A quadruply bonded dimolybdenum compound containing a novel bridging and chelating hexadentate ligand

1983 ◽  
Vol 61 (7) ◽  
pp. 1659-1663 ◽  
Author(s):  
Kenneth R. Breakell ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Physical Properties ◽  
Least Squares ◽  
Complex Anion ◽  
Ion Pair ◽  
Full Matrix ◽  
Coordination Sites ◽  
Hexadentate Ligand ◽  
Ligand Bond

The synthesis, physical properties, and molecular structure of (N2C3H)+[Mo2(μ-CH3CO2)[CH3Ga(N2C3H3)O]4]−•2(C4H8O) are reported. Crystals of pyrazolium (μ-acetato)[1,3,5,7-tetramethyl-1,3,5,7-tetrakis(pyrazol-1-yl)cyclotetragalloxanato(4−)]dimolybdate(II)-bis(tetrahydrofuran) are orthorhombic, a = 10.638(2), b = 32.779(4), c = 12.617(1) Å, Z = 4, space group Cmcm. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to R = 0.032 and Rw = 0.041 for 1957 reflections with I ≥ 3σ(I). The structure consists of THF molecules and (N2C3H5)+[Mo2(μ-CH3CO2)[CH3Ga(N2C3H3)O]4]− ion-pair units, the latter displaying exact C2v symmetry. The pyrazolium cation is joined to the complex anion by a pair of strong [Formula: see text] hydrogen bonds [Formula: see text]. The Mo24+ unit is bridged by a single acetato group, the remaining coordination sites being occupied by the hexadentate bridging and chelating [CH3Ga(N2C3H3)O]44− ligand. Bond lengths are: Mo—Mo = 2.127(I), Mo—N = 2.151(3), Mo—O = 2.090(4) and 2.115(4), Ga—O = 1.853(2) and 1.861(2), Ga—N = 1.961(3), and Ga—C = 1.950(6) Å.

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.

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 3-ethyl-4-hydroxy-1,2,3(4H)-benzotriazine and 6-chloro-4-hydroxy-3-methyl-4-phenyl-1,2,3-benzotriazine

1985 ◽  
Vol 63 (3) ◽  
pp. 581-585 ◽  
Author(s):  
Kwong Khee Lai ◽  
Carl H. Schwalbe ◽  
Keith Vaughan ◽  
Ronald J. Lafrance ◽  
Clive D. Whiston
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Tetrahedral Geometry ◽  
Orthorhombic System ◽  
Full Matrix ◽  
X Ray ◽  
R Factor

The crystal structures of the title compounds have been determined from X-ray data collected on a four-circle diffractometer and refined by the full-matrix least-squares method. The former compound crystallizes in the orthorhombic system, space group Pbcn, with a = 14.346(8), b = 7.239(1), c = 17.276(2) Å, and has been refined to a conventional R factor of 0.043 for 890 observed reflections. Corresponding results for the latter compound are monoclinic, P21/n, a = 12.222(4), b = 7.482(2), c = 14.170(8) Å, β = 94.06(4)°, R = 0.060 for 2128 observed data. The triazine rings of both compounds exhibit short N(1)—N(2) bonds and tetrahedral geometry at C(4); however, the ring is puckered in the first compound but flat in the second. Molecules in both crystals are linked by [Formula: see text] hydrogen bonds.

Synthesis and crystal and molecular structure of ethanolaminogallium dimethyl, H2NCH2CH2O•GaMe2

1979 ◽  
Vol 57 (5) ◽  
pp. 586-590 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Physical Properties ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Space Group ◽  
Bond Lengths ◽  
R Value

Details of the synthesis and physical properties of H2NCH2CH2O•GaMe2 are given. The compound crystallizes in the tetragonal space group P43, a = 12.2771(2), c = 9.7345(4) Å, Z = 8. The structure was solved by Patterson and Fourier syntheses and was refined by fullmatrix least-squares procedures to a final R value of 0.028 and Rw of 0.036 for 1378 reflections with I ≥ 3σ(I). The structure consists of monomeric molecules containing tetrahedrallycoordinated gallium atoms. Molecules are linked by an extensive network of N—H … O hydrogen bonds. Bond lengths (corrected for libration) are: Ga—O, 1.916(5) and 1.917(4), Ga—N, 2.056(6) and 2.072(6), and Ga—C, 1.962–1.974(8–9) Å.

Crystal and Molecular Structure of 2,5-Bis(2′-hydroxyethylamino)-1,4-benzoquinone

1975 ◽  
Vol 53 (5) ◽  
pp. 777-783 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Full Matrix ◽  
Space Group ◽  
Compound C ◽  
Related Compounds ◽  
Centrosymmetric Molecule

Crystals of 2,5-bis(2′-hydroxyethylamino)-1,4-benzoquinone are monoclinic, a = 5.020(1), b = 19.238(3), c = 5.214(1) Å, β = 96.15(3)°, Z = 2, space group P21/n. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.045 for 646 reflections with I ≥ 3σ(I). The benzoquinone ring in the centrosymmetric molecule is slightly, but significantly, nonplanar. Bond distances in the compound (C—C, 1.247 (2) and 1.410 (3), C—N, 1.332 (3) and 1.457 (3), C—C, 1.384–1.514 (3), N—H, 0.89 (3), O—H, 1.07 (5), and C—H, 0.95–1.09 (3) Å) are similar to those in related compounds. The structure features an extensive network of N—H … O (N … O = 2.639 (3) and 3.033 (2) Å) and O—H … O(O … O = 2.757 (3) Å ) hydrogen bonds.

Crystal and molecular structure of L-prolinatodiphenylboron

1977 ◽  
Vol 55 (6) ◽  
pp. 958-965 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Conformational Disorder ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of L-prolinatodiphenylboron are monoclinic, a = 5.9427(5), b = 14.4633(7), c = 8.9654(4) Å, β = 98.423(8)°, Z = 2, space group P21. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.037 and Rw of 0.053 for 1477 reflections with I ≥ 3σ(I). The proline ring exhibits conformational disorder. The crystal structure consists of discrete molecules linked by N—H … O hydrogen bonds (N … O = 2.893(3) Å) along the short a axis. Intramolecular N—B coordination occurs to form a system of two fused five-membered rings. Bond lengths (corrected for libration) are: N—B, 1.630(3), O—B, 1.529(3), O—C, 1.219(3) and 1.300(3), N—C, 1.506(3) and 1.507(3), C(sp3)–C(sp3), 1.525(4), C(sp2)—C(sp3), 1.517(3), and mean C—C(phenyl), 1.394 Å.

Crystal and Molecular Structure of B-Phenyl-diptychboroxazolidine,

1975 ◽  
Vol 53 (10) ◽  
pp. 1393-1401 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Thermal Motion ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of B-phenyl-dictychboroxazolidine are monoclinic, a = 8.4977(4), b = 9.0617(5), c = 7.0105(3) Å, β = 111.627(3)°, Z = 2, space group P21. The structure was solved by direct methods and was refined by full-matrix least squares procedures to a final R of 0.040 for 967 reflections with I ≥ 3σ(I). The bond lengths involving nonhydrogen atoms have been corrected for thermal motion. Bond lengths are: B—O, 1.460(3) and 1.474(3), B—N, 1.666(3), B—C, 1.613(3), C—O, 1.411(3) and 1.419(3), C—N, 1.485(3) and 1.486(3), C(sp3)—C(sp3), 1.514(4) and 1.524(4), C—C(ar), 1.384–1.400(4–6), mean C—H, 0.98(4), and N—H, 0.87(5) Å. The crystal structure consists of discrete molecules of B-phenyl-diptychboroxazolidine each linked to two others by N—H … O hydrogen bonds (O … N = 2.914(3) Å) to form continuous spirals along b.

Crystal and Molecular Structure of (±)-7,7-(2′,2′-Dimethyl)pentamethylene-1-methyl-norbornane-2-oxime

1975 ◽  
Vol 53 (5) ◽  
pp. 765-776 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Full Matrix ◽  
Space Group ◽  
Centrosymmetric Dimers

Crystals of (±)-7,7-(2′,2′-dimethyl)pentamethylene-1-methyl-norbornane-2-oxime are monoclinic, a = 9.202(2), b = 12.852(3), c = 12.698(3) Å, β = 110.83(2)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.048 for 1538 reflections with I ≥ 3σ(I). The crystal structure consists of pairs of molecules linked by N … H—O hydrogen bonds (N … O = 2.821(3) Å ) to form centrosymmetric dimers. Bond distances are as follows: C—N = 1.266(3), N—O = 1.426(3), mean C(sp3)—C(sp3) = 1.540, and mean C(sp3)—C(sp3) = 1.511 Å.

Crystal and Molecular Structure of B,B- Diphenylboroxazolidine (2-Aminoethyl Diphenylborinate),

1973 ◽  
Vol 51 (8) ◽  
pp. 1288-1294 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Electron Density ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Full Matrix ◽  
Bond Lengths

Crystals of the title compound are monoclinic, a = 13.840(1), b = 8.9169(5), c = 10.170(1) Å, β = 98.85(1)°, Z = 4, space group P21/n. The structure was determined by direct methods, and refined by electron-density and full-matrix least-squares procedures to R 0.041 for 1458 observed reflections. The five-membered boroxazolidine ring is in the half-chair conformation. Bond angles in the ring range from 99.7° for OBN to 110.1° for BOC. Bond lengths are as follows: mean B—C, 1.611(2), B—N, 1.653(3), B—O, 1.484(3), C—N, 1.485(3), C—O, 1.413(3), mean C—C (aromatic), 1.383(11), and C—C, 1.505(4) Å. The structure consists of discrete molecules linked by O…H—N hydrogen bonds (2.874(2) Å) to form continuous spirals about the 21 axes.

The Preparation, Physical Properties, and Structure of Oxotetrachloroaquorhenium(VI), ReOCl4(OH2)

1972 ◽  
Vol 50 (12) ◽  
pp. 1811-1818 ◽  
Author(s):  
P. W. Frais ◽  
C. J. L. Lock
Keyword(s):  
Molecular Structure ◽  
Infrared Spectroscopy ◽  
Physical Properties ◽  
Single Crystal ◽  
Least Squares ◽  
Intensity Data ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
First Time

Oxotetrachloroaquorhenium(VI), ReOCl4•H2O, has been prepared and characterized for the first time by analysis, infrared spectroscopy and single crystal X-ray diffraction. The crystals were orthorhombic, a = 10.834(8), b = 11.089(8), c = 5.517(4) Å, Pn21a, Z = 4. Intensity data were recorded by integrating film methods and measured with a Joyce–Loebl microdensitometer, and 624 observable of the 704 measured independent reflections were given non-zero weight in the final cycle of full matrix least-squares refinement where R1 = 0.0572 and R2 = 0.0687. The molecular structure is based on a very distorted octahedron with a strongly bonded oxo-group (Re—O, 1.63(2) Å) trans (177(2)°) to a weakly bonded aquo-group (Re—O, 2.27 (2) Å). The Re—Cl distances do not differ significantly (2.29(1) Å av). The chlorine atoms are bent away from the oxo-group (angles vary from (94–102°(1)).

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