Europium(II) Heptaphosphide EuP7 [1] Europium(II)heptaphosphid EuP7 [1]

1980 ◽  
Vol 35 (7) ◽  
pp. 824-831 ◽  
Author(s):  
Hans Georg von Schnering ◽  
Manfred Wittmann

The novel polyphosphide EuP7 was prepared under controlled conditions by the reaction of the elements in salt melts at 750-800 K. EuP7 forms black prismatic crystals not attacked by diluted mineral acids and bases. The thermal decomposition yields EuP3 at 700 K and in further steps EuP2, Eu3P4 and EuP, respectively. According to the crystal structure as well as the electrical, optical and magnetic properties EuP7 is a semiconductor (EG = 0.9 eV; EG (vert) = 1.1 eV) with divalent europium (μ = 7.55 B.M.). The compound crystallizes in the monoclinic space group P21/n with a = 1148.8(7) pm, b = 570.0(3) pm, c = 1061.0(6) pm, and β= 106.08°(5); (X-ray diffraction data; 1479 hkl, R = 0.031). The P-atoms are connected (P-P) = 218.0-223.5 pm) to a 2-dimensional infinite polyanionic structure with homonuclear 3-bonded and 2-bonded P-atoms in the ratio 5:2. The polyanionic network contains P6-rings (chair conformation) as well as P8-rings and P10-rings. The Eu-atoms are bonded to 9 P-atoms (1,4,4-polyhedra) with bond distances ranging from 306.6 to 326.6 pm. The Eu-atoms complete the tetrahedral environment of the P-atoms

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.


1979 ◽  
Vol 57 (2) ◽  
pp. 174-179 ◽  
Author(s):  
A. Wallace Cordes ◽  
Paul F. Schubert ◽  
Richard T. Oakley

The crystal structure of 1,4-diphenyl-2,2′,3,3′,5,5′,6,6′-octamethylcyclo-1,4-diphospha-2,3,5,6-tetrasilahexane, (PhPSi2Me4)2, has been determined by single crystal X-ray diffraction. The crystals are monoclinic, space group P21/c, with a = 9.866(1), b = 11.921(1), and c = 11.324(2) Å, β = 104.31(1)°, Z = 2, and ρcalcd = 1.15 g/cm3. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to a final R of 0.060 and Rw of 0.078, for 1173 reflections with intensities greater than 3σ. The (PhPSi2Me4)2 molecule lies on a crystallographic centre of symmetry, and the six-membered P2Si4 ring has a chair conformation with equatorial phenyl groups. The endocyclic angles at P (104.4(1)°) and Si (104.9(2)°) are intermediate between those found in cyclic hexaphosphine and hexasilane molecules, and the Si—Si and P—Si distances of 2.345(3) and 2.252(4) Å, respectively, correspond to single bond lengths, with no appreciable evidence for secondary pπ → dπ bonding between phosphorus and silicon. The Si—C (1.867(8) Å) and P—C (1.828(7) Å) bond lengths are also normal. The variations in the Si—P—C (101.6(2)°, 108.6(2)°), P—Si—C (range 106.2(3)–120.0(3)°), and Si—Si—C (range 105.8(3)–113.7(3)°) angles indicate that the positions of the exocyclic methyl and phenyl groups are influenced by both intra- and intermolecular steric forces.


2008 ◽  
Vol 63 (2) ◽  
pp. 139-142 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
Orhan Büyükgüngör

Two new complexes [Ag(sac)(aepip)] (1) and [Ag(sac)(hepip)] (2) have been obtained by the reaction of AgNO3 with Na(sac)・2H2O (sac = saccharinate) in the presence of N-(2-aminoethyl)piperidine (aepip) and N-(2-hydroxyethyl)piperidine (hepip), and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group C2 and triclinic space group P1, respectively. In both complexes, silver( I) is tricoordinated. The sac ligand is N-coordinated, while aepip and hepip behave as N-N and N-O bidentate chelating ligands, respectively. The pip rings of both aepip amd hepip ligands adopt typical ‘chair’ conformation. The individual molecules are linked into one-dimensional chains by two N-H···O hydrogen bonds in 1, and one O-H···O hydrogen bond in 2. TG-DTG curves illustrated that the endothermic elimination of aepip and hepip ligands takes place in the early stages of thermal decomposition, while that of the sac moiety occurs exothermically at higher temperatures to give metallic silver


1997 ◽  
Vol 50 (1) ◽  
pp. 75 ◽  
Author(s):  
Evert J. Ditzel ◽  
K. David Griths ◽  
Glen B. Robertson

The structure of the novel mixed-phosphine complex mer(PMe3)-trans(PEt3)(PPri3)H-trans-Cl2IrIII has been determined by single-crystal X-ray diffraction analysis at 146±3 K. Crystals are monoclinic, space group P 21/c, with a 7·414(4), b 15·073(3), c 9·796(2) Å, β 97·46(1) and Z 4. Structure refinement by constrained (2xC-C distances) full-matrix least-squares analysis (2378 unique reflections, 217 parameters) converged with R 0·049 and ωR 0·055. The PPri3 ligand is face-to-face configured with the unique Pri group eclipsing the hydride ligand. The PEt3 ligand is asymmetrically configured with Ir-P-C-C torsion angles 174, –72 and –146°. Metal{ligand distances are: Ir{P(1,2,3) 2·366(4), 2·372(4), 2·306(4) Å; Ir-Cl(1,2) 2·386(4), 2·372(4) Å. The P-Ir-P(trans) angle is 157·2(1)°.


2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Mihaela Birdeanu ◽  
Mirela Vaida ◽  
Eugenia Fagadar-Cosma

The present study is focused on the obtaining of the Zn3Nb2O8nanomaterial using the hydrothermal method and its characterization through different techniques. X-ray diffraction at room temperature revealed that a novel crystalline form of the nanomaterial forms at 1100°C belonging to monoclinic space group C2/c. Field-emission scanning electron microscopy evidenced the columnar morphology of the particle’s agglomeration and the high resolution electron transmission microscopy confirms the measured interplanar distances calculated from the X-ray diffraction experiments. Using the UV-VIS spectrum and Kubelka-Munk equations, the absorbance and the band gap for the Zn3Nb2O8nanomaterial were calculated. PL spectrum reveals a single peak at 465 nm corresponding to the blue color fluorescence. The novel crystalline nanomaterial might find applications in fluorescence covering of technical devices, due to its capacity to preserve blue fluorescence both in acrylic based paint and after embedding in isopropyl alcohol.


2014 ◽  
Vol 70 (a1) ◽  
pp. C993-C993
Author(s):  
Fernando Cámara ◽  
Linda Pastero ◽  
Rossella Arletti ◽  
Monica Cagnoni

The synthesis, Raman spectroscopy and crystal structure of a novel layered aluminophosphate is described. The new phase was derived by the sol-gel method starting from a modified low hydrothermal ALPO4-34 zeolite synthesis procedure[1].The structure was solved by direct methods using single-crystal X-ray diffraction. The synthesized layered material, with composition [AlPO3(OH)F(H2O)]-(H9C4ON), crystallizes in the monoclinic space group P21/a with a = 9.2282(5) Å, b = 6.9152(4) Å, c = 14.4615(9) Å, β = 101.57(1)0. Layered aluminophosphates with AlO6polyhedra have been previously described [2], although in these compounds Al octahedral share edges. The novel compound has corner sharing AlO4F(H2O) chains along [010], where fluorine is at the shared apex, four oxygen atoms are shared with PO4tetrahedra and the fifth oxygen is a H2O group. This kind of aluminophosphate chains is found in nature in tancoite [3]. Chains are linked along [100] through corner sharing with a PO4group of the adjacent chain plus hydrogen bonding of the H2O group. Layers are stacked along c* through hydrogen bonding with a double layer of morpholine (H9C4ON) molecules. The chemical stability field of the novel materialis strongly dependent from the fluorine/aluminum ratio of the starting gel. At lower fluorine concentrations only ALPO4-34 and/or AlPO4(berlinite) are stable depending on the morpholine content. Crystals growth morphology depends on the supersaturation conditions of the starting gel: at low concentrations crystals are well developed hexagonal like plate shaped and are very thin. At higher concentrations they show a more elongated morphology. A treatment with H2CO3leads to a complete morpholine removal, as shown by in situ Raman spectroscopy. Powder X-ray diffraction reveals that after morpholine extraction, the material diffract still coherently in two dimensions while a strong broadening is shown for basal planes.


Author(s):  
Steffen Klenner ◽  
Maximilian Kai Reimann ◽  
Rainer Pöttgen

Abstract Eu3Pt4Zn12 and Sr3Pt4Zn12 form a complete solid solution Eu3−x Sr x Pt4Zn12. Samples with x = 0, 0.5, 1, 1.5, 2, 2.5 and 3 were synthesized from the elements in sealed tantalum ampoules in an induction furnace. All samples were characterized by powder X-ray diffraction and the structures of Sr3Pt3.93Zn12.07, Eu1.80Sr1.20Pt4Zn12 and Eu3Pt3.68Zn12.32 were refined from single crystal X-ray diffractometer data. The new compounds are isotypic with Gd3Ru4Al12, space group P63/mmc. The striking building units in these phases are the kagome networks occupied by the europium and strontium atoms and Pt1@Zn8 and Pt2@Zn8 distorted cubes. Besides the Eu/Sr mixing within the solid solution, the structure refinements indicated small homogeneity ranges induced by Pt/Zn mixing. The europium containing samples of the solid solution Eu3−x Sr x Pt4Zn12 are Curie–Weiss paramagnets and the experimental magnetic moments manifest stable divalent europium. The samples with x = 0, 0.5 and 2 order magnetically: T N = 15.4(1) K for x = 0, T C = 12.4(1) K for x = 0.5 and T N = 4.0(1) K for x = 2. The 3 K magnetization isotherms tend toward Brillouin type behavior with increasing europium dilution. The divalent ground state of Eu3Pt4Zn12 is further confirmed by 151Eu Mössbauer spectroscopy with an isomer shift of −9.66(2) mm s−1 at 78 K. In the magnetically ordered state Eu3Pt4Zn12 shows full magnetic hyperfine field splitting (23.0(1) T).


1980 ◽  
Vol 33 (5) ◽  
pp. 979 ◽  
Author(s):  
W Choong ◽  
JF McConnell ◽  
NC Stephenson ◽  
JD Stevens

The crystal structure of the title compound was determined by X-ray diffraction and the use of the multi-solution programs MULTAN 74. Crystals are monoclinic, space group C2 with Z = 4 in a unit cell of dimensions: a 21.140(6), b 9.394(3), c 9.765(3) Ǻ, β 108.73(5)°. The structure was refined by full-matrix least-squares methods to a final R of 0.036 for 1858 diffractometer reflections. The seven-membered ring approximates to a twist-chair conformation very similar to that found for the gluco analogue.


2020 ◽  
Vol 58 (5) ◽  
pp. 549-562
Author(s):  
Anatoly V. Kasatkin ◽  
Fabrizio Nestola ◽  
Radek Škoda ◽  
Nikita V. Chukanov ◽  
Atali A. Agakhanov ◽  
...  

ABSTRACT Hingganite-(Nd), ideally Nd2□Be2Si2O8(OH)2, is a new gadolinite group, gadolinite supergroup mineral discovered at Zagi Mountain, near Kafoor Dheri, about 4 km S of Warsak and 30 km NW of Peshawar, Khyber Pakhtunkhwa Province, Pakistan. The new mineral forms zones measuring up to 1 × 1 mm2 in loose prismatic crystals up to 0.7 cm long, where it is intergrown with hingganite-(Y). Other associated minerals include aegirine, microcline, fergusonite-(Y), and zircon. Hingganite-(Nd) is dark greenish-brown, transparent, has vitreous luster and a white streak. It is brittle and has a conchoidal fracture. No cleavage or parting are observed. Mohs hardness is 5½–6. Dcalc. = 4.690 g/cm3. Hingganite-(Nd) is non-pleochroic, optically biaxial (+), α = 1.746(5), β = 1.766(5), γ = 1.792(6) (589 nm). 2Vmeas. = 80(7)°; 2Vcalc. = 84°. Dispersion of optical axes was not observed. The average chemical composition of hingganite-(Nd) is as follows (wt.%; electron microprobe, BeO, B2O3, and Lu2O3 content measured by LA-ICP-MS; H2O calculated by stoichiometry): BeO 9.64, CaO 0.45, MnO 0.10, FeO 3.03, B2O3 0.42, Y2O3 8.75, La2O3 1.63, Ce2O3 12.89, Pr2O3 3.09, Nd2O3 16.90, Sm2O3 5.97, Eu2O3 1.08, Gd2O3 5.15, Tb2O3 0.50, Dy2O3 2.50, Ho2O3 0.33, Er2O3 0.84, Tm2O3 0.10, Yb2O3 0.44, Lu2O3 0.04, ThO2 0.13, SiO2 23.55, H2O 2.72, total 100.25. The empirical formula calculated on the basis of 2 Si apfu is (Nd0.513Ce0.401Y0.395Sm0.175Gd0.145Pr0.096Dy0.068La0.051Ca0.041Eu0.031Er0.022Tb0.014Yb0.011Ho0.009Tm0.003Th0.003Lu0.001)Σ1.979(□0.778Fe2+0.215Mn0.007)Σ1.000(Be1.967B0.062)Σ2.029Si2O8.46(OH)1.54. Hingganite-(Nd) is monoclinic, space group P21/c with a = 4.77193(15), b = 7.6422(2), c = 9.9299(2) Å, β = 89.851(2)°, V = 362.123(14) Å3, and Z = 2. The strongest lines of the powder X-ray diffraction pattern [d, Å (I, %) (hkl)] are: 6.105 (95) (011), 4.959 (56) (002), 4.773 (100) (100), 3.462 (58) (102), 3.122 , 3.028 (61) (013), 2.864 (87) (121), 2.573 (89) (113). The crystal structure of hingganite-(Nd) was refined from single-crystal X-ray diffraction data to R = 0.034 for 2007 unique reflections with I > 2σ(I). The new mineral is named as an analogue of hingganite-(Y), hingganite-(Yb), and hingganite-(Ce), but with Nd dominant among the rare earth elements.


1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.


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