The crystal and molecular structures of two isostructural complexes: [(H3O•18-crown-6)2(ZnCl4)] and [(H3O•18-crown-6)2(MnCl4)]

1990 ◽  
Vol 68 (6) ◽  
pp. 797-803 ◽  
Author(s):  
Robert Chênevert ◽  
Daniel Chamberland ◽  
Michel Simard ◽  
François Brisse
Keyword(s):  
Crown Ether ◽  
Molecular Structures ◽  
The Other ◽  
Tetrahedral Coordination ◽  
Monoclinic System ◽  
Crystal And Molecular Structures ◽  
Hydronium Ion ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Ether Molecule

New macrocycle polyether 18-crown-6 complexes of stoichiometry [(H3O+•18-crown-6)2(MC42−)] have been synthesized for M = Zn and Mn. The two complexes are isostructural and crystallize in the monoclinic system, space group C2/c. The unit cell dimensions are as follows: a = 16.229(9), b = 11.535(3), c = 20.134(8) Å, β = 97.55(4)° and a = 16.255(6), b = 11.625(3), c = 20.122(8) Å, β = 96.54(3)° for the Zn and Mn complexes respectively. In both crystal structures (final Rw = 0.048 with 1817 reflections for Zn and Rw = 0.074 with 728 reflections for Mn), the crown ether molecule and the H3O+ cation to which it is hydrogen-bonded are disordered over two sites. The MCl42− anions, which have tetrahedral coordination, are on crystallographic twofold axes of rotation. The Mn—Cl and Zn—Cl distances average 2.270 and 2.361 Å respectively. The hydronium cation, H3O+, has pyramidal coordination. Of the two disordered crown ether molecules in the Zn and the Mn complexes, one has a slightly deformed (ttg)6 conformation while the other one may be described as having the distorted (ttg)5(ttc) conformation. These observations are in agreement with the infrared analyses of the complexes. Keywords: 18-crown-6 complexes, hydronium ion, ZnCl42−, MnCl42−, crystal structure.

Cyclopentadienyl-Ruthenium and -Osmium Chemistry. XL. X-Ray Crystal Structures of MBr (PPh3)2(η-C5H5).CH2Cl2 (M = Ru, Os)

1995 ◽  
Vol 48 (11) ◽  
pp. 1887 ◽  
Author(s):  
MI Bruce ◽  
PJ Low ◽  
BW Skelton ◽  
ERT Tiekink ◽  
A Werth ◽  
...  
Keyword(s):  
Structural Parameters ◽  
Molecular Structures ◽  
Coordination Geometry ◽  
Chloro Complexes ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structures of MBr (PPh3)2(η-C5H5).CH2Cl2 (M = Ru and Os) have been determined. A revised synthesis of the bromo osmium complex is given. The coordination geometry about the metal atom is based on a distorted octahedron with one face being occupied by the cyclopentadienyl group [average Ru -C(Cp) 2.214(3), Os-C(Cp) 2.177(3)Ǻ] and the other by the bromide [ Ru -Br 2.5683(8), Os-Br 2.5438(9)Ǻ] and the two phosphorus atoms [ Ru -P 2.323(2), 2.329(1); Os-P 2.290(2), 2.297(2)Ǻ]. Structural parameters are compared with those of the corresponding chloro complexes and differ only minimally. Crystals of MBr (PPh3)2(η-C5H5).CH2Cl2 are triclinic, space group Pī , with unit cell dimensions ( Ru [Os]): a 14.374(5) [14.276(4)], b 14.057(4) [13.959(3)], c 10.012(5) [9.903(3)]Ǻ, α 99.43(3) [99.79(2)], β 105.60(3) [105.74(2)], γ 100.42(3) [100.39(2)]°, V 1868(1) [1817.7(9)] Ǻ3, Z 2. The structures were refined by a full-matrix least-squares procedure to R 0.050 [0.036] for 7365 [5108] reflections with I ≥ 3σ(I).

Gold(I) dimers. The synthesis and reactions of [tert-BuC≡CAu(dmpm—P)], and the crystal and molecular structures of [Au2(µ-dmpm)2]X2•2H2O, X = Cl, I

1988 ◽  
Vol 66 (12) ◽  
pp. 3176-3183 ◽  
Author(s):  
N. C. Payne ◽  
R. J. Puddephatt ◽  
R. Ravindranath ◽  
I. Treurnicht
Keyword(s):  
Chlorinated Solvents ◽  
Chloride Ion ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Crystal And Molecular Structures ◽  
Cell Dimensions ◽  
Network Of Hydrogen Bonds ◽  
Final Agreement ◽  
Unit Cell Dimensions

Acetylide complexes of formula [tert-BuC≡CAu(R2PCH2PR2)], R = CH3 (6a) and C6H5 (6b), have been prepared, and characterized by spectroscopic methods. These complexes undergo a fluxional process involving a three-coordinate Au(I) centre. Complex 6a dimerizes by a first-order process in chlorinated solvents, with substitution of the acetylide ligand by chloride ion, to form [Au2(µ-dmpm)2]Cl2•2H2O (7a). The crystal and molecular structures of 7a and the iodide salt 7b have been determined by single crystal X-ray diffraction methods. Both crystallize in the triclinic space group [Formula: see text] with Z = 1; unit cell dimensions are a = 7.962(1), b = 9.987(1), c = 7.895(1) Å, α = 90.11, β = 109.13(1), and γ = 112.84(1)° for 7a; a = 8.243(1), b = 9.057(1), c = 8.167(1) Å, α = 90.23, β = 110.33(1), and γ = 89.92(1)° for 7b. The analyses refined to final agreement factors on F of R = 0.035 based on 3225 unique reflections with I > 3σ (I) for 7a, and R = 0.030 based on 2971 unique reflections with I > 3σ(I) for 7b. The structures are closely related, with the cations containing an eight-membered centrosymmetric ring formed by the Au(I) centres and the bridging dmpm ligands. The Au … Au′ distances are 3.014(1) and 3.019(1) Å in 7a and 7b, respectively. In the solid state, the halide ions bridge the two Au centres, and, together with the water molecules, form a network of hydrogen bonds running at an angle of 104° to the eight-membered Au2P4C2 rings.

The First Molecular Complex Containing Two Azoarenes. The Crystal Structure of Decafluoroazobenzene/Azomesitylene (1 : 1)

1989 ◽  
Vol 42 (5) ◽  
pp. 741 ◽  
Author(s):  
MI Bruce ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
Molecular Complex ◽  
Title Compound ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
Vertical Separation ◽  
Full Matrix ◽  
Crystal And Molecular Structures ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structures of the title compound, C12F10N2.C18H22H2,are reported. The crystal structure is comprised of stacks of alternate decafluoroazobenzene and azomesitylene molecules with the vertical separation between successive molecules being approximately 3.42 � . The stacks are aligned so that the azobenzene molecules of one stack are adjacent to the azomesitylene molecules of the neighbouring stacks; there are no significant intercolumn contacts. Crystals are monoclinic, space group P21/n with unit cell dimensions a 7.197(2), b 15.432(3), c 12.513(3) � , β 96.33(2)� , and Z 2. The structure was refined by a full-matrix least-squares procedure to final R 0.059 for 915 reflections for which 1 ≥ 3.O σ(I).

scholarly journals Synthesis and Characterization of [2-CH3CH2C6H4NH3]6P6O18⋅4H2O

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Houda Marouani ◽  
Salem Slayyem Al-Deyab ◽  
Mohamed Rzaigui
Keyword(s):  
Hydrogen Bonds ◽  
Electrostatic Interactions ◽  
Three Dimensional ◽  
Spectroscopic Studies ◽  
Monoclinic System ◽  
Dimensional Network ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Ir Spectroscopic

Single crystals of [2-CH3CH2C6H4NH3]6P6O18⋅4H2O are synthesized in aqueous solution by the interaction of cyclohexaphosphoric acid and 2-ethylaniline. This compound crystallizes in the monoclinic system with P21/c space group the unit cell dimensions are: a=16.220(4) Å, b=10.220(5) Å, c=20.328(4) Å, β=113.24(3)∘, Z=2, and V=3096.5(18) Å3. The atomic arrangement can be described by layers formed by cyclohexaphosphate anions P6O186− and water molecules connected by hydrogen bonds O–H⋯O. These inorganic layers are developed around bc planes at x=1/2 and are interconnected by the H-bonds created by ammonium groups of organic cations. All the hydrogen bonds, the van der Waals contacts and electrostatic interactions between the different entities give rise to a three-dimensional network in the structure and add stability to this compound. The thermal behaviour and the IR spectroscopic studies of this new cyclohexaphosphate are discussed.

scholarly journals X-ray Crystallographic Study of Ranaconitine

2011 ◽  
Vol 6 (11) ◽  
pp. 1934578X1100601
Author(s):  
Yang Li ◽  
Jun-Hui Zhou ◽  
Gui-Jun Han ◽  
Min-Juan Wang ◽  
Wen-Ji Sun ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Diffraction Analysis ◽  
Critical Role ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
X Ray ◽  
Crystallographic Study ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal structure of natural diterpenoid alkaloid ranaconitine isolated from Aconitum sinomontanum Nakai has been determined by single crystal X-ray diffraction analysis. The crystal presents a monoclinic system, space group C2 with Z = 4, unit cell dimensions a = 30.972(19) Å, b = 7.688(5) Å, and c = 19.632(12) Å. Moreover, the intermolecular O–H···O hydrogen bonds and weak π-π interactions play a critical role in expanding the dimensionality.

scholarly journals An antitrichomonal drug. 2-(2'-Thenoyl)amino-5-nitrothiazole, C8H5O3N3S2. The crystal and molecular structures of a novel monoclinic system solvated with dimethylformamide.

1987 ◽  
Vol 35 (6) ◽  
pp. 2419-2425 ◽  
Author(s):  
BERNARD VIOSSAT ◽  
NGUYEN-HUY DUNG ◽  
JEAN-CHARLES LANCELOT ◽  
FRANCIS ROBERT ◽  
MAX ROBBA
Keyword(s):  
Molecular Structures ◽  
Monoclinic System ◽  
Crystal And Molecular Structures

The crystal and molecular structure of tris-butyl-tin(IV)-(1-pyrrolidinecarbodithioato)-3-propionate

1989 ◽  
Vol 54 (3) ◽  
pp. 684-690 ◽  
Author(s):  
Jan Lokaj ◽  
Viktor Vrábel ◽  
Eleonóra Kellö ◽  
Vladimír Ratay
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Analysis Method ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structure of Bu3Sn(pyrn-dtc-prop) was solved by the X-ray structural analysis method and refined by the block diagonal least squares method to R = 0.053 for 1 930 observed reflections. The compound crystallizes in the monoclinic system with a space group of P21/c, Z = 4, F(000) = 1 056, with unit cell dimensions of a = 1.4758(5), b = 0.9970(3), c = 1.9166(6) nm; β = 113.90(2)°. The measured and calculated crystal densities were Dm = 1.32 and Dc = 1.31.103 kg m-3. The tin atom is coordinated by three carbon atoms at distances of Sn-C 0.2117(8), 0.2133(8), 0.2158(11) nm and two oxygen atoms O(1) and O(2) at distances of Sn-O 0.2210(5) and 0.2399(5) nm. The coordination polyhedron is a deformed trigonal bipyramid. The S2CN ligand is approximately planar.

Structural study in the oligomethylene dithiobenzoate series, nDBS, where n, the number of methylene groups, is odd

1992 ◽  
Vol 70 (3) ◽  
pp. 900-909 ◽  
Author(s):  
Claude Leblanc ◽  
François Brisse
Keyword(s):  
Crystal Structure ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cells ◽  
Methylene Groups ◽  
Unit Cell Dimensions ◽  
Centrosymmetric Dimers

Model compounds of the poly(oligomethylene thioterephthalates) have been synthesized and characterized by X-ray diffraction analyses. The pink n-methylenedithiobenzoates, obtained for n = 3, 5, 7, and 9, all have a low melting point of about 320–330 K. They all crystallize in the monoclinic system, space group P21/c. The a and b unit cell dimensions vary little while the c dimension increases monotonically as n changes from 3 to 9. The crystal structure of the four compounds were established from low-temperature X-ray intensities. Except for the lengthening of the methylenic sequence, the four molecules studied here are isostructural. One of the thiobenzoate groups of the molecules is coplanar with all the methylenic carbons, while the other thiobenzoate group is at 90° from the above plane of atoms. The methylenic sequence has the same conformation. It may be described by g+(t)n, where n is the number of methylene groups. Thus, the four compounds belong to a crystallographically homologous series. The molecules form centrosymmetric "dimers," which, in turn, are herring-bone packed in their respective unit cells. In each "dimmer" two aromatic rings are across from one another while being mutually perpendicular. On the basis of the above results, one proposes three potentially acceptable structures for the parent poly(oligomethylene thioterephthalates). Keywords: dithiobenzoate, methylene sequence, crystal structure, poly(oligomethylene thioterephthalate).

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