Variable-temperature X-ray crystal structure determinations of {Fe[tren(6-Mepy)3]}(ClO4)2and {Zn[tren(6-Mepy)3]}(ClO4)2compounds: correlation of the structural data with magnetic and Mössbauer spectroscopy data

2007 ◽  
Vol 40 (6) ◽  
pp. 1135-1145 ◽  
Author(s):  
Maksym Seredyuk ◽  
Ana B. Gaspar ◽  
Joachim Kusz ◽  
Gabriela Bednarek ◽  
Philipp Gütlich
Keyword(s):  
Crystal Structure ◽  
Cell Volume ◽  
High Spin ◽  
Unit Cell Volume ◽  
Variable Temperature ◽  
Unit Cell ◽  
X Ray ◽  
Cell Parameters ◽  
Bond Lengths ◽  
Structure Determinations

Variable-temperature X-ray crystal structure determinations (80–330 K) on compounds {Fe[tren(6-Mepy)3]}(ClO4)2(1-Fe) {tren(6-Mepy)3is tris[3-aza-4-(6-methyl-2-pyridyl)but-3-enyl]amine} and {Zn[tren(6-Mepy)3]}(ClO4)2(1-Zn) {tren(6-Mepy)3is tris[3-aza-4-(6-methyl-2-pyridyl)but-3-enyl]amine} were carried out together with a detailed analysis of the unit-cell volume and parameters in the spin transition region for (1-Fe). Both compounds crystallize in the monoclinic system and retained the space groupP21/cat all measured temperatures. The Fe and Zn atoms are surrounded by six N atoms belonging to imine groups and pyridine groups of the trifurcated ligand, adopting a pseudo-octahedral symmetry. The average Fe—N bond lengths of 2.013 (1) Å (80 K) and 2.216 (2) Å (330 K) are consistent with a low-spin (LS) and a high-spin (HS) state for the iron(II) ions. In contrast to (1-Fe), the structures of (1-Zn) at low and high temperatures are similar and repeat the structural features of the high-spin structure of (1-Fe). The volume of the unit cell increases on heating from 80 to 330 K for (1-Fe) and (1-Zn). On the other hand, while thea,bandccell parameters increase for (1-Fe), they show less variation for (1-Zn). For (1-Fe), variation of the unit-cell volume with temperature recalculated per Fe atom shows a change ΔV= 27.16 Å3during the spin crossover process. Magnetic susceptibility and Mössbauer spectroscopy studies performed on (1-Fe) reveal an inversion temperature,T1/2of 233 K, where the molar fractions of LS and HS sites are both equal to 0.5. The variation in metal–ligand bond lengths, the distortion parameters and the cell parameters are very close to the character of the magnetic curve and the curve of γHS(the molar fraction of HS molecules) derived from the Mössbauer data; this result shows the correlation between structure and physical properties in (1-Fe).

scholarly journals Crystal Structure Refinements of Four Monazite Samples from Different Localities

Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1028 ◽  
Author(s):  
M. Mashrur Zaman ◽  
Sytle M. Antao
Keyword(s):  
Crystal Structure ◽  
Electron Probe ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters ◽  
Large Unit Cell ◽  
A Site

This study investigates the crystal chemistry of monazite (APO4, where A = Lanthanides = Ln, as well as Y, Th, U, Ca, and Pb) based on four samples from different localities using single-crystal X-ray diffraction and electron-probe microanalysis. The crystal structure of all four samples are well refined, as indicated by their refinement statistics. Relatively large unit-cell parameters (a = 6.7640(5), b = 6.9850(4), c = 6.4500(3) Å, β = 103.584(2)°, and V = 296.22(3) Å3) are obtained for a detrital monazite-Ce from Cox’s Bazar, Bangladesh. Sm-rich monazite from Gunnison County, Colorado, USA, has smaller unit-cell parameters (a = 6.7010(4), b = 6.9080(4), c = 6.4300(4) Å, β = 103.817(3)°, and V = 289.04(3) Å3). The a, b, and c unit-cell parameters vary linearly with the unit-cell volume, V. The change in the a parameter is large (0.2 Å) and is related to the type of cations occupying the A site. The average <A-O> distances vary linearly with V, whereas the average <P-O> distances are nearly constant because the PO4 group is a rigid tetrahedron.

X-ray powder diffraction data for tetrazene nitrate monohydrate, C2H9N11O4

2021 ◽  
pp. 1-3
Author(s):  
J. Maixner ◽  
J. Ryšavý
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

X-ray powder diffraction data, unit-cell parameters, and space group for tetrazene nitrate monohydrate, C2H9N11O4, are reported [a = 5.205(1) Å, b = 13.932(3) Å, c = 14.196(4) Å, β = 97.826(3)°, unit-cell volume V = 1019.8(4) Å3, Z = 4, and space group P21/c]. All measured lines were indexed and are consistent with the P21/c space group. No detectable impurities were observed.

X-ray powder diffraction data for copper(II), bis[(2E)-3-methoxy-2-[(2,6-dimethylphenyl)imino]-4-[(2,6-dimethylphenyl)imino-κN]-3-pentanolato-κO] complex

2013 ◽  
Vol 28 (4) ◽  
pp. 296-298
Author(s):  
R. Pažout ◽  
J. Maixner ◽  
A.S. Jones ◽  
J. Merna
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

X-ray powder diffraction data, unit-cell parameters, and space group for a new bis(β-diiminato) Cu(II) complex, C44H54CuN4O4, are reported [a = 8.683(3) Å, b = 11.216(3) Å, c = 11.753(4) Å, α = 66.27(3), β = 84.61(3), γ = 78.85(3), unit-cell volume V = 1027.77 Å3, Z = 1, and space group P-1]. All measured lines were indexed and are consistent with the P-1 space group. No detectable impurity was observed.

X-ray powder diffraction data for deoxyschisandrin

2013 ◽  
Vol 28 (3) ◽  
pp. 231-233 ◽  
Author(s):  
Li Li Zhang ◽  
Qing Qing Pan ◽  
Dan Xiao ◽  
Xiao Qing Wu ◽  
Qing Wang ◽  
...  
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

X-ray powder diffraction data, unit-cell parameters, and space group for deoxyschisandrin, C24H32O6, are reported [a = 13.083(3) Å, b = 19.563(9) Å, c = 8.805(6) Å, β = 90.472(0)°, unit-cell volume V = 2253.82 Å3, Z = 4, and space group P21]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurity was observed.

X-ray powder diffraction data for 7-ethyl-14-nitro-camptothecin, C22H19N3O6

2018 ◽  
Vol 33 (4) ◽  
pp. 327-329
Author(s):  
Wan Wang ◽  
Zili Suo ◽  
Lidong Liao ◽  
Hui Li
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

X-ray powder diffraction (XRD) data, unit-cell parameters and space group for 7-ethyl-14-nitro-camptothecin, C22H19N3O6, are reported [a = 10.987(5) Å, b = 10.941 (9) Å, c = 8.438 (2) Å, α = 71.321(6)°, β = 96.145(0)°, γ = 95.139(3)°, unit-cell volume V = 953.87 Å3, Z = 2, ρcal = 1.467 g cm−3, and space group P-1]. All measured lines were indexed and are consistent with the P-1 space group. No detectable impurities were observed.

X-ray powder diffraction data for bis (1-amidino-2-ethylisourea) copper(II) nitrate

2013 ◽  
Vol 28 (4) ◽  
pp. 289-292
Author(s):  
J. Maixner
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

X-ray powder diffraction data, unit-cell parameters and space group for C8H20CuN10O8 are presented [a = 5.262 (2) Å, b = 14.051 (3) Å, c = 12.183 (3) Å, β = 96.912 (5)°, unit-cell volume V = 894.3 Å3, Z = 2, space group P21/n]. All measured lines were indexed and are consistent with the P21/n space group. No detectable impurities were observed.

X-ray powder diffraction data for 2-[((3R)-5-oxo-4-phenyltetrahy drofuran-3-yl)methyl]isoindoline-1,3-dione, C19H15NO4

2016 ◽  
Vol 31 (2) ◽  
pp. 155-158
Author(s):  
Shoujun Zheng ◽  
Kailin Xu ◽  
Qing Wang ◽  
XiaoLin Tang ◽  
Yanmei Huang ◽  
...  
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Element Analysis ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

2-[((3R)-5-oxo-4-phenyltetrahydrofuran-3-yl)methyl]isoindoline-1,3-dione, C19H15NO4, was synthesized for the first time. Its structure was characterized by element analysis, ultraviolet spectrometry, nuclear magnetic resonance, and single X-ray diffraction (SXRD). X-ray powder diffraction (XRPD) data of title compound were collected and calculated. The result of SXRD shows that its crystal system is orthorhombic, space group is Pbca, and unit-cell parameters are a = 8.861 57(7), b = 14.6666(10), c = 24.4247(19) Å, α =β =γ =90°, unit-cell volume V = 3174.4 Å3, and Z = 8. All XRPD measured lines were indexed and consistent with the Pbca space group [a = 14.639(7), b = 24.378(3), c = 8.918(1) Å, α = β = γ = 90°, unit-cell volume V = 3182.7(9) Å3, Z = 8]. No detectable impurities were observed.

X-ray powder diffraction data for norethindrone

2013 ◽  
Vol 29 (1) ◽  
pp. 46-47 ◽  
Author(s):  
Pei Xiao Tang ◽  
Xiao Qing Wu ◽  
Li Li Zhang ◽  
Qiang Cheng ◽  
Hui Li
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Experimental X-ray powder diffraction data, unit-cell parameters, and space group for norethindrone, C20H26O2, are reported [a = 20.7484(12) Å, b = 12.1678(9) Å, c = 6.5561(2) Å, α = β = γ = 90°, unit-cell volume V = 1655.17(16) Å3, Z = 4 and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurity was observed.

X-ray powder diffraction data for (1R, 5S, 7R)-7-[(S)-4-tert-Butyl-4,5-dihydrooxazole-2-yl] -1,5,7-trimethyl-3-azabicyclo-[3.3.1]-nonane-2,4-dione, a new chiral Kemp’s acid diamide

2011 ◽  
Vol 26 (4) ◽  
pp. 335-336
Author(s):  
R. Pažout ◽  
J. Maixner ◽  
J. Přech ◽  
P. Kačer
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

X-ray powder diffraction data, unit-cell parameters and space group for a new chiral Kemp’s acid diamide, C18H28N2O3, are reported [a = 12.456(2) Å, b = 12.471(2) Å, c = 12.088(2) Å, β = 99.003(2)°, unit-cell volume V = 1854,48 Å3, Z = 4, space group P21]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurity was observed.

X-ray powder diffraction data for methoxmetamine hydrochloride, C14H20ClNO2

2018 ◽  
Vol 33 (3) ◽  
pp. 242-245 ◽  
Author(s):  
Bronislav Jurasek ◽  
Martin Babor ◽  
Stepan Huber ◽  
Martin Kuchar
Keyword(s):  
Cell Volume ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell Volume ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
Unit Cell Parameters ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

X-ray powder diffraction data, unit-cell parameters and space group for methoxmetamine (C14H20ClNO2) are reported [a = 6.5768(7) Å, b = 14.0830(10) Å, c = 15.0530(10) Å, β = 90.975(2)°, unit-cell volume V = 1394.0(2) Å3, and Z = 4, and space group P21/n]. All measured lines were indexed and are consistent with the P21/n space group. No detectable impurities were observed.

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