Alkaline Earth Metal Organoamide Complexes Displaying Close Ae–F(C) (Ae = Ca, Mg) Interactions

2013 ◽  
Vol 66 (10) ◽  
pp. 1288 ◽  
Author(s):  
Glen B. Deacon ◽  
Peter C. Junk ◽  
Rory P. Kelly
Keyword(s):  
Crystal Structures ◽  
1H Nmr ◽  
Low Temperatures ◽  
Nmr Spectra ◽  
Alkaline Earth ◽  
Earth Metal ◽  
1H Nmr Spectra ◽  
Alkaline Earth Metal ◽  
X Ray ◽  
Bond Lengths

Protolysis of [Ca{N(SiMe3)2(thf)2] (thf = tetrahydrofuran) with the N,N-dialkyl-N′-2,3,5,6-tetrafluorophenylethane-1,2-diamines, p-HC6F4NH(CH2)2NR2 (LRH; R = Me or Et), yields [Ca(p-HC6F4N(CH2)2NR2)2(thf)2], whilst protolysis of di-n-butylmagnesium by the same amines yields [Mg(p-HC6F4N(CH2)2NR2)2] complexes. X-Ray crystal structures show that the calcium derivatives contain eight-coordinate calcium atoms, with tridentate (N,N′,o-F) coordination of the organoamide ligands and cisoid thf donors. It is noteworthy that the Ca–F(C) bond lengths are shorter than the Ca–NR2 bond lengths. By contrast, magnesium forms centrosymmetric, six-coordinate, homoleptic complexes, in which the Mg–NR2 bond lengths are shorter than the Mg–F(C) bond lengths. 19F{1H} NMR spectra of the R = Me complexes support retention of Ae–F(C) linkages in solution at low temperatures. Heating the complexes for a prolonged period in C6D6 at 80°C showed no evidence of C–F activation reactions.

scholarly journals Mixed ligand complexes of alkaline earth metals: Part XII. Mg(II), Ca(II), Sr(II) and Ba(II) complexes with 5-chlorosalicylaldehyde and salicylaldehyde or hydroxyaromatic ketones

2002 ◽  
Vol 67 (4) ◽  
pp. 229-234 ◽  
Author(s):  
R.N. Prasad ◽  
M. Agrawal ◽  
M. Sharma
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Alkaline Earth ◽  
Earth Metal ◽  
Mixed Ligand ◽  
Alkaline Earth Metals ◽  
1H Nmr Spectra ◽  
Mixed Ligand Complexes ◽  
Alkaline Earth Metal ◽  
Metal Chlorides

The reactions of alkaline earth metal chlorides with 5-chlorosalicylaldehyde and salicylaldehyde, 2-hydroxyacetophenone or 2-hydroxypropiophenone have been carried out in 1: 1: 1 mole ratio and the mixed ligand complexes of the type MLL?(H2O)2 (where M = Mg(II), Ca(II), Sr(II) and Ba(II),HL= 5-chlorosalicylaldehyde and HL?= salicylaldehyde, 2-hydroxyacetophenone or 2-hydroxypropiophenone) have been isolated. These complexes were characterized by TLC, conductance measurements, IR and 1H-NMR spectra.

Synthesis and X-ray crystal structures of two new alkaline-earth metal borates: SrBO2(OH) and Ba3B6O9(OH)6

2002 ◽  
pp. 2031-2035 ◽  
Author(s):  
Zhen-Tao Yu ◽  
Zhan Shi ◽  
Wei Chen ◽  
Yu-Sheng Jiang ◽  
Hong-Ming Yuan ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Alkaline Earth ◽  
Earth Metal ◽  
Alkaline Earth Metal ◽  
X Ray

scholarly journals Syntheses and Crystal Structures of the New Ternary Barium Halide Hydrides Ba2H3X (X = Cl or Br)

2007 ◽  
Vol 62 (1) ◽  
pp. 23-27 ◽  
Author(s):  
Olaf Reckeweg ◽  
Jay C. Molstad ◽  
Scott Levy ◽  
Francis J. DiSalvo
Keyword(s):  
Stainless Steel ◽  
Crystal Structures ◽  
Alkaline Earth ◽  
Metal Hydrides ◽  
Earth Metal ◽  
Solid State Reactions ◽  
Alkaline Earth Metal ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Compounds

Single crystals of the isotypic hydrides Ba2H3X (X = Cl or Br) were obtained by solid-state reactions of Ba, NaCl, NaNH2 and metallic Na, or Ba, NH4Br and Na, respectively, in sealed, silicajacketed stainless-steel ampoules. The crystal structures of the new compounds were determined by means of single crystal X-ray diffraction. Ba2H3Cl and Ba2H3Br crystallize in a stuffed anti CdI2 structure and adopt the space group P3̄m1 (No. 164) with the lattice parameters a = 443.00(6), c = 723.00(14) pm and a = 444.92(4), c = 754.48(14) pm, respectively. The hydride positions are derived by crystallographic reasoning and with the help of EUTAX calculations. The results are compared with known data for binary and ternary alkaline earth metal hydrides.

Penta-, Hepta- und Oktaiodid-Anionen in Salzen mit Erdalkalimetall-Kronenether-Kationen / Penta-, Hepta-, and Octaiodide Anions in Salts with Alkaline Earth Metal Crown Ether Cations

2010 ◽  
Vol 65 (9) ◽  
pp. 1077-1083 ◽  
Author(s):  
Christine Walbaum ◽  
Ingo Pantenburg ◽  
Gerd Meyer
Keyword(s):  
Crown Ether ◽  
Single Crystal ◽  
Crystal Structures ◽  
Alkaline Earth ◽  
Earth Metal ◽  
Alkaline Earth Metal ◽  
Iodine Molecule ◽  
X Ray Diffraction ◽  
X Ray ◽  
Secondary Bonding

Salts of alkaline earth metal cations sequestered in dibenzo-18-crown-6 (Db18c6) and benzo-15- crown-5 (B15c5), respectively, with I5−, I7− and I82− as the anions, have been synthesized and their crystal structures determined by single-crystal X-ray diffraction. [Ca(Db18c6)(H2O)3](I5)2- (Db18c6)(H2O) (1): monoclinic, P21 (no. 4), a = 1322.1(2), b = 1849.1(2), c = 1344.0(2) pm, β = 114.70(1)◦, V = 2985.2(6) × 106 pm3, Z = 2; [Sr(B15c5)2](I7)2 (2): triclinic, P1 (no. 2), a = 973.9(5), b = 1244.0(5), c = 1293.3(5) pm, α = 115.28(1), β = 90.18(1), γ = 104.57(1)◦, V = 1360.2(10) × 106 pm3, Z = 2; [Ba(Db18c6)2]I8 (3): orthorhombic, Pbcn (no. 60), a = 1452.0(2), b = 1924.6(2), c = 1912.1(2) pm, V = 5343.3(10) × 106 pm3, Z = 4. Compound 1 contains two crystallographically independent V-shaped pentaiodide anions, I5 −, which are linked to dimers by weak interionic contacts. The unusual heptaiodide anion, I7−, in 2 can be described as a V-shaped pentaiodide unit, which is connected to a slightly widened iodine molecule to give the rare Z form. Secondary bonding distances lead to almost planar ten-membered iodine rings, which are connected through common edges to form ribbons with staircase-like folding. 3 is built of sandwich-like cations and centrosymmetric octaiodide anions, I82−. An inspection for secondary contacts reveals that the iodine substructure of 3 consists of essentially isolated octaiodide units.

The 1H NMR spectra and fluxional behaviour of [Mo(η-C5H5)(CO)(CNR)3][PF6] complexes (R = Me, Et, Pr OR Bu ): the x-ray structure of [Mo(ν-C5H5)(CO)(CNB )3][PF6]

Polyhedron ◽  
1986 ◽  
Vol 5 (11) ◽  
pp. 1741-1746 ◽  
Author(s):  
Gerard Lawless ◽  
Gerard McNally ◽  
A.R. Manning ◽  
Desmond Cunningham ◽  
Patrick McArdle
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
1H Nmr Spectra ◽  
X Ray
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