Five-coordination in complexes of 2-(3,5-Dimethylpyrazol-1-yl)quinoline, a sterically hindered diimine system

1984 ◽  
Vol 37 (12) ◽  
pp. 2421 ◽  
Author(s):  
AT Baker ◽  
NJ Ferguson ◽  
HA Goodwin
Keyword(s):  
Water Molecule ◽  
Cobalt Complex ◽  
X Ray Diffraction ◽  
Iron Cobalt ◽  
Coordination Environment ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Cobalt Nickel ◽  
Metal Atoms ◽  
Sterically Hindered Diimine

The bidentate diimine-type ligand 2-(3,5-dimethylpyrazol-1-yl)quinoline forms mono complexes with the bivalent chlorides of iron, cobalt, nickel and copper. These complexes are magnetically dilute, but electronic spectral data indicate that, except for the cobalt complex which is tetrahedral, the metal atoms are five-coordinate and hence a chloro-bridged structure is proposed. The cobalt(II) complex readily adds a water molecule, and structure determination by X-ray diffraction shows that the complex aquadichloro[2-(3,5-dimethylpyrazol-1-yl)quinoline]cobalt(II) is monomeric and five-coordinate, the coordination environment approximating trigonal bipyramidal.

scholarly journals Synthesis, Characterization, Crystal Structures, and Urease Inhibition of Copper(II) and Zinc(II) Complexes Derived from Benzohydrazones

2020 ◽  
Vol 67 (4) ◽  
pp. 1155-1162
Author(s):  
Fu-Ming Wang ◽  
Li-Jie Li ◽  
Guo-Wei Zang ◽  
Tong-Tong Deng ◽  
Zhong-Lu You
Keyword(s):  
Single Crystal ◽  
Urease Inhibition ◽  
X Ray Diffraction ◽  
Inhibitory Effects ◽  
Strong Activity ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Metal Atoms ◽  
Vis Spectroscopy ◽  
Crystal Structural

A new copper(II) complex [Cu(L1)(NCS)(CH3OH)] (1) and a new zinc(II) complex [ZnCl2(HL2)] · CH3OH (2), derived from 4-bromo-N’-(pyridin-2-ylmethylene)benzohydrazide (HL1) and 4-methoxy-N’-(pyridin-2-ylmethylene)benzohydrazide (HL2), were prepared and characterized by elemental analysis, IR and UV-Vis spectroscopy and single crystal X-ray diffraction. The hydrazone HL1 coordinates to the Cu atom in enolate form, while the hydrazone HL2 coordinates to the Zn atom in carbonyl form. Single crystal structural analyses indicate that the hydrazones coordinate to the metal atoms through the pyridine N, imino N, and enolate/carbonyl O atoms. The Cu atom in complex 1 is in square pyramidal coordination, and the Zn atom in complex 2 is in trigonal-bipyramidal coordination. The inhibitory effects of the complexes on Jack bean urease were studied, which show that the copper complex has strong activity on urease.

scholarly journals Study on the Photoluminescent and Thermal Properties of Zinc Complexes with a N6O4 Macrocyclic Ligand

Molecules ◽  
2018 ◽  
Vol 23 (7) ◽  
pp. 1735 ◽  
Author(s):  
Xingyong Xue ◽  
Qijun Wang ◽  
Fusen Mai ◽  
Xing Liang ◽  
Yichen Huang ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Macrocyclic Ligand ◽  
Quantum Yields ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Fluorescence Quantum Yields ◽  
Solid States ◽  
Trigonal Bipyramidal ◽  
Decomposition Processes

Reactions between a N6O4 macrocyclic ligand (L1) and several Zn(II) salts (trifluoromethane sulfonate, p-toluenesulfonate, acetate, benzoate, o-, m- or p-hydroxybenzoate) led to the formation of seven complexes, [Zn2L1 (DMSO)4](OSO2CF3)4 (1), [Zn2(p-OSO2PhCH3)4L1] (2), [Zn2(OCOCH3)4L1] (3), [Zn2(OCOPh)4L1] (4), [Zn2(o-OCOPhOH)4L1] (5), [Zn2(m-OCOPhOH)4 L1] (6) and [Zn2(p-OCOPhOH)4 L1] (7), which were characterized by elemental analysis, 1H-NMR, 13C-NMR, IR, fluorescence spectroscopies and single crystal X-ray diffraction. In 1, the Zn atom is pentacoordinated with a N3O2 irregular trigonal bipyramidal coordination environment, like the geometries in compounds 3–7, whereas in structure 2 the metal atom is envisaged as possessing a distorted N3O3 octahedronal environment. All the compounds show interesting photoluminescent properties in solid states and solutions in DMF and DMSO, which are reported along with their TG-DTA thermal decomposition processes, UV-vis absorption spectroscopy and fluorescence quantum yields in DMF and DMSO.

More crystal field theory in action: the metal–4-picoline (pic)–sulfate [M(pic) x ]SO4 complexes (M = Fe, Co, Ni, Cu, Zn, and Cd)

2019 ◽  
Vol 75 (5) ◽  
pp. 568-574 ◽  
Author(s):  
Duyen N. K. Pham ◽  
Mrittika Roy ◽  
Ava Kreider-Mueller ◽  
James A. Golen ◽  
David R. Manke
Keyword(s):  
Crystal Structure ◽  
Field Theory ◽  
Crystal Structures ◽  
Crystal Field ◽  
Crystal Field Theory ◽  
Iron Cobalt ◽  
Coordination Environment ◽  
Trigonal Bipyramidal ◽  
Cobalt Nickel ◽  
Sulfate Complexes

Seven crystal structures of five first-row (Fe, Co, Ni, Cu, and Zn) and one second-row (Cd) transition metal–4-picoline (pic)–sulfate complexes of the form [M(pic) x ]SO4 are reported. These complexes are catena-poly[[tetrakis(4-methylpyridine-κN)metal(II)]-μ-sulfato-κ2 O:O′], [M(SO4)(C6H7N)4] n , where the metal/M is iron, cobalt, nickel, and cadmium, di-μ-sulfato-κ4 O:O-bis[tris(4-methylpyridine-κN)copper(II)], [Cu2(SO4)2(C6H7N)6], catena-poly[[bis(4-methylpyridine-κN)zinc(II)]-μ-sulfato-κ2 O:O′], [Zn(SO4)(C6H7N)2] n , and catena-poly[[tris(4-methylpyridine-κN)zinc(II)]-μ-sulfato-κ2 O:O′], [Zn(SO4)(C6H7N)3] n . The Fe, Co, Ni, and Cd compounds are isomorphous, displaying polymeric crystal structures with infinite chains of M II ions adopting an octahedral N4O2 coordination environment that involves four picoline ligands and two bridging sulfate anions. The Cu compound features a dimeric crystal structure, with the CuII ions possessing square-pyramidal N3O2 coordination environments that contain three picoline ligands and two bridging sulfate anions. Zinc crystallizes in two forms, one exhibiting a polymeric crystal structure with infinite chains of ZnII ions adopting a tetrahedral N2O2 coordination containing two picoline ligands and two bridging sulfate anions, and the other exhibiting a polymeric crystal structure with infinite chains of ZnII ions adopting a trigonal bipyramidal N3O2 coordination containing three picoline ligands and two bridging sulfate anions. The structures are compared with the analogous pyridine complexes, and the observed coordination environments are examined in relation to crystal field theory.

scholarly journals First cobalt complexes with methyl pyruvate semi/thiosemicarbazone - synthesis, physico-chemical and structural characterization

2020 ◽  
Vol 85 (4) ◽  
pp. 453-466
Author(s):  
Marko Rodic ◽  
Vukoslava Miskov-Pajic ◽  
Vukadin Leovac ◽  
Mirjana Radanovic ◽  
Ljiljana Vojinovic-Jesic ◽  
...  
Keyword(s):  
Magnetic Measurements ◽  
Magnetic Moments ◽  
Central Metal ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Imine Nitrogen ◽  
Metal Atoms ◽  
Physico Chemical ◽  
Methyl Pyruvate

In the reaction of acetone solutions of CoX2?nH2O (X = Cl, Br) with methyl pyruvate semi/thiosemicarbazone (Hmps, Hmpt) the first Co(II) complexes with these ligands, i.e., [Co(Hmps)(H2O)X2] (X = Cl (1), Br (2)), [Co(Hmpt)2][CoCl4]?2H2? (3) and [Co(Hmpt)2]Br2?Me2CO (4) were obtained. Complexes 1 and 2 represent the first examples of metal complexes of Hmps. All the obtained compounds were characterized by elemental analysis, conductometry, magnetic measurements, and IR spectra, and for complexes 2?4, single crystal X-ray diffraction analysis was also performed. The effective magnetic moments were close to the upper limit (5 ?B) for complexes 1 and 2, and close to the lower limit (4.4 ?B) for complexes 3 and 4, and as such are characteristic for high-spin Co(II) complexes. Structural analysis showed that both ligands coordinate in a neutral form in a tridentate manner, via the ester oxygen, imine nitrogen and the oxygen atom of the ureido (Hmps), or the sulfur atom of the thioureido group (Hmpt). The central metal atoms are situated in a deformed octahedral coordination environment. Complex 2 has cis-Br configuration, while complexes 3 and 4 have mer-configuration.

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

A Simple High-Yield Synthesis of Gallium(I) Tetrachlorogallate(III) and the Reaction of Digallium Tetrachloride Tetrahydrofuran Solvate with 1,2-Diols

2001 ◽  
Vol 56 (4-5) ◽  
pp. 337-341 ◽  
Author(s):  
Eva S. Schmidt ◽  
Annette Schier ◽  
Norbert W. Mitzel ◽  
Hubert Schmidbaur
Keyword(s):  
Crystalline Phase ◽  
Hydrogen Gas ◽  
High Yield ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Atoms ◽  
Gallium Hydride ◽  
Hydroxy Groups ◽  
Tetrahydrofuran Solution ◽  
Analogous Product

Abstract Gallium(I) tetrachlorogallate(III) Ga[GaCU] was prepared in quantitative yield by thermal de­composition of dichlorogallane [HGaCl2]2, which is readily available from Et3SiH and [GaCl3]2. The reaction of catechol with solutions of this gallium(I) tetrachlorogallate(III) in tetrahydrofuran leads to the evolution of hydrogen gas and affords a dinuclear gallium(III) complex with penta-coordinate metal atoms chelated and bridged by mono-deprotonated catechol ligands. In the crystalline phase tetrahydrofuran molecules are hydrogen-bonded to the hydroxy groups: [Ga(1,2 -OC6H4OH)Cl2(C4H8O)]2. The reaction with pinacol also gives hydrogen and the analogous product [Ga(OCMe2CMe2OH)Cl2(C4H8O)]2. The structures of the two compounds have been determined by X-ray diffraction. A mechanism of the new reaction has been proposed which involves oxidative addition of the diol to the solvate (THF)Cl2Ga-GaCl2(THF) present in the tetrahydrofuran solution to give a gallium hydride intermediate.

scholarly journals A Covalent Organic Cage Compound Acting as a Supramolecular Shadow Mask for the Regioselective Functionalization of C60

2020 ◽  
Author(s):  
Viktoria Leonhardt ◽  
Stefanie Fimmel ◽  
Ana-Maria Krause ◽  
Florian Beuerle
Keyword(s):  
Mass Spectrometry ◽  
Single Crystal ◽  
High Selectivity ◽  
Shadow Mask ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Cage Compound ◽  
Vis Spectroscopy ◽  
Regioselective Functionalization

<div><div><div><p>A trigonal-bipyramidal covalent organic cage compound serves as an efficient host to form stable 1:1-complexes with C60 and C70. Fullerene encapsulation has been comprehensively studied by NMR and UV/Vis spectroscopy, mass spectrometry as well as single-crystal X-ray diffraction. Exohedral functionalization of encapsulated C60 via threefold Prato reaction revealed high selectivity for the symmetry-matched all-trans-3 addition pattern.</p></div></div></div>

scholarly journals Crystal structure refinement of magnesium zinc divanadate, MgZnV2O7, from powder X-ray diffraction data

2021 ◽  
Vol 77 (6) ◽  
pp. 588-591
Author(s):  
Stephanie J. Hong ◽  
Jun Li ◽  
Mas A. Subramanian
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Structure Refinement ◽  
Atomic Ratio ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Wyckoff Position ◽  
Distorted Trigonal Bipyramidal

The crystal structure of magnesium zinc divanadate, MgZnV2O7, was determined and refined from laboratory X-ray powder diffraction data. The title compound was synthesized by a solid-state reaction at 1023 K in air. The crystal structure is isotypic with Mn0.6Zn1.4V2O7 (C2/m; Z = 6) and is related to the crystal structure of thortveitite. The asymmetric unit contains two metal sites with statistically distributed magnesium and zinc atoms with the atomic ratio close to 1:1. One (Mg/Zn) metal site (M1) is located on Wyckoff position 8j and the other (M2) on 4h. Three V sites (all on 4i), and eight O (three 8j, four 4i, and one 2b) sites complete the asymmetric unit. The structure is an alternate stacking of V2O7 layers and (Mg/Zn) atom layers along [20\overline{1}]. It is distinct from other related structures in that each V2O7 layer consists of two groups: a V2O7 dimer and a V4O14 tetramer. Mixed-occupied M1 and M2 are coordinated by oxygen atoms in distorted trigonal bipyramidal and octahedral sites, respectively.

Crystal Structure of Calcium Picrate Pentahydrate: A New Eight-Coordinate Stereochemistry for [M(bidentate)2(unidentate)4]

1979 ◽  
Vol 32 (2) ◽  
pp. 301 ◽  
Author(s):  
V Diakiw ◽  
TW Hambley ◽  
DL Kepert ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Title Compound ◽  
Lattice Site ◽  
The Other ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Triangular Face ◽  
X Ray

The crystal structure of the title compound, Ca(C6H2N307)2,5H2O, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.049 for 1513 'observed' reflections. Crystals are orthorhombic, Pmab, a 24.169(6), b l0.292(7), c 8.554(2) �, Z 4. The stereochemistry about the calcium has not been observed previously for the system [M(bidentate)2- (unidentate)4]; in the present structure, the calcium is coordinated by a pair of bidentate picrate ligands and the four water molecules in an array in which three of the water molecules occupy a triangular face of a square antiprism, the overall array having m symmetry. The remaining water molecule occupies a lattice site with no close interaction with the other species.

X-ray diffraction study of oxygen-conducting compoundsLn2Mo2O9(Ln= La, Pr)

2014 ◽  
Vol 70 (4) ◽  
pp. 669-675 ◽  
Author(s):  
Alexander M. Antipin ◽  
Olga A. Alekseeva ◽  
Natalia I. Sorokina ◽  
Alexandra N. Kuskova ◽  
Michail Yu. Presniakov ◽  
...  
Keyword(s):  
Room Temperature ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
Ion Migration ◽  
Transmission Microscopy ◽  
Coordination Environment ◽  
X Ray ◽  
Oxygen Ions ◽  
Oxygen Ion ◽  
Oxygen Ion Migration

The La2Mo2O9(LM) and Pr2Mo2O9(PM) single crystals are studied using precision X-ray diffraction and high-resolution transmission microscopy at room temperature. The crystal structures are determined in the space groupP213. La and Pr atoms, as well as Mo1 and O1 atoms, are located in the vicinity of the threefold axes rather than on the axes as in the high-temperature cubic phase. In both structures studied, the O2 and O3 positions are partially occupied. The coexistence of different configurations of the Mo coordination environment facilitates the oxygen-ion migration in the structure. Based on the X-ray data, the activation energies of O atoms are calculated and the migration paths of oxygen ions in the structures are analysed. The conductivity of PM crystals is close to that of LM crystals. The O2 and O3 atoms are the main contributors to the ion conductivity of LM and PM.

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