Studies of rhenium–carboxylate complexes. III. The crystal and molecular structure of tetra-μ-n-butyratodirhenium(III) diperrhenate

1970 ◽  
Vol 48 (2) ◽  
pp. 219-224 ◽  
Author(s):  
C. Calvo ◽  
N. C. Jayadevan ◽  
C. J. L. Lock ◽  
R. Restivo
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
The Other ◽  
Formula Unit ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
X Ray ◽  
3 Dimensional ◽  
Carboxylate Groups ◽  
R Value

One of the compounds obtained by the reaction of rhenium(III) chloride with n-butyric acid while exposed to oxygen has been shown by single crystal X-ray diffraction to be tetra-μ-n-butyratodi-rhenium(III) diperrhenate. The crystals are triclinic with lattice parameters a = 7.836(8) Å, b = 10.746(8) Å, c = 8.773(8) Å, α = 88.9(1)°, β = 106.5(1)°, and γ = 98.0(1)°. The space group is [Formula: see text] and there is one formula unit per cell. A total of 1593 independent reflections were examined and the structure was refined by full 3-dimensional least-squares to an R value of 0.123. Two rhenium environments are found, one consisting of a dimer unit bridged by 4 carboxylate groups and the other a per-rhenate group. This latter group, showing a mean Re—O distance of 1.75 Å, shares an oxygen atom with a rhenium atom in the dimer unit, and this Re—O bond length is 2.18 Å long. The structure results from packing of short chains, consisting of the dimer unit and the 2 perrhenate groups, running roughly parallel to the [111] direction.

Studies of Rhenium β-Diketone Complexes. III. The Crystal and Molecular Structure of Bis(μ-O-1,3-diphenylpropane-1,3-dionatotricarbonylrhenium(I))

1973 ◽  
Vol 51 (2) ◽  
pp. 317-323 ◽  
Author(s):  
J. C. Barrick ◽  
M. Fredette ◽  
C. J. L. Lock
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Main Part ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
The Other ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
X Ray

One of a series of compounds obtained by the reaction of chloropentacarbonylrhenium(I) with β-diketones has been shown by single crystal X-ray diffraction to be bis(μ-O-1,3-diphenylpropane-1,3-dionatotricarbonylrhenium(I)). The crystals are monoclinic with lattice parameters a = 11.988(A) Å, b = 14.441(9) Å, c = 10.298(7) Å, β = 115.25(7)°. The space group is P21/c and there are two dimers per unit cell. A total of 1563 independent reflections were measured on a single crystal X-ray diffractometer and the structure was refined by least squares analysis to a weighted R2 value of 0.0427. The dimer units are held together by two bridging oxygen atoms, one from each of the β-ketoenolate groups; the distance of the bridging oxygen from the rhenium atom to which it is chelated (2.162(9) Å) is shorter than the distance to the other rhenium atom (2.204(7) Å). The main part of the β-ketoenolate ring is 37° from the OReO plane.

Studies of the rhenium-oxygen bond. III. The crystal and molecular structure of 1-oxo-6-ethoxo-2,4-dichloro-3,5-dipyridinerhenium(V)

1977 ◽  
Vol 55 (2) ◽  
pp. 333-339 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Graham Turner
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Dominant Factor ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Oxygen Bond

The crystal and molecular structure of the title compound has been examined by single crystal X-ray diffraction. The crystals are monoclinic with a = 28.045(10), b = 8.766(3), c = 12.376(5) Å, β = 91.14(3)°. The space group is C2/c and there are eight molecules per unit cell. A total of 5053 independent reflections, of which 2860 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares to an R2 value of 0.0449. The ligands form a very rough octahedron around the rhenium atom with Re—Cl(1), 2.441(3); Re—Cl(2), 2.366(3), Re—O(1), 1.684(7); Re—O(2), 1.896(6); Re—N(1), 2.144(7); Re—N(2), 2.132(7) Å. The pyridine rings are a dominant factor in determining the details of the molecular structure.

scholarly journals Crystal and Molecular Structure of a New Hydroxylamido/Amino Acid Oxovanadium(V) Complex, [VO(NH2O)2(DL-methioninato)]·H2O

2011 ◽  
Vol 66 (7) ◽  
pp. 752-754
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Gabriel Arrambide ◽  
Dinorah Gambino ◽  
Enrique J. Baran
Keyword(s):  
Molecular Structure ◽  
Amino Acid ◽  
Binding Site ◽  
Crystal And Molecular Structure ◽  
Bidentate Ligand ◽  
The Other ◽  
X Ray Diffraction ◽  
Apical Position ◽  
X Ray

The crystal and molecular structure of the [VO(DLmeth)( NH2O)2]・H2O complex has been determined by X-ray diffraction methods (monoclinic, P21/c with a = 5.8138(2), b = 27.3496(8), c = 7.5663(2) A° , β = 103.059(3)◦, and Z = 4). The vanadium(V) cation is in a pentagonal bipyramidal environment axially coordinated to the oxo group and equatorially to two hydroxylamido groups in a side-on fashion. The fifth equatorial binding site and the other apical position are occupied by an N and an O atom, respectively, from the methioninate anion acting as a bidentate ligand.

Synthesis, Crystal Structure and Spectroscopy of Dibutyl Ester-Ether Fluorescein

2011 ◽  
Vol 415-417 ◽  
pp. 1443-1446
Author(s):  
Ke Liang Zhang ◽  
Ning Sheng Zhang ◽  
Chen Tun Qu
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Fluorescence Spectra ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Absorption And Fluorescence Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
3 Dimensional ◽  
Dibutyl Ester

The title compound has been prepared from the reaction of fluorescein and 1-bromobutane in the presence of potassium carbonate. Its crystal and molecular structure is determined by single crystal X-ray diffraction. Its crystal is monoclinic space group P2(1)/n with lattice parameters: a = 8.0460(19) Å, b = 13.198(3) Å, c = 22.208(5) Å, α = 90.00º, β = 94.140(3)º, γ = 90.00º, V= 2352.1(9)Å3, Density (calculated) 1.228 mg /m3, μ(mm-1) = 0.08, absorption coefficient = 0.082m−1, F(000) 1034, Z = 4. In the crystal structure, intermolecular O-H hydrogen bands are responsible for the formation of a 3-dimensional net-work. The UV-vis absorption and fluorescence spectra of both dibutyl ester-ether fluorescein was studied.

Studies of β-Diketone Complexes of Rhenium. VI. The Crystal and Molecular Structure of cis-Dichloropentane-2,4-dionato-trans-bis(triphenylphosphine)rhenium(III)

1974 ◽  
Vol 52 (9) ◽  
pp. 1704-1708 ◽  
Author(s):  
I. D. Brown ◽  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Nearest Neighbours

A compound, obtained in large yields from the reaction of acetylacetone and oxodichloroethoxobis(triphenylphosphine)rhenium(V) in benzene, has been shown by single crystal X-ray diffraction to be cis-dichloropentane-2,4-dionato-trans-bis(triphenylphosphine)rhenium(III). The crystals are monoclinic with a = 13.06(1), b = 18.30(1), c = 16.55(1) Å, and β = 112.7(2)°. The space group is P21/c and there are four molecules per unit cell. A total of 3841 independent reflections, of which 2686 were observed, were examined by film methods, the intensities being measured with a microdensitometer. The structure was refined by full matrix least-squares analysis to an R2 value of 0.068. The ligands are arranged around the rhenium atom in the manner described by the compound name to give a rough octahedron of nearest neighbours and the Re—Cl (2.369 Å av.), Re—O (2.02 Å av.), and Re—P (2.474 Å av.) distances are as expected.

The crystal and molecular structure of syn-2,11-diselena[3,3]metacyclophane and comparison with the dithia-analogue

1982 ◽  
Vol 60 (3) ◽  
pp. 362-367 ◽  
Author(s):  
Gordon W. Bushnell ◽  
Reginald H. Mitchell
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Solid State ◽  
Crystal And Molecular Structure ◽  
State Structure ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Anti Conformer ◽  
R Value

The crystal structure of syn-2,11-diselena[3,3]metacyclophane, 1a, has been determined by single crystal X-ray diffraction and refined to an R-value of 0.039. The crystal structure is monoclinic with a = 1926(1), b = 801.4(3), c = 924(1) pm, β = 98.9(1)°, and is isomorphous with that of the analogous sulphur compound. The space group is P21/n with 4 molecules per cell, D(meas) = 1.733 g cm−3, D(calcd) = 1.726 g cm−3. The molecule has the syn-conformation with the largest possible Se—Se distance of 721.8 pm. The benzenoid rings form a dihedral angle of 19.1°. The distance between the internal aryl hydrogen atoms on rings 1 and 2 is 285.1 pm. The internal aryl C atoms are 314.6 pm apart. The 1Hmr solution spectra of 1a are consistent with the solid state structure, and can be explained without involving equilibration with an anti-conformer.

scholarly journals Studies of rhenium–carboxylate complexes. I. Tris(μ-i-butyrato)di(chlororhenium(III)) perrhenate

1969 ◽  
Vol 47 (22) ◽  
pp. 4213-4220 ◽  
Author(s):  
C. Calvo ◽  
N. C. Jayadevan ◽  
C. J. L. Lock
Keyword(s):  
Oxygen Atom ◽  
Single Crystal ◽  
Bond Length ◽  
Three Dimensional ◽  
Isobutyric Acid ◽  
The Other ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Groups ◽  
R Value

One of the compounds obtained by reacting rhenium(III) chloride with isobutyric acid while exposed to oxygen has been shown by single crystal X-ray diffraction to be tris(μ-i-butyrato)di(chlororhenium(III)) perrhenate. The crystals are monoclinic with lattice parameters a = 8.980(5) Å, b = 17.790(8) Å, c = 15.361(8) Å, and β = 114.4(1)°. The space group is P21/c and there are 4 formula units per cell. A total of 1729 independent reflections were examined and the structure was refined by full three dimensional least squares to an R value of 0.114. Two Re environments are found, one consisting of a dimer unit bridged by three carboxylate groups with a chlorine atom per rhenium and the other as a perrhenate group. This latter group, showing a mean Re—O distance of 1.74 Å, shares an oxygen atom with a Re in the dimer unit, and this Re—O bond length is 2.28 Å long. The structure consists of a packing of chains of alternate dimers and perrhenate groups running parallel to the c axis.

Crystal structures of medium ring compounds. Part III. The crystal and molecular structure of trans-anti-trans-4,5:9,10-biscyclohexano-1,3,6,8-tetraoxecane

1979 ◽  
Vol 57 (16) ◽  
pp. 2154-2158 ◽  
Author(s):  
Aris Terzis ◽  
T. Bruce Grindley
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Chair Conformation ◽  
Membered Ring ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ring Compounds ◽  
R Value ◽  
Medium Ring

The crystal structure of trans-anti-trans-4,5:9,10-biscyclohexano-1,3,6,8-tetraoxecane (3) has been determined by X-ray diffraction. The crystals are monoclinic, a = 11.919(3), b = 17.330(7), c = 7.019(2) Å, β = 98.91(1)°, P21/c, with Z = 4. The structure was solved by application of the tangent formula and refined by large block least squares to a final R value of 0.060 (Rw = 0.058).The ten-membered ring is present in the crystal in a twist-chair-boat-chair conformation — one which has been calculated to be relatively unstable for cyclodecane. Possible reasons why 3 adopts this conformation are discussed.

The conformation of a ten-membered ring: the crystal and molecular structure of trans-syn-trans-4,5:9,10-biscyclohexano-1,3,6,8-tetraoxecane

1977 ◽  
Vol 55 (14) ◽  
pp. 2692-2699 ◽  
Author(s):  
Aris Terzis ◽  
T. Bruce Grindley ◽  
J. Brian Faught
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Membered Ring ◽  
Thermal Parameters ◽  
X Ray Diffraction ◽  
X Ray ◽  
R Value

The crystal structure of trans-sys-trans-4,5:9,10-biscyclohexano-1,3,6,8-tetraoxecane (1) has been determined by X-ray diffraction. The crystals are monoclinic, a = 10.995(2), b = 5.291(1), c = 12.241(2) Å, β = 114.68(1)°, P21/c, with Z = 2. The structure was solved by the application of symbolic addition procedures and refined with anisotropic thermal parameters for all atoms to a final R value of 0.039 (Rw 0.062) for 1135 independent reflections.The ten-membered tetraoxecane ring is present in the crystal in a boat-chair-boat (BCB) conformation, which is somewhat different in geometry than the BCB conformations observed for cyclodecane derivatives. The causes of these differences are discussed. Intramolecular non-bonded interactions cause one CH2 group to be significantly distorted from local C2v symmetry.

The crystal and molecular structure of syn-[4.4.3]propella-2,4,12-trien-11-ol 3,5-dinitrobenzoate

1985 ◽  
Vol 63 (4) ◽  
pp. 862-865 ◽  
Author(s):  
Judith C. Gallucci ◽  
Katsuo Ohkata ◽  
Leo A. Paquette
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Molecular Geometry ◽  
Chair Conformation ◽  
Membered Ring ◽  
Aqueous Acetone ◽  
X Ray Diffraction ◽  
X Ray ◽  
R Value

The crystal structure of syn-[4.4.3]propella-2,4,12-trien-11-ol 3,5-dinitrobenzoate, 2, has been determined by single crystal X-ray diffraction and refined to an R value of 0.051. The crystal structure is triclinic with a = 10.208(2), b = 13.355(2), c = 7.068(1) Å, α = 99.35(1)°, β = 100.63(1)°, γ = 100.79(1)°, and the space group is [Formula: see text] with two molecules per cell, D(calcd) = 1.39 g cm−3. The unsaturated five-membered ring resides in an envelope conformation with C6—C11—C12—C13 lying essentially in a plane. The fifth atom, C1, is positioned 0.47 Å out of this plane on the side opposite O1. The latter is situated 1.38 Å away and projects the 3,5-dinitrobenzoate group above the central portion of the cyclohexadiene unit. Four contiguous carbon atoms in the latter ring are mutually coplanar and the fused cyclohexane ring adopts a chair conformation. The overall molecular geometry is reconcilable with its solvolytic behavior in aqueous acetone.

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