Multiple Metal Coordination by Calixarenes: A Structure Determination of Relevance to the Use of Calixarenes as Solvent Extraction Agents

1999 ◽  
Vol 52 (5) ◽  
pp. 403 ◽  
Author(s):  
Zouhair Asfari ◽  
Jack M. Harrowfield ◽  
Pierre Thuéry ◽  
Martine Nierlich ◽  
Jacques E. Vicens
Keyword(s):  
Solvent Extraction ◽  
Structure Determination ◽  
Metal Coordination ◽  
Monoclinic Space Group ◽  
Sodium Ions ◽  
Space Group ◽  
Axial Coordination ◽  
Carboxylate Oxygen ◽  
Insoluble Material

An insoluble material formed in attempts to extract the copper(II) complex of (R,S)-5,5,7,12,12,14- hexamethyl-1,4,8,11-tetraazacyclotetradecane with the tetraanion of tetrakis(carboxymethyl) p-t-butylcalix[4]arene recrystallizes from pyridine with the composition [Cu(C16H36N4)] [Na2(C52H60O12)].2C5H5N.4·5H2O. The crystals are monoclinic, space group P 21/c (C52h, No. 14); a 26·8524(8), b 12·8151(2), c 25·6525(8) Å; β 115·356(1)°. The structure was refined on F2 (11379 reflections, 955 parameters), giving conventional R1 0·057 (wR2 0·118). The calixarene encapsulates two sodium ions and has only tenuous connection to the copper/macrocycle complex through axial coordination of one carboxylate oxygen.

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.

scholarly journals Synthesis, Crystal Structures, and DNA Binding Properties of Zinc(II) Complexes with 3-Pyridine Aldoxime

2010 ◽  
Vol 2010 ◽  
pp. 1-7 ◽  
Author(s):  
Konstantis F. Konidaris ◽  
Rigini Papi ◽  
Eugenia Katsoulakou ◽  
Catherine P. Raptopoulou ◽  
Dimitrios A. Kyriakidis ◽  
...  
Keyword(s):  
Monoclinic Space Group ◽  
Pyridyl Nitrogen ◽  
Mobility Shift ◽  
Space Group ◽  
Pyramidal Geometry ◽  
Carboxylate Oxygen ◽  
Water Lattice ◽  
Oxygen Atoms

The employment of 3-pyridine aldoxime, (3-py)CHNOH, in ZnIIchemistry has afforded two novel compounds: [Zn(acac)2{(3-py)CHNOH}]⋅H2O(1⋅H2O) [where acac-is the pentane-2,4-dionato(-1) ion] and [Zn2(O2CMe)4{(3-py)CHNOH}2] (2). Complex1⋅H2Ocrystallizes in the monoclinic space groupP21/n. The ZnIIion is five-coordinated, surrounded by four oxygen atoms of two acac-moieties and by the pyridyl nitrogen atom of the (3-py)CHNOH ligand. Molecules of1interact with the water lattice molecules forming a 2D hydrogen-bonding network. Complex2crystallizes in the triclinicP-1space group and displays a dinuclear paddle-wheel structure. Each ZnIIexhibits a perfect square pyramidal geometry, with four carboxylate oxygen atoms at the basal plane and the pyridyl nitrogen of one monodentate (3-py)CHNOH ligand at the apex. DNA mobility shift assays were performed for the determination of thein vitroeffect of both complexes on the integrity and the electrophoretic mobility of pDNA.

Chiral Thioaldehyde Complexes of Rhenium, X-Ray Structure Determination of [Cp(NO)(Ph3P)Re(η2-S=CHPh)]PF6 [1]

1994 ◽  
Vol 49 (12) ◽  
pp. 1633-1639 ◽  
Author(s):  
Wolfdieter A. Schenk ◽  
Nicolai Burzlaff ◽  
Hans Burzlaff
Keyword(s):  
Structure Determination ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Acid Cleavage ◽  
Hydride Abstraction ◽  
Thiolate Complexes

Chiral thiolate complexes [Cp(NO)(Ph3P)ReSCH2R] (R=Ph, 4-C6H4Cl, 4-C6H4OMe, H, Me) are obtained from [Cp(NO)(Ph3P)ReCH3] by acid cleavage in the presence of thiol and subsequent deprotonation. Small amounts of (chloromethyl)thioether complexes [Cp(NO)(Ph3P)ReS(CH2Cl)CH2R]BF4 are formed when dichloromethane is used as a sol­ vent in this reaction. Hydride abstraction using [Ph3C]PF6 converts the thiolate complexes into ionic thioaldehyde complexes [Cp(NO)(Ph3P)Re(η2-S=CHR)]PF6. These are obtained as pure (RR,SS)-diastereomers as shown spectroscopically and by X-ray structure determination of [Cp(NO)(Ph3P)Re(η2-S=CHPh)]PF6. Crystals are monoclinic, space group I2/a (No. 15), a = 25.877(3), b = 18.785(2), c = 13.768(1) Å , β = 104.93(1)°, Z -8.

Bis(4-picoline-κN)gold(I) dibromidoaurate(I) and bis(4-picoline-κN)gold(I) dichloridoaurate(I): space-group ambiguity?

2013 ◽  
Vol 69 (7) ◽  
pp. 709-711 ◽  
Author(s):  
Cindy Döring ◽  
Peter G. Jones
Keyword(s):  
Phase Transformation ◽  
Hydrogen Bonds ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Data Sets ◽  
Asymmetric Unit ◽  
Space Group ◽  
Monoclinic Cell ◽  
Rule Out

Bis(4-picoline-κN)gold(I) dibromidoaurate(I), [Au(C6H7N)2][AuBr2], (I), crystallizes in the monoclinic space groupP21/n, with two half cations and one general anion in the asymmetric unit. The cations, located on centres of inversion, assemble to form chains parallel to theaaxis, but there are no significant contacts between the cations. Cohesion is provided by flanking anions, which are connected to the cations by short Au...Au contacts and C—H...Br hydrogen bonds, and to each other by Br...Br contacts. The corresponding chloride derivative, [Au(C6H7N)2][AuCl2], (II), is isotypic. A previous structure determination of (II), reported in the space groupP\overline{1} with very similar axis lengths to those of (I) [Linet al.(2008).Inorg. Chem.47, 2543–2551], might be identical to the structure presented here, except that its γ angle of 88.79 (7)° seems to rule out a monoclinic cell. No phase transformation of (II) could be detected on the basis of data sets recorded at 100, 200 and 295 K.

Preparation and Crystal Structure Determination of [(C2Η5)4N]2Hg3Cl8

1995 ◽  
Vol 50 (1) ◽  
pp. 66-70 ◽  
Author(s):  
Inge Pabst ◽  
Peter Sondergeld ◽  
Mirjam Czjzek ◽  
Hartmut Fuess
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Analysis ◽  
Structure Determination ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Coordination Type ◽  
X Ray

The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H5)4N]HgCl3 in a mixture of n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H5)4N]2Hg3Cl8, monoclinic, space group P21, a = 7.538(3), b = 19.909(6), c = 10.274(3) Å, β = 95.13(1)°, V = 1535.7(9) A3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The Hg–Cl distances within the [Hg3Cl8]2- clusters range from 2.315(3) to 2.755(4) Å. This is a new coordination type for halomercurates.

Die Röntgenstrukturanalyse der Pyrrolide (CH3)2Al - C4H3NCH3 und (CH3)2Ga - N(CCH3)4 / The X-Ray Structure Determination of the Pyrrolides (CH3)2Al - C4H3NCH3 and (CH3)2Ga - N(CCH3)4

1994 ◽  
Vol 49 (3) ◽  
pp. 430-433 ◽  
Author(s):  
Hans-Dieter Hausen ◽  
Jochen Tödtmann ◽  
Johann Weidlein
Keyword(s):  
Structure Determination ◽  
Unit Cell ◽  
Lattice Parameters ◽  
Metal Ring ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants

AbstractN-M ethyl-2-dimethylaluminium pyrrolide, (CH3)2Al -C4H3NCH3, crystallizes in the triclinic space group P1̄ with the lattice constants a = 700.5(1), b = 725.9(1), c = 886.8(1) pm, α = 67.69(1)°, β = 70.99(1)°, γ = 88.48(1)°, and Z = 2. This compound is isotypic with the gallium homologue [1], the shortest metal-ring contact between the two molecules of one unit cell decreases to 228.6 pm. N-dimethylgallium tetramethylpyrrolide has been synthesized from Li-N (CCH3)4 and (CH3)2GaCl. This “π-associate” crystallizes in the monoclinic space group P21/c with the lattice parameters a = 989.9(2), b = 1305.4(3), c = 878.3(2) pm, β - 112.73(1)° and 4 units per cell. Again two centrosymmetrically orientated molecules form a dimer by short (224.0 pm) intermolecular “Ga - πC ” contacts but the structure differs significant from the structure of the indium homologue [1].

scholarly journals New Synthesis and Structure Determination of 13-Aza-4,4,8,8,12,12-hexamethyl-2,6,10-trioxatricyclo[7,3,1,05,13]tridecane

1995 ◽  
Vol 50 (4) ◽  
pp. 667-670 ◽  
Author(s):  
Konstantina Kehagia ◽  
Alexander Dömling ◽  
Ivar Ugi ◽  
Wolfgang Hiller ◽  
Jürgen Riede
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Space Group ◽  
New Synthesis

A new 13-Aza-4,4,8,8,12,12-hexamethyl-2,6,10-trioxatricyclo[7,3,1,05,13]tridecane synthesis and the crystal structure are reported. It crystallizes in the monoclinic space group P21/n with a = 1201.9(1) pm, b = 1436.6(1) pm, c = 1726.2(2) pm, β = 90.74(1)° and Z = 8.

Neue Mangan(III)-Fluoridhydrate: Na[MnF4(H2O)2] und Na[MnF4(H2O)2] · H2O / New Fluoride Hydrates of Manganese(III): Na[MnF4(H2O)2] and Na[MnF4(H2O)2] · H2O

1990 ◽  
Vol 45 (5) ◽  
pp. 593-597 ◽  
Author(s):  
Werner Massa ◽  
Roland E. Schmidt
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Teller Effect ◽  
Crystal Structure Determination ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Jahn Teller ◽  
Jahn Teller Effect

Crystalline Na[MnF4(H2O)2] and Na[MnF4(H2O)2] · H2O have been precipitated from aqueous HF solution of MnO(OH) and NaF. The crystal structure determination of the trihydrate (space group C 2/c, Z = 8, α = 1638.1(2), b = 667.6(2), c = 1130.3(1) pm, β = 103.78(1)°; R/wR = 0.038/0.033 for 1696 independent reflections) showed the presence of isolated octahedral trans-[MnF4(H2O)2]- anions with an elongation of the H2O-Mn—OH2 axis due to the Jahn-Teller effect (Mn 1-O 224.6(2), Mn 1—F(mean) 183.7(1); Mn2-0 218.3(2), Mn2— F(mean) 184.7(2) pm). As a consequence, an unusual H-bond geometry is observed with a tetrahedral (instead of trigonal) environment of the coordinated O atoms. Na[MnF4(H2O)2] is monoclinic (space group C 2/m, C 2 or Cm, a = 816.6(4), b = 677.1(1), c = 496.8(2), β = 114.45(3)°), the crystals show twinning and 1-dimensional disorder.

Kristallstruktur von Triphenylmethyliodsulfan (C6H5)3CSI [1] / Crystal Structure of Triphenylmethyliodosulfane (C6H5)3 CSI [1]

1988 ◽  
Vol 43 (4) ◽  
pp. 399-402 ◽  
Author(s):  
Rolf Minkwitz ◽  
Hans Preut ◽  
Jürgen Sawatzki
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Space Group

Abstract The crystal structure of (C6H5)3CSI is reported. It is the first structure determination of an iodine sulfane. (C6H5)3CSI crystallizes in the monoclinic space group P21/c with a - 1226.4(7) pm, b = 1398.8(18) pm, c = 941.6(8) pm, β = 96.38(8)° and Z = 4. The sulfur-iodine bond length is 240.6(4) pm corresponding to the sum of the covalent radii with 237 pm. The molecules are linked via short I···S contacts of 321.0(4) pm such that a zig-zag chain is formed.

Funktionelle Trimethylphosphanderivate, XXII [1] Struktur und Reaktivität von Lithium-tris(dimethylphosphino)methanid sowie Molekülstruktur von / Functional Trimethylphosphine Derivatives, X X II [1] Structure and Reactivity of Lithium-tris(dimethylphosphino)methanide and Molecular Structure of

1984 ◽  
Vol 39 (11) ◽  
pp. 1518-1528 ◽  
Author(s):  
Hans Heinz Karsc ◽  
Lothar Weber ◽  
Dietmar Wewers ◽  
Roland Boese ◽  
Gerhard Müller
Keyword(s):  
Least Squares ◽  
Structure Determination ◽  
Solvent Molecule ◽  
Pair Interaction ◽  
Major Product ◽  
Monoclinic Space Group ◽  
Reaction Conditions ◽  
Space Group ◽  
X Ray

Abstract The reaction of Lithium-tris(dimethylphosphino)methanide with methyl iodide is sensitive to the choice of the solvent and reaction conditions; in pentane at room temperature and in the presence of tetramethylethylenediamine, Me3P = C(PMe2)2 is the major product, whereas in tetrahydrofuran, (Me2P)3C -CH3 is formed predominantly. Under similar conditions, Lithium-bis- (dimethylphosphino)methanide reacts with Mel to give (Me2P)2C(CH3)H as the main product. An X-ray structure determination of the tetrahydrofuran solvate of LiC(PMe2)3 reveals this compound to be dimeric with one solvent molecule coordinating to Li. A pseudo tetrahedral coordination sphere around each Li atom is completed by two phosphino groups of one [C(PMe2)3]- anion and a contact ion pair interaction with the carbanionoid center of the second. The crystals are monoclinic, space group P21/n, with a = 928.5(2), b = 1250.8(3), c = 1407.9(3) pm, β = 100.07(1)°, V = 1609.9 • 106 pm3 Dc = 1.13 g/cm3 for Z - 4 at -40 °C. Full-matrix least-squares refinement of 249 parameters based on 2158 reflections converged at R = 0.029. The ligand properties of (Me2P)3CCH3 are tested in its reactions with (CO)4Cr(C7H8) and (CO)5Cr[CH2S(O)Me2] from which and may be isolated. The latter crystallizes in the monoclinic space group P21/c with a - 1218.5(3). b = 881.7(3), c = 1824.1(4) pm, β = 106.66(2)°, V = 1877.6(9) • 106 pm3, Dc = 1.37 g/cm3 for Z = 4. Least-squares refinement of 218 parameters on 1615 reflections produced R = 0.063. The structure determination confirms the molecule to contain a five-membered heterocycle in an approximate envelope conformation.

Sign in / Sign up

Export Citation Format

Share Document