Syntheses, Single-crystal Structure and Vibrational Spectra of Ca15(CBN)6(C2)2H2

2011 ◽  
Vol 66 (11) ◽  
pp. 1092-1096
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvoa
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Vibrational Spectra ◽  
Title Compound ◽  
Cell Parameter ◽  
Single Crystal Structure ◽  
Boron Powder ◽  
Space Group ◽  
Ir And Raman

Single crystals of Ca15(CBN)6(C2)2H2 were obtained either by the reaction of stoichiometric amounts of graphite, hexagonal BN, and CaH2 with an excess of distilled Ca, or by using graphite, boron powder, Ca3N2, and CaH2 with an excess of distilled Ca. Both reactions took place in silicajacketed Ta ampoules at 1400 K. Crystals of the title compound are transparent dark-red and isopointal to Ca15(CBN)6(C2)2O adopting the cubic space group Ia3̄d (no. 230, Z = 8) with the cell parameter a = 1653.30(17) pm. The vibrational spectra were recorded and are compared with IR and Raman data of isotypic compounds

OnemoreCompound Containing the CBN4- Ion – Synthesis, Single-crystal Structure and Vibrational Spectra of Ca15(CBN)6(C2)2F2

2010 ◽  
Vol 65 (12) ◽  
pp. 1409-1415 ◽  
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. Di Salvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Raman Spectra ◽  
Vibrational Spectra ◽  
Title Compound ◽  
Cell Parameter ◽  
Single Crystal Structure ◽  
Space Group ◽  
Ir And Raman

Single crystals of Ca15(CBN)6(C2)2F2 were obtained by the reaction of graphite, hexagonal BN and CaF2 with an excess of distilled Ca metal in silica-jacketed Ta ampoules at 1300 K. The title compound is transparent red and crystallizes isopointal to Ca15(CBN)6(C2)2O adopting the cubic space group Ia 3̄d (no. 230, Z = 8) with the cell parameter a = 1653.6(4) pm. Its vibrational spectra are compared with IR and Raman data of similar compounds from the literature and with the newly measured Raman spectra of Ca5(BC2)(C2)Cl3 and Ca9(BC2)2Cl8.

Kristallstruktur und Schwingungsspektren von Li5CrCl8 / Crystal Structure and Vibrational Spectra of Li5CrCl8

1992 ◽  
Vol 47 (12) ◽  
pp. 1687-1692 ◽  
Author(s):  
Heinz Dieter Lutz ◽  
Peter Kuske ◽  
Arno Pfitzner ◽  
Hermann-Josef Steiner
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Vibrational Spectra ◽  
Title Compound ◽  
Structure Type ◽  
The Novel ◽  
X Ray ◽  
Symmetry Coordinates ◽  
Unknown Structure ◽  
Ir And Raman

The crystal structure of the novel pink Li5CrCl8 oC28 has been determined by both single crystal X-ray and neutron powder studies. The title compound crystallizes in a hitherto unknown structure type (space group C mmm, Z = 2). The final R values are R = 3.4% (715 independent reflections with I > 3aI) and Rwp = 11.5%, respectively (a = 1019.79(3), b = 723.94(2) and c = 726.16(3) pm). The structure consists of edge-connected Li(l)Cl6 and alternating edge-connected Li(2)Cl6 and CrCl6 octahedra, respectively. It is related to the NaCl super structure SnMn2S4 type. IR and Raman spectra as well as symmetry coordinates are given and discussed in terms of CrCl6 and LiCl6 breathing modes.

Filling up another Gap: Synthesis and Crystal Structure of Ba2H3I

2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides

Kristallstruktur von 1,1'-Dimethyl-4,4'-bipyridinium-octachlorodiantimonat(III) / Crystal Structure of 1,1'-Dimethyl-4,4'-bipyridinium-octachlorodiantimonate(III)

1998 ◽  
Vol 53 (5-6) ◽  
pp. 565-568 ◽  
Author(s):  
Bernd Jaschinski ◽  
Roger Blachnik ◽  
Hans Reuter
Keyword(s):  
Crystal Structure ◽  
Phase Transition ◽  
Single Crystal ◽  
Title Compound ◽  
Single Crystal Structure ◽  
Space Group ◽  
Enthalpy Of Transition

Abstract The title compound was prepared by reaction of SbCl3 with 1,1′-dimethyl-4,4′-bipyridinium-chloride in methanol. The single crystal structure gave the following data: [C12H14N2][Sb2Cl8] (1) space group PI, Nr. 1, with a = 570.68(7) pm, b = 938.57(14) pm, c = 1174.27(11)pm, α = 66.72(9)°, β = 89.304(12)°, γ = 78.684(11)°, and Z = 1. The compound has a small SHG effect and a phase transition at 272 °C with an enthalpy of transition of 6.54 kJ mol-1 .

Complete X-ray single-crystal structure determination and Raman spectrum of NH4[C(CN)3]

2017 ◽  
Vol 72 (7) ◽  
pp. 517-521
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Raman Spectrum ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Title Compound ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
X Ray ◽  
Related Compounds

AbstractThe crystal structure of NH4[C(CN)3] has been determined via X-ray single-crystal methods at 203(2) K corroborating earlier results. Additionally, the hydrogen positions have been determined and the Raman spectrum of the title compound recorded on single crystals. The spectroscopic results are compared to those for related compounds.

Synthesis, Raman Spectrum and Single-Crystal Structure of CaBa8[CN2]6O2(N0.5H0.5)

2013 ◽  
Vol 68 (1) ◽  
pp. 39-43
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Raman Spectrum ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Title Compound ◽  
Bond Angle ◽  
Single Crystal Structure ◽  
Oxygen Impurity ◽  
Bond Lengths

Colorless, transparent single crystals of CaBa8[CN2]6O2(N0.5H0.5) (R3̄ (no. 148), a = 996.94(4) and c = 1803.18(8) pm, Z = 3) were obtained by the reaction of Ca3N2, Ba2N and NaHCN2 (of which one of the latter two most likely was contaminated with some oxygen impurity) in arcwelded Nb ampoules at 1200 K. The title compound consists of distorted (H/N)Ba6 octahedra which share two of their opposite faces with OBa4 tetrahedra interconnected by [N=C=N]2- units of Ca(N=C=N)6 octahedra with C=N bond lengths of 121.9(6) and 124.3(6) pm and with a bond angle deviating from linearity with (N-C-N) = 175:9(5)°. A Raman spectrum obtained from the crystal used for the structure determination indicates the presence of the [N=C=N]2- unit.

Synthesis and single-crystal structure of the pseudo-ternary compounds LiA[N(CN)2]2 (A = K or Rb)

2016 ◽  
Vol 71 (2) ◽  
pp. 157-160 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Alkali Metal ◽  
Single Crystal ◽  
Title Compound ◽  
Single Crystal Structure ◽  
Rectangular Plates ◽  
Atmospheric Conditions ◽  
Space Group ◽  
Cell Parameters ◽  
Ternary Compounds

AbstractCrystals of LiA[N(CN)2]2 were obtained from the reaction of LiCl and ACl (A = K or Rb) with Ag[N(CN)2] in water and subsequent evaporation of the filtered solution at 80 °C under normal atmospheric conditions. Crystals of the title compound form thin rectangular plates that are transparent, colorless, and very fragile. Single-crystal structure analyses have shown that both compounds are isotypic and adopt the tetragonal space group I4/mcm (no. 140, Z = 4) with the cell parameters a = 701.53(12) and c = 1413.7(5) pm for LiK[N(CN)2]2 and a = 730.34(10) and c = 1414.4(4) pm for LiRb[N(CN)2]2. The crystal structure is described and compared to that of the pseudo-binary alkali metal dicyanamides.

Cs2NiO2 Revisited. Crystal Structure and Magnetic Properties

2012 ◽  
Vol 67 (1) ◽  
pp. 57-60
Author(s):  
Katarina Đuriš ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
Single Crystal Structure ◽  
Space Group ◽  
Single Crystal Structure Analysis

Single crystals as well as microcrystalline powders of Cs2NiO2 were obtained via the azide/nitrate route from appropriate mixtures of CsN3, CsNO3 and NiO. The single-crystal structure analysis confirmed that Cs2NiO2 crystallizes in the tetragonal space group I4/mmm (Z = 2, a = 4.4090(3), c = 13.576(3) Å , R1 = 0.036, wR2 = 0.093). Above 45 K, Cs2NiO2 is paramagnetic, and an analysis based on the Curie-Weiss law has resulted in μ = 2.89 μB paramagnetic units, θ = −30.8 K and TN ∼ 20 K.

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.

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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