Synthesis, characterization, and structural studies of gallium citrate complexes

1985 ◽  
Vol 63 (9) ◽  
pp. 2545-2549 ◽  
Author(s):  
Gregory A. Banta ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Oxygen Atom ◽  
Physical Properties ◽  
Least Squares ◽  
Ester Group ◽  
Coordination Geometry ◽  
Structural Studies ◽  
Full Matrix ◽  
Heavy Atoms ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers

The synthesis and physical properties of two dimethylgallium citrate triester complexes are reported. Crystals of bis-[(trimethylcitrato)dimethylgallium(III)] are monoclinic, a = 9.839(1), b = 14.496(1), c = 11.125(1) Å, β = 108.31(1)°, Z = 2, space group P21/c. The structure was solved by conventional heavy-atoms methods and was refined by full-matrix least-squares procedures to R = 0.036 and Rw = 0.037 for 1507 reflections with I ≥ 3σ(I). The structure consists of centrosymmetric dimers in which each citrate ligand is coordinated via the hydroxyl oxygen (bridging) and the C=O oxygen atom of the central ester group, forming five-membered chelate rings. Each Ga atom has irregular trigonal bipyramidal coordination geometry with Ga—O(eq) = 1.950(3), Ga—O(ax) = 2.103(3) and 2.395(3), and Ga—C(eq) = 1.953(5) and 1.947(5) Å.

Synthesis and structure of N,N′-ethylenebis(salicylideneiminato)chlorogallium(III) and its methyl analog

1981 ◽  
Vol 59 (1) ◽  
pp. 94-99 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Physical Properties ◽  
Least Squares ◽  
Coordination Geometry ◽  
Form Complex ◽  
Gallium Atom ◽  
Full Matrix ◽  
Trigonal Bipyramidal ◽  
Methyl Analog

The synthesis and physical properties of N,N′-ethylenebis(salicylideneiminato)chlorogallium(III) and N,N′-ethylenebis(salicylideneiminato)methylgallium(III) are described. Crystals of N,N′-ethylenebis(salicylideneiminato)chlorogallium(III) dichloromethane are monoclinic, a = 13.049(1), b = 9.525(1), c = 15.459(2) Å, β = 92.452(5)°, Z = 4, space group P21/a. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to R = 0.042 and Rw = 0.051 for 1815 reflections with I ≥ 3σ(I). The gallium atom is bonded to one chlorine atom and to the tetradentate N,N′-ethylenebis(salicylideneiminato) ligand to give a coordination geometry which is intermediate between square pyramidal and trigonal bipyramidal. Important bond lengths (corrected for libration) are: Ga—Cl, 2.228(2), Ga—O, 1.868(4) and 1.883(4), Ga—N, 2.019(6) and 2.035(5) Å. The crystal structure consists of discrete (C16H14N2O2)GaCl and CH2Cl2 molecules linked by a[Formula: see text]hydrogen bond [Formula: see text]to form complex-solvate units.

Synthesis and structural characterization of bis(tropolonatodimethylgallium), [(C7H5O2)Ga(CH3)2]2

1984 ◽  
Vol 62 (9) ◽  
pp. 1705-1708 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Solid State ◽  
Physical Properties ◽  
Least Squares ◽  
Structural Characterization ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
State Structure ◽  
Full Matrix ◽  
Trigonal Bipyramidal

Details of the synthesis, physical properties, and solid-state structure of [(C7H5O2)Ga(CH3)2]2 are reported. Crystals of bis(tropolonatodimethylgallium) are monoclinic, a = 10.2669(9), b = 9.3237(3), c = 10.8671(10) Å, β = 112.896(4)°, Z = 2, space group P21/n (22°C, λ = 0.70930 Å). The structure was solved by conventional heavy-atom techniques and was refined by full-matrix least-squares procedures to R = 0.034 and Rw = 0.037 for 1746 reflections with I ≥ 3σ(I). The centrosymmetric binuclear dimer features five-coordinate gallium atoms having irregular trigonal bipyramidal coordination geometry and a planar four-membered Ga2O2 ring. Important bond lengths (corrected for libration) are Ga—O(equatorial) = 1.972(2), Ga—O(axial) = 2.025(2) and 2.551(2) Å, and Ga—C = 1.951(4) and 1.954(4) Å.

Structural studies of organoboron compounds. XXXII. 5,5-Difluoro-2,2-pentamethylene-1,4,6-trioxa-3a-azonia-5-borata-1,2,3,4,5,6-hexahydrobenzo[h]azulene and 2,2-pentamethylene-5,5-diphenyl-1,4,6-trioxa-3a-azonia-5-borata-1,2,3,4,5,6-hexahydrobenzo[h]azulene

1988 ◽  
Vol 66 (10) ◽  
pp. 2621-2630 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Mahmood Tajerbashi ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Solid State ◽  
Physical Properties ◽  
Least Squares ◽  
Crystal Structures ◽  
Direct Methods ◽  
Structural Studies ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
Conformational Isomers

Details of the syntheses, physical properties, and crystal structures of the title compounds are reported. Crystals of 5,5-difluoro-2,2-pentamethylene-1,4,6-trioxa-3a-azonia-5-borata-1,2,3,4,5,6-hexahydrobenzo[h]azulene are triclinic, a = 6.1576(3), b = 11.2651(3), c = 10.8118(3) Å, α = 109.747(3), β = 105.807(4), γ = 92.976(4)°, Z = 2, space group [Formula: see text], and those of 2,2-pentamethylene-5,5-diphenyl-1,4,6-trioxa-3a-azonia-5-borata-1,2,3,4,5,6-hexahydrobenzo[h]azulene are monoclinic, a = 9.8549(6), b = 10.9242(6), c = 41.263(2) Å, β = 92.717(6)°, Z = 8, space group P21/n. Both structures were solved by direct methods and were refined by full-matrix least-squares procedures to R = 0.045 and 0.042 for 2344 and 4248 reflections with I ≥ 3σ(I), respectively. The molecules were both found to possess a seven-membered chelate structure, the O,O-chelatїng ligand being strongly bound to the X2B moiety. Two conformational isomers of the X = Ph compound were found in the solid state. The 2-oxazoline N-oxide moieties present in both compounds are the first to be structurally characterized. Important mean libration-corrected bond lengths are: O—B = 1.491 and F—B = 1.387 Å for X = F; O—B = 1.511 and C—B = 1.620 Å for X = Ph.

Structural studies of organoboron compounds. XVI. Preparation and crystal and molecular structures of 4,4-dimethyl-2,5,5-triphenyl-1,3-dioxa-4-azonia-2-bora-5-boratacyclopentane and 4,4,5,5-tetramethyl-2,2-diphenyl-1,3-dioxa-4-azonia-2-boratacyclopentane

1984 ◽  
Vol 62 (5) ◽  
pp. 838-844 ◽  
Author(s):  
W. Kliegel ◽  
H.-W. Motzkus ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Physical Properties ◽  
Least Squares ◽  
Steric Hindrance ◽  
Direct Methods ◽  
Structural Features ◽  
Molecular Structures ◽  
Structural Studies ◽  
Full Matrix ◽  
Space Group ◽  
Crystal And Molecular Structures

Details of the synthesis, physical properties, and molecular structures of 4,4-dimethyl-2,5,5-triphenyl-1,3-dioxa-4-azonia-2-bora-5-boratacyclopentane, 4, and 4,4,5,5-tetramethyl-2,2-diphenyl-1,3-dioxa-4-azonia-2-boratacyclopentane, 5, are reported. Crystals of 4 are triclinic, a = 9.841(2), b = 14.722(3), c = 6.6701(12) Å, α = 86.79(1), β = 102.95(1), γ = 93.89(1)°, Z = 2, space group [Formula: see text]; and those of 5 are monoclinic, a = 14.9164(12), b = 6.4732(3), c = 18.2248(15) Å, β = 117.263(3)°, Z = 4, space group Cc. Both structures were solved by direct methods and were refined by full-matrix least-squares procedures to final R values of 0.032 and 0.035 for 1456 and 1649 observed reflections, respectively. Molecules of 4 contain non-planar BOBON rings with an unusually long N(sp3)—B(sp3) distance of 1.728(3) Å and in 5 there is a long N(sp3)—C(sp3) bond of 1.591(3) Å. These structural features are ascribed to steric hindrance.

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.

Structural studies of organoboron compounds. XXX. 1,9-Dimethyl-3,5,7-triphenyl-2,4,6,8-tetraoxa-1,9-diazonia-5-bora-3,7- diboratatricyclo[5.4.0.03,9]undecane

1988 ◽  
Vol 66 (5) ◽  
pp. 1117-1122 ◽  
Author(s):  
Henning Amt ◽  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Physical Properties ◽  
Least Squares ◽  
Title Compound ◽  
Direct Methods ◽  
Ring System ◽  
Structural Studies ◽  
Organoboron Compounds ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Details of the preparation and physical properties of the title compound are given. Crystals of 1,9-dimethyl-3,5,7- triphenyl-2,4,6,8-tetraoxa-1,9-diazonia-5-bora-3,7-diboratatricyclo[5.4.0.03,9]undecane are orthorhombic, a = 9.4026(3), b = 9.4663(2), c = 24.7462(9) Å, Z = 4, space group P212121. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.036 and Rw = 0.038 for 1536 reflections with I ≥ 3σ(I). The three six-membered and two seven-membered rings comprising the tricyclo[5.4.0.03,9]undecane ring system all have boat or boat-like conformations. Important bond lengths (corrected for libration) are: B(sp3)—N = 1.649(6) and 1.668(6), B(sp3)—O(N) = 1.492(5) and 1.497(6), B(sp3)—O[B(sp2)] = 1.444(6) and 1.438(5), B(sp3)—C = 1.600(6) and 1.594(7), B(sp2)—O = 1.357(6) and 1.370(6), B(sp2)—C = 1.574(6) Å.

The Structure and Physical Properties of μ-oxo-bis{oxotrichloro(O-perrhenylchloride)rhenium(VI)}, and the Non-existence of β-ReOCl3

1972 ◽  
Vol 50 (22) ◽  
pp. 3607-3618 ◽  
Author(s):  
C. Calvo ◽  
P. W. Frais ◽  
C. J. L. Lock
Keyword(s):  
Oxygen Atom ◽  
Infrared Spectrum ◽  
Physical Properties ◽  
Single Crystal ◽  
Least Squares ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
Weak Bond ◽  
X Ray ◽  
Chloride Molecule

The compound previously reported as β-ReOCl3 has been shown by analysis and single crystal X-ray diffraction to be μ-oxo-bis{oxotrichloro(O-perrhenyl chloride)rhenium(VI)}, (Re2O3Cl6)(ReO3Cl)2. The crystals were triclinic, a = 6.112(5), b = 12.876(9), c = 6.020(5) Å, α = 88.30(5), β = 95.88(5), γ = 105.36(5)°, [Formula: see text]. Intensities were measured by a densitometer from photographs recorded on an integrating precession camera. The structure was refined by full matrix least squares to give a final R2 of 0.072. The molecule is composed of a dimeric Re2O3Cl6 unit with a bridging oxygen atom on the center of symmetry and an Re—O (bridge) distance of 1.847(1) Å. The remaining oxo-group on each rhenium is cis to the bridge and is strongly bonded (1.69(2) Å), and the position trans to the terminal oxo-group is filled by a weak bond to an oxygen atom of a perrhenyl chloride molecule. The infrared spectrum of the compound has been explained in terms of the structure.

Structural studies of organoboron compounds. XXXIV. 4-(N-Methoxymethylimino)-2,2-diphenyl-1,3-dioxa-2-borata-1,2,3,4-tetrahydronaphthalene and 4-diethylimino-2,2-diphenyl-1,3-dioxa-2-borata-1,2,3,4-tetrahydronaphthalene

1989 ◽  
Vol 67 (10) ◽  
pp. 1636-1643 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Mahmood Tajerbashi ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Physical Properties ◽  
Least Squares ◽  
Crystal Structures ◽  
Direct Methods ◽  
Structural Studies ◽  
Boron Compounds ◽  
Organoboron Compounds ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Details of the syntheses, physical properties, and crystal structures of the title compounds are reported. Crystals of 4-(N-methoxymethylimino)-2,2-diphenyl-1,3-dioxa-2-borata-1,2,3,4-tetrahydronaphthalene, 4, are monoclinic, a = 9.8072(5), b = 9.6217(7), c = 19.6793(12) Å, β = 94.871(5)°, Z = 4, space group P21/c, and those of 4-diethylimino-2,2-diphenyl-1,3-dioxa-2-borata-1,2,3,4-tetrahydronaphthalene, 9, are orthorhombic, a = 17.0593(7), b = 16.1372(6), c = 14.3753(5) Å, Z = 8, space group Pbca. Both structures were solved by direct methods and were refined by full-matrix least-squares procedures to R = 0.046 and 0.038 for 2198 and 2969 reflections with I ≥ 3σ(I), respectively. In both structures the N,N-dialkylsalicylamidate ligands coordinate the diphenylboron moieties via the phenolate oxygen and amide oxygen atoms, forming six-membered O—B—O chelate rings. The O(ar)—B, O(amide)—B, and mean C—B bond lengths (corrected for libration) are as follows: 1.490(3), 1.549(4), and 1.612 Å for 4 and 1.494(2), 1.550(2), and 1.612 Å for 9. Keywords: crystal structures, boron compounds, organoboron compounds.

Structural studies of organoboron compounds. XXXI. (3-Benzoyl-(+)-camphorato)diphenylboron

1988 ◽  
Vol 66 (8) ◽  
pp. 2007-2013 ◽  
Author(s):  
William R. Cullen ◽  
Steven J. Rettig ◽  
James Trotter ◽  
Eugene B. Wickenheiser
Keyword(s):  
Physical Properties ◽  
Crystal Lattice ◽  
Least Squares ◽  
Structure Analysis ◽  
Title Compound ◽  
Direct Methods ◽  
Structural Studies ◽  
Full Matrix ◽  
Bond Lengths ◽  
Independent Molecules

Details of the synthesis and physical properties of the title compound are reported along with a new preparation of 3-benzoyl-(+)-camphor. Crystals of (3-benzoyl-(+)-camphorato)diphenylboron are triclinic, a = 9.0362(3), b = 9.4679(3), c = 14.2731(7) Å, α = 101.920(3), β = 100.086(3), γ = 93.251(3)°, Z = 2, space group P1. The structure was solved by non-routine application of direct methods and was refined by full-matrix least-squares procedures to R = 0.036 and Rw = 0.039 for 4094 reflections with I ≥ 3σ(I). The unit-cell contains two crystallographically independent molecules, related to one another in the crystal lattice by a pseudo-inversion centre, and having the same configuration but different conformations. The structure analysis shows that the chiral, anionic, 1,3-diketonate ligand derived from 3-benzoyl-(+)-camphor is not symmetrically delocalized like most related ligands, resulting in significantly different O—B bond lengths. Bond lengths (corrected for libration) include: O—B = 1.514(4), 1.522(4); 1.568(4) and 1.567(4) Å; C—B = 1.594(5)−1.616(5) Å.

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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