Synthesis, structure, and properties of poly-bis(μ-diethylphosphinato)copper(II)

1982 ◽  
Vol 60 (15) ◽  
pp. 2017-2022 ◽  
Author(s):  
Katherine W. Oliver ◽  
Steven J. Rettig ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Magnetic Properties ◽  
Magnetic Susceptibility ◽  
Infrared Spectra ◽  
Field Model ◽  
Direct Methods ◽  
Coordination Geometry ◽  
Structure And Properties ◽  
Tetrahedral Coordination ◽  
Full Matrix

The preparation, magnetic properties, electronic and infrared spectra, and molecular structure of poly-bis(μ-diethylphosphinato)copper(II) are described. Crystals of poly-bis(μ-diethylphosphinato)copper(II) are triclinic, a = 7.700(1), b = 9.807(1), c = 10.101(1) Å, α = 90.48(1), β = 104.77(1), γ = 112.21(1)°, Z = 2, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.025 and Rw = 0.032 for 3491 reflections with I ≥ 3σ(I). The polymeric structure consists of Cu atoms with flattened tetrahedral coordination geometry linked by double phosphinate bridges. Mean bond lengths (corrected for libration) are: Cu—O, 1.924(3), P—O, 1.526(4), and P—C, 1.807(4) Å. Assignment of the electronic spectrum using a crystal field model gives Dq = 1665 cm−1 and Cp = 1800 cm−1. Magnetic susceptibility studies give no evidence for magnetic concentration over the temperature range 80 to 300 K.

Crystal and molecular structure of bis[methyltris(1-pyrazolyl)gallato]nickel(II)

1979 ◽  
Vol 57 (14) ◽  
pp. 1823-1825 ◽  
Author(s):  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Nickel Atom ◽  
Exact Formula ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Gallium Atom ◽  
Full Matrix ◽  
Distorted Tetrahedral Coordination

Crystals of bis[methyltris(1-pyrazolyl)gallato]nickel(II) are rhombohedral, a = 9.6670(5), c = 23.893(1) Å, Z = 3, space group [Formula: see text]. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.030 and Rw = 0.035 for 925 reflections with I ≥ 3σ (I). The crystal structure consists of well separated molecules of [MeGa-(N2C3H3)3]2Ni having exact [Formula: see text] (S6) symmetry and approximate D3d symmetry. The coordination geometry about the nickel atom is octahedral with Ni—N = 2.109(2) Å, N—Ni—N = 90.65(6) and 89.35(6)°. The gallium atom has distorted tetrahedral coordination geometry with Ga—N = 1.939(2), Ga—C = 1.940(4) Å, N—Ga—N = 99.55(6), and N—Ga—C = 118.16(5)°.

N,N-Ethylenebis(salicylideneimine) derivatives of gallium trimethyl: crystal and molecular structure of N,N-ethylenebis(salicylideneiminato) bis(dimethylgallium)

1977 ◽  
Vol 55 (13) ◽  
pp. 2540-2546 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Weighted Mean ◽  
Full Matrix ◽  
Derivatives Of ◽  
Distorted Tetrahedral Coordination

Crystals of N,N-ethylenebis(salicylideneiminato)bis(dimethylgallium) are orthorhombic, a = 22.781(1), b = 9.4869(6), c = 19.700(2) Å, Z = 8, space group Pbca. 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 0.029 for 2248 reflections with I ≥ 3σ(I). Details of the preparation and physical properties of (C16H14N2O2)(GaMe2)2 and (C16H15N2O2)(GaMe2) are given. The (C16H14N2O2)(GaMe2)2 molecule is approximately centrosymmetric in the solid state. A "GaMe2" unit is coordinated to each of the two salicylideneiminato moieties of the N,N-ethylenebis(salicylideneiminato) ligand. The gallium atoms have a distorted tetrahedral coordination geometry, with bond angles at gallium ranging from 92.7(1) to 124.6(3)°. Important bond lengths (corrected for libration) are: Ga—O, 1.886(2) and 1.884(2), Ga—N, 2.033(3) and 2.042(3), and weighted mean Ga—C, 1.959(9) Å.

Synthesis, characterization, and X-ray structural analysis of the Cu(I) derivative, [Me2Ga(OCH2CH2NMe2)N2C5H7]Cu• PPh3

1981 ◽  
Vol 59 (3) ◽  
pp. 518-523 ◽  
Author(s):  
Kenneth S. Chong ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Structural Analysis ◽  
Copper Atom ◽  
Direct Methods ◽  
Carbonyl Complex ◽  
Coordination Geometry ◽  
Tetrahedral Coordination ◽  
Full Matrix ◽  
X Ray ◽  
Complex Crystals ◽  
Distorted Tetrahedral Coordination

The Cu(I) complex [Me2Ga(OCH2CH2NMe2)N2C5H7]Cu•PPh3 has been synthesized and its fluxional behavior in solution probed. Attempts have been made to isolate the analogous Cu(I) carbonyl complex. Crystals of [dimethyl(3,5-dimethyl-1-pyrazolyl)(N,N-dimethylethanolamino)gallato (N(2),O,N(3))](triphenylphosphine)copper(I) are monoclinic, a = 18.871(2), b = 9.464(1), c = 18.374(2) Ā, β = 109.62(1)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.028 and Rw = 0.035 for 2729 reflections with I ≥ 3σ(I). The copper atom is bonded to the phosphine and to the tridentate Me2Ga(OCH2CH2NMe2)N2C5H7− ligand resulting in a distorted tetrahedral coordination geometry. The Cu—P distance of 2.156(1) Å is unusually short. Other important bond distances (corrected for libration) are: Cu—O, 2.163(2), Cu—N(pyrazolyl), 2.025(3), Cu—N(amino), 2.144(3), Ga—O, 1.896(3), Ga—N, 2.005(3), and Ga—C, 1.972(5) and 1.987(5) Å.

Crystal and molecular structure of B,B-bis(p-tolyl)boroxazolidine and the orthorhombic form of B,B-diphenylboroxazolidine

1976 ◽  
Vol 54 (20) ◽  
pp. 3130-3141 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Statistical Analysis ◽  
Hydrogen Bonds ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Length Variation ◽  
Full Matrix ◽  
Space Group ◽  
Phenyl Rings ◽  
Related Compounds

Crystals of B,B-bis(p-tolyl)boroxazolidine, 1c, are trigonal, a = 25.1028(9), c = 12.4184(7) Å, Z = 18, space group [Formula: see text]. And crystals of B,B-diphenylboroxazolidine, 1a, are orthorhombic, a = 17.6420(4), b = 14.2527(3), c = 10.205(1) Å, Z = 8, space group Pbca. Both structures were solved by direct methods and were refined by full-matrix least-squares procedures to final R values of 0.057 and 0.040 for 2230 and 1828 reflections with I ≥ 3σ(I) respectively. Both molecules have structures similar to related compounds and feature intermolecular N—H … O hydrogen bonds (N … O = 2.982(2) for 1c and 2.896(2) Å for 1a). Bond lengths are: for 1c; O—C, 1.413(3), O—B, 1.478(3), N—C, 1.488(3), N—B, 1.657(3), C(sp3)—C(sp3), 1.501(4), B—C, 1.616(3) and 1.623(3), mean C—C(ar), 1.395, N—H, 0.93(2) and 0.94(2), mean C(sp3)—H, 1.00, and mean C(ar)—H, 1.00 Å; for 1a; O—C, 1.409(2), O—B, 1.476(2), N—C, 1.489(2), N—B, 1.655(2), C(sp3)—C(sp3), 1.507(3), B—C, 1.613(2) and 1.620(2), mean C—C(ar), 1.391, N—H, 0.93(2) and 0.92(2), mean C(sp3)—H, 1.00, and mean C(ar)—H, 0.98 Å. A statistical analysis of the phenyl C—C distances in compounds 1a, 1b, and 1c has provided an example of statistically significant substituent-induced bond length variation in the phenyl rings.

Crystal and molecular structure of 2,6-dimethyl-3,5-di[N-methyl]carbamoyl-4-[3,4-methoxy]phenyl-l,4-dihydropyridine hemihydrate and 2,6-dimethyl-3,5-di[N-methyl]carbamoyl-4-[furan]1,4-dihydropyridine

1999 ◽  
Vol 214 (12) ◽  
Author(s):  
M. Bidya Sagar ◽  
K. Ravikumar ◽  
Y. S. Sadanandam
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal Structures ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Asymmetric Unit ◽  
Full Matrix

AbstractThe crystal structures of two dihydropyridines were solved by direct methods and refined by full-matrix least-squares procedure. 2,6-Dimethyl-3,5-di[N-methyl]-carbamoyl-4-[3,4-methoxy]phenyl-1,4-dihydropyridine hemihydrate, CBoth compounds crystallize with two molecules in the asymmetric unit. In compound

Basic halides and related species of molybdenum(III). II. Spectroscopic and magnetic properties of MoOF(H2O)3 and MoOCl(H2O)3

1976 ◽  
Vol 29 (4) ◽  
pp. 717 ◽  
Author(s):  
DJ Stabb
Keyword(s):  
Magnetic Properties ◽  
Magnetic Susceptibility ◽  
Absorption Spectroscopy ◽  
Infrared Spectra ◽  
Electronic Spectra ◽  
Related Species ◽  
Bound Water ◽  
Temperature Range ◽  
Field Dependent

Two basic halides of molybdenum(111), namely MoOF(H2O)3 and MoOCl(H2O)3 (some samples containing additional loosely bound water), were investigated by absorption spectroscopy in the range 200-50000 cm-1, and by magnetic susceptibility measurements over a temperature range of 100-300 K. Infrared spectra showed bands at about 670 and 1600 cm-l, but not in the range 800-1100 cm-1. Electronic spectra showed poorly defined bands superimposed on strong general absorption. Very weak paramagnetism was observed: this was field dependent. The results are interpreted to show the compounds to be oxygen-bridged polymers [MOX(H2O)3O]n, rather than species containing Mo=O or Mo-0-H groups.

Synthetic plant growth regulators. V. The synthesis and crystal structure of a hybrid gibberellin-helminthosporic acid

1980 ◽  
Vol 33 (5) ◽  
pp. 1061 ◽  
Author(s):  
JV Turner ◽  
BF Anderson ◽  
LN Mander
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Carboxylic Acid ◽  
Standard Procedure ◽  
Direct Methods ◽  
Detailed Comparison ◽  
Synthesis And Crystal Structure ◽  
Full Matrix ◽  
Cyclopropyl Ketone ◽  
R Value

(3aRS,4RS,6RS,8aSR)-5-Methyleneoctahydro-4H-3a,6-methanoazulene-4-carboxylic acid (7) has been synthesized and a detailed comparison made between its molecular structure and that of gibberellic acid (4). Indane-5-carboxylic acid (8) was converted by an alternating sequence of reduction and isomerization into the hydrindene acid (11). The diazomethyl ketone derived from (11) was transformed to cyclopropyl ketone (12) which was reduced by Li/NH3 with stereochemical inversion at the β-carbon to give a 1:3 mixture of ketones (13) and (14) respectively. Ketone (14) was then converted into the title acid (7) by a standard procedure. ��� Molecules of (7) crystallize in space group P2/c with a 7.782(1), b 11.055(1), c 14.559(3) Ǻ, β 116.05(1)°. The structure was solved by direct methods and refined by full-matrix least squares to a final R value of 0.053.

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.

Crystal and molecular structure of difluoroboron N-methylacethydroxamate (2,2-difluoro-4,5-dimethyl-1,3-dioxa-4-azonia-2-boranatacyclopent-4-ene)

1977 ◽  
Vol 55 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter ◽  
W. Kliegel ◽  
D. Nanninga
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of difluoroboron N-methylacethydroxamate are monoclinic, a = 5.097(1), b = 10.653(2), c = 11.520(2) Å, β = 103.57(2)°, Z = 4, space group P21/c. The structure was solved by direct methods and was refined by full-matrix least squares procedures to a final R of 0.056 and Rw of 0.077 for 988 reflections with I ≥ 3σ(I). The structure features a planar five-membered BO2CN ring. Bond lengths (corrected for libration) are: B—F, 1.374(3) and 1.381(3), O—B, 1.496(3) and 1.497(3), O—N, 1.349(2), O—C, 1.346(2), C—N, 1.298(3) and 1.458(3), and C—C, 1.468(3) Å.

The crystal and molecular structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, a phosphorus–silicon heterocycle

1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Single Bond ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Bond Lengths

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.

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