Crystal structures of some eriostyl/nitrobenzoate derivatives

1980 ◽  
Vol 33 (2) ◽  
pp. 313 ◽  
Author(s):  
PR Jefferies ◽  
BW Skelton ◽  
B Walter ◽  
AH White
Keyword(s):  
Charge Transfer ◽  
Solid State ◽  
Single Crystal ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations

Following the suggestion made earlier, on the basis of solution spectroscopy, that a number of eriostyl/nitrobenzoate compounds form charge-transfer self-complexes, a number of these have been investigated structurally by single-crystal X-ray diffraction methods in order to ascertain the presence or otherwise of such interactions in the solid state. The substances thus studied were eriostyl 3,5-dinitrobenzoate (1), eriostyl p-nitrobenzoate (2), tetrahydroeriostyl 3,5-dinitrobenzoate (3), and eriostemyl 3,5-dinitrobenzoate (4);* structure determinations in all cases, although displaying the presence of strong charge-transfer interactions from the two moieties of each molecule, show that the interactions in the solid state are intermolecular in nature.

Lewis-Base Adducts of Group 11 Metal(I) Compounds. LIX. Crystal Structure Determinations of Tetrakis(trimethylphosphine)copper(I) Halides and Tetrakis(triphenylphosphine)-copper(I) and -silver(I) Hexafluorophosphates

1990 ◽  
Vol 43 (10) ◽  
pp. 1697 ◽  
Author(s):  
GA Bowmaker ◽  
PC Healy ◽  
LM Engelhardt ◽  
JD Kildea ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Coordination Environment ◽  
X Ray ◽  
Bond Lengths ◽  
Cu Complex ◽  
Structure Determinations

The crystal structures of [Cu(Pme3)4]X (X = Cl , Br, I) and of [M(PPh3)4] [PF6] (M = Cu, Ag) have been determined by single-crystal X-ray diffraction methods at 295 K. The former compounds contain nearly tetrahedral [Cu(PMe3)4]+ ions on sites of m symmetry with mean Cu-P bond lengths of 2.270, 2.271 and 2.278 Ǻ for X = Cl , Br and I respectively. The latter compounds contain [M(PPh3)4]+ ions on sites of 3 symmetry. In the M =Ag complex the coordination environment is close to tetrahedral, but in the M =Cu complex the length of the axial Cu-P bond [2.465(2)Ǻ] is significantly shorter than that of the off-axis bonds [2.566(2)Ǻ]. Possible reasons for this are discussed.

Structure, Stereochemistry and Novel 'Hydrogen Bonding' in Two Bipyridinium Salts of the B10H102- Anion

1987 ◽  
Vol 40 (12) ◽  
pp. 2097 ◽  
Author(s):  
DJ Fuller ◽  
DL Kepert ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Charge Transfer ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
X Ray ◽  
Structure Determinations ◽  
Positively Charged

Crystal structure determinations of (LH)2(B10H10), (1), and (LH2)(B10H10), (2), L = 2,2'- bipyridine , have been carried out by single-crystal X-ray diffraction methods at 295 K, being refined by full-matrix least squares to residuals of 0.041, 0.047 for 1758, 1771 'observed' independent reflections respectively. Crystals of (1) are monoclinic, P21/n, a 12.040(7), b 17.71(1), c 11.142(4) �, β 101.78(4)�, Z 4. Crystals of (2) are monoclinic, P21/c, a 9.937(4), b 10.837(3), c 14.856(5) �, β 109 2l(3)�, Z 4. The colour of the compounds is accounted for by charge-transfer interactions of a novel type, namely between the positively charged cationic acid hydrogen atoms and the negatively charged non-apical hydrogen atoms of the anion. In yellow (1), these distances are 2.26(5) �, while in red (2), they are much shorter, being 1.89(4), 1.97(3) �.

scholarly journals Crystal structures of cristobalite-type and coesite-type PON redetermined on the basis of single-crystal X-ray diffraction data

2015 ◽  
Vol 71 (11) ◽  
pp. 1325-1327 ◽  
Author(s):  
Maxim Bykov ◽  
Elena Bykova ◽  
Vadim Dyadkin ◽  
Dominik Baumann ◽  
Wolfgang Schnick ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Crystal Structures ◽  
Rotation Axis ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Anisotropic Displacement Parameters

Hitherto, phosphorus oxonitride (PON) could not be obtained in the form of single crystals and only powder diffraction experiments were feasible for structure studies. In the present work we have synthesized two polymorphs of phosphorus oxonitride, cristobalite-type (cri-PON) and coesite-type (coe-PON), in the form of single crystals and reinvestigated their crystal structures by means of in house and synchrotron single-crystal X-ray diffraction. The crystal structures ofcri-PON andcoe-PON are built from PO2N2tetrahedral units, each with a statistical distribution of oxygen and nitrogen atoms. The crystal structure of thecoe-PON phase has the space groupC2/cwith seven atomic sites in the asymmetric unit [two P and three (N,O) sites on general positions, one (N,O) site on an inversion centre and one (N,O) site on a twofold rotation axis], while thecri-PON phase possesses tetragonalI-42dsymmetry with two independent atoms in the asymmetric unit [the P atom on a fourfold inversion axis and the (N,O) site on a twofold rotation axis]. In comparison with previous structure determinations from powder data, all atoms were refined with anisotropic displacement parameters, leading to higher precision in terms of bond lengths and angles.

Structural studies in the iron(III)/chloride/α,α'-diimine system. II. Ionic derivatives of stoichiometry FeCl3(phen,bpy)1,1.5

1983 ◽  
Vol 36 (10) ◽  
pp. 2043 ◽  
Author(s):  
BN Figgis ◽  
JM Patrick ◽  
PA Reynolds ◽  
BW Skelton ◽  
AH White ◽  
...  
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Derivatives Of

The crystal structures of the 1 : 1 adducts of FeCl3 with 2,2'-bipyridine (bpy) (1) and 1,10-phenanthroline (phen) (2), as recrystallized from nitromethane, have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to residuals of 0.038 and 0.032 for 1341 and 3968 'observed' reflections; the result for (2) is a redetermination. Crystals of (1) are orthorhombic, Pbnb, a 15.013(4), b 13.510(5), c 12.471(3) Ǻ, Z 4. Crystals of (2) are triclinic, P1, a 15.823(5), b 11.021(5), c 8.200(3) Ǻ, α 80.27(3), β 76.78(3), γ 89.64(3)°, Z 2. Both complexes haw the stoichiometry (FeCl3)1(bpy,phen)1, but are formulated as cis-[Fe(bpy,phen)2Cl2] [FeCl4]; in both compounds, the Fe-N distance is c. 2.20, (trans to Cl), 2.1, Ǻ(cis to Cl), while Fe-Cl, c. 2.2, Ǻ, is short. The structure determinations of Fe2Cl6(phen,bpy)3 as [Fe(phen)2Cl2]+ [Fe(phen)Cl4]- (3) and [Fe(bpy)2Cl2]+ [Fe(bpy)Cl4]- (4) are also reported. Compound (3) (from acetonitrile solution) is triclinic, P1, a 16.502(5), b 11.857(3), c 10.653(3) Ǻ, α 84.92(2), β 72.66(2), γ 74.80(2)°, Z 2, and was refined to a residual of 0.034 for 5540 'observed' reflections. The cation geometry is similar to that of (2); in the anion, the two Fe-CI bonds trans to each other are long [2.377(1) and 2.365(1) Ǻ] while those trans to the Fe-N bonds are short [2.287(1) and 2.318(1) Ǻ]. Fe-N distances are 2.216(3) and 2.220(3) A. Compound (4) (as its nitromethane solvate) is also triclinic, P1, a 14.480(7), b 12.645(5), c 10.678(4) Ǻ, α 95.68(3), β 109.21(3), γ 9258(3)°, Z 2; a residual of 0.042 was obtained for 4962 'observed' reflections. Cation and anion metal geometries are similar to those of (3).

Crystal structures of rac- and meso-o-Phenylenebis(iodomethylarsine), the latter as its lattice complex with the methiodide of 1,3-Dimethyl-1,3-dihydro-2,1,3-benzoxadiarsole

1977 ◽  
Vol 30 (11) ◽  
pp. 2417 ◽  
Author(s):  
K Henrick ◽  
CL Raston ◽  
AH White ◽  
SB Wild
Keyword(s):  
Charge Transfer ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths ◽  
Iodine Species ◽  
Iodide Anion ◽  
The Mean

The crystal structures of the title compounds, o-C6H4(AsMeI)2 (1), and o- C6H4(AsMeI)2- [o-C6H4(AsMe)(As+Me2)O] I- (2), have been determined at 295 K by single-crystal X-ray diffraction and refined by least squares to residuals of 0.037 and 0.067 for 2095 and 2913 reflections respectively. Crystals of (1) are triclinic, Pī, a 9.865(5), b 9.837(7), c 7.765(4) Ǻ, α 98.89(5), β 96.71(4), γ 60.72(4)�, Z 2. <As- I> is 2.585 Ǻ and <As-C> 1.97 Ǻ. The angles about the arsenic differ only trivially, the mean being 98.4�. Crystals of (2) are monoclinic, P21/n, a 15.315(4), b 21.511(8), c 7.952(2) Ǻ, β 98.19(2)�, Z 4. In the cation As-O distances are unequal [1.75(1) (quaternary As), 1.86(2) Ǻ]; As-O-As is very small being 115.8(8)�. Charge-transfer interactions between iodine species are present in both derivatives; in (2), there is an interaction between the tertiary arsenics of the meso molecule and the iodide anion, As...I being 3.307(3), 3.551(3) Ǻ, with the geometry of the arsenics approaching that of a tetrahedral disposition. Within the cation, the geometry about the quaternary arsenic is typical of arsenic(v), the bond lengths being shorter than those about the ternary arsenic.

A quinoxaline-fused tetrathiafulvalene derivative and its semiconducting charge-transfer salt: synthesis, crystal structures and physical properties

2014 ◽  
Vol 38 (5) ◽  
pp. 2052-2057 ◽  
Author(s):  
Yan Geng ◽  
Christoph Fiolka ◽  
Karl Krämer ◽  
Jürg Hauser ◽  
Vladimir Laukhin ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Charge Transfer ◽  
Physical Properties ◽  
Single Crystal ◽  
Crystal Structures ◽  
Single Crystal Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Donor Acceptor ◽  
Tetrathiafulvalene Derivative

A quinoxaline-fused tetrathiafulvalene (TTF) derivative 1 has been synthesized to form a compact and planar π-conjugated donor–acceptor (D–π–A) ensemble, and its single crystal structure has been determined by X-ray diffraction.

scholarly journals Cooperativity in the Reaction of 9-Methylanthracene With a 1,4-Dithiin Molecule

2014 ◽  
Vol 70 (a1) ◽  
pp. C913-C913
Author(s):  
Sanaz Khorasani ◽  
Manuel Fernandes
Keyword(s):  
Charge Transfer ◽  
Solid State ◽  
Single Crystal ◽  
Lattice Energy ◽  
Alder Reaction ◽  
Diels Alder ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diels Alder Reaction

Solid-state chemistry involves the manipulation of molecules and materials through photochemical, thermal, or mechanical reaction methods. Single-crystal-to-single-crystal (SCSC) reactions are rare, but offer the opportunity to study reaction mechanisms and molecular motions in the solid state at the atomic level using single crystal X-ray diffraction. This allows the effect of the surrounding molecules, and hence the reaction cavity, on the reacting molecules to be examined which may ultimately lead to postcrystallization methods for creating new materials or reaction products that cannot easily be obtained via solution. SCSC reactions involving two different molecules are relatively uncommon. A convenient system that allows the study of such reactions is the [4+2] Diels-Alder reaction of 1,4-dithiintetracarboxylic type compounds with anthracene derivatives. In the work reported here, electron donor to acceptor interactions between 9-Methylanthracene and bis(N-cyclobutylimino)-1,4-dithiin lead to the formation of chiral charge transfer (CT) crystals [1]. These undergo a topochemical thermal SCSC [4 + 2] Diels-Alder reaction in the solid state. CT crystals were reacted at 400C, their structures determined by X-ray diffraction at various degrees of conversion, and examined using Hirshfeld surfaces and lattice energy calculations to find evidence of reaction cooperativity and feedback mechanisms. In this case, a maximum reaction conversion of around 96% was obtained indicating that the reaction is non-random within the charge transfer stacks, with close contacts between product molecules in the reacted crystal also providing some evidence for reaction cooperativity along the b axis perpendicular to the CT stacking axis.

Crystal structures of (S)- and (R,S)-2,2′-bipyridine-3,3′-dicarboxylic acid 1,1′-dioxides and of their barium salts: absolute configuration and molecular distortion enforced by supramolecular self-assembly

1997 ◽  
Vol 212 (3) ◽  
Author(s):  
P. Vojtíšek ◽  
I. Císařová ◽  
J. Podlaha ◽  
Z. Žák ◽  
S. Böhm ◽  
...  
Keyword(s):  
Single Crystal ◽  
Dicarboxylic Acid ◽  
Crystal Structures ◽  
Absolute Configuration ◽  
Self Assembly ◽  
Barium Salt ◽  
X Ray Diffraction ◽  
X Ray

AbstractCrystal structures of the title compounds were determined by single crystal X-ray diffraction. Absolute configuration of the barium salt of (+)-(

Die Kristallstrukturen der isotypen Verbindungen Ba3[MoN4] und Ba3[WN4] / The Crystal Structures of the Isotypic Compounds Ba3[MoN4] and Ba3[WN4]

1991 ◽  
Vol 46 (5) ◽  
pp. 566-572 ◽  
Author(s):  
Axel Gudat ◽  
Peter Höhn ◽  
Rüdiger Kniep ◽  
Albrecht Rabenau
Keyword(s):  
Transition Metals ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ternary Compounds ◽  
The Third

The isotypic ternary compounds Ba3[MoN4] and Ba3[WN4] were prepared by reaction of the transition metals with barium (Ba3N2, resp.) under nitrogen. The crystal structures were determined by single crystal X-ray diffraction: Ba3[MoN4] (Ba3[WN4]): Pbca; Z = 8; a = 1083.9(3) pm (1091.8(3) pm), b = 1030.3(3) pm (1037.5(3) pm), c = 1202.9(3) pm (1209.2(4) pm). The structures contain isolated tetrahedral anions [MN4]6- (M = Mo, W) which are arranged in form of slightly distorted hexagonal layers and which are stacked along [010] with the sequence (···AB···). Two of the three Ba atoms are situated between, the third one is placed within the layers of [MN4]-groups. In this way the structures can be derived from the Na3As structure type.

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