Crystal structure and stereoisomerism of Tris(O-ethylxanthato)antimony(III) in its lattice hemiadduct with 4,4'-bipyridyl

1978 ◽  
Vol 31 (4) ◽  
pp. 757 ◽  
Author(s):  
DL Kepert ◽  
CL Raston ◽  
AH White ◽  
G Winter
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Electron Pair ◽  
Complex Molecule ◽  
Lone Pair ◽  
Antimony Atom ◽  
The Other ◽  
Mirror Plane ◽  
Crystallographic Symmetry

The preparation and crystal structure determination of the adduct [Sb(S2COEt)3],0.5C10H8N2 is reported. Crystals are triclinic, Pī, a 6.064(3), b 10.825(6), c 17.723(7) Ǻ, α 104.77(4), β 96.78(3), γ 97.14(4)°, Z 2. The compound is a lattice adduct, the bipyridyl molecule being located about a crystallographic centre of symmetry. The complex molecule geometry is unlike that of the compound [Sb(S2COEt)3]; in the latter the molecule has crystallographic symmetry 3, the three equivalent ligands being unsymmetrically coordinated, while in the present molecule the chirality is lost, the molecule conforming to approximate pseudo-m symmetry: two ligands are similar [Sb-S, 2.615(2), 2.892(2); 2.612(2), 2.878(2) Ǻ] and the other, located in the pseudo-mirror plane, is different [Sb-S, 2.477(2), 3.091(2) Ǻ]. Electron-pair repulsion theory shows that the bond angles, the relative bond lengths, and the coexistence of different stereoisomers of this molecule, can be ascribed to the stereochemically active lone pair of electrons being close to the antimony atom.

scholarly journals Bis(acetylacetonato-κ2O,O′)(pyridine-κN)(thiocyanato-κN)manganese(III): a redetermination using data from a single crystal

2013 ◽  
Vol 69 (12) ◽  
pp. m657-m657
Author(s):  
Stefan Suckert ◽  
Inke Jess ◽  
Christian Näther
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Complex Molecule ◽  
Mirror Plane ◽  
Asymmetric Unit ◽  
Pyridine Ligand ◽  
Thiocyanate Anion ◽  
Using Data

In the crystal structure of the title compound, [Mn(C5H7O2)2(NCS)(C5H5N)], the Mn3+cation is coordinated by two acetylacetonate anions, one terminal thiocyanate anion and one pyridine ligand within a slightly distorted octahedron. The asymmetric unit consists of half a complex molecule with the Mn3+cation, the thiocyanate anion and the pyridine ligand located on a mirror plane. The acetylacetonate anion is in a general position. The title compound was previously described [Stultset al.(1975).Inorg. Chem.14, 722–730] but could only be obtained as a powder. Suitable crystals have now been obtained for a high-precision single-crystal structure determination.

Methylzinn- und Methylindium-bis(trimethylsilyl)amide / Methyltin and Methylindium Bis(trimethylsilyl)amides

1991 ◽  
Vol 46 (4) ◽  
pp. 459-467 ◽  
Author(s):  
Michael Rannenberg ◽  
Johann Weidlein ◽  
Axel Obermeyer
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Homologous Series ◽  
Nmr Spectra ◽  
The Other ◽  
Crystal Structure Determination ◽  
New Compounds

BrSn[N(SiMe3)2]3 and ClIn[N(SiMe3)2]2 react with LiMe · O(C2H5)2 (Me = CH3) in toluene or hexane to give the corresponding amido derivatives MeM[N(SiMe3)2]x (M = Sn, x = 3 and M = In, x = 2). These new compounds and the other members of the homologous series MenM[N(SiMe3)2]4 or 3-n are characterized by their IR, Raman und NMR spectra. In addition, the results of the crystal structure determination of MeSn[N(SiMe3)2]3 are reported.

scholarly journals Redetermination of nickel(II) formate dihydrate

IUCrData ◽  
2018 ◽  
Vol 3 (3) ◽  
Author(s):  
Matthias Weil
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Three Dimensional ◽  
The Other ◽  
Water Molecules ◽  
Hydrogen Bonding Pattern ◽  
Medium Strength

In comparison with the previous structure determination of poly[diaquadi-μ-formato-nickel(II)], [Ni(HCOO)2(H2O)2]n, based on Weissenberg film data [Krogmann & Mattes (1963).Z. Kristallogr.118, 291–302], the current redetermination from modern CCD data revealed the positions of the H atoms, thus making a detailed description of the hydrogen-bonding pattern possible. Both Ni2+cations in the crystal structure are located on inversion centres and are octahedrally coordinated. One Ni2+cation is bound to six O atoms of six formate anions whereas the other Ni2+cation is bound to four O atoms of water molecules and to two formate O atoms. In this way, the formate anions bridge the two types of Ni2+cations into a three-dimensional framework. O—H...O hydrogen bonds of medium strength between water molecules and formate O atoms consolidate the packing.

Mossbauer spectrum, molecular and crystal structure of tin(II) diethyldithiocarbamate

1976 ◽  
Vol 29 (1) ◽  
pp. 213 ◽  
Author(s):  
BF Hoskins ◽  
RL Martin ◽  
NM Rohde
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Quadrupole Splitting ◽  
Structure Determination ◽  
Lone Pair ◽  
Molecular And Crystal Structure ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The syntheses and Mossbauer spectra of four sulphur-chelated compounds of tin(11) are reported. A single-crystal X-ray structure determination of Sn(dedtc)2 has established that the molecule possesses a strongly distorted trigonal bipyramidal configuration with a sterically active lone pair of electrons occupying an equatorial coordination position. While the Mossbauer quadrupole splitting for tin(11) compounds, in general, is consistent with a sterically active pair of electrons, its magnitude appears to be more sensitive to the nature of the ligand rather than the tin stereochemistry.

The protonation of the ethylenediphosphinetetraacetate anion and the crystal structure of the bis (hydrogen bromide) of ethylenediphosphinetetraacetic acid

1981 ◽  
Vol 46 (12) ◽  
pp. 3063-3073 ◽  
Author(s):  
Jana Podlahová ◽  
Bohumil Kratochvíl ◽  
Vratislav Langer ◽  
Josef Šilha ◽  
Jaroslav Podlaha
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Free Acid ◽  
Hydrogen Bromide ◽  
Carboxyl Groups ◽  
Spectroscopic Methods ◽  
X Ray ◽  
Partial Formation

The equilibria and mechanism of addition of protons to the ethylenediphosphinetetraacetate anion (L4-) were studied in solution by the UV, IR, 1H and 31P NMR spectroscopic methods. A total of six protons can be bonded to the anion. They are added stepwise, first with partial formation of zwitterions containing P-H bonds, which then dissociate with formation of the free acid, H4L, where all four protons are bonded in carboxyl groups. The formation of zwitterions is strongly dependent on the concentration. In the final stage, the acid bonds two additional protons to form the bis-phosphonium cation, H6L2+. A number of isostructural salts containing this cation, H4L.2 HX (X = Cl, Br, I), have been prepared. The X-ray crystal structure determination of the bromide confirmed the expected arrangement. The bromide crystals are monoclinic, a = 578.2, b = 1 425.0, c = 1 046.7 pm, β = 103.07° with a space group of P21/c, Z = 2. The final R factor was 0.059 based on 1 109 observed reflections. The structure consists of H6L2+ cations containing protons bonded to phosphorus atoms (P-H distance 134 pm) and of bromide anions, located in gaps which are also sufficiently large for I- anions in the isostructural iodide. The interbonding of phosphonium cations proceeds through hydrogen bonds, C-OH...O=C, in which the O...O distance is 275.3 pm.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

Wechselwirkungen in Molekülkristallen, 160 [1,2]. Kristallzüchtung und Strukturbestimmung der verschiedenartigen Polyphenyl-Kontaktionenmultipel [p-Quaterphenylee⊖⊖][Na⊕(DME)3]2, [p-Quaterphenyl⊖⊖(Na⊕(THF)3)2] und [p-Terphenyl⊖⊖Na⊕(DME)2Na⊕(DME)]2 / Interaction in Molecular Crystals, 160 [1, 2]. Crystallization and Structure Determination of the Different Polyphenyl Contact Ion Multiples [p-Quaterphenylee⊖⊖][Na⊕(DME)3]2, [p-Quaterphenyl⊖⊖(Na⊕(THF)3)2] und [p-Terphenyl⊖⊖Na⊕(DME)2Na⊕(DME)]2

2000 ◽  
Vol 55 (12) ◽  
pp. 1103-1113 ◽  
Author(s):  
Hans Bock ◽  
K. Gharagozloo-Hubmann ◽  
M. Sievert
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Sodium Salt ◽  
Structure Determination ◽  
Metal Cation ◽  
Molecular Crystals ◽  
Sodium Salts ◽  
Structure Determinations ◽  
Cation Coordination

The π-hydrocarbons p-terphenyl and p-quaterphenyl are reduced to their dianions in aprotic solutions of different ethers at sodium metal mirrors. Single crystal structure determinations of the solvent-separated or solvens-shared contact ion multiples, [p-terphenyl⊖⊖ Na⊕(DME)2Na⊕DME]2, p-quaterphenyl⊖⊖ ][Na⊕(DME)3]2 and [p-quaterpheny⊖⊖( Na⊕(THF)3)2], prove the essential cation solvation by the chelating dimethoxyethane (DME) versus the bulky tetrahydrofuran (THF) ligands: The solution network of equilibria between solvent separated and solvent shared ion aggregates can be considerably and transparently modified by the ether solvent selected. In addition, the structures of the monomeric sodium salts reveal partly novel details of metal cation coordination by contacts Na⊕ ··· O as well as Na⊕ ··· Cπ such as in the dimeric sodium salt of p-terphenyl dianion, [(DME)2Na⊕ (terphenyl⊖⊖)(Na⊕ DME)(terphenyl⊖⊖)Na⊕ (DME)2].

Sign in / Sign up

Export Citation Format

Share Document