(CH3)3CCOOSbCl4: Structure Determination by Zeeman Perturbed NQR

1986 ◽  
Vol 41 (1-2) ◽  
pp. 129-133 ◽  
Author(s):  
Maria L. S. Garcia ◽  
Edwin A. C. Lucken
Keyword(s):  
Molecular Structure ◽  
Magnetic Field ◽  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Organic Ligand ◽  
Coupling Constants ◽  
Zero Field ◽  
Quadrupole Coupling ◽  
Asymmetry Parameters

A single crystal of tetrachloro(0,0-pivaloylato)antimony(V) has been studied at 77 K, byZeeman perturbed 35Cl NQR, using a FT-NQR pulsed spectrometer. The four lines at zero-field, ν1 = 27.6468, ν2= 27.3070, ν3= 25.7341 and ν4= 25.3438 MHz yield eight EFG tensors in themagnetic field, related by a twofold symmetry element in the crystal. The correspondingasymmetry parameters are η1, = 0.134, η2 = 0.13, η3= 0.07, and η4 = 0.09. The molecular structurededuced from the relative orientations of the principal Z-axes of the EFG tensors confirms that thehigher quadrupole coupling constants are associated with the chlorine atoms in equatorial positions,relative to the plane of the organic ligand, as predicted from NQR powder studies. It is concludedthat the crystal structure is monoclinic with two (class m or 2) or four (class 2/m) moleculesper unit cell. The molecular packing is such that the planes formed by equatorial or axial chlorineatoms are approximately at right angles to their symmetry related images.

scholarly journals Hydrogen Bond Studies. 125. A Deuteron Magnetic Resonance Study of Strontium Formate Dihydrate, Sr(HCOO)2 · 2D2O

1977 ◽  
Vol 32 (9) ◽  
pp. 1025-1029 ◽  
Author(s):  
Bo Berglund ◽  
Jörgen Tegenfeldt
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Magnetic Resonance ◽  
Electric Field Gradient ◽  
Room Temperature ◽  
Coupling Constants ◽  
Water Molecules ◽  
Magnetic Resonance Study ◽  
Quadrupole Coupling ◽  
Asymmetry Parameters

AbstractA room temperature (25 °C) deuteron magnetic resonance (DMR) study of a single crystal of Sr (HCOO)2 · 2 D2O is reported. Signals from all water molecules in the unit cell have been detected, and all four independent electric field gradient (EFG) tensors at the water deuterons have been determined from 409 quadrupole splittings. All spectra were recorded by rotating the crystal about one arbitrarily selected axis. The following quadrupole coupling constants and asymmetry parameters for the deuterons were obtained: 213.5(4), 189.3(4), 195.7(4) and 200.7(5) kHz and 0.117(3), 0.110(4), 0.116(4) and 0.098(3). The directions of the eigenvalues are qualitatively consistent with the crystal structure refined by Galigné 1; the result is in disagreement, however, with the earlier DMR study of Sr (DCOO)2 · 2 D2O (Reference 2).

Kristallstruktur und molekulare Dynamik eines Stereoisomeren von (P,P′,P″,P‴-Tetraphenyl)-1,1,2,2-ethantetrakisphosphinsäuretetraisopropylester / Crystal Structure and Molecular Dynamics of a Stereoisomer of (P,P′,P″,P‴-Tetraphenyl)-1,1,2,2-ethane-tetraphosphinic Acid Tetraisopropylester

1992 ◽  
Vol 47 (5) ◽  
pp. 725-731 ◽  
Author(s):  
Gerhard Hägele ◽  
Peter Reinemer ◽  
Michael Batz ◽  
Dietrich Mootz
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Molecular Dynamics ◽  
Single Crystal ◽  
Spectroscopic Data ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Structural Data ◽  
Coupling Constants ◽  
Type Relation

The crystal and molecular structure of (P,P′,P″,P‴-tetraphenyl)-1,1,2,2-ethane-tetraphosphinic acid tetraisopropylester has been determined from single-crystal MoKa diffractometer data. The crystals are monoclinic with space group C 2/c, Ζ = 4, a = 2054.5(9), b = 1189.8(5), c = 1800.8(8) pm, β = 110.07(3)°. The structure was solved by direct methods and refined to R = 0.046. A 250 ps-vacuo-trajectory was calculated using the Molecular Dynamics program GROMOS. Structural data and MD results are compared to NMR spectroscopic data. A Karplus-type relation was confirmed for coupling constants 3JPP.

NUCLEAR MAGNETIC RESONANCE SPECTRUM OF B11 IN KERNITE

1955 ◽  
Vol 33 (5) ◽  
pp. 156-175 ◽  
Author(s):  
H. H. Waterman ◽  
G. M. Volkoff
Keyword(s):  
Magnetic Field ◽  
Coupling Constants ◽  
Monoclinic Crystal ◽  
X Ray ◽  
Principal Axes ◽  
Quadrupole Coupling ◽  
Radio Frequency Spectrum ◽  
Asymmetry Parameters ◽  
Crystallographic Axes ◽  
The Magnetic Field

The radio-frequency spectrum of B11 in a single crystal of Na2B4O7∙4H2O (kernite) is examined experimentally as the monoclinic crystal is rotated in an external magnetic field of 7060 gauss in turn about each of three axes (b, c crystallographic axes, and a third perpendicular direction) held normal to the magnetic field. A maximum of 21 lines (some of which show small additional splitting) is observed, which reduces to 11 when the b symmetry axis is perpendicular or parallel to the magnetic field. The results are interpreted in terms of four essentially non-equivalent B11 sites in kernite characterized respectively by quadrupole coupling constants [Formula: see text], 0.588 ± 0.003, 2.563 ± 0.007, 2.567 ± 0.010 Mc./sec, and asymmetry parameters 77 [Formula: see text], 0.60 ± 0.02, 0.163 ± 0.010, 0.116 ± 0.010. The orientations of the principal axes of the four [Formula: see text] tensors are also determined. These observations on boron are consistent with previous X-ray results, but preliminary observations on Na23 in kernite contradict previous X-ray position assignments.

scholarly journals The Bond Sn-Cl in SnIV Complex Salts A2 [(C2H5 )SnCl 5]. A Single Crystal 35Cl NQR Study of Bis(methylammonium)- pentachloroethylstannate, (CH3NH3 )2](C2H5 )SnCl5]

1990 ◽  
Vol 45 (3-4) ◽  
pp. 229-236 ◽  
Author(s):  
Peter Storck ◽  
Norbert Weiden ◽  
Alarich Weiss
Keyword(s):  
Single Crystal ◽  
Charge Distribution ◽  
Coupling Constants ◽  
General Tendency ◽  
Quadrupole Coupling ◽  
35Cl Nqr ◽  
Complex Salts ◽  
The Asymmetry ◽  
Asymmetry Parameters

AbstractZeeman 35Cl NQR spectroscopy has been applied to determine the magnitude and orientation of the EFG tensors at the chlorine sites in a single crystal of(CH3NH3)2[(C2H5)SnCl5] at 293 K. The assignment of the NQR frequencies vi(35Cl), the corresponding quadrupole coupling constants eQΦ(i)zz h-1 , and the asymmetry parameters ηi(35Cl) to certain Cl(k) atoms is discussed. The most probable assignment is (no. i of vi(35Cl), vi(35Cl)/MHz, eQΦ(i)zz h-1 / MHz ηi, (35Cl), no. k of assigned Cl(k), d(Sn-Cl(k) )/pm, ∢ (Φ(i)zz , d(Sn-Cl(k) )) :i = 1,17.032, 34.046,0.056, k= 1, 242.6, 3.1°; i = 2, 12.072, 24.089, 0.117, k = 3, 250.7, 1.9°; i = 3, 11.537, 22.992, 0.146, k = 2, 253.1, 2.8°; i = 4, 10.770, 21.455, 0.154, k = 4, 249.7, 2.9 °; i = 5,9.969,19.842,0.171, k=5,254.9,1.7°. The orientation of the tensor axes Φ(i)jj , j = x, y, z,i= 1 - 5 , in space is mainly determined by the geometry of the [(C2H5)SnCl5]2⊖ anion. The Φ(i)zz are nearly parallel to the assigned bond directions Sn-Cl(k) · η (35CI) is low, increasing with decreasing v(35Cl). The reason for the asymmetry seems not to be a π-character in the Sn-Cl bond, but the charge distribution within the anion. The rule that a longer bond corresponds to a lower NQR frequency is valid as a general tendency, but not strict.

scholarly journals Crystal Structure Refinement and Single Crystal 81Br Zeeman NQR Study of KHgBr3· H2O

1996 ◽  
Vol 51 (12) ◽  
pp. 1197-1202 ◽  
Author(s):  
Hiromitu Terao ◽  
Tsutomu Okuda ◽  
Sachiyo Uyama ◽  
Hisao Negita ◽  
Shi-qi Dou ◽  
...  
Keyword(s):  
Single Crystal ◽  
Room Temperature ◽  
Structure Refinement ◽  
Zeeman Effect ◽  
Coupling Constants ◽  
X Ray ◽  
Quadrupole Coupling ◽  
Nuclear Quadrupole ◽  
Asymmetry Parameters ◽  
Good Agreement

Abstract Three 81Br NQR resonance lines of KHgBr3 ·H2O were detected between 77 K and room temperature. From the Zeeman effect measurement on a single crystal the nuclear quadrupole coupling constants (e2qQ/h) and the asymmetry parameters (ƞ) were obtained, which are 228.42 MHz and 0.005, 226.24 MHz and 0.005, and 108.76 MHz and 0.465 for e2qQ/h and ƞ at 295 K, respectively. Large deviations of the observed directions of electric field gradient tensors from the directions expected from previous X-ray results have been found. With the present X-ray redetermination, 81Br NQR and structure are in good agreement. The structure and bonding in the compound are discussed.

The C—CI Bonds in α -2,4,6-tris(trichIoromethyl)-1,3,5-trioxane, α -Parachloral, (Cl3CCHO)3. A 35Cl-NQR Single Crystal Study

1985 ◽  
Vol 40 (4) ◽  
pp. 324-334 ◽  
Author(s):  
Masao Hashimoto ◽  
Norbert Weiden ◽  
Alarich Weiss
Keyword(s):  
Single Crystal ◽  
Coupling Constants ◽  
X Ray Diffraction ◽  
X Ray ◽  
Principal Axes ◽  
Quadrupole Coupling ◽  
35Cl Nqr ◽  
Single Crystal Study ◽  
Nuclear Quadrupole ◽  
Asymmetry Parameters

By single crystal 35C1-NQR Zeeman spectroscopy, the five independent 35Cl nuclear quadrupole coupling tensors in a-parachloral, (Cl3CCHO)3, have been studied at 24 ± 2 °C. The directions of the electric field gradient (EFG) tensor components have been determined. The principal axes Φ are within ± 0.8° parallel to the C-Cl bond directions found by X-ray diffraction. Very small asymmetry parameters in the range 0.002 ≦ η ≦ 0.046 are characteristic for the EFG tensors of chlorine atoms bound to carbon atoms in aliphatic systems. The five nuclear quadrupole coupling constants are in the range 76.752 ≦ e2qQh-1/MRz ≦ 78.155. The orientation of the principal axes Φxx and Φyy can be correlated to the molecular structure.

scholarly journals Molekül- und Kristallstruktur von 1.1-Dimethylsilylentitanocendichlorid, (CH3)2Si(C5H4)2TiCl2 / Molecular and Crystal Structure of l,r-Dimethylsilylene Titanocene Dichloride, (CH3)2Si(C5H4)2TiCl2

1981 ◽  
Vol 36 (10) ◽  
pp. 1208-1210 ◽  
Author(s):  
Hartmut Köpf ◽  
Joachim Pickardt
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structure Determination ◽  
Titanocene Dichloride ◽  
Molecular And Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Space Group ◽  
X Ray ◽  
Structural Dimensions

Abstract The molecular structure of the bridged [1]-titanocenophane 1,1'-dimethylsilylene titanocene dichloride, (CH3)2Si(C5H4)2TiCl2, has been investigated by an X-ray structure determination. Crystal data: monoclinic, space group C2/c, Z = 4, a = 1332.9(3), 6 = 988.7(3), c = 1068.9(3) pm, β = 113.43(2)°. The results are compared with the structural dimensions of similar compounds: 1,1'-methylene titanocene dichloride, CH2(C5H4)TiCl2, with the unbridged titanocene dichloride, (C5H5)2TiCl2 and the ethylene-bridged compound (CH2)2(C5H4)2TiCl2

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

Wechselwirkungen in Molekülkristallen, 160 [1,2]. Kristallzüchtung und Strukturbestimmung der verschiedenartigen Polyphenyl-Kontaktionenmultipel [p-Quaterphenylee⊖⊖][Na⊕(DME)3]2, [p-Quaterphenyl⊖⊖(Na⊕(THF)3)2] und [p-Terphenyl⊖⊖Na⊕(DME)2Na⊕(DME)]2 / Interaction in Molecular Crystals, 160 [1, 2]. Crystallization and Structure Determination of the Different Polyphenyl Contact Ion Multiples [p-Quaterphenylee⊖⊖][Na⊕(DME)3]2, [p-Quaterphenyl⊖⊖(Na⊕(THF)3)2] und [p-Terphenyl⊖⊖Na⊕(DME)2Na⊕(DME)]2

2000 ◽  
Vol 55 (12) ◽  
pp. 1103-1113 ◽  
Author(s):  
Hans Bock ◽  
K. Gharagozloo-Hubmann ◽  
M. Sievert
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Sodium Salt ◽  
Structure Determination ◽  
Metal Cation ◽  
Molecular Crystals ◽  
Sodium Salts ◽  
Structure Determinations ◽  
Cation Coordination

The π-hydrocarbons p-terphenyl and p-quaterphenyl are reduced to their dianions in aprotic solutions of different ethers at sodium metal mirrors. Single crystal structure determinations of the solvent-separated or solvens-shared contact ion multiples, [p-terphenyl⊖⊖ Na⊕(DME)2Na⊕DME]2, p-quaterphenyl⊖⊖ ][Na⊕(DME)3]2 and [p-quaterpheny⊖⊖( Na⊕(THF)3)2], prove the essential cation solvation by the chelating dimethoxyethane (DME) versus the bulky tetrahydrofuran (THF) ligands: The solution network of equilibria between solvent separated and solvent shared ion aggregates can be considerably and transparently modified by the ether solvent selected. In addition, the structures of the monomeric sodium salts reveal partly novel details of metal cation coordination by contacts Na⊕ ··· O as well as Na⊕ ··· Cπ such as in the dimeric sodium salt of p-terphenyl dianion, [(DME)2Na⊕ (terphenyl⊖⊖)(Na⊕ DME)(terphenyl⊖⊖)Na⊕ (DME)2].

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.

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