Structural and Solid-State 31P N.M.R. Studies on a Novel Fluorotris(triphenyl-phosphine)copper(I) Adduct

1991 ◽  
Vol 44 (3) ◽  
pp. 427 ◽  
Author(s):  
PC Healy ◽  
JV Hanna ◽  
JD Kildea ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Single Crystal ◽  
Copper Atom ◽  
Title Compound ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
Threefold Axis ◽  
X Ray ◽  
R Value

The synthesis of the title compound as its triphenylphosphine /methanol solvate, [(PPh3)3CuF].- 4PPh3.4MeOH, is reported together with characterization by solid-state 31P CP-MAS n.m.r. and single-crystal X-ray diffraction. Crystals are trigonal, space group P3, with a 14.453(5), c 15.388(6)Ǻ. The structure refined to a final R value of 0.049 for 1926 'observed' [I> 3σ(I)] reflections. The (PPh3)3CuF molecule lies on a crystallographic threefold axis. Cu-F is 2.115(9)Ǻ, and Cu-P 2.323(3)Ǻ. The solid-state 31P n.m.r. spectrum is dominated by peaks from each of the four solvated PPh3 molecules at -1.6, -5.4, -10.6 and -14.2 ppm with respect to 85% H3PO4. The quartet of lines arising from the ligands coordinated to the copper atom shows an average chemical shift of -5 ppm and approximately equal line spacings of 1.0 kHz.

Crystal structure of 2,4-Di-t-butyl-6-(3,5-di-t-butyl-2-hydroxyphenyl)-6-morpholinocyclohexa-2,4-dienone

1978 ◽  
Vol 31 (12) ◽  
pp. 2721 ◽  
Author(s):  
SR Hall ◽  
DG Hewitt ◽  
CL Raston ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Chemical Shift ◽  
Single Crystal ◽  
Least Squares ◽  
Structure Determination ◽  
Title Compound ◽  
X Ray Diffraction ◽  
X Ray

The crystal structure of the title compound, C32H49NO3, has been determined by single-crystal X-ray diffraction at 295(1) K and refined by least squares to a residual of 0.061 for 1721 'observed' reflections. Crystals are orthorhombic, Pcab, a 18.63(2), b 18.58(2), c 18.19(2) Ǻ, Z 8. The structure determination confirms that proposed on chemical grounds and shows an unusual t-butyl N.M.R. chemical shift to be a consequence of an unusual orientation.

Dimeres Di(N-lithium–tert–butylamino)bis(dimethylamino)silan - [Si(N(CH3)2)2(NLiC(CH3)3)2]2 – Darstellung und Kristallstruktur / Dimeric Di(N -lithio-tert-butylamino)bis(dimethylamino)silane - [Si(N(CH3)2)2(NLiC(CH3)3)2]2 – Synthesis und Crystal Structure

2001 ◽  
Vol 56 (1) ◽  
pp. 90-94 ◽  
Author(s):  
Josef Engering ◽  
Eva-Maria Peters ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Title Compound ◽  
Solution Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solution Nmr Spectroscopy

Abstract [Si(N(CH3)2)2(NLiC(CH3)3)2]2 results from the reaction of silicon tetrachloride with excess terf-butylamine, followed by halogen substitution with LiN(CH3)2, and treatment with n-butyllithium in hexane. The title compound, found to be dimeric in the solid state, was characterised by single crystal X-ray diffraction (triclinic, Pi , a = 10.208(2), b = 12.140(2), c = 15.658(3) Å , a = 79.02(3), ß = 82.80(3), γ = 67.19(3)°, Z = 2, C24H60Li4N8Si2 ), and by solid state and solution NMR-spectroscopy and mass spectrometry.

Crystal structure of Diaqua(1,10-phenanthroline)copper(II) sulfate

1984 ◽  
Vol 37 (5) ◽  
pp. 1111 ◽  
Author(s):  
PC Healy ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Copper Atom ◽  
Title Compound ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Axial Coordination ◽  
Square Planar

The crystal structure of the title compound, [Cu(OH2)2(phen)] (SO4) (phen = 1,10-phenanthroline), has been determined by single-crystal X-ray diffraction methods at room temperature, being refined by full matrix least-squares methods to a residual of 0.033 for 1445 'observed' reflections. Crystals are monoclinic, C2/c, a 14.883(8), b 13.843(9), c 7.019(4) �, β 108.60(4)�, Z 4. As in a number of other copper(II) and nickel(II) derivatives with (CuL4)(SO4) stoichiometry, the pseudo-square planar copper environments [Cu-N,O: 2.009(2), 1.970(2) � in the present case] are bridged through the two axial coordination positions by sulfate groups: O.SO2.O[Cu(OH2)2(phen)]O.SO2.0, etc. to give a linear polymeric array [Cu-O(SO4), 2.468(3) �]; a crystallographic twofold axis passes through the copper atom.

Preparation and Structure of Dibromobis(N,N-diethyldithiocarbamato)-thionitrosyltechnetium(III)

1991 ◽  
Vol 44 (8) ◽  
pp. 1125 ◽  
Author(s):  
J Baldas ◽  
SF Colmanet ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Trans Influence ◽  
R Value

The title compound, [Tc (NS)(S2CNEt2)2Br2], has been prepared by the reaction of [ TcN (S2CNEt2)2] with SOBr2, and its crystal structure has been determined by single-crystal X-ray diffraction methods at 23�1°C. Crystals are orthorhombic, space group Pnma , with a 14.864(7), b 15.857(7), c 8.938(4)Ǻ, and Z 4. Full-matrix least-squares refinement gave a final R value of 0.047 for 1685 independent reflections. The technetium atom is seven-coordinate with a distorted pentagonal- bipyramidal coordination geometry. The thionitrosyl ligand and a bromo ligand occupy the axial positions, with the thionitrosyl group exerting a small trans influence with Tc-Brtrans 2.595(1) and Tc-Brcis 2.564(1)Ǻ. The coordination of the thionitrosyl group is essentially linear with Tc -N=S 177.2(7)°, Tc -N 1.754(9), and N=S 1.504(9)Ǻ.

Solid-State 31P N.M.R. and Crystal Structure of Binuclear Di-μ-chloro-bis[(4-methylpyridine)(triphenyl-phosphine)copper(I)]

1991 ◽  
Vol 44 (5) ◽  
pp. 729 ◽  
Author(s):  
PC Healy ◽  
AK Whittaker ◽  
JD Kildea ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Chemical Shift ◽  
Single Crystal ◽  
Structure Determination ◽  
Molecular Fragment ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Tetrahedral Environment ◽  
Analogous Data

The 1 : 1 : 1 adduct of 4-methylpyridine (MeC5H4N), triphenylphosphine and copper(I) chloride has been synthesized, and characterized by solid-state 31P CP-MAS n.m.r. and a single-crystal X-ray structure determination. The structure determination reveals the presence of two crystallographically independent but pseudo-symmetrically related [(PPh3)(MeC5H4N) CuCl ]2 molecules in the unit cell, with the [(MeC5H4N) CuCl ]2 core and PPh3 ligands adopting different dispositions in each dimer. Crystals of the compound are triclinic, with space group Pī , a 16.884(5), b 14.898(4), c 9.501(3)Ǻ , α 104.28(2), β 89.95(2), γ 111.25(2)°. This structure refined to a final residual of 0.041 for 3022 'observed' [I> 3σ(I)] reflections. Cu- P,Cl,Cl,N are 2.196(2), 2.395(2), 2.402(3), 2.061(5)Ǻ for molecule 1 and 2.197(2), 2.420(2), 2.386(3), 2.061(5)Ǻ for molecule 2. The n.m.r. data show quartets arising from two crystallographically independent phosphorus atoms coupled to copper(I) atoms. The chemical shift difference between the quartets is 2.5 ppm. Line spacings of 1.546-1.746 kHz are indicative of [PPh3Cu]+ with the copper atoms in a tetrahedral environment. n.m.r. data have been recorded also for the analogous dimeric systems, [(PPh3)(RC5H4N) CuCl ]2 (R = H, 4-CN). Comparison of the n.m.r. data is made with analogous data for other compounds containing the [(PPh3)Cu]+ molecular fragment.

[Bis(3-methyl-2-thioxo-2,3-dihydro-1H-imidazolyl)borato-κ2 S,S′]dibromoindium(III)

2006 ◽  
Vol 62 (4) ◽  
pp. m702-m704 ◽  
Author(s):  
Sarah C. Hill ◽  
Daniel S. Jones ◽  
Daniel Rabinovich
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Bond Length ◽  
Title Compound ◽  
Bond Distance ◽  
Mirror Plane ◽  
X Ray Diffraction ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Distorted Tetrahedral Geometry

The structure of the title compound, [InBr2(C8H12N4BS2)], the first bis(mercaptoimidazolyl)borate (BmMe) complex of indium to be structurally characterized, has been determined by single-crystal X-ray diffraction. The four-coordinate In atom displays a distorted tetrahedral geometry in the solid state and is surrounded by the two thione groups of a BmMe ligand and two bromides, with an average In—Br bond distance of 2.494 Å. The presence of a crystallographically imposed mirror plane results in the observation of a unique In—S bond length of 2.4407 (11) Å.

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXI The Crystal and Molecular Structures of the Unsolvated Forms of Dibromotris(triphenylphosphine)dicopper(I) and 'step' Tetrabromotetrakis(triphenyl-phosphine)tetracopper(I)

1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Lewis Base ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.

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