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.

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.

scholarly journals Synthesis and structural characterization of glycinatodimethylgallium, (C2H4NO2)Ga(CH3)2

1987 ◽  
Vol 65 (6) ◽  
pp. 1349-1352 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structural Characterization ◽  
Title Compound ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Full Matrix ◽  
Independent Molecules

Details of the preparation and crystal structure of the title compound are given. Crystals of glycinatodimethylgallium are monoclinic, a = 12.502(1), b = 12.023(1), c = 10.732(1) Å, β = 110.05(1)°, Z = 8, space group P21/c. The structure was solved by conventional heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.033 and Rw = 0.039 for 1172 reflections with I ≥ 3σ(I). The structure consists of monomeric (C2H4NO2)GaMe2 molecules which are linked together by an extensive network of [Formula: see text] hydrogen bonds. The Ga atoms have tetrahedral coordination geometry with bond lengths averaged over the two crystallographically independent molecules: Ga—O = 1.958(18), Ga—N = 2.031(5), and Ga—C = 1.937(7) Å.

Pyrazagaboles, pyrazolyl-bridged heterocycles containing boron and gallium

1990 ◽  
Vol 68 (1) ◽  
pp. 59-63 ◽  
Author(s):  
Steven J. Rettig ◽  
Mark Sandercock ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Structural Characterization ◽  
Heavy Atom ◽  
Full Matrix ◽  
Space Group ◽  
The Mean

The synthesis and structural characterization of representative and novel pyrazagaboles, boron- and gallium-containing compounds with a central six-membered heterocyclic B—(N—N)2—Ga ring feature, are detailed. Crystals of dimethylgallium-bis(μ-pyrazolyl)dimethylboron are orthorhombic, a = 7.6135(5), b = 16.2917(5), c = 22.331(1) Å, Z = 8, space group Pbca, and those of hydroxy(methyl)galliumbis(μ-pyrazolyl)dimethylboron are orthorhombic, a = 7.6197(3), b = 16.2184(7), c = 22.190(1) Å, Z = 8, space group Pbca. Both structures were solved by conventional heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.054 and 0.040 for 1243 and 1272 reflections with I ≥ 1.5 and 3σ(I), respectively. The crystal structures are isomorphous and both feature six-membered B—(N—N)2—Ga rings having highly asymmetric boat conformations, unlike those observed for the majority of the homobinuclear analogs previously reported. The mean Ga—N and B—N distances in the two compounds are 1.977 and 1.61 Å. Keywords: pyrazagaboles, pyrazolyl-bridged heterocycles, crystal structures, synthesis of pyrazagaboles.

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 characterization of [Me2Ga(3,5-Me2pz)2]Rh(CO)PPh3 and the X-ray structure of its toluene solvate

1985 ◽  
Vol 63 (2) ◽  
pp. 503-508 ◽  
Author(s):  
Brenda M. Louie ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Physical Properties ◽  
Least Squares ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Boat Conformation ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Square Planar

Details of the synthesis and physical properties of [Me2Ga(3,5-Me2pz)2]Rh(CO)PPh3 are given. Crystals of [dimethylbis(3,5-dimethyl-1-pyrazolyl)gallato-N,N′](triphenylphosphine)carbonylrhodium(I) – toluene (1:1) are triclinic, a = 10.690(2), b = 12.928(2), c = 13.998(2) Å, α = 77.44(1), β = 83.50(1), γ = 72.70(1)°, Z = 2, 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 = 0.039 and Rw = 0.048 for 5987 reflections with I ≥ 3σ(I). The Rh(I) is in a distorted square planar environment with Rh—N = 2.090(3) and 2.097(2), Rh—CO = 1.815(4), and Rh—P = 2.2700(8) Å. The central six-membered RhGaN4 ring has a steep boat conformation with a [Formula: see text] separation of 3.3819(4) Å.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

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.

Crystal and molecular structure of [dimethyl(1-pyrazolyl)(2-pyridyl-methoxy)gallato-N2,O,N3](η3-allyl)dicarbonylinolybdenum(II)

1988 ◽  
Vol 66 (3) ◽  
pp. 355-358 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Nitrogen Atom ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Coordination Geometry ◽  
Pyridyl Nitrogen ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of [dimethyl(1-pyrazolyl)(2-pyridylmethoxy)gallato-N2,O,N3](η3-allyl)dicarbonylmolybdenum(II) are triclinic, a = 9.632(2), b = 9.798(2), c = 10.255(2) Å, α = 80.16(1), β = 87.38(1), γ = 81.75(1)°, Z = 2, 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 = 0.033 and Rw = 0.037 for 3000 reflections with I ≥ 3σ(I). The molecule has pseudo-octahedral coordination geometry with the tridentate [Me2Ga(N2C3H3)(OCH2(C5H4N))]− ligand facially coordinated and the η3-allyl ligand occupying one coordination site trans to the pyridyl nitrogen atom. Important bond lengths are Mo—O = 2.219(2), Mo—N(py) = 2.212(3), Mo—N(pz) = 2.232(2), Mo—C(allyl) = 2.290(4), 2.189(4), 2.341(4), Mo—CO (trans to O) = 1.928(4), and Mo—CO (trans to N) = 1.952(4) Å.

Molecular “Texas Longhorn”: An expanded Schiff base oligopyrrolic macrocycle

2021 ◽  
pp. A-G
Author(s):  
Chenxing Guo ◽  
Vincent M. Lynch ◽  
Jonathan L. Sessler
Keyword(s):  
Schiff Base ◽  
Solid State ◽  
Structural Characterization ◽  
Building Blocks ◽  
State Structure ◽  
Architectural Form ◽  
Molecular Building Blocks ◽  
Texas Longhorn ◽  
Porphyrin Analogues

We report here the synthesis and structural characterization of a novel expanded Schiff base oligopyrrolic macrocycle TxLH (i.e. compound 2) along with its smaller congener hemi-TxLH (i.e. compound 1). The solid-state structure of TxLH is reminiscent of the shape of a Texas Longhorn[Formula: see text]. It thus defines a new architectural form for porphyrin analogues. The present study thus underscores the potential of using functionalized oligopyrroles as readily accessible molecular building blocks for the construction of structurally non-trivial molecules.

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