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.

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.

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.

The Last Missing Member of the AE2[BN2]Cl Series – Synthesis, Structural and Spectroscopic Characterization of Ba2[BN2]Cl

2008 ◽  
Vol 63 (5) ◽  
pp. 525-529 ◽  
Author(s):  
Olaf Reckeweg ◽  
Jesse Reiherzer ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Title Compound ◽  
Spectroscopic Characterization ◽  
X Ray ◽  
Fundamental Frequencies ◽  
Raman And Ir Spectra

Pale grey-blue, transparent single crystals of Ba2[BN2]Cl (I4132 (no. 214), a = 1462.88(1) pm, Z = 24) are obtained by the reaction of Ba, BaCl2, BN and NaN3 in arc-welded Ta ampoules at 1200 K. The crystal structure was determined by single crystal X-ray structure analysis. The Raman and IR spectra of the title compound show the expected fundamental frequencies (νs = 1038; νas = 1969 and 2087; δ = 616 / 636 cm−1) for a nitridoborate unit with D∞h symmetry. The [N-B-N] structure obtained by X-ray single crystal structure determination corroborates this finding within the standard deviations of the measurement with d(B-N) = 132.3(8) pm and ∡ (N-B-N) = 178.5(13)°. Our results compare well to the data reported for cubic and orthorhombic Ba3[BN2]2 as well as to the isotypic compound Ba2[BN2]Br.

A Metal Nitride Carbodiimide with a Stuffed Skutterudite-type Structure: Synthesis, Crystal Structure and IR Spectra of (Ba6N5/6)2[NbN4][CN2]6

2007 ◽  
Vol 62 (10) ◽  
pp. 1246-1250 ◽  
Author(s):  
Olaf Reckeweg ◽  
Mehmet Somer ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Single Crystals ◽  
Ir Spectrum ◽  
Title Compound ◽  
Bond Angle ◽  
Type Structure ◽  
Bond Lengths ◽  
Structure Synthesis ◽  
Bending Modes

Coppery-red, transparent single crystals of (Ba6N5/6)2[NbN4][CN2]6 (Im¯3, no. 204, a =1125.83(3) pm, Z = 2) are obtained by the reaction of Ba2N and ZnCN2 with the container walls of the arc-welded Nb ampoules at 1100 K. The title compound assumes a stuffed skutterudite-type structure in which edge-sharing (Ba6N5/6) octahedra form large voids which are occupied by either [NbN4] tetrahedra or by [N=C=N]2− units with symmetric C=N bond lengths of d = 121.8(6) pm but a bond angle deviating significantly from linearity (∡ (N-C-N) = 175.3(9)°). The IR spectra corroborate this crystallographic result by the fact that all fundamental vibrations are visible in the IR spectrum [ν1 = 1262 (symmetric stretching mode); ν2 = 1957/2009 (antisymmetric stretching mode); ν3 = 611/633/653 cm−1 (bending modes)], which is symmetry forbidden for [N=C=N]2− units having D∞h symmetry but expected for the C2v symmetry found in the title compound.

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

Single-crystal Structure Determination and Spectroscopic Characterization of KSr4(BO3)3

2013 ◽  
Vol 68 (4) ◽  
pp. 338-344 ◽  
Author(s):  
Gerhard Sohr ◽  
Doris Clara ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Normal Pressure ◽  
Spectroscopic Characterization ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
Raman Spectroscopic ◽  
Pressure Phase

During attempts to synthesize a high-pressure phase of KSr4(BO3)3 using pressures of up to 12 GPa, single crystals of the normal-pressure phase KSr4(BO3)3 with sufficient quality for singlecrystal diffraction experiments could be obtained at 3 GPa and 1300 °C in a Walker-type multianvil apparatus. The single-crystal structure determination verified the published powder diffraction data of KSr4(BO3)3 revealing the non-centrosymmetric space group Ama2 with a = 1104:8(2), b=1199:1(2), c=688:8(2) pm and Z =4. Additionally, IR- and Raman-spectroscopic investigations were performed on single crystals of the compound.

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

Synthesis and Single Crystal Structure Determination of Bis(carbido)bis(μ-diphenylphosphido)heptadecacarbonyloctaruthenium-Dichloromethane (1/1), Ru8(μ6-C)(μ5-C)(μ-PPh2)2(CO)17.CH2Cl2

1993 ◽  
Vol 46 (11) ◽  
pp. 1811 ◽  
Author(s):  
CJ Adams ◽  
MI Bruce ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Room Temperature ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
Triangular Face ◽  
X Ray

The synthesis and room-temperature single-crystal X-ray structure determination of the title compound are recorded. Crystals are monoclinic, P 21/c, a 14.43(2), b 18.39(1), c 23.64(3) Ǻ, β 123.16(7)°, Z = 4, isostructural with the recently described Fe3Ru5 analogue; R was 0.048 for 6892 'observed' data [I > 3σ(I)]. The cluster is one of the few containing separated carbide ligands within a polyhedral metal skeleton, consisting of an Ru5C square pyramid and an Ru6C octahedron sharing a triangular face, with two PPh2 groups bridging opposite Ru-Ru vectors in each polyhedron.

Ba9[NbN4]2O[Cn2] – Synthesis, Crystal Structure and Raman Spectrum

2003 ◽  
Vol 58 (1) ◽  
pp. 201-204 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Raman Spectrum ◽  
Single Crystal ◽  
Single Crystals ◽  
Title Compound ◽  
Single Crystal Diffraction ◽  
X Ray

Abstract Red transparent single crystals of Ba9[NbN4]2O[CN2] were synthesised by the reaction of BaO coated Ba metal, C and Nb powder in arc-welded Nb ampoules at 1300 K. The title compound was characterised by X-ray single crystal diffraction (P1̅ , a = 799.05(2), b = 962.61(2) and c = 1264.38(4) pm; α = 75.859(1), β = 85.745(1) and γ = 87.8621(8)°; Z = 2) and Raman spectroscopy (νsym = 1234 and δ = 632/658/668 cm−1). It now seems likely that a nitride-azide compound we previously reported, Ba9[NbN4]2N[N3], does not exist, but is in fact the title compound.

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