Color and Conformation of Some Derivatives of Benzil in the Solid-State: Crystal-Structures of 2,2′-Dimethoxy- 4,4′-Dimethoxy- , 4-4′Diethoxy- and 4,4'-Dibenzyloxy-benzil

1989 ◽  
Vol 42 (10) ◽  
pp. 1631 ◽  
Author(s):  
JR Cannon ◽  
VA Patrick ◽  
AH White
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Aromatic Ring ◽  
Full Matrix ◽  
X Ray ◽  
Derivatives Of ◽  
Least Squares Techniques

The crystal structures of the colourless 2,2'-dimethoxybenzil (2) and 4,4'-diethoxybenzil (6), the yellow 4,4'-dimethoxybenzi (5), and the yellow polymorph of 4,4'-dibenzyloxybenzil (7) have been determined by single-crystal X-ray studies from diffractometer data at 295 K, and refined by full matrix least-squares techniques to residuals of 0.048 (1281 'observed' reflections), 0.041 (610), 0.052 (662) and 0.043 (2140) respectively. Crystals of 2,2′-dimethoxybenzil (2) are monoclinic, P21/c, a 7.861(4), b 7.991(2), c 21.557(9)�, β90.37(4)�, Z 4. Crystals of 4,4'-dimethoxybenzil (6) are monoclinic C2/c, a 21.912(9), b 4.055(2), c 15.197(5) �,β 102 13(3)� Z 4. Crystals of 4,4′-diethoxybenzil (6) are monoclinic C21/c, a 14.544(7), b 4.781(2), c 22.128(7), β 99.06(3)�, Z 4. Crystals of the yellow modification of 4,4'-dibenzyloxybenzil (7) are monoclinic P21/c, a 19.126(4), b 6.91 1(2), c 16.673(7) � β 99.52(3)�, Z 4. It has been found that there is a correlation between the colour of the crystal and the conformation adopted by the molecule in the solid state with the colourless derivatives of benzil having the aromatic ring planes orthogonal.

scholarly journals Crystal structure of Tetraaqua(ethylenediamine)nickel(II) sulfate dihydrate and of Tetraaqua(2,2'-bipyridyl)nickel(II) sulfate dihydrate

1984 ◽  
Vol 37 (5) ◽  
pp. 921 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Water Molecule ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Oxygen Atoms

The crystal structures of the title compounds, [Ni(OH2)4(en)] [SO4].2H2O, (1), and [Ni(OH2)4(bpy)]- [SO4].2H2O, (2), have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by full matrix least-squares methods to residuals of 0.028,0.031 for 1852, 4323 independent 'observed' reflections respectively. Crystals of (1) are monoclinic, C2/c, a 9.459(4), b 12.192(7), c 12.294(3) �, β 119.84(4)�, Z 4. In the cation, Ni-N is 2.061(2) �; Ni-O (trans to O, N respectively) are 2.106(2), 2.063(2) �. Instead of being enlarged above 90� as predicted from repulsion theory, the angle between the pair of oxygen atoms trans to nitrogen is diminished, being 87 14(7)�. Crystals of (2) are triclinic, P1, a 11.476(5), b 9.351(5), c 7.793(4) �, α 77.63(4), β 83.52(3), γ87.40(4)�, Z 2. In the cation, Ni-N are both 2.063(2) �. Ni-O (trans to N, O respectively) are 2.060(2), 2.O42(2); 2.O80(2), 2�. The short Ni-O distance [2.042(2)�] is associated with the coordination of a trigonal water molecule.

The Conformation of Some 1,1,2,2-Tetraacylethanes in the Solid-State: Crystal-Structures of 1,1,2,2-Tetrabenzoylethane, 1,2-Diacetyl-1,2-Dibenzoylethane and 1,1,2,2-Tetraethoxycarbonylethane

1986 ◽  
Vol 39 (11) ◽  
pp. 1811 ◽  
Author(s):  
JR Cannon ◽  
VA Patrick ◽  
AH White
Keyword(s):  
Solid State ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Keto Form ◽  
Carbon Bond ◽  
X Ray ◽  
Carbon Carbon Bond ◽  
Central Carbon ◽  
Least Squares Techniques

The crystal structures of 1,1,2,2-tetrabenzoylethane (3), 1,2-diacetyl- 1,2-dibenzoylethane (4) and 1,1,2,2-tetraethoxycarbonylethane (tetraethyl ethanetetracarboxylate ) (5) have been determined by X-ray diffraction from diffractometer data at 295 K and were refined by least-squares techniques to residuals of 0.050 (1077 'observed' reflections), 0.056 (3020) and 0.041 (480), respectively. Crystals of (3) are triclinic, Pī , Z 1, a 6.145(2), b 9.002(3), c 11.261(3) Ǻ; α 101.91(3), β 91.88(3), γ 105.94(3)°. Crystals of (4) are also triclinic, Pī , Z 2, a 17.119(5), b 7.210(1), c 7.175(2) Ǻ, α 89.59(2), β 72.92(2), γ 87.87(2)°. Crystals of (5) are tetragonal, P42/n, Z 4, a 17.748(6), c 5.515(1)Ǻ. In the solid state each compound exists in the keto form which adopts the antiperiplanar conformation about the central carbon-carbon bond.

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).

Isolation and Crystal Structure of Limonidilactone—a Labdane Diterpene From Vitex limonifolia

1995 ◽  
Vol 48 (1) ◽  
pp. 133 ◽  
Author(s):  
S Aphaijitt ◽  
K Nimgirawath ◽  
A Suksamrarn ◽  
U Tooptakong
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Structure Determination ◽  
Spectroscopic Methods ◽  
Full Matrix ◽  
X Ray ◽  
Labdane Diterpene ◽  
Least Squares Techniques

The structure of a new labdane diterpene, limonidilactone , from the leaves of Vitex limonifolia Wall. ( Verbenaceae ) has been established by spectroscopic methods and a single-crystal X-ray structure determination. Crystals are orthorhombic, P212121, a 19.373(10), b 10.871(7), c 8.207(3) Ǻ, Z 4. Diffractometer data were refined by full-matrix least-squares techniques to a residual of 0.043 for 1436 independent 'observed' reflections.

Crystal structures of N,N,N',N'-Tetramethylthiuram monosulphide and Diiodo(N,N,N',N'-tetramethylthiuram monosulphide)mercury(II)

1977 ◽  
Vol 30 (8) ◽  
pp. 1693 ◽  
Author(s):  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Metal Atom ◽  
X Ray Diffraction ◽  
Sulphur Atom ◽  
Full Matrix ◽  
X Ray ◽  
The Common ◽  
Trigonal Prismatic

The crystal structures of the title compounds, Me2NC(S)SC(S)NMe2 (tmtm) and I2Hg(tmtm), have been determined by single-crystal X-ray diffraction at 295 K and refined by full-matrix least squares to residuals of 0.038 and 0.050 respectively for 1080 and 1532 ?observed? reflections. ��� The ligand tmtm is monoclinic, P21/a, a 14.096(4), b 7.457(3), c 10.178(3)Ǻ, β 110.55(3)�, Z4. The complex I2Hg(tmtm) is orthorhombic, P212121, a 12.910(3), b 12.441(3), c 9.863(2) Ǻ, Z4. ��� The structure of the ligand comprises a pair of planar Me2NCS2 fragments linked at the common central sulphur atom with a dihedral of 78.4�. As in the related tetraethylthiuram disulphide, the ?CS2- geometry is very asymmetric: <C=S> 1.657; <C-S> 1.793 Ǻ; <S-C-S> 119.3; <S-C-N> 115.2; <S=C-N> 125.4�; with C-S-C, 103.2(2)�. The metal-atom geometry in I2Hg(tmtm) is pseudo-trigonal prismatic, as in I2Hg(Me2NCS2- S2CNMe2), the prism apex being occupied by a ligand sulphur atom, but considerable changes are observed in the geometry about the metal as a consequence of the change in the ligand ?bite?.

Lewis-Base Adducts of Group-11 Metal(I) Compounds. XXIX. Crystal Structures of Bis(Pyridine-4-carbonitrile)silver(I) Nitrate and Bis(4-benzoylpyridine)Silver(I) Nitrate Monohydrate

1987 ◽  
Vol 40 (9) ◽  
pp. 1603 ◽  
Author(s):  
S Gotsis ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Complex Cation ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Silver Atoms ◽  
Close Contacts

The crystal structures of the title compounds, [Ag(C6H4N2),] (NO3), (I), and [Ag(C12H9NO)2] (NO3).H2O, (2), have been determined by single-crystal X-ray diffraction methods at ~295 K, being refined by full-matrix least-squares methods to residuals of 0.042 and 0.044 for 1814 and 3434 independent 'observed' reflections respectively. Crystals of (1) and (2) are triclinic P1; for (1) a, 27.954(7), b 6.354(2), c 3.710(1)�, α 87.55(3), β 86.21(2), γ 89.35(2)�, Z 2; for (2), a 17.036(5), b 8.691(3), c 7.849(3) �, α � 107.74(2), β 97 53(2), γ 91 .11(2)�, Z 2. In both structures the formulation is basically a linearly coordinated complex cation/anion as shown above: in (I), Ag-N are 2.214(4), 2.203(4) � with N-Ag-N, 162.2(2)"; in (2), Ag-N are 2.146(3), 2.147(3) �, N-Ag-N, 175.3(1)�. The shortest Ag-O contact is found in (1) at 2.693(4)�. No close contacts are found between the silver atoms and cyano or ketonic ligand substituents.

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.

Crystal structure of 2,3-Dichloro-5,8-dihydroxynaphtho-1,4-quinone

1978 ◽  
Vol 31 (3) ◽  
pp. 555 ◽  
Author(s):  
GI Feutrill ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Benzene Ring ◽  
Title Compound ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
X Ray ◽  
The One ◽  
Least Squares Techniques

The crystal structure of the title compound has been determined at 295 K by single-crystal X-ray diffraction methods and refined by least- squares techniques to a residual of 0.049 for 1046 'observed' reflections. Crystals are monoclinic, P21/c, a 11.584(6), b 5.449(7), c 15.273(8) Ǻ, β 92.44(4)°, Z4. The pair of quinol hydrogen atoms are both located on the one benzene ring as the title indicates.

A REFINEMENT OF THE CRYSTAL STRUCTURES OF (NH4)2TeBr6 AND Cs2TeBr6

1966 ◽  
Vol 44 (8) ◽  
pp. 939-943 ◽  
Author(s):  
A. K. Das ◽  
I. D. Brown
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Bromine Atom ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Anisotropic Temperature ◽  
Temperature Factors

(NH4)2TeBr6 and Cs2TeBr6 crystals have the cubic K2PtCl6 structure with space group: [Formula: see text] with a0 = 10.728 ± 0.003 Å and 10.918 ± 0.002 Å respectively. The positional coordinate of the bromine atom, and the anisotropic temperature factors of all atoms in the unit cell, have been refined for both crystals by a full matrix least-squares analysis of the three dimensional X-ray diffraction data (R = 0.08). The Te—Br distance, corrected for probable thermal motions of atoms forming the bond, is 2.70 ± 0.01 Å in both crystals.

Crystal structures of optically active naphthidine (4,4′-diamino-1,1′-binaphthyl) and 1,1′-binaphthyl

1983 ◽  
Vol 61 (1) ◽  
pp. 69-71 ◽  
Author(s):  
Richard A. Pauptit ◽  
James Trotter
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Direct Methods ◽  
Optically Active ◽  
Dihedral Angles ◽  
Full Matrix ◽  
Bond Lengths ◽  
Least Squares Techniques

Crystals of optically active naphthidine and of binaphthyl are tetragonal, P41212 (or P43212), a = 7.945(1), 7.164(2), c = 24.264(5), 27.70(1) Å, respectively, Z = 4. The structures were solved by direct methods and refined by full-matrix least-squares techniques to respective R = 0.068 and 0.030 for 548 and 562 reflexions. The dihedral angles between the planes of the naphthalene residues are 87 and 102°, respectively. Bond lengths and angles are normal.

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