refinement converged to R (Rw) = 0.042 (0.039). The anions of the compounds 1—4 contain five-coordinated metal centers which reside in distorted trigonal-bipyramidal (1, 2, and 3) or square pyramidal (4) S4Cl-environments. The neutral complex [Fe{S2P(OMe)2}3] (5) with six-coordinated metal sites was isolated from the reaction system FeCl3/K{S2P(OMe)2} in CH2Cl2. 5 is monoclinic, space group C 2/c (Z = 4) with a = 14.211(2), b = 11.115(2), c = 12.823(2) Å, β = 97.23(1)°. The refinement converged to R (Rw) = 0.022 (0.031). The anions of 1, 2, and 3 represent the first examples of structurally defined mononuclear Fe(II) and Co(II) complexes containing 1,1-dithiolate groups and halide ions simultaneously.

Synthesis, structural and magnetic properties of macrocyclic aza-amido binuclear copper(II) complexes

1989 ◽  
Vol 67 (4) ◽  
pp. 662-670 ◽  
Author(s):  
Sanat K. Mandal ◽  
Laurence K. Thompson ◽  
Michael J. Newlands ◽  
Amal K. Biswas ◽  
Bibhutosh Adhikary ◽  
...  
Keyword(s):  
Variable Temperature ◽  
Complex Iii ◽  
Azomethine Nitrogen ◽  
X Ray Diffraction ◽  
Binuclear Copper ◽  
Magnetic Studies ◽  
Monoclinic System ◽  
Space Group ◽  
Pyramidal Geometry ◽  
Square Planar

Binuclear, antiferromagnetically coupled, macrocyclic copper(II) complexes, [Cu2(C28H32N4O4)]•H2O (II) and [Cu2(C36H32N4O4)]•CH3CN•H2O (III), involving asymmetric ligands with two deprotonated amide, two azomethine nitrogen, and two phenoxide donors at the binuclear centre, have been synthesized and characterized by single-crystal X-ray diffraction and variable temperature magnetic studies. Complex II crystallizes in the monoclinic system, space group P21/n, with a = 16.4854(9) Å, b = 7.6005(13) Å, c = 21.1617(11) Å, β = 104.090(5)°, Z = 4, Rf = 0.068 for 2062 significant reflections. The two copper(II) centres have square planar N2O2 donor sets with two phenoxide oxygen atoms bridging the copper centres with a copper–copper separation of 2.898(2) Å. A long copper–oxygen (amide) contact (2.808(10) Å) forms a weak dimer association. Complex III crystallizes in the triclinic system, space group [Formula: see text], with a = 8.7771(9) Å, b = 12.3983(16) Å, c = 15.7299(16) Å, α = 85.003(11)°, β = 84.574(8)°, γ = 76.838(10)°, Z = 2, Rf = 0.041 for 2966 significant reflections. The two copper(II) centres have distorted square-pyramidal geometry involving an N2O2 in plane donor set and two phenoxide oxygen bridges with a copper–copper separation of 3.018(1) Å. The fifth coordination site at each copper centre involves an amide oxygen from a neighbouring molecule (Cu(1)—O 2.371(4), Cu(2)—O 2.413(3) Å) in a staggered intermolecular array. Very strong antiferromagnetic exchange is observed in both cases (−2J = 689 ± 7 cm−1 (II), −2J = 816 ± 8 cm−1 (III)). Keywords: macrocycles, binuclear copper(II) complexes.

scholarly journals The crystal and molecular structure of the bis(N,N,N′,N′-tetramethylethanediamine) adduct of I(Br)InInBr2, In2Br3I•2C6H16N2, an indium–indium bonded molecule

1984 ◽  
Vol 62 (3) ◽  
pp. 601-605 ◽  
Author(s):  
Masood A. Khan ◽  
Clovis Peppe ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Orthorhombic Space Group ◽  
Trigonal Bipyramidal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Distorted Trigonal Bipyramidal

The crystal structure of the title compound has been determined by the heavy atom method. The crystals are orthorhombic, space group Pbca, with unit cell dimensions a = 22.795(3) Å, b = 17.518(2) Å, c = 12.396(3) Å, Z = 8; R = 0.0409 for 1527 unique "observed" reflections. The structure is disordered, with each halogen site (X) occupied by 75% Br, 25% I. The molecule consists of two X2(tmen)In units (tmen = N,N,N′,N′-tetramethylethanediamine) with distorted trigonal bipyramidal geometry, joined by an In—In bond 2.775(2) Å in length.

scholarly journals Syntheses, Structures, Magnetic Properties and Antibacterial Activities of Two Copper(II) Azido Complexes with Varied Nuclearities Containing Symmetrical 1,3-Diammine as Chelator

2021 ◽  
Vol 33 (2) ◽  
pp. 359-366
Author(s):  
Habibar Chowdhury ◽  
Chandan Adhikary
Keyword(s):  
Hydrogen Bonds ◽  
Variable Temperature ◽  
Antibacterial Activities ◽  
Metal Centers ◽  
X Ray ◽  
Pyramidal Geometry ◽  
Azide Ion ◽  
3D Network ◽  
Square Pyramidal Geometry ◽  
Dinuclear Structure

Two copper(II) azido complexes of the types mononuclear [Cu(TMEDA)2(N3)2] (1) and dinuclear [Cu(TMEDA)(μ1,1-N3)(N3)]2 (2) [TMEDA = trimethylenediamine; N3 – = azide ion] have been synthesized and characterized. X-ray structural analysis revealed that each copper(II) center in complex 1 adopts a distorted octahedron geometry with a CuN6 chromophore ligated through four N atoms of two different symmetrical TMEDA ligands as bidentate chelator and two N atoms of two terminal azides. In complex 2, each copper(II) center adopts a distorted square pyramidal geometry with a CuN5 chromophore ligated through two N atoms of TMEDA as bidentate chelator and two N atoms of two different azides as μ1,1-N3 bridging mode and one N atom of terminal azide ion. The two copper centers are connected through double μ1,1-N3 bridges affording a dinuclear structure with Cu···Cu separation 3.327(2) Å. In crystalline state, mononuclear units in complex 1 are associated through intermolecular N-H···N and C-H···N hydrogen bonds to form a 2D sheet structure viewed along crystallographic b-axis, whereas dinuclear entities in complex 2 are propagated through intermolecular N-H···N and C-H···N hydrogen bonds to form a 3D network structure viewed along crystallographic a-axis. The Variable-temperature magnetic susceptibility measurement evidenced a dominant antiferromagnetic interaction between the metal centers through μ1,1-azide bridges in complex 2 with J = − 0.40 cm-1. The antibacterial activities of the complexes have also been studied.

scholarly journals Chiral crystallization of a zinc(II) complex

2021 ◽  
Vol 77 (5) ◽  
pp. 542-546
Author(s):  
Shabana Noor ◽  
Shintaro Suda ◽  
Tomoyuki Haraguchi ◽  
Fehmeeda Khatoon ◽  
Takashiro Akitsu
Keyword(s):  
Hydrogen Bond ◽  
Schiff Base ◽  
Complex Molecule ◽  
Solvent Molecule ◽  
Hirshfeld Surface ◽  
Supramolecular Interactions ◽  
Orthorhombic Space Group ◽  
Complex Molecules ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The compound, {6,6′-dimethoxy-2,2′-[(4-azaheptane-1,7-diyl)bis(nitrilomethanylidyne)]diphenolato}zinc(II) methanol monosolvate, [Zn(C22H27N3O4)]·CH3OH, at 298 K crystallizes in the orthorhombic space group Pna21. The Zn atom is coordinated by a pentadentate Schiff base ligand in a distorted trigonal–bipyramidal N3O2 geometry. The equatorial plane is formed by the two phenolic O and one amine N atom. The axial positions are occupied by two amine N atoms. The distorted bipyramidal geometry is also supported by the trigonality index (τ), which is found to be 0.85 for the molecule. In the crystal, methanol solvent molecule is connected to the complex molecule by an O—H...O hydrogen bond and the complex molecules are connected by weak supramolecular interactions, so achiral molecules generate a chiral crystal. The Hirshfeld surface analysis suggests that H...H contacts account for the largest percentage of all interactions.

Sign in / Sign up

Export Citation Format

Share Document