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 (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 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.

Reaction of N,N′-dihydroxy-.N,N′-dimethylmethanediamine with phenylboronic acid and the crystal and molecular structure of N,N′-dihydroxy-N,N′-dimethylmethanediamine

1989 ◽  
Vol 67 (11) ◽  
pp. 1959-1963 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Phenylboronic Acid ◽  
Direct Methods ◽  
Exact Formula ◽  
Full Matrix ◽  
Space Group ◽  
Hydrogen Bonded

The reaction of N,N′-dihydroxy-N,N′-dimethylmethanediamine with phenylboronic acid leads to the product 1,7-dimethyl-3,5-diphenyl-2,4,6-trioxa-7-aza-1-azonia-3-bora-5-boratabicyclo[3.3.0]octane rather than the expected product 1,5-dimethyl-3-phenyl-1,5-diaza-2,4-dioxa-3-boracyclohexane. The structure of N,N′-dihydroxy-N,N′-dimethylmethanediamine has been determined and is discussed in terms of its reaction with PhB(OH)2. Crystals of N,N′-dihydroxy-N,N′-dimethylmethanediamine are tetragonal, a = 8.5346(3), c = 8.4178(7) Å, Z = 4, space group P421c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.036 and Rw of 0.038 for 333 reflections with I ≥ 3σ(I). The structure consists of hydrogen-bonded dimers having exact [Formula: see text] symmetry. Keywords: N,N′-dihydroxy-N,N′-dimethylmethanediamine, crystal structure.

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.

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.

Complexes of the methyl tris(3,5-dimethylpyrazol-1-yl) gallate ligand, MeGa(N2C5H7)3−, and its hydroxy derivative, MeGa(N2C5H7)2(OH)−. Crystal and molecular structure of [MeGa(N2C5H7)2(OH)]Mo(CO)2(η3-C4H7)

1979 ◽  
Vol 57 (2) ◽  
pp. 139-146 ◽  
Author(s):  
Kenneth R. Breakell ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Structure Determination ◽  
Carbonyl Compounds ◽  
Crystal And Molecular Structure ◽  
Hydroxy Derivative ◽  
Full Matrix ◽  
Sterically Demanding

The synthesis and coordinating properties of the tridentate tris-chelating ligand, methyl tris(3,5-dimethylpyrazol-1-yl)gallate, MeGa(N2C5H7)3−, are described. Carbonyl and nitrosyl carbonyl compounds of manganese, molybdenum, and tungsten incorporating this ligand are detailed. The ready conversion of the above ligand to the less sterically demanding tris-chelating 'hydroxy' ligand [MeGa(N2C5H7)2(OH)]− occurs in attempted syntheses of the 'η3-allyl' complexes, [MeGa(N2C5H7)3]M(CO)2'η3-allyl', (where M = Mo or W, 'η3-allyl' = η3-C3H5, η3-C4H7). The tridentate chelating nature of this 'hydroxy' ligand is conclusively demonstrated in the crystal structure determination of the complex, [MeGa(N2C5H7)2(OH)]-Mo(CO)2(η3-C4H7). Crystals of this complex are monoclinic, a = 14.020(4), b = 10.110(1), c = 15.493(7) Å, β = 111.58(3)°, Z = 4, space group P21/n. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to a final R of 0.40 and Rw of 0.043 for 3374 reflections with I ≥ 3.5σ(I).

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).

Zinc 3,5-dimethylpyrazolate complexes: synthesis and structural studies. The crystal and molecular structure of [Zn2(dmpz)4(Hdmpz)2]

1990 ◽  
Vol 68 (9) ◽  
pp. 1494-1498 ◽  
Author(s):  
Martin K. Ehlert ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
High Yield ◽  
Coordination Geometry ◽  
Structural Studies ◽  
Full Matrix ◽  
Space Group

Zinc metal reacts with excess 3,5-dimethylpyrazole (Hdmpz) in the presence of O2 to produce materials of composition Zn(dmpz)2(Hdmpz)y. Thermolysis of these materials results in the loss of Hdmpz and the formation of the [Zn(dmpz)2]x polymer. Under appropriate conditions the pure dimer [Zn2(dmpz)4(Hdmpz)2] can be obtained in high yield. Crystals of bis[μ-(3,5-dimethylpyrazolyl-N1,N2)]bis[(3,5-dimethylpyrazolyl)(3,5-dimethylpyrazole)zinc(II)] are orthorhombic, a = 17.009(2), b = 29.239(2), c = 13.590(2) Å, Z = 8, space group Fddd. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.037 and Rw = 0.042 for 913 reflections with I ≥ 3σ(I). The structure of [Zn2(dmpz)4(Hdmpz)2] contains nearly planar doubly dmpz bridged Zn2 units capped at each end by strongly hydrogen-bonded [Formula: see text] units. The zinc atoms display pseudotetrahedral coordination geometry with Zn—N = 1.991(3) (bridging) and 2.025(3) Å (terminal), and N—Zn—N = 99.6(2)–113.8(2)°. Keywords: zinc 3,5-dimethylpyrazolate complexes, crystal structure.

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