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Volumn 47, Issue 30, 2008, Pages 5654-5657

Mineralization routes to polyphosphides: Cu2P20 and Cu5InP16

Author keywords

Coinage metals; Indium; Mineralization reactions; Phosphorus; Polyphosphides

Indexed keywords

COPPER;

EID: 53549125819     PISSN: 14337851     EISSN: None     Source Type: Journal    
DOI: 10.1002/anie.200705540     Document Type: Article
Times cited : (51)

References (64)
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    • Black Phosphorus is commercially available: http://www.chem-pur.de. See also: T. Nilges, M. Kersting, T. Pfeiffer, J. Solid State Chem. 2008, DOI: 10.1016/j.jssc.2008.03.008.
    • Black Phosphorus is commercially available: http://www.chem-pur.de. See also: T. Nilges, M. Kersting, T. Pfeiffer, J. Solid State Chem. 2008, DOI: 10.1016/j.jssc.2008.03.008.
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    • X-ray powder diffraction data were collected by using a Stoe STADIP powder diffractometer fitted with CuKα1 radiation (λ, 1.54051 Å, germanium monochromator, transmission geometry, 298 K, 7.0 < 2θ < 70.0°, linear 5° PSD (Braun, A comparison of calculated and measured powder diffractograms of the samples is given in the Supporting Information. Lattice parameters derived from the powder data were used for the single-crystal structure determinations. Semiquantitative EDX analyses were performed by using a Leica 420i scanning electron microscope (Zeiss) fitted with an energy-dispersive detector unit (EDX, Oxford, Cu, In, and GaP were used as standards for calibration. A voltage of 20 kV was applied to the samples. Data were averaged for more than five independent measurements collected from crystals separated from different reaction batches. Cu 2P20 (in atom , Cu 9(2, P 912, calcd: Cu 9.1, P 90.9; Cu5
    • 16 is stable in air for several months and can stored without the need for an inert gas atmosphere.
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    • 53549129817 scopus 로고    scopus 로고
    • Crystallographic data for Cu2P20: M, 746.6 g mol-1; dark red, nontransparent crystals, 0.01 x 0.02 x 1.0 mm3, triclinic, space group P1, a, 7.131(4, b, 11.437(4, c, 11.750(4) Å, α, 68.53(3, β, 83.60(4, γ, 84.39(4)°, V, 884.6(7) Å3, Z, 2, ρcalcd, 2.80 g cm-3, Stoe IPDS II, Mo Kα radiation (λ, 0.71073 Å, graphite monochromator, F(000, 716, μ, 4.2 mm-1, T, 293(1) K, 2487 independent reflections between 1.87 < θ < 26.74°, 1939 reflections I > 3σI, and 199 parameters, Rint, 0.0321, numerical absorption correction, full-matrix least-squares refinement against F2 with Jana 2000,[22c] R1, 0.0585, wR2, 0.0818 for I > 3σI and R
    • [22c] R1 = 0.0585, wR2 = 0.0818 for I > 3σI and R1 = 0.0792, wR2 = 0.0837 for all data.
  • 37
    • 53549107019 scopus 로고    scopus 로고
    • Crystallographic data for Cu5InP16: refined composition Cu4.9(1)In1.1(1)P16; M, 933.9 g mol-1; dark red, nontransparent crystal 0.45 x 0.40 x 0.18 mm3, monoclinic, space group C2/c, a, 11.124(3, b, 9.663(3, c, 7.533(2) Å, β, 109.96(1)°, V, 761.1(3) Å3, Z, 2, ρcalcd, 4.07 g cm-3, Stoe IPDS II, MoKα-radiation (λ, 0.71073 Å, graphite monochromator, F(000, 872, μ, 10.0 mm-1, T, 293(1) K, 642 independent reflections between 2.87 < θ < 29.17°, 362 reflections I > 3σI, and 53 parameters, Rint, 0.0450, numerical absorption correction, full-matrix least-squares refinement against F2 with Jana 2000,[22c] R1, 0.0240, wR2, 0.0386 for I
    • 16);
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    • Magnetic measurements were performed by using a commercially available physical property measurement system PPMS Quantum Design, The samples for magnetic measurements were mounted on a VSM sample holder and measured in the temperature range from 5 to 305 K. For details see Supporitng Information
    • Magnetic measurements were performed by using a commercially available physical property measurement system PPMS (Quantum Design). The samples for magnetic measurements were mounted on a VSM sample holder and measured in the temperature range from 5 to 305 K. For details see Supporitng Information.
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    • The electronic structure was calculated based on the experimental structure data by applying the LCAO scheme as implemented in CRYSTAL06 [25a,b] within the framework of density functional theory (DFT, 25c] Calculations were performed with the GGA functional PBE, 25d] A shrinking factor scheme of 4 4 resulting in 36 k-points for the IBZ and 260 points for the Gilat net was used. The electronic structure input was given by all-electron basis sets according to Doll et al, 25e] for Cu and Zicovich-Wilson et al. for P.[25f] Additional information on the computational procedure can be found in reference [25g] and in the Supporting Information; a) R. Dovesi, V. R. Saunders, C. Roetti, R. Orlando, C. M. Zicovich-Wilson, F. Pascale, B. Civalleri, K. Doll, N. M. Harrison, I. J. Bush, Ph. D'Arco, M. Llunell, CRYSTAL06, Torino, Italy, 2007;
    • [25f] Additional information on the computational procedure can be found in reference [25g] and in the Supporting Information; a) R. Dovesi, V. R. Saunders, C. Roetti, R. Orlando, C. M. Zicovich-Wilson, F. Pascale, B. Civalleri, K. Doll, N. M. Harrison, I. J. Bush, Ph. D'Arco, M. Llunell, CRYSTAL06, Torino, Italy, 2007;
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    • 8 unit is given in the Supporting Information.
    • 8 unit is given in the Supporting Information.
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    • An overview on the topological relationship between polyphosphides and ultraphosphates can be found in: R. Glaum, Neue Untersuchungen an wasserfreien Phosphaten der Übergangsmetalle, Habilitationsschrift, Universisty Gießen, 1999, p. 86
    • An overview on the topological relationship between polyphosphides and ultraphosphates can be found in: R. Glaum, Neue Untersuchungen an wasserfreien Phosphaten der Übergangsmetalle, Habilitationsschrift, Universisty Gießen, 1999, p. 86.
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    • 16 is given in the Supporting Informaiton; a) A. Olbertz, D. Stachel, I. Svoboda, H. Fuess, Acta Crystallogr. Sect. C 1995, 51, 1047-1049;
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    • [29c] with X = Cl, Br. a A. V. Shevelkov, E. V. Dikarev, B. A. Popovkin, Z. Kristallogr. 1994, 209, 583-585;
    • [29c] with X = Cl, Br. a) A. V. Shevelkov, E. V. Dikarev, B. A. Popovkin, Z. Kristallogr. 1994, 209, 583-585;
  • 61
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    • [32d] (Q = Te, Se, S; X = Cl, Br); a) S. Lange, T. Nilges, Chem. Mater. 2006, 18, 2538-2544;
    • [32d] (Q = Te, Se, S; X = Cl, Br); a) S. Lange, T. Nilges, Chem. Mater. 2006, 18, 2538-2544;


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.