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.

Heavy-Metal Complexes With (2-Chlorophenoxy)acetic Acid: The Crystal Structures of Polymeric Mercury(II) (2-Chlorophenoxy)acetate and the Thallium(I) (2-Chlorophenoxy)acetate(2-Chlorophenoxy)acetic Acid Adduct

1990 ◽  
Vol 43 (8) ◽  
pp. 1431 ◽  
Author(s):  
TCW Mak ◽  
WH Yip ◽  
CHL Kennard ◽  
G Smith
Keyword(s):  
Acetic Acid ◽  
Crystal Structures ◽  
Rotational Symmetry ◽  
Ligand Molecule ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
Acid Proton ◽  
Square Planar ◽  
A Cell

The crystal structures of the mercury(II) and thallium(I) complexes with (2-chlorophenoxy)acetic acid have been determined by X-ray diffraction, and refined to residual values R 0.040 and 0.060 for 1130 and 1612 observed reflections respectively. catena-[ Bis {(2- chlorophenoxy ) acetato }mercury(II)] is monoclinic, space group Cc with Z 4 in a cell of dimensions a 25.449(7), b 7.335(2), c 10.154(1) Ǻ, β 112.83(2)°. Mercury is bonded linearly to two carboxylate oxygens [Hg-O, 2.02(1), 2.04(1)Ǻ; O-Hg-O, 175.5(6)°] and forms a polymer link to a third oxygen [Hg-O, 2.60(2)Ǻ; O-Hg-O, 88.8(6), 87.6(7)°] giving triangular coordination about the mercury. The complex adduct {(2-chlorophenoxy) acetato }thallium(I)-(2-chlorophenoxy)acetic acid is monoclinic, space group C2/c with a 27.97(1), b 4.798(1), c 13.389(6) Ǻ, β 94.23(3)° and Z 4. This is an example of an ML.LH compound, having twofold rotational symmetry with the acid proton not located. The Tl -O bonds to each ligand molecule are 2.826(7)Ǻ with two longer bonds to adjacent carboxylate oxygens [3.002(7)Ǻ] completing a distorted square-planar stereochemistry about thallium. This results in a linear polymer structure.

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.

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.

Copper complexes of Picloram: The crystal and molecular structures of Bis(4-amino-3,5,6-trichloropyridine-2-carboxylato)aquacopper(II) dihydrate and Bis(4-amino-3,5,6-trichloropyridine-2-carboxylato)bis(pyrimidin-2-amine)copper(II)

1983 ◽  
Vol 36 (1) ◽  
pp. 183 ◽  
Author(s):  
EJ O'Reilly ◽  
G Smith ◽  
CHL Kennard ◽  
AH White
Keyword(s):  
Copper Complexes ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Trigonal Bipyramidal ◽  
Distorted Octahedral ◽  
A Cell ◽  
Amine Ligands

The crystal structures of two copper(II) complexes of the herbicide Picloram (4-amino-3,5,6-trichloro- pyridine-2-carboxylic acid) have been determined by single-crystal X-ray diffractometry. Bis(4-amino- 3,5,6-trichloropyridine-2-carboxylato)aquacopper(II) dihydrate (1) is monoclinic, space group C2/c, with Z 4 in a cell of dimensions a 15.593(6), b 7.940(6), c 16.983(6) �, β 107.58(3)�. The structure was refined to a residual R 0.046 for 905 'observed' reflections. Complex (1) is trigonal bipyramidal with the trigonal plane consisting of oxygens from two picolinate ligands [Cu-O 1.995(5) �] and a water molecule [Cu-O 2.080(5) �]. The apical positions are occupied by pyridine ring nitrogens from the Picloram ligands [Cu-N 2.021(5) �]. Bis(4-amino-3,5,6-trichloropyridine- 2-carboxylato)bis(pyrimidin-2-amine)copper(II) (2) is monoclinic, space group P2,/c, with Z 4 in a cell of dimensions a 12.3 11(5), b 15.435(5), c 15.320(6) �, β 115.95(3)�, and gave a final R 0.059 for 2429 'observed' reflections. In complex (2), the copper(II) atom has a tetragonally distorted octahedral stereochemistry with the Picloram ring nitrogens once again occupying the two axial positions [Cu-N 2.586(7) and 2.611(7) �]. The square plane consists of two carboxylato oxygens [Cu-O 1.941(6) and 1.960(7) �] and two hetero-nitrogens from pyrimidin-2-amine ligands [Cu-N 2.048(6) and 2.054(6) �].

Monomere und dimere Oxotrihalogenoselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C6H5)4]SeOCl3 und [N(C2H5)4]SeOCl3 / Monomerie and Dimeric Oxotrihalogenoselenates(IV): Preparation, Structure and Properties of [As(C6H5)4]SeOCl3 and [N(C2H5)4]SeOCl3

1983 ◽  
Vol 38 (1) ◽  
pp. 20-29 ◽  
Author(s):  
Bernt Krebs ◽  
Marita Hucke ◽  
Michael Hein ◽  
Andreas Schäffer
Keyword(s):  
Polymer Chains ◽  
Monoclinic Space Group ◽  
Structure And Properties ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers

Abstract The monomeric SeOCl3- ion, which can be prepared as the tetraphenylarsonium salt from SeOCl2 and As(C6H5)4Cl, was structurally characterized by a low-temperature single crystal X-ray diffraction analysis. [As(C6H5)4]SeOCl3 is monoclinic, space group P21/c, with a = 9,332(3), b = 13,761(4), c = 18,985(6) Å, β = 110,97(3)° (at -135 °C), Z = 4; it contains a novel type of ψ-trigonal bipyramidal oxotrichloroselenate(IV) anion which is not associated to dimers or polymer chains as in known structures. The equatorial positions are occupied by doubly bonded oxygen (Se-O 1,601(3) Å) and by one Cl(Se-Cl 2,234(1) Å), the axial Se-Cl bonds (2,430(1) and 2,475(1) Å) being significantly longer. [N(C2H5)4]SeOCl3, which was obtained as crystals by oxidation of trichloroselenate(II), is triclinic, space group P1̄, with a = 10,607(3), b = 8,950(2), c = 8,862(2) Å, α = 119,79(2)°, β = 101,07(2)°, γ = 96,28(2)°, Z = 2. The X-ray structure analysis shows the anions to be present as centrosymmetric dimers Se2O2Cl62- like in the [P(C6H5)4]+ salt, with two tetragonal SeOCl4 pyramids linked through a Cl···Cl edge and the lone pairs trans to the axial Se-O bonds (1,589(4) Å). Se-Cl bond lengths are 2.270(1) and 2,351(2) Å (terminal); 2,698(1) and 2,920(1) Å (bridging). The results show that the nature of the reaction products of the Lewis acid SeOCl2 with halogenides as bases changes very sensitively with small variations in cations and environment. The vibrational spectra are discussed.

Coordination of 6-Methyl-2,2'-bipyridine. Structure of Bivalent Copper and Palladium Complexes

1991 ◽  
Vol 44 (2) ◽  
pp. 219 ◽  
Author(s):  
D Onggo ◽  
DC Craig ◽  
AD Rae ◽  
HA Goodwin
Keyword(s):  
Palladium Complexes ◽  
Partial Hydrolysis ◽  
Monoclinic Space Group ◽  
Coordination Environment ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Square Planar ◽  
Bivalent Copper ◽  
Hydrolysis Of

Bis ( ligand ) complexes of 6-methyl-2,2′-bipyridine (L) with copper(II) and palladium(II) have been prepared, and their structures have been determined by single-crystal X-ray diffractometry . In the formation of the complex fromcopper(II) tetrafluoroborate and L, partial hydrolysis of a coordinated fluoroborate ion to the hydroxytrifluoroborate ion occurs. The stereochemistry about copper in [CuL2OHBF3][BF4] is essentially trigonal bipyramidal with an axial compression. The nitrogens of the methyl-substituted pyridine rings coordinate in the axial sites. In [PdL2Cl][BF4] the coordination environment about palladium is square planar and one of the 6-methylbipyridine molecules functions as a unidentate group, the nitrogen of the methyl-substituted pyridine ring being uncoordinated. The average metal-nitrogen distance is 2.032 Ǻ in the copper complex and 2.042 Ǻ in the palladium complex. [CuL2OHBF3][BF4] is monoclinic, space group P21/c, Z = 4, a 9.005(2), b 17.868(2), c 15.298(3) Ǻ, β 104.13(1)°. [PdL2Cl][BF4] is monoclinic, space group P21/c, Z = 4, a 9.606(5), b 14.748(2), c 16.311(8)Ǻ, β 96.13(2)°.

The crystal structures of two isomers of a macrocyclic binuclear compound each containing both divalent and trivalent cobalt

1975 ◽  
Vol 28 (12) ◽  
pp. 2593 ◽  
Author(s):  
BF Hoskins ◽  
GA Williams
Keyword(s):  
Bromine Atom ◽  
Fourier Method ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
R Factor ◽  
A Cell ◽  
Coordinated Water

The compound Lco2Br3,2H2O (where L is a binucleating ligand derived from the macrocycle LH2 formed by condensation of two molecules each of propane-1,3-diamine and 2-hydroxy-5- methylisophthalaldehyde) was found to occur in two crystalline forms. The structures of both have been determined by single-crystal X-ray diffraction techniques, revealing that each corresponds to a different geometrical isomer of composition Lco2Br3,2H2O. Each structure was determined by the conventional Patterson-Fourier method and refined by a least-squares procedure, with only the Co, Br, N and O atoms being refined anisotropically. The first form, designated the A-isomer, crystallizes in the orthorhombic space group Pn21a with four formula units in a cell of dimensions a 15.173(1), b 17.370(2) and c 10.493(1) Ǻ. The structure refined to a conventional R-factor of 0.074 by means of 1883 unique reflections collected by counter methods. The second form, or B-isomer, crystallizes in the monoclinic space group P21 with two formula units in a cell of dimen- sions a 10.676(1), b 15.235(2), c 9.304(1) Ǻ and β 111.83(2)°. The structure refined to a conventional R-factor of 0.101 by means of 2006 independent reflections collected by counter methods. Both isomers are composed of discrete bromide anions together with discrete binuclear cations of com- position [Lco2Br2,2H2O]+, each containing one cobalt(II) and one cobalt(III) atom with a Co...Co distance of 3.13 Ǻ. In both isomers the cobalt atoms are in octahedral environments. In the A-isomer two bromine atoms are bonded to the cobalt(III) atom in positions perpendicular to the ligand N2O2 donor plane, with the two water molecules occupying similar positions about the cobalt((II). But in the B-isomer, one water molecule and one bromine atom are bonded to each of the cobalt(III) and the cobalt((II) atoms in the comparable positions. In both structures the ionic bromide is involved in a hydrogen-bonding scheme with the coordinated water molecules.

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 and molecular structures of N,N′-di(2-acetylcyclohexenyl)ethylenediamine and its copper(II) complex

1993 ◽  
Vol 71 (3) ◽  
pp. 358-363 ◽  
Author(s):  
Juan N. Fernández-G. ◽  
Raúl G. Enríquez ◽  
Amalia Tobón-Cervantes ◽  
Margarita I. Bernal-Uruchurtu ◽  
René Villena-I ◽  
...  
Keyword(s):  
Solvent Molecule ◽  
Molecular Structures ◽  
Isomeric Form ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Nmr Study ◽  
Square Planar

The crystal structures of N,N′-di(2-acetylcyclohexenyl)ethylenediamine (L1) and its copper(II) complex, which crystallizes with one solvent molecule of chloroform (Cu(L1-2H)•CHCl3), were determined. Crystallographic details are as follows: L1 is monoclinic, space group P21/c, with a = 8.280(2), b = 11.692(2), and c = 9.355(2) Å, β = 114.10(2)°, V = 826.7(3) Å3, Z = 2; ρc = 1.22 g cm−3, μ(Cu Kα) = 5.93 cm−1, with the final residual indices of R = 0.046 and Rw = 0.070 for 991 unique reflections. Cu(L1-2H)•CHCl3 is triclinic, space group[Formula: see text] with a = 11.121(3), b = 11.713(3), and c = 8.974(2) Å, α = 99.35(2)°, β = 110.83(2)°, γ = 82.33(2)°, V = 1074(1) Å3, Z = 2; ρc = 1.50 g cm−3, μ(Cu Kα) = 50.74 cm−1, with the final residual indices of R = 0.048 and Rw = 0.077 for 2369 unique reflections. The X-ray diffraction study shows that in the crystal state the ligand L1 is in the methylketonecyclohexanonenamine isomeric form. For the copper complex Cu(L1 2H)•CHC13, the geometry around the metal atom is distorted square planar, and the angle between the chelate ring planes in the complex is 15.1°. An NMR study shows that L1 in solution has the same structure as that observed in the solid state by X-ray diffraction.

Darstellung und Kristallstruktur von Zinkazid · 4-Methylpyridin / Preparation and Crystal Structure of Zinc Azide · 4-Methylpyridine

1988 ◽  
Vol 43 (3) ◽  
pp. 253-256 ◽  
Author(s):  
Franz A. Mautner ◽  
Harald Krischner ◽  
Christoph Kratky
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Single Crystal ◽  
Zinc Atom ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

Zinc azide · 4-methylpyridine (1) is formed by the reaction of zinc azide with the corresponding pyridine in aqueous solution. The crystal structure was determined by single crystal X-ray diffraction methods. The crystals of 1 are monoclinic, space group C2/c, Z = 4, a = 1085.5(2), b = 1692.7(11), c = 619.7(6) pm, β = 113.47(5)°. Each zinc atom is surrounded by five nitrogen atoms (four from azide groups and one from the pyridine adduct) in a distorted trigonal bipyramidal fashion. The ZnN5-polyhedra share common edges to form chains along the crystallographic c-axis.

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