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.

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.

Darstellung und Kristallstrukturanalyse von K3BiO3 und Rb3BiO3 / Synthesis and Crystal Structure Determination of K3BiO3 and Rb3BiO3

1997 ◽  
Vol 52 (9) ◽  
pp. 1031-1036 ◽  
Author(s):  
Nicola Zoche ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Single Crystal ◽  
Structure Determination ◽  
Solid State Reactions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Binary Compounds ◽  
First Time

K3BiO3 and Rb3BiO3 have been synthesized for the first time by solid state reactions of the respective binary compounds. K3BiO3 was obtained from Bi2O3 and K2O at 550 °C, Rb3BiO3 from Bi2O3 and Rb2O at 650 °C. The compounds were structurally examined by single-crystal X -ray investigations (K3BiO3: I 4̅ 3 m, a = 1070.15(2) pm, Z = 8; Rb3BiO3: P 21 3, a = 875.48(2) pm, Z = 4). The structures reveal “isolated” BiO33- groups. While K3BiO3 is isostructural to Na3BiO3, Rb3BiO3 has the same crystal structure as Cs3BiO3.

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.

Calcium Carbodiimide Compounds Revisited – Syntheses, Single Crystal Structure Determination and Vibrational Spectra of Ca11N6[CN2]2, Ca4N2[CN2] and Ca[CN2]

2008 ◽  
Vol 63 (5) ◽  
pp. 530-536 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Raman Spectrum ◽  
Single Crystal ◽  
Single Crystals ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
X Ray ◽  
Characteristic Features ◽  
Reported Data ◽  
Correct Data

Single crystals of Ca11N6[CN2]2 (dark red needles, tetragonal, P42/mnm (no. 136), a = 1456.22(5), and c = 361.86(2) pm, Z = 2), Ca4N2[CN2] (transparent yellow needles, orthorhombic, Pnma (no. 62), a = 1146.51(11), b = 358.33(4), and c = 1385.77(13) pm, Z = 4) and Ca[CN2] (transparent, colorless, triangular plates, rhombohedral, R3̅m (no. 166), a = 369.00(3), and c = 1477.5(3) pm, Z = 3) were obtained by the reaction of Na2[CN2], CaCl2 and Ca3N2 (if demanded by stoichiometry) in arc-welded Ta ampoules at temperatures between 1200 - 1400 K. Their crystal structures were re-determined by means of single crystal X-ray structure analyses. Additionally, the Raman spectra were recorded on these same single crystals, whereas the IR spectra were obtained with the KBr pellet technique. The title compounds exhibit characteristic features for carbodiimide units with D∞h symmetry (d(C-N) = 121.7 - 123.8 pm and ∡ (N-C-N) = 180°). The vibrational frequencies of these units are in the expected range (Ca11N6[CN2]2: νs = 1230, νs = 2008; δ = 673/645/624 cm−1; Ca4N2[CN2]: νs = 1230, νs = 1986; δ = 672/647 cm−1; Ca[CN2]: νs = 1274, νs = 2031, δ = 668 cm−1). The structural results are more precise than the previously reported data, and with the newly attained Raman spectrum of Ca11N6[CN2]2 we correct data reported earlier.

On the Origin of the Red Color of Aqueous-Solutions of 2,3-Dichloro-5,6-Dicyano-1,4-Benzoquinone (ddq). Crystal Structure of the Ammonium Salt of 2-Cyano-5,6-Dichloro-3-Hydroxy-1,4-Benzoquinone

1987 ◽  
Vol 40 (3) ◽  
pp. 625 ◽  
Author(s):  
HD Becker ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Structure Determination ◽  
Aqueous Ethanol ◽  
X Ray ◽  
Red Color ◽  
Hydrolysis Of

Hydrolysis of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone in aqueous ethanol gives the deep-red coloured ammonium salt of a monocyano-dichloro-monohydroxy-benzoquinone which crystallizes in the tetragonal space group I41 /a, a 20.832(5), c 8.618(2) �, Z 16. Single-crystal X-ray structure determination (R 0.036 for 1185 'observed' reflections) show the presence of ammonium cations forming hydrogen bonds in the lattice alternatingly with the tautomeric anion of 2-cyano-5,6-dichloro-3-hydroxy-1,4-benzoquinone and 3-cyano-5,6-dichloro-4-hydroxy-1,2-benzoquinone.

Kristallzucht und Strukturaufklärung von K2[Pt(CN)4Cl2], K2[Pt(CN)4Br2], K2[Pt(CN)4I2] und K2[Pt(CN)4Cl2] · 2H2O/ Crystal Growth and Crystal Structure Determination of K2[Pt(CN)4Cl2], K2[Pt(CN)4Br2], K2[Pt(CN)4I2] and K2[Pt(CN)4]Cl2] · 2H2O

2004 ◽  
Vol 59 (5) ◽  
pp. 567-572 ◽  
Author(s):  
Claus Mühle ◽  
Andrey Karpov ◽  
Jürgen Nuss ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Crystal Growth ◽  
Single Crystal ◽  
Structure Determination ◽  
Spectroscopy Data ◽  
Crystal Data ◽  
X Ray ◽  
Raman And Infrared Spectroscopy

Abstract Crystals of K2Pt(CN)4Br2, K2Pt(CN)4I2 and K2Pt(CN)4Cl2 ·2H2O were grown, and their crystal structures have been determined from single crystal data. The structure of K2Pt(CN)4Cl2 has been determined and refined from X-ray powder data. All compounds crystallize monoclinicly (P21/c; Z = 2), and K2Pt(CN)4X2 with X = Cl, Br, I are isostructural. K2Pt(CN)4Cl2: a = 708.48(2); b = 903.28(3); c = 853.13(3) pm; β = 106.370(2)°; Rp = 0.064 (N(hkl) = 423). K2Pt(CN)4Br2: a = 716.0(1); b = 899.1(1); c = 867.9(1) pm; β = 106.85(1)°; R(F)N′ = 0.026 (N’(hkl) = 3757). K2Pt(CN)4I2: a = 724.8(1); b = 914.5(1); c = 892.1(1) pm; β = 107.56(1)°; R(F)N′ = 0.025 (N’(hkl) = 2197). K2Pt(CN)4Cl2 ·2H2O: a = 763.76(4); b = 1143.05(6); c = 789.06(4) pm; β = 105.18(1)°; R(F)N′ = 0.021 (N’(hkl) = 2281). Raman and infrared spectroscopy data are reported.

Structural Properties of a Dimeric Phenylcyanamidocopper(I) Complex, [{Cu(PPh3)2(C6H5NCN)}2]

2000 ◽  
Vol 53 (12) ◽  
pp. 971 ◽  
Author(s):  
Eric W. Ainscough ◽  
Andrew M. Brodie ◽  
Peter C. Healy ◽  
Joyce M. Waters
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structural Properties ◽  
Structure Determination ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Cross Polarization ◽  
X Ray ◽  
Angle Spinning

The X-ray crystal structure determination of bis[-(phenylcyanamido)bis(triphenylphosphine)copper(I)], [{Cu(PPh3)2(C6H5NCN)}2], (1) is reported. The complex has a centrosymmetric dimeric structure with the phenylcyanamide ligands bridging the copper atoms in a -1,3-fashion. The structure is compared with that of the 4-methylphenylcyanamido complex, [{Cu(PPh3)2(4-MeC6H4NCN)}2] (2), and the differences observed in the Cu–P bond lengths compared with changes in the solid state 31P cross-polarization magic-angle spinning (CPMAS) spectra of the two complexes.

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