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)°.

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.

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.

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.

Characterization and nonrigid behaviour of a carboxylate-bridged rhodium dimer

1994 ◽  
Vol 72 (5) ◽  
pp. 1294-1301 ◽  
Author(s):  
William R. Cullen ◽  
Steven J. Rettig ◽  
Eugene B. Wickenheiser
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Variable Temperature ◽  
Heavy Atom ◽  
Molecular Rearrangement ◽  
Full Matrix ◽  
Space Group ◽  
H Nmr ◽  
Nmr Data ◽  
Nmr Study

Bis(μ-t-butylacetato)bis(norbornadiene)dirhodium(I) 1 is prepared by a reaction between pivaloyl camphor and (norbornadiene)rhodium(I) chloride dimer. A molecular rearrangement takes place in which the pivaloyl groups of the pivaloyl camphor starting material are incorporated into the end product as bridging t-butylcarboxylate ligands. A variable temperature 1H NMR study and corresponding dynamic computer fit of the NMR data, and crystal structure are reported for the structurally nonrigid dimer. Crystals of 1 are triclinic, a = 10.454(1), b = 10.817(1), c = 12.424(1) Å, α = 64.904(7), β = 100.320(7), γ = 109.382(8)°, Z = 2, space group [Formula: see text] The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.070 and Rw = 0.081 for 3093 reflections with I ≥ 3σ(I).

The crystal structure and vibrational spectra of cis-dichlorobis(cyclopropylamine)-platinum(II), PtCl2(C3H5NH2)2

1981 ◽  
Vol 59 (18) ◽  
pp. 2737-2745 ◽  
Author(s):  
Helen Elaine Howard-Lock ◽  
Colin James Lyne Lock ◽  
Graham Turner ◽  
Maruta Zvagulis
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Vibrational Spectra ◽  
Vibrational Analysis ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
Deuterated Analogue

Crystals of cis-dichlorobis(cyclopropylamine)platinum(II), PtCl2(C3H5NH2)2, are monoclinic, a = 12.770(5), b = 5.838(2), c = 15.113(6) Å, β = 104.46(3)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares to R = 0.057, Rw = 0.055 for 1577 reflections with I > 3σ(I). Bond lengths and angles are normal. A vibrational analysis of the compound and its d2-deuterated analogue was performed.

Reaction of N,N′-dihydroxy-.N,N′-dimethylmethanediamine with phenylboronic acid and the crystal and molecular structure of N,N′-dihydroxy-N,N′-dimethylmethanediamine

1989 ◽  
Vol 67 (11) ◽  
pp. 1959-1963 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Phenylboronic Acid ◽  
Direct Methods ◽  
Exact Formula ◽  
Full Matrix ◽  
Space Group ◽  
Hydrogen Bonded

The reaction of N,N′-dihydroxy-N,N′-dimethylmethanediamine with phenylboronic acid leads to the product 1,7-dimethyl-3,5-diphenyl-2,4,6-trioxa-7-aza-1-azonia-3-bora-5-boratabicyclo[3.3.0]octane rather than the expected product 1,5-dimethyl-3-phenyl-1,5-diaza-2,4-dioxa-3-boracyclohexane. The structure of N,N′-dihydroxy-N,N′-dimethylmethanediamine has been determined and is discussed in terms of its reaction with PhB(OH)2. Crystals of N,N′-dihydroxy-N,N′-dimethylmethanediamine are tetragonal, a = 8.5346(3), c = 8.4178(7) Å, Z = 4, space group P421c. 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 0.038 for 333 reflections with I ≥ 3σ(I). The structure consists of hydrogen-bonded dimers having exact [Formula: see text] symmetry. Keywords: N,N′-dihydroxy-N,N′-dimethylmethanediamine, crystal structure.

The Crystal Structure of Dimedone

1975 ◽  
Vol 53 (7) ◽  
pp. 1046-1050 ◽  
Author(s):  
Ishwar Singh ◽  
Crispin Calvo
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Symmetry ◽  
Enolic Form ◽  
Full Matrix ◽  
Space Group ◽  
Least Squares Techniques

Dimedone, C8H12O2, crystallizes with monoclinic symmetry, a = 10.079(7), b = 6.835(3), c = 12.438(4) Å, β = 110.24(5)°, space group P21/n and Z = 4. The structure of this compound was solved by direct methods and refined by full-matrix least-squares techniques using 1205 unique reflections to a final R of 0.047. In the solid state it exists in the enolic form and these molecules pack in the crystal in systems of infinite chains linked together by hydrogen bonds in the y direction. These results are virtually the same as recently reported by Semmingsen.

Refinement of the structure of Mg2As2O7

1970 ◽  
Vol 48 (6) ◽  
pp. 890-894 ◽  
Author(s):  
C. Calvo ◽  
K. Neelakantan
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Unit Cell ◽  
Full Matrix ◽  
Space Group ◽  
Cell Dimensions ◽  
Central Oxygen ◽  
R Value ◽  
Unit Cell Dimensions

The crystal structure of Mg2As2O7 has been refined by full matrix least squares procedures using 587 observed reflections. The structure of Mg2As2O7 is of the thortveitite type, as reported by Łukaszewicz, with space group C2/m and unit cell dimensions a = 6.567(2) Å, b = 8.524(4) Å, c = 4.739(1) Å, β = 103.8(1)°, and Z = 2. The As—O—As group in the anion appears to be linear but the central oxygen atom undergoes considerable disorder in the plane perpendicular to this group. The AsO bond distances uncorrected for thermal motion are 1.67 Å for the As—O(—As) bond and 1.66 and 1.65 Å for the terminal As—O bonds. The final R value obtained is 0.088.

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.

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