Crystal and Molecular Structure of [2,3-Bis(dimethylarsino)-1,1,1,4,4,4,-hexafluorobut-2-ene-As, As]tricarbonyldiiodotungsten(II)

1974 ◽  
Vol 52 (19) ◽  
pp. 3331-3336 ◽  
Author(s):  
Anthony Mercer ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Bidentate Ligand ◽  
The Other ◽  
Carbonyl Groups ◽  
Arsenic Atom ◽  
Tungsten Atom ◽  
Full Matrix ◽  
Octahedral Environment

Crystals of the title compound, Me2AsC(CF3):C(CF3)AsMe2WI2(CO)3, are monoclinic, a = 15.37(2), b = 9.529(1), c = 15.967(3) Å, β = 112.03(2)°, Z = 4, space group P21/c. The structure was determined by Patterson and Fourier syntheses and refined by full-matrix least-squares procedures to a final R of 0.069 for 1823 observed (of a total of 2778) reflexions. The tungsten atom is seven-coordinate with a distorted capped octahedral environment, the capping group being a carbonyl (W—C, 1.94(3) Å). The capped face consists of the two remaining carbonyl groups (W—C, 1.97(4) and 2.00(4) Å) and one of the arsenic atoms from the bidentate ligand (W—As, 2.556(3) Å). The uncapped face contains the two iodine atoms (W—I, 2.848(2) and 2.856(2) Å) and the remaining arsenic atom (W—As, 2.618(3) Å), this bond length (trans to CO), being significantly longer (by 0.062 Å) than the other (trans to I) W—As distance.

The crystal and molecular structure of lead(II)bromide-bis-dimethylsulphoxide, PbBr2•2[(CH3)2SO]

1977 ◽  
Vol 55 (5) ◽  
pp. 849-855 ◽  
Author(s):  
Anthony D. Baranyi ◽  
Mario Onyszchuk ◽  
Yvon Le Page ◽  
Gabrielle Donnay
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Title Compound ◽  
Lone Electron Pair ◽  
Electron Pair ◽  
Crystal And Molecular Structure ◽  
Crystal Packing ◽  
The Other ◽  
Full Matrix ◽  
A Cell

The title compound has two PbBr2•2[(CH3)2SO] units, Z = 2, in a cell with a = 11.093(2), b = 12.382(3), c = 4.540(1) Å, belonging to space group Pmmn. The structure was solved by Patterson functions and was refined by full-matrix least-squares calculations to a final R of 0.054 for 348 observed diffractometer intensities. Passing through the unit cell are two antiparallel, infinite polar chains, each with symmetry mm2, extending along z and interacting with each other by weak van der Waals forces. Lead(II) is six-coordinate with a close, covalent hemisphere consisting of two bromine atoms [Pb—BrIBrII 2.93(1) Å], and two oxygen atoms [Pb—O,O′ 2.50(3) Å] which subtend an angle of 157.9(9)° at lead, located at the intersection of the O—Pb—O′ and BrI—Pb—BrII perpendicular mirror planes. The other hemisphere consists of bridging bromine atoms from the neighboring PbBr2•2dmso unit [Pb—BrIII,BrIV 3.24(1) Å], resulting in a rectangle of bromine atoms around lead [BrI—Pb—BrII 90.5(1)°, BrIII—Pb—BrIV 80.2(1)°]. The distortion of the octahedral coordination sphere around lead is discussed in terms of (a) a repulsive effect of the Pb(II) valence lone electron-pair, (b) weak Br—S bonding, and (c) crystal packing forces.

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.

Crystal and molecular structure of [dimethyl(3,5-dimethyl-1-pyrazolyl)(ethanol-amino)gallato (N(2),O,N(3))](η3-cycloheptatrienyl)dicarbonylmolybdenum

1981 ◽  
Vol 59 (11) ◽  
pp. 1665-1670 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Amino Nitrogen ◽  
Full Matrix ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Unusual Type

Crystals of [dimethyl(3,5-dimethyl-l-pyrazolyl)(ethanolamino)gallato(N(2),O,N(3))](η3-cycloheptatrienyl)dicarbonylmolybdenum are monoclinic, a = 10.511(1), b = 8.335(1), c = 24.138(3) Å, β = 102.22(1)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was reflned by full-matrix least-squares procedures to R = 0.028 and Rw = 0.046 for 3708 reflections with I ≥ 3σ(I). The crystal structure consists of discrete molecules linked by N—H … O hydrogen bonds (N … O = 2.929(5) Å). The Mo atom is in a distorted octahedral environment with the η3-C7H7 ligand occupying one coordination site, trans to the amino nitrogen, as a π-donating ligand. Important bond distances (corrected for libration) are: Mo—O, 2.245(2), Mo—N(amino), 2.249(3), Mo—N(pyrazolyl), 2.270(3), Mo—C(O), 1.950(4) and 1.947(4), Mo—C(C7H7), 2.176(4), 2.364(4), and 2.380(4), Ga—O, 1.919(3), Ga—N, 1.984(3), and Ga—C, 1.982(5) and 1.983(5) Å. An unusual type of disorder is present in which a second image of the molecule, approximately mirrored by the plane y = 1/4, is in evidence at low occupancy.

Crystal and molecular structure of 8,8-dimethyl-3,5-diphenyl-2,4,6-trioxa-1-azonia-3-bora-5-boranatabicyclo[3.3.0]octane

1976 ◽  
Vol 54 (20) ◽  
pp. 3142-3151 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter ◽  
W. Kliegel ◽  
H. Becker
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Boron Atom ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
The Other ◽  
Full Matrix ◽  
Atom Bond ◽  
Tetrahedral Boron

Crystals of 8,8-dimethyl-3,5-diphenyl-2,4,6-trioxa-1-azonia-3-bora-5-boranatabicyclo[3.3.0]-octane are monoclinic, a = 22.323(1), b = 9.555(1), c = 16.0027(6) Å, β = 109.055(4)°, Z = 8, space group C2/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.048 and Rw of 0.066 for 2629 reflections with I ≥ 3σ(I). The central part of the molecule consists of two fused five-membered rings. One of them is a familiar BOCCN ring while the other is a novel and nearly planar BOBON ring containing one tetrahedral boron atom and one trigonal planar boron atom. Bond lengths are: O—B, 1.337(2)–1.467(2), N—B, 1.692(2), O—N, 1.440(2), O—C, 1.426(2), N—C, 1.513(2), B—C, 1.557(2) and 1.599(2), C(sp3)—C(sp3), 1.520(2)–1.530(2), C—C(ar), 1.372(4)–1.407(2), N—H, 0.89(2), mean C(ar)—H, 0.97(1), and mean C(sp3)—H, 1.01(1) Å. The crystal structure consists of discrete molecules each linked to two others by N—H … O hydrogen bonds (N … O = 2.853(2) Å).

Organometalloidal Compounds with o-Phenylene Substituents, VII [1] Crystal and Molecular Structure of 10,15-Dihydro-5H-5,10,15-trioxa-tribenzo [a,d,g] cyclononene (Trimeric o-Phenylene Oxide) and its Implications Concerning Preferred Conformations of Compounds (Arylene)3X3

1981 ◽  
Vol 36 (12) ◽  
pp. 1526-1531 ◽  
Author(s):  
Klaus von Deuten ◽  
Günter Klar
Keyword(s):  
Molecular Structure ◽  
Title Compound ◽  
Molecular Conformation ◽  
Crystal And Molecular Structure ◽  
The Other ◽  
Bond Lengths ◽  
Π Interactions ◽  
Phenylene Oxide ◽  
Steric Factors ◽  
Oxygen Atoms

The title compound crystallizes with an orthorhombic P cell, a = 893.5(1), b = 949.2(2), c = 1520.6(3) pm; Z = 4, space group Pnab. Its molecular conformation has crystallographic C2-symmetry with one phenylene ring in the plane of the three oxygen atoms, the other rings extending almost perpendicularly above and below this plane. The two kinds of oxygen atoms in the molecule show characteristic differences with respect to CO bond lengths and COC bond angles; only the oxygen lying on the C2-axis (joining the "perpendicular" rings) exhibits π-interactions with its phenylene rings. The influence of electronic and steric factors on the preferred conformation of the class of compounds (arylene)3X3 is pointed out.

The crystal and molecular structure of (4-diethylaminophenyl)diazenyltriphenylphosphonium tetrafluoroborate

1978 ◽  
Vol 56 (7) ◽  
pp. 891-895 ◽  
Author(s):  
Frederick W. B. Einstein ◽  
Derek Sutton ◽  
Peter L. Vogel
Keyword(s):  
Molecular Structure ◽  
Electronic Structure ◽  
Least Squares ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Hydrogen Atoms ◽  
Full Matrix ◽  
Bond Lengths ◽  
A Cell ◽  
Automatic Diffractometer

The title compound crystallizes in the space group P21/c with four formula units in a cell of dimensions a = 10.146(6) Å, b = 10.593(4) Å, c = 26.31(1) Å, β = 103.14(3)°. Using 1496 observed reflections (I = 2.3σ(I)) in the range 0° < 2θ < 40° measured on a Picker FACS-1 automatic diffractometer with Mo-Kα radiation, the structure was solved (symbolic addition) and refined (full-matrix least-squares procedure) to R = 0.062 (Rw = 0.058), with all hydrogen atoms included and all non-hydrogen atoms having anisotropic thermal parameters. The dimensions within the cation are consistent with a delocalized electronic structure which is intermediate between valence formulations involving benzenoid or quinonoid structures for the (4-diethylaminophenyl)diazenyl residue. Some important bond lengths are N3—C22 1.336(7) Å, N2—C19 1.356(7) Å, N1—N2 1.308(6) Å, and P—N1 1.648(5) Å.

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.

Crystal and Molecular Structure of Benzylidenimine Tetrasulfide, (C6H5CHN)2S4

1973 ◽  
Vol 51 (22) ◽  
pp. 3691-3696 ◽  
Author(s):  
James C. Barrick ◽  
Crispin Calvo ◽  
Fredric P. Olsen
Keyword(s):  
Molecular Structure ◽  
Bond Length ◽  
Least Squares ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Aromatic Rings ◽  
Intensity Measure ◽  
Full Matrix ◽  
Space Group

The structure of the title compound has been determined. Crystals are monoclinic with space group P21/a, Z = 4, a = 13.83(1), b = 19.66(2), c = 5.983(5) Å, β = 101.4(1)°, dcalcd = 1.404, dobs = 1.40(1). A full-matrix least-squares refinement on 1085 unique reflections of positive intensity measure produced a conventional R of 0.066. The spiral arrangement of the S4 chains (nearly generating a 31 axis) is such that the two aromatic rings are eclipsed. Alternation in bond length along the sulfur chain was observed, the long inner bond being 2.083(4) Å and the shorter outer bonds averaging 2.026(3) Å in length. No intermolecular non-bonding interactions involving sulfur were found.

Crystal and molecular structure of (η3-2-methylallyl)[dimethyl(ethanolamino)-(3,5-dimethyl-1-pyrazolyl)gallato(N(2),N(3),O)] dicarbonylmolybdenum, [Me2Ga(N2C5H7)(OCH2CH2NH2)]Mo(CO)2(η3-C4H7)

1979 ◽  
Vol 57 (11) ◽  
pp. 1335-1340 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Full Matrix ◽  
Distorted Octahedral Environment ◽  
Coordination Sites ◽  
Octahedral Environment ◽  
Distorted Octahedral

Crystals of (η3-2-methylallyl)[dimethyl(ethanolamino)(3,5-dimethyl-1-pyrazolyl)gallato-(N(2),N(3),O)]dicarbonylmolybdenum are triclinic, a = 7.6047(5), b = 10.882(1), c = 12.633(1) Å, α = 77.07(1), β = 89.19(1), γ = 71.91(1)°, Z = 2, space group [Formula: see text]. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to R = 0.024 and Rw = 0.030 for 3835 reflections with I ≥ 3σ(I). The crystal structure consists of discrete molecular units, each linked to four others by weak [Formula: see text] hydrogen bonds [Formula: see text] The Mo atom is in a distorted octahedral environment with the η3-C4H7 ligand occupying one of the six coordination sites as a π-donating ligand. Important bond distances (corrected for libration) are: Mo—C(allyl), 2.335(3), 2.372(3), 2.324(3); Mo—C(O), 1.902(3) and 1.961(2); Mo—O, 2.269(2); Mo—N(pz), 2.222(2); Mo—N(amino), 2.285(2); Ga—O, 1.924(2); Ga—N, 2.006(2); and Ga—C, 1.968(4) and 1.981(4) Å.

Studies of the rhenium–oxygen bond. II. The crystal and molecular structure of µ-oxobis(cis-dichloro-cis-di(pyridine)-trans-oxorhenium(V)), ORe(C5H5N)2Cl2ORe(C5H5N)2Cl2O

1978 ◽  
Vol 56 (2) ◽  
pp. 179-188 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Graham Turner
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
The Other ◽  
Full Matrix ◽  
X Ray ◽  
Ray Methods ◽  
Oxygen Bond

The crystal structure of µ-oxobis(cis-dichloro-cis-di(pyridine)-trans-oxorhenium(V)), ORe(C5H5N)2Cl2•O•Re(C5H5N)2Cl2O bas been studied by single crystal X-ray methods. The crystals were orthorhombic with lattice parameters a = 15.367(2), b = 10.283(2), c = 16.685(2) Å. The space group was Pna21 and there were four formula weights per unit cell. A total of 3339 reflections, of which 2990 were observed, were examined, and the structure refined by full matrix least squares (treating the pyridine rings as groups) to an R2 value of 0.0449. The dimer had a roughly rectilinear O—Re—O—Re—O backbone with pairs of chlorine atoms and pyridine molecules arranged cis in each half of the dimer. The two halves of the dimer were arranged such that the pairs of cis atoms in one half were rotated about the Re(1)–Re(2) axis almost 113 ° when compared to the corresponding pair in the other half. Important bond lengths (Re—O(terminal), 1.715(16), 1.764(16); Re—O(bridging), 1.943(16), 1.903(16); Re—Cl, 2.356(5)–2.390(5); Re—N, 2.116(16)–2.180(16)) were close to previously observed values. The molecule was markedly disturbed from the idealized structure and this was caused by intramolecular non-bonded interactions.

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