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, 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 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 XL. 4,7-Dicyclohexyl-2,2,5,6-tetraphenyl- 1,3-dioxa-4-aza-7-azonia-2-boratacycloheptane

1990 ◽  
Vol 68 (10) ◽  
pp. 1797-1802 ◽  
Author(s):  
Henning Amt ◽  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Least Squares ◽  
Direct Methods ◽  
Organoboron Compound ◽  
Chair Conformation ◽  
Membered Ring ◽  
Structural Studies ◽  
Full Matrix ◽  
Bond Lengths

The synthesis of 4,7-dicyclohexyl-2,2,5,6-tetraphenyl-1,3-dioxa-4-aza-7-azonia-2-boratacycloheptane is reported. Crystals of the compound are orthorhombic, a = 10.893(1), b = 28.072(1), c = 10.596(1) 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 = 0.043 for 2480 reflections with I ≥ 3σ(I). The molecule has a seven-membered chelate structure. The seven-membered ring, which has a twisted chair conformation, is stabilized by an intramolecular [Formula: see text] hydrogen bond. Bond lengths O—B = 1.468(4) and 1.554(4), C—B = 1.621(5) and 1.626(4) Å are consistent with moderately strong binding of the diphenylboron moiety by the O,O-chelating ligand. Keywords: crystal structure, organoboron compound, boron compound.

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.

Five-coordinate iron and manganese dinitrosyl complexes incorporating tridentate chelating dimethyl(N,N-dimethylethanolamino)(pyrazolyl)gallate ligands: crystal and molecular structure of [Me2Ga(N2C5H7)(OCH2CH2NMe2)]Fe(NO)2

1979 ◽  
Vol 57 (23) ◽  
pp. 3113-3118 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Iron Complex ◽  
Coordination Geometry ◽  
Full Matrix ◽  
Trigonal Bipyramidal ◽  
Dinitrosyl Complexes ◽  
Molecular Dimensions ◽  
Iron And Manganese ◽  
Distorted Trigonal Bipyramidal

Novel neutral monomeric five-coordinate manganese and iron dinitrosyl compounds incorporating asymmetric tridentate anionic gallate ligands are described. The crystal structure of the formally "19-electron" iron complex [Me2Ga(N2C5H7)(OCH2CH 2NMe2)]Fe(NO)2 has been determined. Crystals of [dimethyl(N,N-dimethylethanolamino)(3,5-dimethylpyrazolyl)gallato (N(2),N(3),O)]dinitrosyliron(I) are monoclinic, a = 7.3079(6), b = 14.274(1), c = 17.076(1) Å, β = 91.709(4)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to R = 0.034 and Rw = 0.046 for 2848 reflections with I ≥ 3σ(I). The crystal structure consists of discrete monomeric units. The coordination geometry about the iron atom is distorted trigonal-bipyramidal with the tridentate gallate ligand acting in a meridional fashion, occupying one equatorial and both axial positions. The two nitrosyl groups occupy the other two equatorial sites and both Fe—N—O groupings are considerably bent toward one another in the equatorial plane. Important mean molecular dimensions (distances corrected for libration) are: Fe—O, 2.037(3), Fe—N(pyrazolyl), 2.112(3), Fe—N(amino), 2.279(3), Fe—NO, 1.710(3), N—O, 1.153(5), Ga—O, 1.916(3), Ga—N, 1.975(3), Ga—C, 1.972(6) Å, and Fe—N—O, 158.6(7)°.

Catalytic decarbonylation of aldehydes using iron(II) porphyrin complexes, and the crystal structure of (5,10,15,20-tetraphenylporphinato)bis(tri-n-butylphosphine)iron(II)

1988 ◽  
Vol 66 (8) ◽  
pp. 2072-2078 ◽  
Author(s):  
Ramesh M. Belani ◽  
Brian R. James ◽  
David Dolphin ◽  
Steven J. Rettig
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Hydrogen Abstraction ◽  
Heavy Atom ◽  
Crystal Form ◽  
Coordination Geometry ◽  
Full Matrix ◽  
Space Group ◽  
Initiation Reaction ◽  
Trace Water

The complex (5, 10, 15, 20-tetraphenylporphinato)bis(tri-n-butylphosphine)iron(II), 1, has been isolated in a triclinic crystal form, a = 12.499(3), b = 12.528(2), c = 12.039(2) Å, α = 116.39(1), β = 109.79(1), γ = 98.13(1)°, Z = 1, space group [Formula: see text]. The structure was solved by conventional heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.060 and Rw = 0.070 for 3551 reflections with I ≥ 3σ(I). The molecule, which has crystallographic [Formula: see text], symmetry, displays a relatively undistorted pseudo-octahedral coordination geometry with Fe—P = 2.346(1) and Fe—N = 1.998(3) and 1.993(3) Å. In CH2Cl2 solution, 1 reacts with CO and aldehydes to generate the carbonyl(phosphine) derivative, and decarbonylation of phenylacetaldehyde to toluene becomes catalytic under an Ar stream. The aldehyde decarbonylations involve radical pathways via carbonyl loss from [Formula: see text]. The hydrogen abstraction/initiation reaction probably utilizes trace O2 (and possibly trace (water); speculative mechanisms are discussed.

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 structure of the spirophosphorane (OCMe2C(O)O)2PH

1998 ◽  
Vol 76 (7) ◽  
pp. 1060-1063 ◽  
Author(s):  
Craig D Montgomery ◽  
Steven J Rettig ◽  
Bryn Shurmer
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Trigonal Bipyramid ◽  
Full Matrix ◽  
Space Group ◽  
Trigonal Bipyramidal Geometry ◽  
Trigonal Bipyramidal ◽  
Independent Molecules ◽  
Distorted Trigonal Bipyramidal

The crystal structure of the spirobicyclic phosphorane (OCMe2C(O)O)2PH, 1, has been determined. Crystals of C8H13O6P, 1, are orthorhombic, a = 10.515(2), b = 10.623(2), c = 20.552(2) Å, Z = 8, space group Pca21. The structure was solved by direct methods and refined by full-matrix least-squares procedures to R = 0.037 (Rw = 0.033) for 1616 reflections with I > 3sigma(I). The structure consists of two independent molecules each displaying a distorted trigonal bipyramidal geometry; the distortion follows closely the Berry pseudorotation coordinate.Key words: crystal structure, phosphorane, Berry pseudorotation, trigonal bipyramid.

Complexes of the dimethylgallium-1-pyrazolyl-o-aminophenolato ligand, [Me2Ga(pz)(o-NH2C6H4O)]−. Formation and crystal structure of the molybdenum amidine complex, Mo(CO)2Br(η3-C3H5)[η2-HN=CMe(pz)] (where pz = pyrazolyl, N2C3H3)

1987 ◽  
Vol 65 (10) ◽  
pp. 2469-2477 ◽  
Author(s):  
G. D. Gracey ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Physical Properties ◽  
Least Squares ◽  
Heavy Atom ◽  
Full Matrix ◽  
Space Group ◽  
Benzene Solvate

The synthesis, characterization, and structures of complexes containing the o-aminophenolato ligand are detailed. A novel molybdenum amidine complex is also described. Crystals of (o-aminophenolato)dimethylgallium are monoclinic, a = 10.1970(9), b = 9.7597(7), c = 18.778(2) Å, β = 100.810(7)°, Z = 8, space group C2/c, those of bis(dimethylgallium-1-pyrazolyl-o-aminophenolato)nickel(II) benzene solvate are monoclinic, a = 20.491(1), b = 11.789(1), c = 15.789(1) Å, β = 103.413(7)°, Z = 4, space group C2/c, and those of η3-allyl(bromo)[2-(1-pyrazolyl)ethylidenarnino]dicarbonylmolybdenum(II) are monoclinic, a = 11.0278(4), b = 8.4461(2), c = 15.3747(5) Å, β = 109.208(3)°, Z = 4, space group P21/c. The structures were solved by conventional heavy atom methods and refined by full-matrix least-squares procedures to R = 0.030, 0.053, and 0.038 for 1980, 1684, and 1901 reflections, respectively. Reaction of the [Me2Ga(pz)(OC6H4NH2)]− ligand, L−, with [Re(CO)4Cl]2 results in the formation of LRe(CO)3 whose physical properties indicate a fac arrangement of the organogallate ligand.

Synthesis and crystal structure of tri(μ-carbonyl)bis[methyltris(1-pyrazolyl)gallato]dirhodium – benzene (1:1)

1984 ◽  
Vol 62 (4) ◽  
pp. 633-643 ◽  
Author(s):  
Brenda M. Louie ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Physical Properties ◽  
Least Squares ◽  
Structural Parameters ◽  
Heavy Atom ◽  
Molecular Symmetry ◽  
Single Bond ◽  
Synthesis And Crystal Structure ◽  
Full Matrix ◽  
Space Group

The synthesis, physical properties, and crystal structure of the dirhodium species [MeGa(N2C3H3)3]2Rh2(μ-CO)3 containing three carbonyl bridges are reported. Crystals of tri(μ-carbonyl)bis[methyltris(1-pyrazolyl)gallato]dirhodium – benzene (1:1) are monoclinic, a = 11.660(4), b = 15.2917(7), c = 11.750(4) Å, β = 119.09(1)°, Z = 2, space group P21. The structure was solved by conventional heavy-atom techniques and was refined by full-matrix least-squares procedures to R = 0.030 and Rw = 0.033 for 2604 reflections with I ≥ 3σ(I). The molecule contains a Rh—Rh single bond of 2.5818(8) Å bridged by three CO ligands, the overall molecular symmetry being close to D3h. Other important mean structural parameters are: Rh—C = 2.007(10), Rh—N = 2.181(14) Å, Rh—C—Rh = 80.1(5)°, and Rh—C—O = 140.0(7)°.

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