Studies of the synthesis, structure, and reduction of trans-dichloro bis(2,3-dihydro-4- and 7-methylbenzo[b]thiophene)palladium(II) complexes

1993 ◽  
Vol 71 (2) ◽  
pp. 199-205 ◽  
Author(s):  
Peter D. Clark ◽  
Martin J. Kirk ◽  
Massood Parvez
Keyword(s):  
Single Crystal ◽  
Molecular Hydrogen ◽  
Nmr Spectra ◽  
Hydrogen Donor ◽  
Ambient Conditions ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Sulfur Containing ◽  
C Nmr

trans-Dichlorobis(2,3-dihydro-4- and -7-methylbenzo[b]thiophene)palladium(II), 1b and 1c, have been prepared by reaction of 2,3-dihydro-4- and -7-methylbenzo[b]thiophenes with palladium(II) chloride. Both 1b and 1c exhibit complex 1H and 13C NMR spectra as a result of inversion of the sulfur-containing ligands. Their structures were confirmed by single crystal X-ray studies. 1b crystallized in the triclinic space group [Formula: see text] (a = 7.219(2), b = 8.441(5), c = 8.494(7) Å, α = 61.47(5)°, β = 88.85(4)°, γ = 84.40(3)°, and R = 0.067 for 1372 observed of 1760 unique reflections). 1c also crystallized in the triclinic space group [Formula: see text] (a = 7.730(3), b = 8.056(3), c = 8.516(4) Å, α = 62.87(3)°, β = 82.31(3)°, γ = 88.82(3)°, and R = 0,040 for 1425 observed of 1825 unique reflections), 1b and 1c and the complex 1a (prepared from 2,3-dihydrobenzo[b]thiophene) were unstable in the presence of molecular hydrogen at ambient conditions, liberating the parent dihydrobenzothiophenes and forming elemental palladium. 1a was also unstable to the organic hydrogen donor tetrahydronaphthalene, again forming Pd and 2,3-dihydrobenzothiophene. Complexes 1a–c were shown to promote the shift of CO/H2O to hydrogen and CO2 although most of the hydrogen was consumed by the reduction of Pd(II) to Pd0.

Bis[dicarbonyl(cyclopentadienyl)ruthenium(I)] Komplexe / Bis[dicarbonyl(cyclopentadienyl)ruthenium(I)] Complexes

2002 ◽  
Vol 57 (9) ◽  
pp. 1017-1026 ◽  
Author(s):  
Herbert Schumann ◽  
Susanne Stenz ◽  
Frank Girgsdies ◽  
Stefan H. Mühle
Keyword(s):  
Single Crystal ◽  
Nmr Spectra ◽  
X Ray ◽  
Tert Butyl ◽  
New Compounds ◽  
C Nmr

Ru3(CO)12 reacts with 1-tert-butyl-2,4-cyclopentadiene (1), 1-trimethylsilyl-2,4-cyclopentadiene (2), 1-tert-butyl-3-methyl-2,4-cyclopentadiene (3), 1,3-di(tert-butyl)-2,4-cyclopentadiene (4), 1-iso-propyl-2,3,4,5-tetramethyl-2,4-cyclopentadiene (5), 1-tert-butyl-2,3,4,5-tetramethyl- 2,4-cyclopentadiene (6), 1-phenyl-2,3,4,5-tetramethyl-2,4-cyclopentadiene (7), 2,5- diphenyl-2,4-cyclopentadiene (8), or 2,3,4,5-tetraphenyl-2,4-cyclopentadiene (9) with formation of the corresponding bis[dicarbonyl(cyclopentadienyl) ruthenium(I)] complexes [RuCp# (CO)2]2 1a to 9a. The 1H and 13C NMR spectra of the new compounds 3a and 5a to 9a as well as the single crystal X-ray structures of 1a, 4a, 5a, 7a, 8a, and 9a are reported and discussed

Zur Darstellung und Struktur des 1.3-Dichloro-5-N.N-dimethylamino-1.3-dithia-2.4.6-triazins / Synthesis and Structure of 1,3-Dichloro-5-N,N-dimethylamino-1,3-dithia-2,4,6-triazine

1983 ◽  
Vol 38 (3) ◽  
pp. 347-349 ◽  
Author(s):  
Herbert W. Roesky ◽  
Pierre Schäfer ◽  
Mathias Noltemeyer ◽  
George M. Sheldrick
Keyword(s):  
Structure Analysis ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cl Atoms ◽  
C Nmr

Abstract The six membered ring of composition (CH3)2NCN3S2Cl2 3 a was prepared from N,N-dimethylguanidinhydrochloride and trithiadiazindichloride. 3 a was characterized on the basis of mass, 1H, 13C NMR spectra and X-ray structure analysis. Crystals of 3 a are monoclinic, space group P21/c, with a = 660.3(6), b = 834.5(7), c = 1774.7(15) pm, β = 112.83(6)° and Z = 4. The C2N unit lies approximately in the plane of the [-CNSNSN-] ring, with both Cl atoms on the same side of the ring.

One-dimensional ribbons of solvated Ag sulfonates

1999 ◽  
Vol 77 (3) ◽  
pp. 313-318 ◽  
Author(s):  
George KH Shimizu ◽  
Gary D Enright ◽  
Gabriela S Rego ◽  
John A Ripmeester
Keyword(s):  
Coordination Polymer ◽  
Single Crystal ◽  
The Other ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Structure Determinations

Single crystal X-ray structure determinations of two solvated silver sulfonates have been obtained and these compounds have been shown to adopt infinite one-dimensional motifs. {AgOTs(MeCN)}[Formula: see text] (OTs = p-toluenesulfonate) crystallizes in the monoclinic space group, P21, a = 8.4278(5) Å, b = 5.7413(3) Å, c = 12.1057(7) Å, β = 109.24(1)°. {Ag(NDSA)(MeCN)2(H3O)(H2O)2}[Formula: see text] (NDSA = 1,5-naphthalenedisulfonate) crystallizes in the triclinic space group, P[Formula: see text], a = 8.3407(4) Å, b = 10.4374(5) Å, c = 12.3399(6) Å, α = 101.941(8)°, β = 109.24(1)°, γ = 102.190(8)°. Despite one compound containing a monosulfonate and the other a disulfonate, both complexes form infinite one-dimensional arrays.Key words: silver, sulfonates, coordination polymer.

Crystal Structure and Spectroscopic Behaviour of a Binuclear Copper(II) Complex of Mefenamic Acid and Dimethylsulfoxide

1998 ◽  
Vol 53 (8) ◽  
pp. 871-874 ◽  
Author(s):  
G. Facchin ◽  
M. H. Torre ◽  
E. Kremer ◽  
O. E. Piro ◽  
E. J. Baran
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Mefenamic Acid ◽  
Electronic Spectra ◽  
Anthranilic Acid ◽  
Binuclear Copper ◽  
Triclinic Space Group ◽  
Spectroscopic Behaviour ◽  
Space Group ◽  
X Ray

Abstract The crystal structure of the binuclear Cu(II) complex [Cu(mef)2DMSO]2 (mef = deprotonated N-2,3-dimethylphenyl-anthranilic acid; DMSO = dimethylsulfoxide) has been determined by single-crystal X-ray diffractometry. It crystallizes in the triclinic space group P1̄ with Z = 1. IR and electronic spectra of the compound are also discussed briefly.

Synthesis and structural characterization of donor-stabilized disubstituted diphenyldithiophosphates of nickel(II)

2014 ◽  
Vol 70 (4) ◽  
pp. 761-767 ◽  
Author(s):  
Sandeep Kumar ◽  
Ruchi Khajuria ◽  
Amanpreet Kaur Jassal ◽  
Geeta Hundal ◽  
Maninder S. Hundal ◽  
...  
Keyword(s):  
Single Crystal ◽  
Chelate Ring ◽  
Donor Ligands ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Donor-stabilized addition complexes of nickel(II) with disubstituted diphenyldithiophosphates, [{(ArO)2PS2}2NiL2] {Ar = 2,4-(CH3)2C6H3[(1), (5)], 2,5-(CH3)2C6H3[(2), (6)], 3,4-(CH3)2C6H3[(3), (7)] and 3,5-(CH3)2C6H3[(4), (8)];L= C5H5N [(1)–(4)] and C7H9N [(5)–(8)]}, were successfully isolated and characterized by elemental analysis, magnetic moment, IR spectroscopy and single-crystal X-ray analysis. Compound (4) crystallizes in the monoclinic space groupP21/nwhereas compounds (7) and (8) crystallize in the triclinic space group P\bar 1. The single-crystal X-ray diffraction analysis of (4), (7) and (8) reveals a six-coordinated octahedral geometry for the NiS4N2chromophore. Two diphenyldithiophosphate ions act as bidentate ligands with their S atoms coordinated to the Ni centre. Each of them forms a four-membered chelate ring in the equatorial plane. The N atoms from two donor ligands are axially coordinated to the Ni atom.

Metallaborane Reaction Chemistry. Part 3. Reaction of Carbon Monoxide with [6-H-6-(PPh3)-6P,5C-μ-(2-Ph2PC6H4)-nido-6-IrB9H12] and the Isolation and Characterisation of Two arachno-6-Monoiridadecaboranes [6-(CO)-6-H-6,9-(PPh3)2-6P,5C-μ-(2-Ph2PC6H4)-arachno-6-IrB9H11] and sym-[6-(CO)-6-H-6,6-(PMe2Ph)2-9-(PPh3)-arachno-6-IrB9H11]

1997 ◽  
Vol 62 (8) ◽  
pp. 1239-1253 ◽  
Author(s):  
Jonathan Bould ◽  
Paul Brint ◽  
John D. Kennedy ◽  
Mark Thornton-Pett ◽  
Lawrence Barton ◽  
...  
Keyword(s):  
Carbon Monoxide ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Reaction System ◽  
Structural Type ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

[6-(CO)-6-H-6,9-(PPh3)2-6P,5C-μ-(2-Ph2PC6H4)-arachno-6-IrB9H11] (1) results from the reaction of [6-H-6-(PPh3)-6P,5C-μ-(2-Ph2PC6H4)-nido-6-IrB9H12] (2) with carbon monoxide in refluxing benzene. It is characterised by NMR spectroscopy and by single-crystal X-ray diffraction analysis. Crystals were triclinic, space group P1, with a = 10.688(2), b = 13.114(3), c = 22.356(5) Å, α = 78.33(2), β = 89.482(10), γ = 70.884(12)°, and Z = 2. The compound is of the little-examined arachno ten-vertex metallaborane structural type. A second compound of this type, [6-(CO)-6-H-6,6-(PMe2Ph)2-9-(PPh3)-arachno-6-IrB9H11] (3), isolated from a reaction system involving [Ir(CO)Cl(PPh3)2], PMe2Ph and the [nido-B9H12]- anion, has also been characterised crystallographically. Crystals were triclinic, space group P1, with a = 10.389(1), b = 10.511(1), c = 19.699(3) Å, α = 75.03(1), β = 85.53(1), γ = 74.88(1)°, and Z = 2.

Beiträge zur Strukturchemie phosphorhaltiger Ketten und Ringe, XIII [1]. Die Molekül- und Kristallstruktur von 3,4,9,10-Tetraisopropylpentacyclo[ 6.4.0.02,6.05,12.07,11]dodecaphosphan, P12(i-Pr)4 / Structural Chemistry of Phosphorus-Containing Chains and Rings, XIII [1]. The Molecular and Crystal Structure of 3,4,9,10-Tetraisopropylpentacyclo[6.4.0.02,6.05,12.07,11]dodecaphosphane, P12(iPr)4

1986 ◽  
Vol 41 (5) ◽  
pp. 548-552 ◽  
Author(s):  
Karl-Friedrich Tebbe ◽  
Magda Fehér
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structural Unit ◽  
Structural Chemistry ◽  
Molecular And Crystal Structure ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Phosphorus Containing

Abstract The structure of P12(iPr)4, C12H28P12 , has been determined by single crystal X-ray techniques (Rf = 0.026, wRf = 0.029 for 3549 observed reflections with |Fo| ≥ 4σ(Fo)). The compound crystallizes in the triclinic space group P1 with a = 879.8, b = 1088.5, c = 1414.1 pm, α = 93.01, β - 107.61, γ = 92.92° and Z = 2. The molecule contains a polycyclic P12-unit of nearly C2v symmetry, which represents an essential structural unit of Hittorf’s phosphorus.

Structural Systematics of Metal Acetylide Complexes. II. X-Ray Studies of Some Nickel σ-Acetylide Complexes

1998 ◽  
Vol 51 (3) ◽  
pp. 219 ◽  
Author(s):  
Ian R. Whittall ◽  
Mark G. Humphrey ◽  
David C. R. Hockless
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Trans Influence

The structures of Ni(C≡CR)(PPh3)(η-C5H5) (R = Ph (1), C6H4-4-NO2 (2), 4-C6H4C6H4-4′-NO2 (3), (E)-4-C6H4CH=CHC6H4-4′-NO2 (4), 4-C6H4C≡CC6H4-4′-NO2 (5), 4-C6H4N=CHC6H4-4′-NO2 (6)) have been determined by single-crystal X-ray diffraction studies, refining by full-matrix least-squares analysis. For (1), crystals are triclinic, space group P-1, with a 10·094(2), b13·429(3), c 18·835(5) Å,α 103·24(2), β 91·50(2), γ 90·10(2)°, Z 4, 5844 unique reflections (595 parameters), converging at R 0·033 and Rw 0·024. For (2), crystals are orthorhombic, space group Pna21, with a 16·799(2), b 8·681(2), c 17·485(2) Å, Z 4, 1774 unique reflections (325 parameters), converging at R 0·031 and Rw 0·029. For (3), crystals are monoclinic, space group P 21/c, with a 11·140(3), b 18·282(4), c 15·296(2) Å, β 105·18(2)°, Z 4, 3132 unique reflections (397 parameters), converging at R 0·039 and Rw 0·024. For (4), crystals are monoclinic, space group P 21/n, with a 12·929(7), b 16·953(8), c 15·601(7) Å, β 112·55(3), Z 4, 3023 unique reflections (397 parameters), converging at R 0·039 and Rw 0·025. For (5), crystals are monoclinic, space group P 21/n, with a 12·710(5), b 16·882(3), c 15·693(4) Å, β 111·37(3)°, Z 4, 3216 unique reflections (397 parameters), converging at R 0·035 and Rw 0·030. For (6), crystals are monoclinic, space group P 21/n, with a 12·594(1), b 16·936(2), c 15·611(1) Å, β 112·476(5)°, Z 4, 3564 unique reflections (397 parameters), converging at R 0·038 and Rw 0·041. For structurally characterized 18-electron (cyclopentadienyl)nickel(II) acetylide complexes, statistically insignificant decreases in the average Ni-C(1) distance and trans influence and an increase in the average C(1)-C(2) parameter are observed on introduction of an acceptor substituent at the alkynyl ligand.

Reactions between Co(II), 1,2-bis(diphenylphosphino)ethane, and NaBH3CN in the presence and absence of CO. The crystal structure of bis(cyanotrihydroborato)tetrakis(N,N-dimethylformamide)cobalt(II)

1988 ◽  
Vol 66 (7) ◽  
pp. 1770-1775 ◽  
Author(s):  
David J. Elliot ◽  
Sanna Haukilahti ◽  
David G. Holah ◽  
Alan N. Hughes ◽  
Stanislaw Maciaszek ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
R Factor

Reactions between Co(II), Diphos, and NaBH3CN lead to Co(BH3CN)2(Diphos)2, 1, or [Co(BH3CN)(Diphos)2]X, 2 (X = ClO4 or BPh4), and, in certain solvents, 2 reacts to produce [Co(CN)(Diphos)2](ClO4). Compound 1 can be reversibly converted to Co(BH3CN)2(DMF)4, 4, via Co(BH3CN)2(Diphos)(DMF). In addition, 1 reacts with CO to form the Co(I) and Co(III) compounds [Co(Diphos)2](CO)]X and [Co(Diphos)2(CN)2]X (X = BH3CN or BPh4). Single crystal X-ray diffraction studies of 4 show that the compound crystallizes in the triclinic space group [Formula: see text], with unit cell parameters a = 7.572(6), b = 9.695(6), c = 9.395(6) Å, α = 81.06(4), β = 68.46(5), γ = 68.19(5)°, V = 595.5 Å3, Z = 1, and dcalcd = 1.202 g cm−3. The structure converged to a conventional R factor of 0.040 for 2841 observations and showed an octahedral arrangement of four O atoms from DMF molecules and two trans N-bound BH3CN groups around the Co(II) center.

scholarly journals Synthesis, Crystal Structure, and Fungicidal Activity of 5-(4-cyclopropyl-5-((3-fluorobenzyl)thio)-4H-1,2,4-triazol-3-yl)-4-methyl-1,2,3-thiadiazole

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Xing-Hai Liu ◽  
Jian-Quan Weng ◽  
Cheng-Xia Tan
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Fungicidal Activity ◽  
Herbicidal Activity ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Compound C

A new 1,2,3-thiadiazole compound was synthesized and characterized. The crystal structure of the title compound (C15H14FN5S2, Mr = 347.43) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P-1 witha=7.0490(14),b=9.0212(18),c=12.799(3) Å,α= 89.97(3)°,β= 82.27(3)°,γ= 73.17(3)°,V= 771.3(3)  Å3, Z = 2, F(000) = 360, Dc = 1.496 g/cm3,μ= 0.036 mm−1, the finalR1= 0.0358, andwR2= 0.0986 for 2204 observed reflections withI>2σ(I). A total of 5697 reflections were collected, of which 2719 were independent (Rint=0.0028). The herbicidal activity of title compound was determined; the results showed that the title compound displayed excellent fungicidal activity.

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