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.

Crystal structures of (Z)-O-β-D-xylopyranosyl(1 → 6)-→-D-glucopyranosyloxy-NNO-azoxymethane (Macrozamin) and 5-O-methyl-myo-inositol (Sequoyitol)

1980 ◽  
Vol 33 (10) ◽  
pp. 2229 ◽  
Author(s):  
JR Cannon ◽  
CL Raston ◽  
RF Toia ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Least Squares Techniques

Crystal structures of (Z)-O-β-D-xylopyranosyl(1→6)-β-D- glucopyranosyloxy-NNO-azoxymethane (macrozamin) (1) and 5-O-methy-myo-inositol (sequoyitol) (4)-both of which are constituents of Macrozamia riedlei (Fisch. ex Gaud.) C. A. Gardn.-have been determined by X-ray diffraction. Diffractometer data at 295 K were refined by least-squares techniques to residuals of 0.050 (1537 'observed' reflections) for macrozamin and 0.060 (1052) for sequoyitol. Crystals of macrozamin are monoclinic, P2I, a 8.315(3), b 10.410(4), c 10.423(5) Ǻ, β 106.42(3)°, Z 2. Crystals of sequoyitol are triclinic, Pī, a 4.780(5), b 6.502(6), c 14.668(10) Ǻ, α 96.43(7), β 94.20(8), γ 109.31(8)°, Z 2.

Selective O-Demethylation of 5,8-Dihydroxy-2,3-Dimethoxy-6-Methylnaphtho-1,4-Quinone: The Crystal Structures of 5,8-Dihydroxy-2,3-Dimethoxy-6-Methylnaphtho-1,4-Quinone and 2,5,8-Triacetoxy-3-Methoxy-6-Methylnaphtho-1,4-Quinone

1987 ◽  
Vol 40 (7) ◽  
pp. 1191 ◽  
Author(s):  
JR Cannon ◽  
Y Matsuki ◽  
VA Patrick ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Sodium Hydroxide ◽  
Crystal Structures ◽  
Hydrolysis Product ◽  
Aqueous Sodium Hydroxide ◽  
X Ray Diffraction ◽  
Aqueous Sodium ◽  
X Ray ◽  
Least Squares Techniques

It has been confirmed that treatment of 5,8-dihydroxy-2,3-dimethoxy-6-methylnaphtho-1,4- quinone (1) with dilute aqueous sodium hydroxide leads to selective O- demethylation. The hydrolysis product has been identified as 2,5,8-trihydroxy-3-methoxy-6-methylnaphtho1,4- quinone (3) from the crystal structure of the corresponding triacetate (4). The crystal structures of 5,8-dihydroxy-2,3-dimethoxy-6-methylnaphtho-1,4-quinone (1) and 2,5,8-triacetoxy-3-methoxy-6-methylnaphtho-1,4-quinone (4) were determined by X-ray diffraction; diffractometer data at 295 K were refined by least squares techniques to residuals of 0.074 (583 'observed' reflections) for (1) and 0.049 (2005) for (4). Crystals of (1) are monoclinic, P2l/c, a 3.873(4), b 20.21(1), c 15.OO(2) �, β 96.05(6)�, Z 4. Crystals of (4) are also monoclinic, P2l/c, a 10.532(5), b 14.596(6), c 12.097(6) �, β 109.74(4)�, Z 4.

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.

The crystal structures of 1,3-Diphenylpropane-1,2,3-trione, 1,4-Diphenylbutane-1,2,3,4-tetraone, 2,4-Dihydroxy-2,5-diphenylfuran-3(2H)-one and 3,3-Dihydroxy- 1,4-diphenylbutane-1,2,4-trione

1982 ◽  
Vol 35 (3) ◽  
pp. 543 ◽  
Author(s):  
RL Beddoes ◽  
JR Cannon ◽  
M Heller ◽  
OS Mills ◽  
VA Patrick ◽  
...  
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Carbonyl Groups ◽  
X Ray Diffraction ◽  
X Ray ◽  
Least Squares Techniques

As a contribution towards a study of the relative disposition of adjacent carbonyl groups in polycarbonyl compounds, the crystal structures of 1,3-diphenylpropane-1,2,3-trione (1), 1,4-diphenyl- butane-1,2,3,4-tetraone (3), 2,4-dihydroxy-2,5-diphenylfuran-3(2H)-one (benzoylformoin) (7) and 3,3-dihydroxy-1,4-diphenylbutane-1,2,4-trio (8) have been determined by X-ray diffraction from diffractometer data at 295 K and refined by least-squares techniques to residuals of 0.036 (942 'observed' reflections), 0.029 (979), 0.067 (941) and 0.045 (1661), respectively. Crystals of 1,3-diphenylpropane-1,2,3-trione are triclinic, P1, a 9.756(4), b 8.813(3), c 8.303(3) �,α 68.56(2), β 67.53(3), γ 89.11(3)�, Z 2. Crystals of 1,4-diphenylbutane-1,2,3,4-tetraone are monoclinic P21/c, a 10.641(2), b 8.381(2), c 14.710(4) �, β 91.70(2)�, Z 4. 2,4-Dihydroxy-2,5- diphenylfuran-3(2H)-one also forms monoclinic crystals, P21/c, a 5.741(4), b 9.276(7), c 24.31(2) �, β 106.26(5)�, Z 4. Crystals of 3,3-dihydroxy-1,4-diphenylbutane-1,2,4-trine are triclinic, P1, a 13.08(1), b 12.43(1), c 8.895(8) �, α 82.54(8), β 81.87(7), γ 78.61(7)�, Z 4.

Dimethyl-, Disilyl- and Digermylsulfide: Different Intermolecular Contacts in the Solid State

2004 ◽  
Vol 59 (6) ◽  
pp. 635-638 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Udo Losehand
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intermolecular Contacts

The compounds (H3C)2S, (H3Si)2S and (H3Ge)2S have been crystallised in situ on a diffractometer and their crystal structures determined by low-temperature X-ray diffraction. The molecules are present as monomers in the crystals. The aggregation of the molecules through secondary intermolecular contacts in the crystal is different: (H3C)2S is weakly associated into dimers by S···S contacts, whereas (H3Si)2S and (H3Ge)2S form Si···S and Ge···S contacts in an ice-analogous aggregation motif. Important geometry parameters are (H3C)2S: C-S 1.794(av) Å , C-S-C 99.2(1)°; (H3Si)2S: Si- S 2.143(1) Å , Si-S-Si 98.4°; (H3Ge)2S Ge-S 2.223(2) and 2.230(2) Å , Ge-S-Ge 98.2(1)◦.

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.

Supramolecular architectures in two 1:1 cocrystals of 5-fluorouracil with 5-bromothiophene-2-carboxylic acid and thiophene-2-carboxylic acid

2017 ◽  
Vol 73 (6) ◽  
pp. 481-485 ◽  
Author(s):  
Marimuthu Mohana ◽  
Packianathan Thomas Muthiah ◽  
Colin D. McMillen
Keyword(s):  
Solid State ◽  
Carboxylic Acid ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Base Pairs ◽  
X Ray ◽  
Supramolecular Architectures ◽  
Acid Acid ◽  
Carboxylic Acid Dimer

In solid-state engineering, cocrystallization is a strategy actively pursued for pharmaceuticals. Two 1:1 cocrystals of 5-fluorouracil (5FU; systematic name: 5-fluoro-1,3-dihydropyrimidine-2,4-dione), namely 5-fluorouracil–5-bromothiophene-2-carboxylic acid (1/1), C5H3BrO2S·C4H3FN2O2, (I), and 5-fluorouracil–thiophene-2-carboxylic acid (1/1), C4H3FN2O2·C5H4O2S, (II), have been synthesized and characterized by single-crystal X-ray diffraction studies. In both cocrystals, carboxylic acid molecules are linked through an acid–acid R 2 2(8) homosynthon (O—H...O) to form a carboxylic acid dimer and 5FU molecules are connected through two types of base pairs [homosynthon, R 2 2(8) motif] via a pair of N—H...O hydrogen bonds. The crystal structures are further stabilized by C—H...O interactions in (II) and C—Br...O interactions in (I). In both crystal structures, π–π stacking and C—F...π interactions are also observed.

Crystal Structures of New Compounds Na0.5Sm4.5Ti4O15 and Na0.5Eu4.5Ti4O15

2011 ◽  
Vol 415-417 ◽  
pp. 468-471
Author(s):  
Qiao Hong Yu ◽  
Zheng Fa Li ◽  
Yong Xiang Li ◽  
Ping Zhan Si ◽  
Jiang Ying Wang ◽  
...  
Keyword(s):  
Solid State ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Diffraction Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ordinary Temperature ◽  
Europium Titanate ◽  
New Compounds

New compounds of sodium samarium titanate Na0.5Sm4.5Ti4O15and sodium europium titanate Na0.5Eu4.5Ti4O15were synthesized successfully by solid state reaction at 1300 oC and 1200 oC, respectively. The lattice parameters of Na0.5Sm4.5Ti4O15and Na0.5Eu4.5Ti4O15were determined at ordinary temperature by using X-ray powder diffraction method. Their Lattice types were determined, and their patterns were indexed. Polycrystalline X-ray diffraction data of sodium samarium titanate were listed. Differences of their crystal structures were analyzed and discussed.

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