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.

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.

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.

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.

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.

The Flavonoids of Combretum quadrangulare: Crystal structures of the Polymorphic Forms of 5-Hydroxy-2-(4'-hydroxy-3',5'-dimethoxyphenyl)-3,7-dimethoxy-4H-1-benzopyran-4-one

1985 ◽  
Vol 38 (8) ◽  
pp. 1177 ◽  
Author(s):  
IR Castleden ◽  
SR Hall ◽  
S Nimgirawath ◽  
S Thadaniti ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Β Phase ◽  
Α Phase ◽  
Polymorphic Forms

The following substituted 2-phenyl-4H-1-benzopyran-4-ones have been isolated from the dried flowers of Combretum quadrangulare Kurz ( Combretaceae ): 5-hydroxy-3,3′,4′,5′,7-pentamethoxy ( combretol ) (1), 3′,5-dihydroxy-3,4′,7-trimethoxy ( ayanin ) (2) and 4′,5-dihydroxy- 3,3′,5′,7-tetramethoxy (3). The last substance (3) was obtained as a mixture of two polymorphic forms (α and β) each of which was characterized by X-ray diffraction. Diffractometer data at 295 K were refined by full matrix least squares to residuals of 0.043 (1181 'observed' reflections) for the α-phase and 0.044 (1421) for the β phase of (3). Crystals of the α-phase of (3) are triclinic, Pī, a 12.663(6), b 9.592(4), c 7.444(4) Ǻ, α 102.48(3), β 101.39(4), γ 91.72(4)°,Z 2. Crystals of the β-phase of (3) are monoclinic P21/n, a 17.139(8), b 12.728(6), c 7.845(7) Ǻ, β 95.07(6)°, Z 4. An unambiguous synthesis of (3) was also achieved.

Crystal structures of hexa(N-methylurea)cobalt(II) sulfate and thiosulfate

1980 ◽  
Vol 33 (2) ◽  
pp. 425 ◽  
Author(s):  
BN Figgis ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Complex Cation ◽  
X Ray Diffraction ◽  
Threefold Axis ◽  
X Ray

The crystal structures of the title compounds, [Co(C2H6N2O)6](SO4)(1) and[Co(C2H6N2O)6](S2O3) (2), have been determined at 295 K by X-ray diffraction using diffractometer data and refined by least squares to residuals of 0.042 (1), 0.043 (2) [875 and 926 reflections with I > (3σ(I)]. Crystals are trigonal, R 3c, a 1.4890(1) nm, α 43.34(1)° (1); a 1.4760(3) nm, α 44.53(1)° (2), Z 2. The compounds are isostructural; the complex cation has 3 symmetry, Co-O, 209.6(2) (1), 209.9(2) pm (2); the geometry of the ligand is well defined and precise, but the anions, located at sites of symmetry 32, are disordered. ��� The cobalt environment is distorted from Oh symmetry, being compressed along the threefold axis.

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.

Crystal structures of (RS)-Di-μ-chloro-tetrakis(ethane-1,2-diamine)nickel(II) dichloride and diperchlorate

1978 ◽  
Vol 31 (2) ◽  
pp. 285 ◽  
Author(s):  
GA Bottomley ◽  
LG Glossop ◽  
CL Raston ◽  
AH White ◽  
AC Willis
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Complex Cation ◽  
Dimeric Complex ◽  
X Ray Diffraction ◽  
X Ray ◽  
Coordination Sites

The crystal structures of [(en)2NiCl2Ni(en)2] Cl2 (1) and [(en)2NiCl2Ni(en)2] (ClO4)2 (2) have been redetermined from single- crystal X-ray diffraction data at 295(1) K and refined by least squares to residuals of 0.073 and 0.052 respectively for 1345 and 1605 'observed' reflections respectively. Crystals of (1) are monoclinic, P21/n, a 14.053(4), b 11.309(3), c 6.326(1) Ǻ, β 94.22(2)�, Z 2. Crystals of (2) are monoclinic, P21/n, a 8.885(12), 6 19.707(20), c 7.120(8) Ǻ, β 108.99(4)�, Z 2. In both (1) and (2), a dimeric complex cation is observed, a pair of cis coordination sites about the nickel in each case being occupied by the bridging chlorines; the latter are asymmetric (Ni-Cl, 2.461(3), 2.551(3)(1); 2.461(3), 2.512(3) Ǻ (2)).

Crystal structures of Bis[(ethane-1,2-diyl)bis(diphenylphosphine)]-palladium(II) and -platinum(II) dichloride dichloromethane and Dichloro[(ethane-1,2-diyl)bis(diphenylphosphine)]platinum(II) dichloromethane

1984 ◽  
Vol 37 (11) ◽  
pp. 2193 ◽  
Author(s):  
LM Engelhardt ◽  
JM Patrick ◽  
CL Raston ◽  
P Twiss ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Centrosymmetric Molecule ◽  
Platinum Analogue

The crystal structures of the title compounds have been established by single-crystal X-ray diffraction techniques at 295 K, being refined by least squares to residuals of 0.043, 0.036, 0.036 for 2057, 3176 and 3468 independent 'observed' reflections respectively. Crystals of [Pd(diphos)2] C12 (1) (diphos = Ph2P(CH2)2PPh2) are monoclinic, P21/c, with a 12.779(9), b 18.084(10), c 12.942(6) �, β 119.29(5)�, 22; for the isostructural platinum analogue (2), a 12.789(4), b 18.099(7), c 12.965(4) �, β 1l9.39(2)�. Crystals of [PtCl2(diphos)].CH2Cl2, (3), are orthorhombic, P212121, with a 21.360(6), b 13.499(4), c 9.551(5)� Z 4. Complexes (1) and (2) are also solvated but the nature of the solvation is complicated by disorder and less clearcut than in (3). In (1), Pd-P distances are 2.342(2), 2.347(2) � in a centrosymmetric molecule; in (2), Pt-P distances are 2.332(2), 2.335(2) �, while in (3), Pt-P distances are 2.230(2), 2.224(3) � and Pt-Cl are both 2.355(2) � [cf. 2.233(2), 2.226(2), (2.361(2), 2.357(2))� respectively for the previously studied palladium analogue].

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