Crystal and molecular structure of an unusual unsymmetrical isomer of 1,2-Os3(CO)10{P(C6H5)[(η-C5H4)Fe(η-C5H5)]2}2

1992 ◽  
Vol 70 (9) ◽  
pp. 2329-2334 ◽  
Author(s):  
William R. Cullen ◽  
Steven J. Rettig ◽  
Tu Cai Zheng
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Full Matrix ◽  
Space Group

The reaction of Os3(CO)10(MeCN)2 with PFc2Ph (Fc = (η-C5H4)Fe(η-C5H5)) affords the unsymmetrical isomer of 1,2-Os3(CO)10(PFc2Ph)2, 2. Crystals of 2 are monoclinic, a = 27.846(4), b = 11.253(4), c = 38.520(3) Å, β = 107.813(9)°, Z = 8, space group C2/c. The structure was solved by heavy atom methods, and was refined by full-matrix least-squares procedures to R = 0.030 and Rw = 0.027 for 5073 reflections with I ≥ 3σ(I).

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.

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.

Crystal and molecular structure of fac-[dimethylbis(1-pyrazolyl)gallato-N,N′]-(triphenylphosphine)tricarbonylrhenium(I)

1985 ◽  
Vol 63 (3) ◽  
pp. 703-707 ◽  
Author(s):  
Brenda M. Louie ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths ◽  
Independent Molecules ◽  
Twisted Boat ◽  
Chelate Rings

Crystals of fac-[dimethylbis(1-pyrazolyl)gallato-N,N′](triphenylphosphine)tricarbonylrhenium(I) are triclinic, a = 9.479(2), b = 16.258(4), c = 20.412(6) Å, α = 110.06(1), β = 95.46(1), γ = 92.65(2)°, Z = 4, 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 = 0.027 and Rw = 0.031 for 5965 reflections with I ≥ 3σ(I). The two crystallographically independent molecules have nearly identical structures. The coordination about Re is distorted fac-octahedral with mean bond lengths: Re—P = 2.538(4), Re—N = 2.201(5), Re—CO(trans to P) = 1.931(1), and Re—CO(trans to N) = 1.913(9) Å. The ReGaN4 chelate rings have twisted boat conformations with cross-ring [Formula: see text] separations of 3.9396(7) and 3.8981(8) Å.

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.

Crystal and Molecular Structure of 2,5-Bis(2′-hydroxyethylamino)-1,4-benzoquinone

1975 ◽  
Vol 53 (5) ◽  
pp. 777-783 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Full Matrix ◽  
Space Group ◽  
Compound C ◽  
Related Compounds ◽  
Centrosymmetric Molecule

Crystals of 2,5-bis(2′-hydroxyethylamino)-1,4-benzoquinone are monoclinic, a = 5.020(1), b = 19.238(3), c = 5.214(1) Å, β = 96.15(3)°, Z = 2, space group P21/n. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.045 for 646 reflections with I ≥ 3σ(I). The benzoquinone ring in the centrosymmetric molecule is slightly, but significantly, nonplanar. Bond distances in the compound (C—C, 1.247 (2) and 1.410 (3), C—N, 1.332 (3) and 1.457 (3), C—C, 1.384–1.514 (3), N—H, 0.89 (3), O—H, 1.07 (5), and C—H, 0.95–1.09 (3) Å) are similar to those in related compounds. The structure features an extensive network of N—H … O (N … O = 2.639 (3) and 3.033 (2) Å) and O—H … O(O … O = 2.757 (3) Å ) hydrogen bonds.

Crystal and molecular structure of L-prolinatodiphenylboron

1977 ◽  
Vol 55 (6) ◽  
pp. 958-965 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Conformational Disorder ◽  
Full Matrix ◽  
Space Group ◽  
Bond Lengths

Crystals of L-prolinatodiphenylboron are monoclinic, a = 5.9427(5), b = 14.4633(7), c = 8.9654(4) Å, β = 98.423(8)°, Z = 2, space group P21. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.037 and Rw of 0.053 for 1477 reflections with I ≥ 3σ(I). The proline ring exhibits conformational disorder. The crystal structure consists of discrete molecules linked by N—H … O hydrogen bonds (N … O = 2.893(3) Å) along the short a axis. Intramolecular N—B coordination occurs to form a system of two fused five-membered rings. Bond lengths (corrected for libration) are: N—B, 1.630(3), O—B, 1.529(3), O—C, 1.219(3) and 1.300(3), N—C, 1.506(3) and 1.507(3), C(sp3)–C(sp3), 1.525(4), C(sp2)—C(sp3), 1.517(3), and mean C—C(phenyl), 1.394 Å.

Structural studies of organoboron compounds. LX. Reaction of sterically hindered arylboronic acids with 2-(hydroxyamino)alkanols. Crystal and molecular structure of 2-mesityl-6,6-pentamethylene-1,3-dioxa-4-aza-2-boracyclohexane

1994 ◽  
Vol 72 (4) ◽  
pp. 1154-1161 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Gottfried Lubkowitz ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Structural Studies ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Arylboronic Acids ◽  
Sterically Hindered

Three 2-(hydroxyamino)alkanols have been reacted with sterically hindered arylboronic acids, ArB(OH)2. When Ar = o-tolyl, 1:2 condensates having bicyclic structures are formed but when Ar = mesityl (2,4,6-(CH3)3C6H2), 1:1 condensates having six-membered cycloboronate structures result. These 1:1 condensates represent the first examples of N-unsubstituted 1,3-dioxa-4-aza-2-boracyclohexane derivatives. An X-ray analysis of one example provides unambiguous proof of the structure. Crystals of 2-mesityl-6,6-pentamethylene-1,3-dioxa-4-aza-2-boracyclohexane, 3c, are monoclinic, a = 11.076(9), b = 23.94(2), c = 13.414(9) Å, β = 109.40(5)°, Z = 8, space group P21/n. The structure was solved by direct methods and refined by full-matrix least-squares procedures to R = 0.051 and Rw = 0.058 for 2037 reflections with I ≥ 3σ(F2).

Crystal and molecular structure of diphenylboron N-methylacethydroxamate (4,5-dimethyl-2,2-diphenyl-1,3-dioxa-4-azonia-2-boratacyclopent-4-ene)

1978 ◽  
Vol 56 (12) ◽  
pp. 1676-1680 ◽  
Author(s):  
Steven J. Rettig ◽  
James Trotter ◽  
W. Kliegel ◽  
D. Nanninga
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Heterocyclic Ring ◽  
Mirror Plane ◽  
Full Matrix ◽  
Space Group ◽  
Carbon And Nitrogen ◽  
Bond Lengths

Crystals of diphenylboron N-methylacethydroxamate are orthorhombic, a = 12.5478(8), b = 7.8735(3), c = 13.6809(5) Å, Z = 4, space group Pnam. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.037 and Rw = 0.054 for 1265 reflections with I ≥ 3σ(I). The molecule features a five-membered BO2CN ring which lies in the crystallographic mirror plane. The carbon and nitrogen atoms of the heterocyclic ring are positionally disordered. Mean bond lengths (corrected for libration) are: O—B, 1.550(2), B—C, 1.609(2), O—C/N, 1.340(3), C—N, 1.300(2), C/N—CH, 1.470(2), and C—C(phenyl), 1.394(8) Å.

The Crystal and Molecular Structure of Chloro-mer-Tris(dimethylphenylphosphine)-cis-dihydridoiridium(III) by X-Ray and Neutron Diffraction

1988 ◽  
Vol 41 (5) ◽  
pp. 641 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Molecular Structure ◽  
Neutron Diffraction ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Neutron Data ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The structure of mer-(Pme2Ph)3Cl-cis-H2IrIII (1) has been determined by single-crystal X-ray and neutron diffraction analyses. Crystals are monoclinic, space group P21, with a 11.476(4), b 14.069(5), c 8.286(3)Ǻ, β 92.45(1)° and Z 2. Full-matrix least-squares analyses converged 0.022 for 7773 X-ray data and R(F2) = 0.062 for 1538 neutron data. Ir -H [1.557(11)Ǻ trans to Cl, 1.603(10) Ǻ trans to P] and Ir -P distances [2.292(1)Ǻ trans to P, 2.328(1)Ǻ trans to H] both exhibit trans lengthening effects. Consistent with the increased hydride content the Ir -P distances in (1) are c. 0.04 Ǻ shorter than for the corresponding bonds in its dichloro monohydrido analogues and c. 0.08 Ǻ shorter than those in the trichloride . In contrast Ir-Cl [2.505(1)Ǻ] is not significantly different to the corresponding distance (2.504 Ǻ av.) in mer -(PMe2Ph)3-cis-Cl2HIrIII.

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