scholarly journals Synthesis and Crystal Structure Differences between Fully and Partially Fluorinated β-Diketonate Metal (Co2+, Ni2+, and Cu2+) Complexes

2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Akiko Hori ◽  
Masaya Mizutani

Coordination complexes, [Co2(1)4(H2O)2] (2), [Ni2(1)4(H2O)2] (3), and [Cu(1)2] (4), by using an asymmetric and partially fluorinated 3-hydroxy-3-pentafluorophenyl-1-phenyl-2-propen-1-one (H1) have been prepared, and the structures were investigated to compare with the corresponding fully fluorinated complexes of [Co2(5)4(H2O)2] (6), [Ni2(5)4(H2O)2] (7), and [Cu(5)2] (8) with bis(pentafluorobenzoyl)methane (H5) and to understand the fluorine-substituted effects. While the coordination mode of the partially fluorinated complexes was quite similar to the fully fluorinated complexes, the intra- and intermolecular π-interactions of the ligand moieties were highly influenced by the fluorination effects; the arene-perfluoroarene interactions were observed in complexes 2 and 3 as a reason of the dinucleation. In this paper, we describe detail structures of the protonated form of the ligand, H1, and complexes 2–4 by X-ray crystallographic studies.

1977 ◽  
Vol 32 (9) ◽  
pp. 1001-1002 ◽  
Author(s):  
T. Stanley Cameron

The title complex was synthesised and its structure determined by x-ray crystallography. The structure contains two hydrogen bonds between the phosphoryl oxygen atom and the two meta-toluidinium ions. The P–N bond lengths are significantly different and the differences, attributed to varying p π-d π interactions along the bonds, confirm earlier observations on tri-para-toluidylphosphazenyl oxide.


2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.


2013 ◽  
Vol 803 ◽  
pp. 80-84
Author(s):  
Yu Qi Liu ◽  
Yong Yang ◽  
Rui Yang ◽  
Xiao Jun Xu

A novel metalorganic coordination polymer, namely [Co3(bpd)5.5(NCS)6(NH3)]n2H2O (1) (bpd=1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene), has been synthesized and characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. Compound 1 presents 2D[3,4,-connected 3-nodal net with the point symbol (4268210)(4462)(8210). In addition, four identical 2D single nets is interlocked with each other in parallel, thus directly leading to the formation of a polycatenated layer (2D2D).


2011 ◽  
Vol 396-398 ◽  
pp. 2338-2341
Author(s):  
Xing Chuan Wei ◽  
Zhi Li Liu ◽  
Kun Zhang ◽  
Zhi Yun Du ◽  
Xi Zheng

In this paper, (2E,6E)-2,6-Bis(2,3,4-tri-methoxy -benzylidene)cyclohexanone (omitted as tmbcho) (1) was obtained by the reaction of acetic acid, tetrahydrofuran, cyclohexanone and 2,3,4-tri-methoxy-benzaldehyde. Three non-classic hydrogen bonds were observed in the compound. X-ray crystallography shows that the crystal structure is stabilized by intermolecular C-H•••π interactions and it contains plenty of conjugated double bonds. The title compound was characterized by UV-vis and fluorescent spectral studies.


2013 ◽  
Vol 28 (1) ◽  
pp. 13-17 ◽  
Author(s):  
F. Laufek ◽  
A. Vymazalová ◽  
D.A. Chareev ◽  
A.V. Kristavchuk ◽  
J. Drahokoupil ◽  
...  

The (Ag,Pd)22Se6 phase was synthesized from individual elements by silica glass tube technique and structurally characterized from powder X-ray diffraction data. The (Ag,Pd)22Se6 phase crystallizes in Fm$\overline3$m symmetry, unit-cell parameters: a = 12.3169(2) Å, V = 1862.55(5) Å3, Z = 4, and Dc = 10.01 g/cm3. The crystal structure of the (Ag,Pd)22Se6 phase represents a stuffed 3a.3a.3a superstructure of the Pd structure (fcc), where only 4 from 108 available octahedral holes are occupied. Its crystal structure is related to the Cr23C6 structure type.


2013 ◽  
Vol 68 (2) ◽  
pp. 161-167 ◽  
Author(s):  
Muhammad Monim-ul-Mehbooba ◽  
Muhammad Ramzan ◽  
Tobias Rüffe ◽  
Heinrich Lang ◽  
Shafqat Naddem ◽  
...  

A cyanido-bridged Zn(II)-Ag(I) bimetallic coordination polymer, {[Zn(phen)2(H2O){Ag(CN)2}] [Ag(CN)2]·MeOH}n (1), was prepared using ZnCl2, 1,10-phenanthroline (phen) and K[Ag(CN)2] and characterized by IR spectroscopy, thermal analysis and X-ray crystallography. The crystal structure of 1 consists of dinuclear [Zn(phen)2(H2O){Ag(CN)2}]+ cations, [Ag(CN)2]- anions and a methanol molecule. The non-coordinated [Ag(CN)2]- anions are linked to the [Zn(phen)2(H2O){Ag(CN)2}]+ complex cations through argentophilic interactions leading to the formation of chains. The chains are connected by hydrogen bonds and π-π interactions to give a 3D network.


2009 ◽  
Vol 64 (1) ◽  
pp. 141-144 ◽  
Author(s):  
Yong Nie ◽  
Thomas Oeser ◽  
Walter Siebert

The dimer [(η5-C5Me5)Ru(C3B2Me5)RhCl]2 (2) reacts with 1,2-bis(diphenylphosphino)ethane (dppe) to give the triple-decker complex [(η5-C5Me5)Ru(C3B2Me5)Rh- (dppe)Cl] (3). Its constitution follows from NMR and MS data, and a single-crystal X-ray diffraction study.


1992 ◽  
Vol 47 (3) ◽  
pp. 301-304 ◽  
Author(s):  
Stefan Vogler ◽  
Kurt Dehnicke

The title compound has been prepared by the reaction o f [WCl4(NSeCl)]2 with PPh4Cl in CH2Cl2 solution. It forms red crystals, which were characterized by an X-ray structure determination. Space group P21/c, Z = 4, 3856 observed unique reflections, R = 0.073. Lattice dimensions at 25 °C: a = 2266.0(5), b = 1121.0(2), c = 2013.0(4) pm, β = 109.66(3)°. The structure consists o f PPh4+ ions and anions [WCl5(NSeCl2)]2-, in which the tungsten atom is surrounded in a distorted octahedral way by five chlorine atoms and by the nitrogen atom of the (NSeCl2)3- ligand. The W = N = SeCl2 group is characterized by WN and SeN double bonds; the selenium atom has a pseudo trigonal-bipyramidal coordination with the N atom and two lone pairs in equatorial and the chlorine atoms in axial positions.


1990 ◽  
Vol 45 (10) ◽  
pp. 1393-1397 ◽  
Author(s):  
Gerlinde Frenzen ◽  
Werner Massa ◽  
Thilo Ernst ◽  
Kurt Dehnicke

[VCl2(15-crown-5)]+[VOCl4]- has been prepared by the reaction of VCl4 with 15-crown-5 in acetonitrile solution in the presence of water, forming black-brown single crystals. They were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1530 observed unique reflexions, R = 0.052. Lattice dimensions at -120°C: a = 1128.5(4), b = 1063.3(3), c = 1680(1) pm. The compound forms ions, in which the cation contains vanadium(+III), which is seven coordinate by the five oxygen atoms of the crown ether molecule and by two chlorine atoms in axial positions of a pentagonal bipyramide. The [VOCl4]- anion contains vanadium (+V) with approximately tetragonal symmetry


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