L-Proline derivatives of gallium trimethyl and gallium triethyl: crystal and molecular structure of L-prolinatodimethylgallium

1977 ◽  
Vol 55 (24) ◽  
pp. 4174-4179 ◽  
Author(s):  
Kenneth R. Breakell ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Gallium Atom ◽  
Full Matrix ◽  
Trigonal Bipyramidal ◽  
A Chain ◽  
Proline Derivatives ◽  
Derivatives Of ◽  
Distorted Trigonal Bipyramidal

Crystals of L-prolinatodimethylgallium are orthorhombic, a = 10.624(2), b = 10.567(4), c = 8.2268(6) Å, Z = 4, space group P212121. The structure was solved by direct methods and was refined by full-matrix least squares procedures to a final R of 0.029 and Rw of 0.035 for 1109 reflections with I ≥ 3σ(I). Details of the preparation and physical properties of L-prolinatodimethylgallium and L-prolinatodiethylgallium are given. The crystal structure of L-prolinatodimethylgallium consists of molecules each linked to two others by weak Ga—O bonds (2.695(3) Å) and N—H … O hydrogen bonds (N … O = 2.901(4) Å) to form a chain-like polymeric structure extending along the b axis. The gallium atom is five-coordinate and has distorted trigonal bipyramidal geometry. Important bond lengths are: Ga—O (axial), 2.044(3) and 2.695(3); Ga—N, 2.035(3); and Ga—C, 1.942(5) and 1.958(5) Å

Crystal and Molecular Structure of a Novel Polycyclic Ga, O, N Cage Compound: (GaH)6(GaH2)2(μ3-O)2(μ3-NCH2CH2NMe2)4(μ-NHCH2CH2NMe2)2

1975 ◽  
Vol 53 (5) ◽  
pp. 753-764 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Cage Structure ◽  
Gallium Atom ◽  
Full Matrix ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Cage Compound ◽  
Distorted Trigonal Bipyramidal

Crystals of 11H,22H-10,10,21,21-tetramethyl-3,5,14,16-tetra(N,N-dimethyl-2-aminoethyl)-1,12-dioxonia-3,5,7,10,14,16,18,21 -octaazonia-2,4,6,11,13,15,17,22-octagallanata-nonacyclo-[13.7.0.02,7.03,22.04,12.07,11.011,14.013,18.018,22]docosane are triclinic, a = 13.358(1), b = 9.300(1), c = 9.545(1) Å, α = 92.16(2), β = 107.49(1), γ = 89.23(2)°, Z = 1, space group [Formula: see text]. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to a final R of 0.038 for 3393 reflections with I ≥ 4σ(I). The bond lengths involving nonhydrogen atoms have been corrected for thermal motion. The molecular structure features a novel Ga, O, N cage structure which includes the first crystallographic examples of four-membered Ga2NO and six-membered Ga3N2O rings. Three of the four crystallographically independent gallium atoms are tetrahedrally four-coordinate with bond lengths: Ga—O, 1.869 and 1.879(2), Ga—N, 1.945–2.001 (3), and Ga—H, 1.40–1.52(4–5) Å. The remaining gallium atom is five-coordinate with distorted trigonal bipyramidal geometry (Ga—O(ax), 1.960(3), Ga—N(ax), 2.779(3), Ga—N(eq), 1.949 and 1.999(3), and Ga—H(eq), 1.49(5)Å). Other bond lengths in the molecule are: N—C, 1.449–1.493(4–10), C—C, 1.486–1.528(6–7), N—H, 0.85(5), and mean C—H, 1.03 Å. The errors quoted above are those arising from the least-squares analysis and do not reflect uncertainties introduced by the thermal analysis.

Crystal and molecular structure of the salicylaldehydatogallium dimethyl dimer

1976 ◽  
Vol 54 (8) ◽  
pp. 1278-1284 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Gallium Atom ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers ◽  
Distorted Trigonal Bipyramidal

Crystals of the salicylaldehydatogallium dimethyl dimer, [C7H5O2•GaMe2]2, are triclinic, a = 9.845(1), b = 8.6892(8), c = 7.4153(6) Å, α = 118.236(5), β = 92.46(1), γ = 115.81(1)°, Z = 1, space group [Formula: see text] The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to a final R of 0.050 and Rw of 0.064 for 1644 reflections with I ≥ 3σ(I). The structure features a five-coordinate gallium atom having distorted trigonal bipyramidal geometry. Monomer units link via the formation of a four-membered Ga2O2 ring to form the centrosymmetric dimers. Bond lengths in the molecule are: Ga—O(eq), 1.933(3), Ga—O(ax), 2.127(3) and 2.469(3), Ga—C, 1.944(6) and 1.946(5), C—O, 1.333(4) and 1.231(6), C(ar)—C(sp2), 1.432(7), mean C—C(ar), 1.395(8), mean C(sp3)—H, 0.92(4), and mean C(sp2)—H, 0.93(2) Å. Bonds not involving hydrogen have been corrected for thermal motion.

Crystal and molecular structure of diorganoammonium oxalatotrimethylstannate, [R2NH2][Me3Sn(C2O4)] (R=i-Bu, cyclohexyl)

2011 ◽  
Vol 34 (5-6) ◽  
pp. 127-130 ◽  
Author(s):  
Yaya Sow ◽  
Libasse Diop ◽  
Kieran C. Molloy ◽  
Gabrielle Kociok-Köhn
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Diffraction Study ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Trans Complex ◽  
A Chain ◽  
Distorted Trigonal Bipyramidal

Abstract The title compounds [R2NH2][C2O4SnMe3](R=i-Bu, Cy), in which tin atoms adopt a distorted trigonal bipyramidal configuration, have been prepared and submitted to an X-ray diffraction study. These compounds have been obtained from the reaction of (Cy2NH2)2C2O4·H2O or (i-Bu2NH2)2C2O4 with SnMe3Cl. In both [R2NH2][C2O4SnMe3] compounds, the trans complex has an almost regular trigonal bipyramidal geometry around the tin atom. The SnMe3 residues are connected as a chain with bridging oxalate anions in a trans-SnC3O2 framework, the oxygen atoms being in axial positions. The cations connect linear adjacent chains through NH…O hydrogen bonds giving layered structures.

Crystal and molecular structure of bis[methyltris(1-pyrazolyl)gallato]nickel(II)

1979 ◽  
Vol 57 (14) ◽  
pp. 1823-1825 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Nickel Atom ◽  
Exact Formula ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Gallium Atom ◽  
Full Matrix ◽  
Distorted Tetrahedral Coordination

Crystals of bis[methyltris(1-pyrazolyl)gallato]nickel(II) are rhombohedral, a = 9.6670(5), c = 23.893(1) Å, Z = 3, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.030 and Rw = 0.035 for 925 reflections with I ≥ 3σ (I). The crystal structure consists of well separated molecules of [MeGa-(N2C3H3)3]2Ni having exact [Formula: see text] (S6) symmetry and approximate D3d symmetry. The coordination geometry about the nickel atom is octahedral with Ni—N = 2.109(2) Å, N—Ni—N = 90.65(6) and 89.35(6)°. The gallium atom has distorted tetrahedral coordination geometry with Ga—N = 1.939(2), Ga—C = 1.940(4) Å, N—Ga—N = 99.55(6), and N—Ga—C = 118.16(5)°.

Synthesis and characterization of octahedral and trigonal bipyramidal transition metal complexes incorporating chelating gallate ligands: crystal and molecular structure of [Me2Ga(N2C5H7)(OCH2CH2NMe2)]Ni[(N2C5H7)2GaMe2]

1980 ◽  
Vol 58 (11) ◽  
pp. 1091-1100 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
Synthesis And Characterization ◽  
Chelating Ligands ◽  
Full Matrix ◽  
Trigonal Bipyramidal ◽  
Distorted Trigonal Bipyramidal

The preparation and physical properties of octahedral and trigonal bipyramidal complexes incorporating the tris-chelating ligands [Me2Ga(N2C5H7)(OCH2CH2NR′2)]− (R′ = H or Me) are described. Crystals of [dimethylbis(3,5-dimethyl-1-pyrazolyl)gallato (N(2),N′(2))][dimethyl (3,5 - dimethyl-1-pyrazolyl) (N,N-dimethylethanolamino(gallato (N(2), O, N(3))]nickel(II) are triclinic, a = 20.8562(11), b = 9.1536(4), c = 8.2798(4) Å, α = 100.204(3), β = 85.513(4), γ = 101.989(3)°, 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 = 0.048 and Rw = 0.078 for 5508 reflections with I ≥ 3σ(I). The coordination about the Ni atom is distorted trigonal bipyramidal with the two nitrogen atoms from the Me2Ga(N2C5H7)2 ligand occupying equatorial positions. The tridentate Me2Ga(N2C5H7)(OCH2CH2NMe2) ligand is meridionally coordinated with the oxygen in the equatorial and the two nitrogens in the axial positions. Important bond lengths (corrected for libration) are: Ni—N(eq), 2.005(3) and 2.006(3), Ni—O, 1.993(3), Ni—N(pz—ax), 2.072(3), Ni—N(amino), 2.229(3), Ga—O, 1.913(3), Ga—N, 1.971(3)–1.989(3), and Ga—C, 1.961(10)–1.986(6) Å.

Crystal and Molecular Structure of the N-Methyldiethanolaminogallane Dimer, [CH3N(CH2CH2O)2GaH]2

1974 ◽  
Vol 52 (12) ◽  
pp. 2206-2215 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Experimental Error ◽  
Crystal And Molecular Structure ◽  
Fourier Synthesis ◽  
Full Matrix ◽  
Axial Ligands ◽  
Trigonal Bipyramidal ◽  
The Mean ◽  
Distorted Trigonal Bipyramidal

Crystals of the N-methyldiethanolaminogallane dimer are orthorhombic, a = 19.112(4), b = 9.947(2), c = 7.709(2) Å, Z = 4, space group P212121. The structure was determined by Patterson and Fourier synthesis and was refined by full-matrix least-squares procedures to a final R of 0.056 for 1477 observed reflections. The structure provides the first1 known crystallographic example of pentacoordinate gallium, the dimerization of MeN(CH2CH2O)2GaH occurring via the formation of a four-membered Ga2O2 ring. The coordination about the gallium is distorted trigonal bipyramidal with an angle of 151.2(4)° between the axial substituents. The mean bond distances are: Ga—N, 2.192(5), and Ga—O, 2.018(2) for axial ligands; Ga—O, 1.847(2), 1.960(8), and Ga—H, 1.41(4) for equatorial ligands; O—C, 1.419(14), C—N, 1.470(7), C—C, 1.520(12), and C—H, 1.00(13) Å. The molecule has C2 symmetry to within experimental error. There are possible [Formula: see text] hydrogen bonds ([Formula: see text] 3.13(1)–3.44(1) Å) in the structure.

N,N-Ethylenebis(salicylideneimine) derivatives of gallium trimethyl: crystal and molecular structure of N,N-ethylenebis(salicylideneiminato) bis(dimethylgallium)

1977 ◽  
Vol 55 (13) ◽  
pp. 2540-2546 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Weighted Mean ◽  
Full Matrix ◽  
Derivatives Of ◽  
Distorted Tetrahedral Coordination

Crystals of N,N-ethylenebis(salicylideneiminato)bis(dimethylgallium) are orthorhombic, a = 22.781(1), b = 9.4869(6), c = 19.700(2) Å, Z = 8, space group Pbca. 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 0.029 for 2248 reflections with I ≥ 3σ(I). Details of the preparation and physical properties of (C16H14N2O2)(GaMe2)2 and (C16H15N2O2)(GaMe2) are given. The (C16H14N2O2)(GaMe2)2 molecule is approximately centrosymmetric in the solid state. A "GaMe2" unit is coordinated to each of the two salicylideneiminato moieties of the N,N-ethylenebis(salicylideneiminato) ligand. The gallium atoms have a distorted tetrahedral coordination geometry, with bond angles at gallium ranging from 92.7(1) to 124.6(3)°. Important bond lengths (corrected for libration) are: Ga—O, 1.886(2) and 1.884(2), Ga—N, 2.033(3) and 2.042(3), and weighted mean Ga—C, 1.959(9) Å.

scholarly journals The crystal and molecular structure of the bis(N,N,N′,N′-tetramethylethanediamine) adduct of I(Br)InInBr2, In2Br3I•2C6H16N2, an indium–indium bonded molecule

1984 ◽  
Vol 62 (3) ◽  
pp. 601-605 ◽  
Author(s):  
Masood A. Khan ◽  
Clovis Peppe ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Orthorhombic Space Group ◽  
Trigonal Bipyramidal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Distorted Trigonal Bipyramidal

The crystal structure of the title compound has been determined by the heavy atom method. The crystals are orthorhombic, space group Pbca, with unit cell dimensions a = 22.795(3) Å, b = 17.518(2) Å, c = 12.396(3) Å, Z = 8; R = 0.0409 for 1527 unique "observed" reflections. The structure is disordered, with each halogen site (X) occupied by 75% Br, 25% I. The molecule consists of two X2(tmen)In units (tmen = N,N,N′,N′-tetramethylethanediamine) with distorted trigonal bipyramidal geometry, joined by an In—In bond 2.775(2) Å in length.

Crystal and molecular structure of B,B-bis(p-tolyl)boroxazolidine and the orthorhombic form of B,B-diphenylboroxazolidine

1976 ◽  
Vol 54 (20) ◽  
pp. 3130-3141 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Statistical Analysis ◽  
Hydrogen Bonds ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Length Variation ◽  
Full Matrix ◽  
Space Group ◽  
Phenyl Rings ◽  
Related Compounds

Crystals of B,B-bis(p-tolyl)boroxazolidine, 1c, are trigonal, a = 25.1028(9), c = 12.4184(7) Å, Z = 18, space group [Formula: see text]. And crystals of B,B-diphenylboroxazolidine, 1a, are orthorhombic, a = 17.6420(4), b = 14.2527(3), c = 10.205(1) Å, Z = 8, space group Pbca. Both structures were solved by direct methods and were refined by full-matrix least-squares procedures to final R values of 0.057 and 0.040 for 2230 and 1828 reflections with I ≥ 3σ(I) respectively. Both molecules have structures similar to related compounds and feature intermolecular N—H … O hydrogen bonds (N … O = 2.982(2) for 1c and 2.896(2) Å for 1a). Bond lengths are: for 1c; O—C, 1.413(3), O—B, 1.478(3), N—C, 1.488(3), N—B, 1.657(3), C(sp3)—C(sp3), 1.501(4), B—C, 1.616(3) and 1.623(3), mean C—C(ar), 1.395, N—H, 0.93(2) and 0.94(2), mean C(sp3)—H, 1.00, and mean C(ar)—H, 1.00 Å; for 1a; O—C, 1.409(2), O—B, 1.476(2), N—C, 1.489(2), N—B, 1.655(2), C(sp3)—C(sp3), 1.507(3), B—C, 1.613(2) and 1.620(2), mean C—C(ar), 1.391, N—H, 0.93(2) and 0.92(2), mean C(sp3)—H, 1.00, and mean C(ar)—H, 0.98 Å. A statistical analysis of the phenyl C—C distances in compounds 1a, 1b, and 1c has provided an example of statistically significant substituent-induced bond length variation in the phenyl rings.

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