The surprisingly elusive crystal structure of sodium metabisulfite

2004 ◽  
Vol 60 (2) ◽  
pp. 155-162 ◽  
Author(s):  
Kay L. Carter ◽  
Tasneem A. Siddiquee ◽  
Kristen L. Murphy ◽  
Dennis W. Bennett
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Low Temperature ◽  
Unit Cell ◽  
Sodium Metabisulfite ◽  
Asymmetric Unit ◽  
Space Group ◽  
Crystal Fragment ◽  
First Time ◽  
Correct Structure

The crystal structure of Na2S2O5, a simple and common ionic compound, is reported here for the first time. The crystals form non-merohedral twins, with the twin domains related by a twofold axis which bisects the angle between the a and c axes of each unit cell. The structure was determined from a single-crystal fragment of a twinned crystal that had undergone cleavage along the twin boundary. In addition to the problems associated with twinning, space-group determination proved difficult as well, with the structure initially determined in the P21 space group appearing to be disordered with two rotational conformers of the metabisulfite ion occupying equivalent sites in the lattice. An analysis at low temperature provided new weak reflections which were inconsistent with the original unit cell, but indexed to the correct unit cell, allowing for space group and crystal structure determination. The apparent structure, which appeared disordered in P21, seems to have resulted from an apparently fortuitous superposition of two conformationally inequivalent S2O_5^{2-} anions in the asymmetric unit of the correct structure in the P21/n space group. The metabisulfite ions in this structure do not adopt the Cs geometry observed in previously determined crystal structures containing S2O_5^{2-}. The structures of both ions in the asymmetric unit are effectively conformational mirror images of one another with two of the O atoms on each S atom in the ion approaching an eclipsed geometry. This observation provides further evidence that the structures of sulfur-oxy anions in the solid state are dictated mainly by interionic coulombic forces rather than by intraionic bonding interactions

Darstellung und Kristallstruktur von [(Me3Si)2CH(i-Pr)InCl]2 / Synthesis and Crystal Structure of [(Me3Si)2CH(i-Pr)InCl]2

1991 ◽  
Vol 46 (11) ◽  
pp. 1539-1543 ◽  
Author(s):  
Bernhard Neumüller
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Solid State ◽  
Title Compound ◽  
Unit Cell ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Cell Parameters

The title compound 1 has been prepared by the reaction of i-PrInCl2 with LiCH(SiMe3)2 in diethylether at -30 °C. The colorless substance 1 was characterized by NMR, IR, and RE spectroscopy, as well as by mass spectrometry. 1 is dimer in solution and the solid state and crystallizes in the space group P21/c with the cell parameters a = 1206.4(3) pm, b = 905.7(2) pm, c = 1591.2(5) pm, and β = 101.18(2)°. The unit cell contains two centrosymmetrical dimeric molecules.

scholarly journals Crystal structure of strontium dinickel iron orthophosphate

2015 ◽  
Vol 71 (10) ◽  
pp. 1255-1258 ◽  
Author(s):  
Said Ouaatta ◽  
Abderrazzak Assani ◽  
Mohamed Saadi ◽  
Lahcen El Ammari
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Solid State Reaction ◽  
Title Compound ◽  
Three Dimensional ◽  
The Other ◽  
Asymmetric Unit ◽  
Space Group ◽  
Edge Sharing Octahedra ◽  
Wyckoff Position

The title compound, SrNi2Fe(PO4)3, synthesized by solid-state reaction, crystallizes in an ordered variant of the α-CrPO4structure. In the asymmetric unit, two O atoms are in general positions, whereas all others atoms are in special positions of the space groupImma: the Sr cation and one P atom occupy the Wyckoff position 4e(mm2), Fe is on 4b(2/m), Ni and the other P atom are on 8g(2), one O atom is on 8h(m) and the other on 8i(m). The three-dimensional framework of the crystal structure is built up by [PO4] tetrahedra, [FeO6] octahedra and [Ni2O10] dimers of edge-sharing octahedra, linked through common corners or edges. This structure comprises two types of layers stacked alternately along the [100] direction. The first layer is formed by edge-sharing octahedra ([Ni2O10] dimer) linked to [PO4] tetrahedraviacommon edges while the second layer is built up from a strontium row followed by infinite chains of alternating [PO4] tetrahedra and FeO6octahedra sharing apices. The layers are held together through vertices of [PO4] tetrahedra and [FeO6] octahedra, leading to the appearance of two types of tunnels parallel to thea- andb-axis directions in which the Sr cations are located. Each Sr cation is surrounded by eight O atoms.

A reexamination of the low-temperature crystal structure of the p-tert-butylcalix[4]arene–toluene inclusion compound. Differences in spatial averaging with Cu and Mo Kα radiation

2002 ◽  
Vol 58 (6) ◽  
pp. 1032-1035 ◽  
Author(s):  
Gary D. Enright ◽  
Eric B. Brouwer ◽  
Konstantin A. Udachin ◽  
Christopher I. Ratcliffe ◽  
John A. Ripmeester
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Inclusion Compound ◽  
Incident Radiation ◽  
Unit Cell ◽  
Spatial Averaging ◽  
Space Group ◽  
Compound C ◽  
Low Temperature Crystal Structure ◽  
Diffraction Peaks

The low-temperature crystal structure of the p-tert-butylcalix[4]arene–toluene inclusion compound, C44H56O4·C7H8, exhibits significant guest-induced distortion of the host calixarene molecule. This distortion persists long enough to establish a correlation in the orientation of guests in adjacent host molecules. Remarkably, the space group and unit cell that best describe the structure appear to depend on the wavelength of the incident radiation. This behaviour appears to arise from spatial averaging over the different scattering volumes required to establish the diffraction peaks.

scholarly journals The Synthesis and Crystal Structure of N-tert-Butyl-3-(tert-butylimino)-2-nitropropen-1 -amine

1993 ◽  
Vol 48 (8) ◽  
pp. 1138-1142 ◽  
Author(s):  
Daryl L. Ostercamp ◽  
Lisa M. Preston ◽  
Kay D. Onan
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Solid State ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Tert Butyl ◽  
Intramolecular Hydrogen ◽  
Hydrolysis Of

The unit cell of N-tert-butyl-3-(tert-butylimino)-2-nitropropen-1-amine (4) is monoclinic, space group P21/C, with a = 9.669(4), b = 16.415(6), c = 17.341 (7) Å, and Z = 4. Hydrolysis of 4 leads to (E)-3-(N-tert-butylamino)-2-nitro-2-propenal (5), whose unit cell is monoclinic, space group P21/n, with a = 6.821(1), b = 20.707(6), c = 6.303(1)Å, and Z = 4. Compounds 4 and 5 both possess C2 symmetry in the solid state, their “U-shaped” conjugated cores being essentially planar. In each case this planarity is enforced by an intramolecular hydrogen bond.

THE CRYSTAL STRUCTURE OF 1,4-DIBROMONAPHTHALENE

1961 ◽  
Vol 39 (8) ◽  
pp. 1574-1578 ◽  
Author(s):  
J. Trotter
Keyword(s):  
Crystal Structure ◽  
Detailed Examination ◽  
Unit Cell ◽  
Asymmetric Unit ◽  
Space Group ◽  
Bond Lengths ◽  
Sufficient Precision ◽  
Molecular Dimensions

Crystals of 1,4-dibromonaphthalene are monoclinic with eight molecules in a unit cell of dimensions a = 27.45, b = 16.62, c = 4.09 Å; β = 91.9°; space group P21/a The high proportion of bromine in the crystal probably precludes location of the carbon atoms with sufficient precision to give accurate molecular dimensions, and it has therefore not been considered worth while proceeding beyond the detailed examination of the projection along the short c-axis. There are two molecules in the asymmetric unit, and the solution of the structure from hk0 Patterson and Fourier projections has indicated that these two molecules are related, at least in projection, by a pseudo center of symmetry. The projected bond distances indicate significant deviations of the bromine atoms from the aromatic plane. Approximate values of the bond lengths in the molecule have been deduced from the projected distances and estimated orientation angles.

scholarly journals Synthesis and Crystal Structure of 1-Methyl-3-(2-pyridyl)imidazolium Hexafluorophosphate

2014 ◽  
Vol 2014 ◽  
pp. 1-4
Author(s):  
Elango Kandasamy
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Weak Interactions ◽  
Unit Cell ◽  
State Structure ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Cell Parameters

Compound 1-Methyl-3-(2-pyridyl)imidazolium hexafluorophosphate was crystallized in monoclinic system with space group P21/c and unit cell parameters a=7.3740(8) Å, b=15.5931(16) Å, c=10.4787(11) Å, β= 105.3102°, and  ν=1162.12Å3. The obtained solid state structure of 1-Methyl-3-(2-pyridyl)imidazolium hexafluorophosphate shows CH⋯F type weak interactions and was analyzed.

The Crystal Structure of Bis(2,2′:6′,2″-terpyridine)nickel(II) Perchlorate Hydrate

1995 ◽  
Vol 48 (7) ◽  
pp. 1373 ◽  
Author(s):  
AT Baker ◽  
DC Craig ◽  
AD Rae
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
Least Squares ◽  
Axial Compression ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Octahedral Symmetry ◽  
Space Group ◽  
X Ray

The crystal structure of bis (2,2′:6′,2″-terpyridine)nickel(II) bis (perchlorate) hydrate has been determined by single-crystal X-ray diffractometry . The compound is monoclinic, space group P21, with two molecules in a unit cell of dimensions a 8.827(4), b 8.910(2), c 20.148(9) Ǻ, β 98.71(2)°. The structure was refined by least-squares to a residual of 0.065 for 2184 observed reflections. The compound is found to be isomorphic with the iron(II) analogue previously reported: the cation has approximate D2d symmetry, with the main distortion from octahedral symmetry being an axial compression. Both the solid state reflectance and solution spectra have been measured and some significant differences are noted.

Synthesis and Crystal Structure of 5,10,15,20-Tetrakis(3,5-dinitrophenyl)porphyrin

1998 ◽  
Vol 02 (05) ◽  
pp. 391-396 ◽  
Author(s):  
P. BHYRAPPA ◽  
K. S. SUSLICK
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Data ◽  
Crystal Structure Data ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

The synthesis, characterization and crystal structure of the octanitro-substituted porphyrin 5,10,15,20-tetrakis(3,5-dinitrophenyl)porphyrin, H 2 T (3,5- DNP ) P , are described. The solid state structure has two porphyrins in the unit cell with eight pyridine solvates and is made up from columnar arrays of the porphyrins. X-ray crystal structure data: monoclinic, space group P1 21/n1, a = 14.9996(9) Å, b = 8.2489(5) Å, c = 24.818(2) Å, α = 90 °, β = 104.172(1) °, γ = 90 °, V = 2977.3(3) Å3, dcalc = 1.440 g m-3, Z = 2.

A low-temperature polymorph ofm-quinquephenyl

2012 ◽  
Vol 68 (12) ◽  
pp. o492-o497 ◽  
Author(s):  
Ligia R. Gomes ◽  
R. Alan Howie ◽  
John Nicolson Low ◽  
Ana S. M. C. Rodrigues ◽  
Luís M. N. B. F. Santos
Keyword(s):  
Low Temperature ◽  
Cell Volume ◽  
Room Temperature ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Geometric Parameters ◽  
Asymmetric Unit ◽  
Cell Axis ◽  
Space Group ◽  
Π Interactions

A low-temperature polymorph of 1,1′:3′,1′′:3′′,1′′′:3′′′,1′′′′-quinquephenyl (m-quinquephenyl), C30H22, crystallizes in the space groupP21/cwith two molecules in the asymmetric unit. The crystal is a three-component nonmerohedral twin. A previously reported room-temperature polymorph [Rabideau, Sygula, Dhar & Fronczek (1993).Chem. Commun.pp. 1795–1797] also crystallizes with two molecules in the asymmetric unit in the space groupP\overline{1}. The unit-cell volume for the low-temperature polymorph is 4120.5 (4) Å3, almost twice that of the room-temperature polymorph which is 2102.3 (6) Å3. The molecules in both structures adopt a U-shaped conformation with similar geometric parameters. The structural packing is similar in both compounds, with the molecules lying in layers which stack perpendicular to the longest unit-cell axis. The molecules pack alternately in the layers and in the stacked columns. In both polymorphs, the only interactions between the molecules which can stabilize the packing are very weak C—H...π interactions.

Zwei neue Tetraphosphor-trichalkogeno-diiodide α′-P4Se3I2 und α′-P4S3I2 / Two New Tetraphosphorus-trichalcogeno-diiodies α′-P4Se3I2 and α′-P4S3I2

1984 ◽  
Vol 39 (6) ◽  
pp. 778-782 ◽  
Author(s):  
R. Blachnik ◽  
G. Kurz ◽  
U. Wickel
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Unit Cell ◽  
Lattice Parameters ◽  
Molten State ◽  
Asymmetric Unit ◽  
Space Group ◽  
Nmr Data ◽  
Structure In Solution

Abstractα′-P4Se3I2 and α′-P4S3I2 were prepared by the reaction of P4S3 (P4Se3) with I2 in the molten state. The structure of α′-P4Se3I2 was determined. The compound crystallizes in the tetragonal space group I4̄2d with a - 1200.5(2) pm, c = 1518.8(4) pm, and eight molecules per unit cell. The structure was refined with 814 of 1402 observed reflections to a conventional residual of R = 0.045. One half of a molecule is forming the asymmetric unit. α′-P4S3l2 is isotypic with the lattice parameters a = 1182.2(2) pm and c = 1496.8(4) pm. 31P NMR data confirm that both modifica­tions have the same bicyclic molecular structure in solution as in the solid state and form an AA′BB′ system. Evidence is presented that the α-isomer is stabilized by the formation of two additional weak P-X bonds in this molecule.

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