Preparation and Crystal Structure of Silver(I) Anthranilate

1999 ◽  
Vol 52 (4) ◽  
pp. 325 ◽  
Author(s):  
Graham Smith ◽  
Colin H. L. Kennard ◽  
Karl A. Byriel
Keyword(s):  
Major Constituent ◽  
Monoclinic Space Group ◽  
Zigzag Chain ◽  
Aminobenzoic Acid ◽  
X Ray Diffraction ◽  
Amine Nitrogen ◽  
Chain Polymer ◽  
X Ray ◽  
A Cell ◽  
Planar Angle

Silver(I) anthranilate, [Ag2(C7H6NO2)2]n, was isolated as the major constituent in the attempted preparation of the adduct of anthranilic acid (2-aminobenzoic acid) with silver(I) p-toluenesulfonate and its structure has been determined by using single-crystal X-ray diffraction. Crystals of the complex are monoclinic, space group P 21/n, with two dimers in a cell of dimensions a 5·3516(8), b 4·9746(2), c 25·386(5) Å, β 91· 547(8)°. The complex repeating unit comprises a distorted centrosymmetric biscarboxylato(-O,O′)-bridged dimer [Ag−O, 2·223, 2·409(4) Å; Ag---Ag 2·9128(9) Å] but has, in addition, a third bond to an adjacent amine nitrogen [Ag−N, 2·301(5) Å], which extends the structure into a zigzag chain polymer. The stereochemistry about each Ag centre is distorted trigonal planar [angle range, 89·9−142·9(2)°]. Relatively short inter-dimer Ag---Ag separations [2·989(1) Å] are also present.

A New Supramolecular Synthon Using N-Methylaniline. The Crystal Structure of the 1 : 1 Adduct of N-Methylaniline with 5-Nitrofuran-2-carboxylic Acid

1998 ◽  
Vol 51 (9) ◽  
pp. 867 ◽  
Author(s):  
Daniel E. Lynch ◽  
Lisa C. Thomas ◽  
Graham Smith ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Proton Transfer ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Supramolecular Synthon ◽  
X Ray ◽  
C 23 ◽  
A Cell

The crystal structure of the 1 : 1 adduct of N-methylaniline with 5-nitrofuran-2-carboxylic acid has been determined by single-crystal X-ray diffraction. Crystals are monoclinic, space group P21/c with Z 4 in a cell of dimensions a 8·467(5), b 6·106(2), c 23·95(1) Å, β 94·48(3)°. The molecules associate in a tetrameric, proton-transfer formation which has potential as a new supramolecular synthon.

Crystal and molecular structure of Z- and E-1,2-dichloro-1,2-bis(2-chlorophenyl)ethylene. An X-ray and NMR study

1995 ◽  
Vol 73 (9) ◽  
pp. 1520-1525
Author(s):  
Luciano Antolini ◽  
Ugo Folli ◽  
Dario Iarossi ◽  
Adele Mucci ◽  
Silvia Sbardellati ◽  
...  
Keyword(s):  
Chemical Shifts ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Nmr Study ◽  
Phenyl Rings ◽  
A Cell ◽  
C Nmr

The crystal structures of the title compounds were determined by single crystal X-ray diffraction techniques. The molecule of the Z isomer, which crystallizes in the monoclinic space group C2/c with Z = 4 in a cell of dimensions a = 14.891 (2), b = 10.780(2), c = 8.769(1) Å, β = 97.47(2)°, V = 1395.7(7) Å3 has crystallographic twofold symmetry. The E form crystallizes in the orthorhombic space group Pbca with a = 11.730(1), b = 6.932(1), c = 16.841(1) Å, V = 1369.4(2) Å3 and Z = 4. Its molecules have crystallographically dictated [Formula: see text] symmetry. In both isomers the phenyl rings are roughly perpendicular to the average ethylene plane. The atoms characterizing this plane show significant deviations from planarity in the Z isomer. Marked bond-angle distortions at the ethene carbons of both structures are observed. The 1H and 13C NMR spectra of the compounds were measured and, particularly in the case of the 1H chemical shifts, fall into two quite separate spectral regions. At low temperature, two conformational isomers, those with different relative orientation of the C—Cl bonds of the phenyl rings, are observed in the spectrum of each compound. Keywords: chlorostilbenes, overcrowded molecules. X-ray structure, conformations, NMR spectroscopy.

Metal complexes of dicamba: the crystal and molecular structures of dicamba(3,6-Dichloro-2-methoxybenzoic acid) and catena-μ-Aqua-diaquabis(3,6-dichloro-2-methoxybenzoato)zinc(II) dihydrate

1983 ◽  
Vol 36 (11) ◽  
pp. 2175 ◽  
Author(s):  
G Smith ◽  
EJ O'Reilly ◽  
CHL Kennard
Keyword(s):  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bridging Ligand ◽  
Methoxy Groups ◽  
A Cell ◽  
Methoxybenzoic Acid

The crystal structures of the herbicide, dicamba (3,6-dichloro-2-methoxybenzoic acid) and the zinc(II) complex of this acid, {[Zn(dicamba)2(H2O)3].2H2O}}n (1), have been determined from X-ray diffraction data and refined by least squares to final residuals of 0.034 and 0.043 respectively. Dicamba is triclinic, space group P1, Z 2 with a cell a 7.232(1), b 7.971(1), c 9.050(3) �, α 102.76(3), β 91.33(3), γ 110.38(1)�, while (1) is monoclinic, space group P21/n, Z 4 with a cell a 10.467(1), b 8.135(3), c 28.079(2) �, β 96.497(7)�. Dicamba forms hydrogen-bonded cyclic dimers [O---O, 2.655(7) �] with the carboxyl and the methoxy groups synclinal to the benzene ring. The dicamba ligands retain their conformation in the ZnII complex and are cis-related and unidentate [Zn-0,2.083,2.095(4) �]. Three of the waters are coordinated [Zn-0, 2.036, 2.055, 2.099(4) �] with one of these also acting as a bridging ligand between the octahedral zinc centres [Zn-0, 2.326(4) �], giving a 'linear' polymer structure [Zn-0-Zn bridge angle, 133.6(3)�]. The MnII and CoII complexes of dicamba [(2) and (3)] have been confirmed as isomorphous and isostructural with the ZnII analogue.

The crystal structure of a binuclear cobalt(II) complex of a macrocyclic ligand

1975 ◽  
Vol 28 (12) ◽  
pp. 2607 ◽  
Author(s):  
BF Hoskins ◽  
GA Williams
Keyword(s):  
Crystal And Molecular Structure ◽  
Bromine Atom ◽  
Macrocyclic Ligand ◽  
Cobalt Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
R Factor ◽  
Central Carbon ◽  
A Cell

The crystal and molecular structure of LCo2Br2,CH3OH (where LH2 represents the macrocycle obtained by condensation of two molecules each of propane-1,3-diamine and 2-hydroxy-5-methyl-isophthalaldehyde) has been determined by single-crystal X-ray diffraction techniques. The compound crystallizes in the monoclinic space group P21/c with two molecules in a cell of dimensions a 9.8723(5), b 16.891(1), c 8.0745(5)Ǻ and 102.06(1)�. Counter methods were used to collect the 2004 independent reflections above background and the structure was refined by least-squares methods to a conventional R-factor of 0.049. The structure is molecular, consisting of discrete binuclear units LCo2Br2,CH3OH, containing two cobalt(II) atoms separated by 3.158(2) Ǻ. Each cobalt atom is in an identical pseudo-square-pyramidal environment, in agreement with the conclusion drawn from the electronic spectrum of the complex, with an N2O2 basal plane and a bromine atom coordinated at the apex. The methanol molecule is disordered and partially occupies the sixth coordination site of each cobalt, with a long bond of 2.503(9) Ǻ between the cobalt and the methanol oxygen atom. The central carbon atom of the propane-1,3-diamine residue is also disordered, occupying partially each of two positions.

Crystal structure of 9-Oxofluorene-4-carboxylic acid

1981 ◽  
Vol 34 (5) ◽  
pp. 1143 ◽  
Author(s):  
CHL Kennard ◽  
G Smith ◽  
GF Katekar
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
A Cell

The crystal structure of 9-oxofluorene-4-carboxylic acid has been determined by direct methods using three-dimensional X-ray diffraction data, and refined to R0·068 for 1323 'observed' reflections. Crystals are monoclinic, space group P21/c with 24 in a cell of dimensions a 3·843(3), b 7·986(5), c 3269(2) �, β 96·64(4)�. The molecules form centrosymmetric hydrogen-bonded cyclic dimers [O···O 2·642(3) �] with the plane of the carboxylic acid making an angle of 26·5� with that of the 9-oxofluorene group. Stacks of molecules form down the a axis with 3.843 �. separation.

Synthesis and Characterization of a Zinc(II) Complex of Bispicen

2013 ◽  
Vol 68 (12) ◽  
pp. 1327-1332 ◽  
Author(s):  
Beatriz S. Parajón-Costa ◽  
Gustavo A. Echeverría ◽  
Oscar E. Piro ◽  
Enrique J. Baran
Keyword(s):  
Crystal And Molecular Structure ◽  
Chloride Ion ◽  
Monoclinic Space Group ◽  
Tetradentate Ligand ◽  
X Ray Diffraction ◽  
Amine Nitrogen ◽  
X Ray ◽  
Octahedral Environment ◽  
Distorted Octahedral

The synthesis of a Zn(II) complex of bispicen, the tetradentate ligand N,N′-bis(2-pyridylmethyl)- ethylenediamine, of composition [Zn(bispicen)Cl(H2O)]2[ZnCl4] is reported. Its crystal and molecular structure was determined by single-crystal X-ray diffraction methods. It crystallizes in the monoclinic space group C2=c with Z =4 molecules per unit cell. The Zn(II) cation in the [Zn(bispicen)Cl(H2O)]+ complex is in a distorted octahedral environment, coordinated to a neutral bispicen molecule acting as a tetradentate ligand through its two amine nitrogen atoms, at cis positions, and its two pyridyl N atoms, at trans positions. The six-fold coordination is completed by a chloride ion and a water molecule. The tetrahedral [ZnCl4]2- counter-ion lies on a crystallographic twofold axis. The complex was further characterized by FTIR spectroscopy, and its vibrational behavior compared with that of the dihydrated tetrahydrochloride of free bispicen

Preparation of Some Pyrrole-3,4-dicarboxylic Acid Derivatives and the Crystal Structure of 2-Methylpyrrolo[3,4-c]pyrrole-1,3(2H,5H)-dione

1991 ◽  
Vol 44 (2) ◽  
pp. 323 ◽  
Author(s):  
DP Arnold ◽  
LJ Nitschinsk ◽  
CHL Kennard ◽  
G Smith
Keyword(s):  
Crystal Structure ◽  
Dicarboxylic Acid ◽  
Substituent Effects ◽  
Ring System ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Fused Ring ◽  
A Cell ◽  
Fused Ring System

A series of pyrrole-3,4-dicarboxylic acid derivatives has been prepared, and the crystal structure of one, 2-methylpyrrolo[3,4-c]pyrrole-1,3(2H,5H)- dione, has been determined by X-ray diffraction and refined to a residual R 0.049 for 1415 observed reflections. Crystals are monoclinic, space group P21/c, with Z= 8 in a cell of dimensions a 14.775(3), b 7.0692(5), c 15.151(3)Ǻ, β 118.82(8)�. Strain in the planar fused ring system is evident from the widening of the external interring angles to 143°, and from the unusual substituent effects in the 13C n.m.r. spectra.

The Preparation and Crystal Structure of Ammonium Bis[citrato(3-)]cuprate(II)

1991 ◽  
Vol 44 (10) ◽  
pp. 1495 ◽  
Author(s):  
RC Bott ◽  
DS Sagatys ◽  
DE Lynch ◽  
G Smith ◽  
CHL Kennard ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Citric Acid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Teller Distortion ◽  
Space Group ◽  
X Ray ◽  
Jahn Teller ◽  
A Cell ◽  
Jahn Teller Distortion

The copper(II) complex with citric acid (NH4)4 [Cu(C6H5O7)2] has been prepared, and its structure determined by X-ray diffraction, giving a residual R 0.035 for 1208 observed reflections. Crystals are monoclinic, space group P21/c with Z 2 in a cell of dimensions a 8.755(3), b 13.185(4), c 9.364(2)Ǻ, β 113.73(2)°. The complex is a centrosymmetric six-coordinate monomer which is isomorphous with ammonium zinc(II) citrate. However, the Cu-O(hydroxyl) bonds [2.341(3)Ǻ] show Jahn-Teller distortion relative to the Cu-O(carboxyl) bonds [1.969(3) and 1.977(3)Ǻ].

Reactions of benzo[b]thiophene with some aqueous platinum metal species at elevated temperatures

1991 ◽  
Vol 69 (4) ◽  
pp. 590-598 ◽  
Author(s):  
Peter D. Clark ◽  
James F. Fait ◽  
Colin G. Jones ◽  
Martin J. Kirk
Keyword(s):  
Elevated Temperatures ◽  
Fourier Method ◽  
Platinum Metal ◽  
Metal Species ◽  
Monoclinic Space Group ◽  
Mechanistic Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
A Cell

The desulfurization of benzo[b]thiophene 1 with aqueous transition metal species in the presence of various hydrocarbons at elevated temperatures is described. Mechanistic studies have shown that treatment of 1 with solutions of RuCl3 and other platinum metal species results in the formation of 2,3-dihydrobenzo[b]thiophene 2 and ethylbenzene 3 as major products. Metal coordinated species are probable intermediates in the formation of 2 and hydrocarbon products. 2 readily coordinates to PdCl2 to form square-planar trans-dichlorobis(2,3-dihydrobenzo[b]thiophene) palladium(II), which decomposes to ethylbenzene at 300 °C. The crystal structure of the complex was determined by a single crystal X-ray diffraction study. The complex crystallized in the monoclinic space group C 2/c with Z = 8 in a cell of dimensions a = 23.057 (3), b = 9.711 (1), c = 15.227 (2) Å and β = 99.74(1)°. The structure was solved by the Fourier method and was refined by full-matrix least-squares calculations to R = 0.042 for 2537 observed data with I > 2.5σ(I). Key words: benzo[b]thiophene, desulfurization, platinum metal species.

Preparation and Crystal Structures of the Urea Adducts of Silver(I) Perchlorate and Silver(I) p-Toluenesulfonate

1997 ◽  
Vol 50 (7) ◽  
pp. 741 ◽  
Author(s):  
Graham Smith ◽  
Brett A. Cloutt ◽  
Karl A. Byriel ◽  
Colin H. L. Kennard
Keyword(s):  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Urea Molecule ◽  
Amine Nitrogen ◽  
Space Group ◽  
Trigonal Bipyramidal ◽  
Square Planar ◽  
A Cell ◽  
Ribbon Structure ◽  
Urea Adducts

The urea adducts with silver(I) perchlorate (2 : 1) (1) and silver(I) p-toluenesulfonate (1 : 1) (2) have been prepared and their structures determined by single-crystal X-ray diffraction methods. Crystals of adduct (1) are monoclinic, space group P21/a, with four molecules in a cell with dimensions a 7·806(2), b 15·929(2), c 7·861(3) Å, β 113·35(1)°, while (2) is also monoclinic, space group P21, with two dimer units in a cell with a 5·380(3), b 25·72(2), c 7·926(5) Å, β 94·22(3)°. Both form polymer structures which are stabilized by extensive hydrogen bonding. Adduct (1) is based upon a square planar trans-AgN2O2 repeating unit involving bonds to the two independent urea molecule with the perchlorate anion uncoordinated, while with (2), the oxygens of two urea molecules bridge two trigonal bipyramidal (AgNO4) silver centres, forming cyclic pseudo-centrosymmetric four-membered dimer repeats. The silver coordination of (2) also includes two cis-related sulfonate oxygens from bridging p-toluenesulfonate ligands, as well as a third bridging urea amine nitrogen. The result is a step-polymer ribbon structure.

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