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.

Heavy transition metal complexes of biologically important molecules. I. The crystal and molecular structure of trans-dichloro(bis(isopropyl)-sulfoxide-S)(1-methylcytosine-N)platinum(II)

1976 ◽  
Vol 54 (1) ◽  
pp. 53-58 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Robert Anthony Speranzini ◽  
John Powell
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Least Squares ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal and molecular structure of trans-dichloro(bis(isopropyl)sulfoxide-S)(1-methylcytosine-N)platinum(II) has been determined by single crystal X-ray diffraction. The crystals are triclinic with a = 16.205(5), b = 8.078(2), c = 6.776(2) Å, α = 106.53(2), β = 96.35(2), γ = 98.54(2)°. The space group is [Formula: see text] and there are two molecules per unit cell. A total of 2294 independent reflections, of which 2023 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares analysis to an R2 value of 0.0427. The ligands form a rough square around the platinum atom with Pt—Cl(1), 2.304(3), Pt—Cl(2), 2.287(4), Pt—S, 2.232(2), Pt—N, 2.058(7). Distances within the ligands are normal. The plane of the cytosine ring is at 84.4° to the plane formed by the ligands around platinum.

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.

Synthesis and characterization of dinuclear trihydride complexes of platinum with chelating ligands. Crystal and molecular structure of [Pt2H3(Ph2P(CH2)2PPh2)2][BPh4]

1983 ◽  
Vol 22 (16) ◽  
pp. 2324-2331 ◽  
Author(s):  
Carolyn B. Knobler ◽  
Herbert D. Kaesz ◽  
Giovanni Minghetti ◽  
Anna Laura Bandini ◽  
Guido Banditelli ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Synthesis And Characterization ◽  
Chelating Ligands

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.

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