Reactivity of electron-rich binuclear hydrides. Synthesis, structure, and reactions of [{(i-Pr)2PCH2CH2P(i-Pr)2}Rh]2(μ-H)(μ-OC6H5)

1986 ◽  
Vol 64 (1) ◽  
pp. 174-179 ◽  
Author(s):  
Michael D. Fryzuk ◽  
May-Ling Jang ◽  
Terry Jones ◽  
Frederick W. B. Einstein
Keyword(s):  
Single Crystal ◽  
Diffraction Study ◽  
Mononuclear Complex ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Fourier Methods ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonded

The reaction of phenol with the binuclear rhodium hydride [{(i-Pr)2PCH2CH2P(i-Pr)2}Rh]2(μ-H)2 generates [{(i-Pr)2PCH2CH2P(i-Pr)2}Rh]2(μ-H)(μ-OC6H5), 2, which was characterized by both solution spectroscopic techniques and a single crystal X-ray diffraction study. The structure was solved using Patterson and Fourier methods and refined to R = 0.019 (Rw = 0.027) for 6062 reflections; crystals of the compound are triclinic, space group [Formula: see text], with a = 9.018(2), b = 12.988(2), c = 17.558(3) Å, α = 99.42(1), β = 92.62(2), γ = 91.85(2)°, and Z = 2. Further reaction with excess phenol leads to the mononuclear complex (η5-C6H5O)Rh{(i-Pr)2PCH2CH2P(i-Pr)2}•2C6H5OH, which contains two phenol units hydrogen bonded to the oxygen of the η5-cyclohexy]dienylone ligand. The presence of the bridging phenoxide ligand in 2 results in reduced reactivity as compared to the starting binuclear hydride dimer.

Confacial bioctahedral complexes of tungsten(IV) containing tungsten-to-tungsten bonds: X-ray crystal structures of di-μ-ethanethiolato-μ-sulfidobis[dichloro(dimethyl sulfide)-tungsten(IV) (W—W)] and tetraphenylphosphonium di-μ-ethane thiolato-μ-sulfido- bis[trichlorotungstate(IV) (W—W)]

1982 ◽  
Vol 60 (11) ◽  
pp. 1333-1338 ◽  
Author(s):  
P. Michael Boorman ◽  
Penelope W. Codding ◽  
K. Ann Kerr ◽  
Kelly J. Moynihan ◽  
Vikram D. Patel
Keyword(s):  
Single Crystal ◽  
Bond Length ◽  
Diffraction Study ◽  
Crystal Structures ◽  
Dimethyl Sulfide ◽  
Heavy Atom ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The complex (Me2S)Cl2W(μ-S)(μ-SEt)2WCl2(Me2S), 1, has been prepared by reaction of [WCl4(Me2S)2] with 1 mol-equiv. of SiMe3(SEt) in CH2Cl2 solution. A single-crystal X-ray diffraction study shows that the molecule has a confacial bioctahedral structure with a W—W bond length of 2.526(2) Å. The structure was solved by heavy atom methods and refined to R = 0.061 and Rw = 0.061 for 2715 reflections with I ≥ 3σ(1). Crystals of 1 are triclinic, space group [Formula: see text], with a = 9.661(1), b = 10.695(1), c = 13.253(4) Å, α = 61.84(2), β = 66.98(2), and γ = 66.44(1)°, Z = 2.Reaction of 1with 2 mol-equiv. of Ph4PCl in CH2Cl2 solution yields (Ph4P)2[Cl3W(μ-S)(μ-SEt)2WCl3], 2. Crystals of 2 are triclinic, space group [Formula: see text], with a = 10.153(1), b = 13.043(1), c = 21.876(3) Å, α = 95.16(1), β = 96.48(2), and γ = 108.90(1)°, Z = 2. The structure was refined to R = 0.041, Rw = 0.048 for 2384 reflections with I ≥ 3σ(1); 2 also has a confacial bioctahedral structure with a W—W bond length of 2.522(1) Å.

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.

X-RAY DIFFRACTION STUDY OF THE MODULATED STRUCTURE IN SUPERCONDUCTING SINGLE-CRYSTAL Bi2Sr2CaCu2Oy

1988 ◽  
Vol 02 (08) ◽  
pp. 985-991 ◽  
Author(s):  
X. CHU ◽  
Z.H. MAI ◽  
Y.F. YAN ◽  
J.H. WANG ◽  
D.N. ZHENG ◽  
...  
Keyword(s):  
Experimental Data ◽  
Single Crystal ◽  
Diffraction Study ◽  
Basic Structure ◽  
X Ray Diffraction ◽  
Modulated Structure ◽  
Space Group ◽  
One Dimensional ◽  
X Ray ◽  
Average Structure

X-ray precession technique1 has been utilized to study the reciprocal space of the superconducting single crystal Bi 2 Sr 2 CaCu 2 O y. An average structure with space group of Pnnn and a real structure with the superspace group of [Formula: see text] or [Formula: see text] have been found for this one dimensional modulated incommensurate material. As well, a basic structure with the space group of Fmmm is derived from the experimental data.

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.

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 of Transition-Metal Sigma-Acetylides. V. Synthesis and X-Ray Structure of Co2(µ-η2-PhC2Fe(Co)2(η-C5h5))(Co)6

1986 ◽  
Vol 39 (1) ◽  
pp. 159 ◽  
Author(s):  
MI Bruce ◽  
DN Duffy ◽  
MG Humphrey
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Single Crystal ◽  
Diffraction Study ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Independent Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The reaction between Co2(CO)8 and Fe(C2Ph)(CO)2(η-C5H5) gave the title complex in 44% yield. The molecular structure was determined from a single-crystal X-ray diffraction study, and consists of the transition metal acetylide acting as a conventional μ- alkyne ligand to a Co2(CO)6 unit. Crystals are monoclinic, space group P21/n, with a 11.610(8), b 14.657(4), c 12.526(6)Ǻ, β 90.30(5)°, and Z 4; 1683 independent data were refined to R 0.080, Rw 0.087.

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.

Die Kristallstruktur des Tetraphenylphosphonium-Monoiodohexahydroc/ oso-Hexaborats [P(C6H5)4][B6H6I] / The Crystal Structure of Tetraphenylphosphonium Monoiodohexahydro-closo-hexaborate [P(C6H5)4][B6H6I]

1994 ◽  
Vol 49 (12) ◽  
pp. 1809-1812 ◽  
Author(s):  
W. Preetz ◽  
D. Sonnak
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

The crystal structure of [P(C6H5)4][B6H6I] has been determined by single crystal X-ray diffraction analysis; triclinic, space group P1 with a = 7.5137(9), b = 12.623(2), c = 13.6363(13) Å, α = 87.787(13)°, β = 83.836(13)°, γ = 88.156(10)°. The additional H atom could be refined with B-H distances of 1.13 to 1.31 A above one of the facettes of the B6 octahedron opposite to the I substituent.

scholarly journals Crystal Structures of Two Macrocyclic Bischalcones Possessing 26-Membered Rings

2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Rina Mondal ◽  
Nayim Sepay ◽  
Debajyoti Ghoshal ◽  
Asok K. Mallik
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Crystal Structures ◽  
Membered Ring ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonding Interactions

Single crystal X-ray diffraction of two macrocyclic bischalcones, namely, (2E,25E)-11,17,33,37-tetraoxapentacyclo[36.4.0.05,10.018,23.027,32]dotetraconta-1(42),2,5,7,9,18,20,22,25,27,29,31,38,40-tetradecaene-4,24-dione(1) and (2E,24E)-11,16,32,37-tetraoxapentacyclo[36.4.0.05,10.017,22.026,31]dotetraconta-1(42),2,5,7,9,17,19,21,24,26,28,30,38,40-tetradecaene-4,23-dione(2), each containing a 26-membered ring, has been studied. Compound 1 belongs to the monoclinic system, space group C2/c with a = 34.3615(9) Å, b = 12.7995(3) Å, c = 14.6231(3) Å, β = 96.912(2)°,  V = 6,384.6(3) Å3, and Z = 8. Compound 2 is triclinic, space group P-1 with a = 10.066(2) Å, b = 10.670(3) Å, c = 16.590(3) Å, α = 85.95(2), β = 89.244(14), γ = 62.211(13), V = 1572.0(6) Å3, and Z = 2. Intermolecular C–H⋯O hydrogen bonding interactions are present in both compounds.

Sign in / Sign up

Export Citation Format

Share Document