Preparation and characterization of the osmium cluster complexes H2Os3(CO)8L(EtFcPCMe) (L = CO or PEt2Fc) and H2Os3(CO)8[(η-C5H3PEt2)Fe(η-C5H4)]

1993 ◽  
Vol 71 (3) ◽  
pp. 399-409 ◽  
Author(s):  
William R. Cullen ◽  
Steven J. Rettig ◽  
Tu Cai Zheng
Keyword(s):  
Least Squares ◽  
Heavy Atom ◽  
Molar Ratio ◽  
Asymmetric Unit ◽  
Full Matrix ◽  
Space Group ◽  
Cluster Complexes ◽  
Unit Space

Thermolysis of Os3(CO)11(PEt2Fc) (Fc = (η-C5H4)Fe(η-C5H5)) in octane for 8 h affords H2Os3(CO)9(EtFcPCMe), 10, and H2Os3(CO)8[(η-C5H3PEt2)Fe(η-C5H4)], 9e, in 15 and 65% yield, respectively. Heating Os3(CO)12 and PEt2Fc in 1:2 molar ratio in xylene for 10 h gives two isomers of H2Os3(CO)8(PEt2Fc)(EtFcPCMe), 11, in about 40% yield. Two crystalline modifications of the complex 9e have been obtained from the same solvent: 9eA, triclinic, a = 15.653(1), b = 15.799(1), c = 11.257(1) Å, α = 90.388(7)°, β = 109.740(6)°, γ = 82.445(6)°, Z = 4 (two molecules per asymmetric unit), space group [Formula: see text]; and 9eB, monoclinic, a = 9.889(2), b = 13.632(3), c = 18.927(4) Å, β = 97.36(2)°, Z = 4, space group P21/n. The structures were solved by heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.033 and 0.037 for 8131 and 5145 reflections with I ≥ 3σ(I), respectively.

Synthesis and characterization of LMo(CO)3M(PPh3)x (where L = tridentate pyrazolyl-gallate or -borate ligand; M = Rh, x = 2; M = Cu, x = 1). X-ray crystal structures of [MeGapz3]Mo(CO)3Rh(PPh3)2 and [MeGapz3]Mo(CO)3Cu(PPh3) (where pz = pyrazolyl, N2C3H3)

1986 ◽  
Vol 64 (2) ◽  
pp. 373-386 ◽  
Author(s):  
Gregory A. Banta ◽  
Brenda M. Louie ◽  
Emmanuel Onyiriuka ◽  
Steven J. Rettig ◽  
Alan Storr
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Octahedral Structure ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The reactions of the LMo(CO)3− ions (L = MeGapz3, HBpz3, Me2Gapz(OCH2CH2NMe2)) with [Cu(PPh3)Cl]4 and Rh(PPh3)3Cl have yielded complexes with Mo—Cu and Mo—Rh bonds. The X-ray crystal structures of two such complexes have been determined. Crystals of [MeGapz3]Mo(CO)3Cu(PPh3) are monoclinic, a = 17.071(2), b = 16.738(1), c = 23.641(3) Å, β = 104.899(6)°, Z = 8, space group P21/n, and those of [MeGapz3]Mo(CO)3Rh(PPh3)2, are triclinic, a = 12.519(3), b = 17.182(4), c = 12.071(2) Å, α = 105.02(1), β = 109.87(1), γ = 97.10(2)°, Z = 2, space group [Formula: see text]. Both structures were solved by conventional heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.040 and Rw = 0.035 for 6296 reflections with I ≥ 2σ(I) and R = 0.036 and Rw = 0.037 for 5642 reflections with I ≥ 3σ(I), respectively. The former complex provides a rare example of a 3:3:1, or capped octahedral structure, with a short (mean) Mo—Cu distance of 2.513(9) Å. The latter compound displays one terminal and two bridging CO ligands and a Mo—Rh distance of 2.6066(5) 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 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.

Studies in aryltin chemistry. Part 6. Crystal and molecular structures of tetra(p-methylsulphonylphenyl)tin(IV) and tetra(p-methylsulphinylphenyl)tin(IV) monohydrate

1990 ◽  
Vol 68 (8) ◽  
pp. 1277-1282 ◽  
Author(s):  
Ivor Wharf ◽  
Michel G. Simard ◽  
Henry Lamparski
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Direct Method ◽  
Molecular Structures ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
Molecular Symmetry ◽  
Asymmetric Unit ◽  
Full Matrix ◽  
Space Group

Tetrakis(p-methylsulphonylphenyl)tin(IV) and tetrakis(p-methylsulphinylphenyl)tin(IV) n-hydrate have been prepared and their spectra (ir 1350–400 cm−1; nmr, 1H, 13C, 119Sn) and X-ray crystal structures are reported. The first compound is monoclinic, space group C2/c, Z = 4, with a = 21.589(6), b = 6.207(3), c = 22.861(11) Å, β = 93.80(3)° (22 °C); the structure was solved by the direct method and refined by full-matrix least squares calculations to R = 0.043 for 2755 observed reflections. It has 2 molecular symmetry with the methyl group and one oxygen atom completely disordered in both CH3S(O2) groups in the asymmetric unit. The second compound is tetragonal, space group P42/n, Z = 2, with a = b = 15.408(6), c = 6.379(2) Å (−100 °C); the structure was solved by the Patterson method and refined by full-matrix least squares calculations to R = 0.060 for 1209 observed reflections. It has [Formula: see text] molecular symmetry with the whole asymmetric unit disordered. Water molecules occupy positions on parallel 42 axes but molecular packing requirements prevent all sites having 100% occupancy giving n ~ 1 for the hydrate. Keywords: Tetra-aryltins, crystal structures, sulphone, sulphoxide, hydrogen-bonding.

scholarly journals Synthesis and Molecular Structure of cis-Tetracarbonyl[N-(diphenylphosphino-kP)-naphthalen-1-yl-P,P-diphenylphosphinous amide-kP]chromium(0)

2014 ◽  
Vol 2014 ◽  
pp. 1-4
Author(s):  
Harbi Tomah Al-Masri
Keyword(s):  
Molecular Structure ◽  
Least Squares ◽  
Direct Methods ◽  
Molar Ratio ◽  
Planar Geometry ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
Distorted Octahedral ◽  
Least Squares Techniques

The reaction of N,N-bis(diphenylphosphanyl)naphthylamine C10H7-1-N(PPh2)2 with (C5H10NH)2Cr(CO)4 (1 : 1 molar ratio) in dichloromethane afforded cis-[Cr(CO)4{C10H7-1-N(PPh2)2}] (1). This complex was crystallized in the monoclinic space group P21/n. The structure was solved by direct methods and refined by full-matrix least squares techniques to an R factor of 0.0313 for 6488 observed reflections. The Cr-metal is coordinated by four terminal CO molecules and a P,P′-bidentate N,N-bis(diphenylphosphanyl)naphthylamine ligand in a distorted octahedral array. The N-atom adopts a planar geometry with the two P-atoms and C-atom attached to it. The four-membered metallacycle ring P2CrN is nearly planar.

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.

Synthesis and X-ray crystal structure of the 3,5-dimethylpyrazolato copper(I) trimer, [Cu(pz″)]3

1990 ◽  
Vol 68 (8) ◽  
pp. 1444-1449 ◽  
Author(s):  
Martin K. Ehlert ◽  
Steven J. Rettig ◽  
Alan Storr ◽  
Robert C. Thompson ◽  
James Trotter
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Heavy Atom ◽  
High Yield ◽  
Asymmetric Unit ◽  
Temperature Synthesis ◽  
Full Matrix ◽  
X Ray ◽  
Unit Space ◽  
High Temperature Synthesis

A moderately high-yield, high temperature synthesis of the title compound is reported. Crystals of tris[(3,5-dimethylpyrazolato-N1,N2)copper(I)] are triclinic, a = 12.360(4), b = 14.637(4), c = 12.358(4) Å, α = 105.29(2), β = 119.83(2), γ = 93.99(3)°, Z = 4 (trimers, two per asymmetric unit), space group [Formula: see text]. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures to R = 0.034 and Rw = 0.038 for 3877 reflections with I ≥ 3σ(I). The structure consists of trimeric molecules with an unusually short average Cu—N distance of 1.852 Å. The central Cu3N6 nine-membered rings are planar to within 0.07 Å. The trimer units are linked in pairs about centres of symmetry by weak [Formula: see text] interactions averaging 2.946 Å. Keywords: pyrazolato copper (I) timer, copper (I) pyrazolate.

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).

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.

Structural studies of organoboron compounds. LII. N-Ethylhydroxylamine- (O-B)1,7-diethyl-3,5-diphenyl-2,4,6-trioxa-7-aza-1-azonia-3-bora-5- boratabicyclo[3.3.0]octane

1992 ◽  
Vol 70 (7) ◽  
pp. 2015-2021 ◽  
Author(s):  
Wolfgang Kliegel ◽  
Gottfried Lubkowitz ◽  
Steven J. Rettig ◽  
James Trotter
Keyword(s):  
Least Squares ◽  
Good Yield ◽  
Direct Methods ◽  
Structural Studies ◽  
Asymmetric Unit ◽  
Open Chain ◽  
Full Matrix ◽  
Unit Space ◽  
Boron Complex ◽  
Ethanol Yields

The reaction of N,N′-diethyl- N,N′-dihydroxymethanediamine with oxybis(diphenylborane) in absolute ethanol yields N-ethylhydroxylamine(O-B)1,7-diethyl-3,5-diphenyl-2,4,6-trioxa-7-aza-1-azonia-3-bora-5-boratabicyclo[3.3.0]octane [3-(1-oxa-2-azoniabutyl)-1,7-diethyl-3,5-diphenyl-2,4,6-trioxa-7-aza-1-azonia-3,5-diboratabicyclo[3.3.0]octane], 7b, in good yield. Crystals of this material are monoclinic, a = 16.396(2), b = 11.303(2), c = 22.898(4) Å, β = 92.78(1)°, Z = 8 (two molecules per asymmetric unit), space group P21/a. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.041 and Rw = 0.050 for 3602 reflections with I ≥ 3σ(I). The product 7b is formed by O→B coordination between N-ethylhydroxylamine and the bicyclic bis-phenylboronate of N,N′-diethyl-N,N′-dihydroxymefhanediamine. Compound 7b is only the second structurally characterized example of an N-alkylhydroxylamine(O-B)boron complex having an open-chain B,N-betaine structure. Bond lengths about boron are: B—O(N) = 1.467(4)–1.527(4), B—O(B) = 1.433(4)–1.451(4), B—N = 1.688(4) and 1.707(4), B—C = 1.586(4)–1.606(5) Å.

Sign in / Sign up

Export Citation Format

Share Document