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Starting materials for the preparation of CaFe4As3 were Ca (Alfa Aesar, granules, 99.5, Fe (Cerac, powder, 99.9, As (Alfa Aesar, powder, 99.99, and Sn (Cerac, shot, 99.9, All of the manipulations were done in a nitrogen-filled glove box with moisture and oxygen levels less than 1 ppm. Ca (0.0407 g, 1 mmol, Fe (0.223 g, 4 mmol, As 0.225 g, 3 mmol, and 5 g of Sn pieces were added to an alumina crucible, which was placed in a quartz ampoule and subsequently sealed under a reduced pressure of 10 -4 Torr. This assembly was heated to 650 °C for 12 h, held there for a period of 6 h, then heated to 1123 K for 12 h, held for 6 h, and slowly cooled to 873 K for 12 h. At this temperature, the liquid Sn flux was filtered by centrifugation. The resulting product was metallic needlelike crystals
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-4 Torr. This assembly was heated to 650 °C for 12 h, held there for a period of 6 h, then heated to 1123 K for 12 h, held for 6 h, and slowly cooled to 873 K for 12 h. At this temperature, the liquid Sn flux was filtered by centrifugation. The resulting product was metallic needlelike crystals.
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84869588207
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57Co(Rh) source calibrated with α-Fe, relative to which isomer shift values are reported.
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57Co(Rh) source calibrated with α-Fe, relative to which isomer shift values are reported.
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14
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84869588209
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Magnetization measurements were carried out using a SQUID magnetometer (Quantum Design MPMS-XL) over the temperature range 5-300 K. Anisotropic magnetization measurements on CaFe4As3 single crystals were performed using a Quantum Design MPMS SQUID magnetometer. Temperature-dependent data were collected in both the ZFC and FC modes between 2 and 300 K, with an applied field of 2000 Oe. Field-dependent magnetic measurements were acquired at 5, 32, and 105 K with the field swept from-50 to 50 kG. No background correction for the sample holder (straw and kapton tape) was performed. Space group, Pnma; a, 11.8953(12) Å, b, 3.7430(3) Å, c, 11.6100(10, V, 516.92(8) Å3; dcalcd, 6.274 g/cm3; R1, 0.0308, wR2, 0.0628 see the Supporting Information for details
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3; R1 = 0.0308, wR2 = 0.0628 (see the Supporting Information for details).
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3 were performed with a Quantum Design PPMS commercial instrument over the temperature range 4.6-100 K in zero field by a relaxation method using the Two-Tau Model (ref 14b). Single crystals were mounted on the sample puck using special low-temperature grease (Quantum Design). Specific heat data were corrected for background (stage and grease).
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3 were performed with a Quantum Design PPMS commercial instrument over the temperature range 4.6-100 K in zero field by a relaxation method using the "Two-Tau Model" (ref 14b). Single crystals were mounted on the sample puck using special low-temperature grease (Quantum Design). Specific heat data were corrected for background (stage and grease).
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