The stuctural nature of a Bender's salt: an X-ray study of potassium O-methyl monothiocarbonate

1975 ◽  
Vol 28 (6) ◽  
pp. 1195 ◽  
Author(s):  
BF Hoskins ◽  
CN Murphy
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Least Squares Method ◽  
Potassium Ions ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

The structure of the Bender's salt, potassium O-methyl monothiocarbonate (C2H3O2S-K+), has been determined by single crystal X- ray diffraction methods. The crystals are monoclinic of space group P21/c with a 6.7295(5), b 6.9438(5), c 11.1520(10) Ǻ, β 110.93(2)� and Z 4. The structure was solved using a direct phasing programme in conjunction with the Patterson synthesis and refined by a full-matrix least-squares method to R 0.041 for the 788 independent statistically significant reflections collected by counter methods. The crystals are composed of potassium ions and O-methyl monothiocarbonate anions. Each anion is essentially planar with bond lengths and angles having values very similar to those of related systems.

Crystal Structure of Tetraethylammonium Bromopentacarbonyltungstate(0)

1995 ◽  
Vol 48 (5) ◽  
pp. 1045 ◽  
Author(s):  
T Whyte ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
R Value

The crystal structure of tetraethylammonium bromopentacarbonyltungstate (0), [NEt4] [W(CO)5Br], has been determined by single-crystal X-ray diffraction methods at 22�1°C. Crystals are tetragonal, space group P4/n, with a 9.206(2), c 10.484(2) Ǻ, and Z 2. Full-matrix least-squares refinement gave a final R value of 0.034 for 820 independent reflections. The [W(CO)5Br]- anion possesses exact C4v symmetry, with bond lengths W-Br 2.736(1), W-COtrans 1.93(1) and W-COcis 2.034(6) Ǻ.

Structural Systematics of Metal Acetylide Complexes. II. X-Ray Studies of Some Nickel σ-Acetylide Complexes

1998 ◽  
Vol 51 (3) ◽  
pp. 219 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Trans Influence

The structures of Ni(C≡CR)(PPh3)(η-C5H5) (R = Ph (1), C6H4-4-NO2 (2), 4-C6H4C6H4-4′-NO2 (3), (E)-4-C6H4CH=CHC6H4-4′-NO2 (4), 4-C6H4C≡CC6H4-4′-NO2 (5), 4-C6H4N=CHC6H4-4′-NO2 (6)) have been determined by single-crystal X-ray diffraction studies, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a 10·094(2), b13·429(3), c 18·835(5) Å,α 103·24(2), β 91·50(2), γ 90·10(2)°, Z 4, 5844 unique reflections (595 parameters), converging at R 0·033 and Rw 0·024. For (2), crystals are orthorhombic, space group Pna21, with a 16·799(2), b 8·681(2), c 17·485(2) Å, Z 4, 1774 unique reflections (325 parameters), converging at R 0·031 and Rw 0·029. For (3), crystals are monoclinic, space group P 21/c, with a 11·140(3), b 18·282(4), c 15·296(2) Å, β 105·18(2)°, Z 4, 3132 unique reflections (397 parameters), converging at R 0·039 and Rw 0·024. For (4), crystals are monoclinic, space group P 21/n, with a 12·929(7), b 16·953(8), c 15·601(7) Å, β 112·55(3), Z 4, 3023 unique reflections (397 parameters), converging at R 0·039 and Rw 0·025. For (5), crystals are monoclinic, space group P 21/n, with a 12·710(5), b 16·882(3), c 15·693(4) Å, β 111·37(3)°, Z 4, 3216 unique reflections (397 parameters), converging at R 0·035 and Rw 0·030. For (6), crystals are monoclinic, space group P 21/n, with a 12·594(1), b 16·936(2), c 15·611(1) Å, β 112·476(5)°, Z 4, 3564 unique reflections (397 parameters), converging at R 0·038 and Rw 0·041. For structurally characterized 18-electron (cyclopentadienyl)nickel(II) acetylide complexes, statistically insignificant decreases in the average Ni-C(1) distance and trans influence and an increase in the average C(1)-C(2) parameter are observed on introduction of an acceptor substituent at the alkynyl ligand.

Studies of β-Diketone Complexes of Rhenium(V). The Molecular and Crystal Structure of trans-Dichlorobis(pentane-2,4-dionato)rhenium(IV)

1973 ◽  
Vol 51 (13) ◽  
pp. 2073-2076 ◽  
Author(s):  
I. D. Brown ◽  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Molecular And Crystal Structure ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths ◽  
Dimeric Structure

One of the compounds obtained by reacting acetylacetone with oxoethoxodichlorobis(triphenylphosphine)rhenium(V) has been shown by single crystal X-ray diffraction to be trans-dichlorobis(pentane-2,4-dionato)rhenium(IV). The crystals are triclinic, a = 8.032(4), b = 8.344(6), c = 7.429(6) Å, α = 118.1(2), β = 92.3(2), γ = 55.5(2)°, [Formula: see text], Z = 1. Intensities were measured with a microdensitometer from photographs recorded on an integrating precession camera. Of the 991 measured reflections all were observed and 984 were used in the refinement. The structure was refined by full matrix least squares to an R2 value of 0.0685. The compound was found to be a trans-monomer, in contrast to the dimeric structure claimed to exist in solution. The ligand atoms bonded to rhenium lie almost exactly at the apices of an octahedron and the bond lengths (Re—Cl, 2.326(8); Re—O1, 1.97(1); Re—O2, 2.01(1) Å) are in the range expected.

Crystal structure of Tris(N,N-diethyldithiocarbamato)thallium(III)

1978 ◽  
Vol 31 (9) ◽  
pp. 1927 ◽  
Author(s):  
DL Kepert ◽  
CL Raston ◽  
NK Roberts ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
Electron Pair ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The crystal structure of the title compound, [Tl(S2CNEt2)3], has been determined by single-crystal X-ray diffraction methods at 295 K and refined by full-matrix least squares to a residual of 0.050 for 2517 'observed' reflections. Crystals are monoclinic, with space group A2/a, a 14.789(7), b 10.428(4), c 18.207(9) Ǻ, β 118.11(4)°, Z 4, and are isostructural with those of the previously determined gallium and indium analogues, the molecule having 2 symmetry with <Tl-S> 2.666 Ǻ. As in the dimethyl/thallium analogue, the departure of the TlS6 core symmetry from 3 is large and is examined in terms of electron-pair repulsion theory.

Crystal Structure of ζ2' Martensite in Au-49.5at%Cd Alloy

1991 ◽  
Vol 246 ◽  
Author(s):  
Yutaka Emura ◽  
Takuya Ohba ◽  
Kazuhiro Otsuka
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Least Squares ◽  
Least Squares Method ◽  
Diffraction Method ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Lattice Constants

AbstractCrystal structure of the ζ2' martensite in a Au-49.5at%Cd ally has been analyzed by the single crystal x-ray diffraction method. The crystal lattice was trigonal and the lattice constants were a:0.8095(3) and c=o.57940(6) nm. There were 18 atoms in a unit cell. The space group was P3, which was different from that previously determined by Vatanayon and Hehemann. The structure was refined by the full matrix least squares method to a final R factor of 7.8% and a weighted R factor of 4.1%.

Crystal structure of zerumbone [(E,E,E)-2,6,9,9-Tetramethylcycloundeca-2,6,10-trien-1-one]

1981 ◽  
Vol 34 (10) ◽  
pp. 2243 ◽  
Author(s):  
SR Hall ◽  
S Nimgirawath ◽  
CL Raston ◽  
A Sittatrakul ◽  
S Thadaniti ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Zingiber Zerumbet ◽  
Space Group ◽  
X Ray ◽  
Considerable Distortion

The crystal structure of zerumbone, C15H22O, extracted from the rhizomes of Zingiber zerumbet Smith, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.051 for 925 'observed' reflections. Crystals are monoclinic, space group P21/c, a 9.036(3), b 9.712(5), c 15.643(6) �, β 97.19(3)�, Z = 4. Although the molecule has no chiral centre, the presence of the three trans double bonds confers considerable distortion and rigidity on the eleven-membered ring and renders the whole molecule chiral and potentially resolvable.

Filling up another Gap: Synthesis and Crystal Structure of Ba2H3I

2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides

Ring contraction of 4-substituted 2,6-dichlorophenols. The crystal structure of 2,2,4α,5α-Tetrachloro-1α,3α-dihydroxycyclopentane-1,4-carbolactone

1977 ◽  
Vol 30 (10) ◽  
pp. 2195 ◽  
Author(s):  
RM Christie ◽  
RW Rickards ◽  
KJ Schmalzl ◽  
D Taylor
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Major Product ◽  
X Ray Diffraction ◽  
Ring Contraction ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Counter Data

Alkaline chlorination of the 4-alkyl-2,6-dichlorophenols (2b) and (2c) proceeds through ring contraction and halolactonization to form the 4α- alkyl-2,2,5α-trichloro-1α,3α-dihydroxycyclopentane-1,4-carbolactones (4b) and (4c). Under similar conditions, 2,4,6-trichlorophenol affords the analogous 2,2,4α,5α-tetrachloro-1α,3α-dihydroxycyclopentane-1,4- carbolactone (4a) in low yield, in addition to the Hantzsch acid (3a) as the major product. The acid (3a) upon further treatment undergoes chloro-lactonization to give the lactone (4a). The structures of the lactones (4b) and (4c) follow from spectroscopic comparison with (4a), the structure of which has been established by X-ray diffraction (C6H4Cl4O4 orthorhombic a 13.485(1), b 12.348(1), c 11.371(1) Ǻ, space group Pccn, Z 8, solved by direct methods and refined by block-diagonal and full-matrix least squares to R 0.031, Rw 0.043 for 1313 unique counter data with I/σ(I) ≥ 3.0).

Crystal structure of 8-Hydroxy-1H-naphtho[2,1,8-mna]xanthen-1-one

1984 ◽  
Vol 37 (8) ◽  
pp. 1763
Author(s):  
IR Castleden ◽  
LM Engelhardt ◽  
SR Hall ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Charge Transfer ◽  
Single Crystal ◽  
Least Squares ◽  
Interplanar Spacing ◽  
Charge Transfer Complexes ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal structure of 8-hydroxy-1H-naphtho[2,1,8-mna]xanthen-1-one, C19H10O3, obtained as an indefinite methanolsolvate, has been determined at 295K by single-crystal X-ray diffraction methods, being refined by full matrix least squares to a residual of 0.056 for 892 independent 'observed' reflections. Crystals are monoclinic, P21/c, a 5.128(4), b 10.024(9), c 27.45(2) �, β 107.73(6)�, Z 4. The packing of the molecules is typically that of charge-transfer complexes, with an interplanar spacing of c.3.5 �.

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.

Sign in / Sign up

Export Citation Format

Share Document