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As part of a study of the long-term operation of solid-oxide fuel cells, three (Mn,Co,Cr)3O4 samples have been synthesized and characterized. X-ray and neutron diffraction patterns from the powder samples at room temperature were measured and the data were co-refined. The neutron data were indispensible in locating Mn, Co and Cr within the crystallographic unit cell with their respective atomic occupancies. Two of these samples have been identified as cubic Mn0.76Co0.58Cr1.66O4 and Mn1.28Co1.72O4. The third is a two-phase sample containing cubic Mn1.66Co1.34O4 and tetragonal Mn2.05Co0.91O4 in a 59.1 (6):40.9 (6)% mass fraction ratio. Cr, which might be introduced from reaction with chromia during oxidation of interconnect materials, exhibits a preference for the octahedral site rather than the tetrahedral site. Without Cr, Mn dominates the octahedral site.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889810008150/db5075sup1.cif
Contains datablocks MN0_4CO0_6CR2O4_publ, MN0_4CO0_6CR2O4_overall, MN0_4CO0_6CR2O4_phase_1, MN0_4CO0_6CR2O4_p_01, MN0_4CO0_6CR2O4_p_02, MNCO2O4_publ, MNCO2O4_overall, MNCO2O4_phase_1, MNCO2O4_p_01, MNCO2O4_p_02, MN1_5CO1_5O4_publ, MN1_5CO1_5O4_overall, MN1_5CO1_5O4_phase_1, MN1_5CO1_5O4_phase_2, MN1_5CO1_5O4_p_01, MN1_5CO1_5O4_p_02

Experimental top

S$_1$ was prepared by mixing MnO (99°, Alfa Aesar), Co$_3$O$_4$ (99.83°, Fisher) and Cr$_2$O$_3$ (99°, Acros) according to the nominal molar proportions 0.4 MnO, 0.2 Co$_3$O$_4$ and 1 Cr$_2$O$_3$ which should result in Mn$_{0.4}$Co$_{0.6}$Cr$_2$O$_4$ The powders mixed with water were ball milled for 48 hours. The ball-milled powders were dried overnight and then sintered in air at 1200${µbox{σmall o}}$C (S$_1$) for 10 hours. The phase purity was checked by a Rigaku X-ray diffractometer with Cu$_{µbox{τiny K}_{αlpha}}$ radiation at the Materials Research and Education Center, Auburn University, U.S.A, which indicated a single-phase character of S$_1$.

Refinement top

The neutron-powder-diffraction experiments were undertaken with the high-resolution powder diffractometer HRPD ($λambda=1.8214 (2)˛$AA) at the Neutron Scattering Laboratory of BATAN, Serpong, Indonesia. S$_1$, with the weight of 10.13 g, was loaded in cylindrical vanadium sample holders. The data were collected in the angular range $2τheta$ of $2.5\,{χirc}$ up to $157\^,{χirc}$ in an interval of approximately $0.05\,{χirc}$ at room temperature. The exact detector positions, which were not always $0.05\^,{χirc}$, were confirmed by the electronic encoder. The data reduction, including the detector efficiency correction, were performed after the measurements. Both the X-ray and neutron diffraction data of each sample were co-refined using the Rietveld refinement program GSAS χite{GSAS2000,GSAS2001}. The co-refinement provides a complementary contrast of X-ray and neutron diffraction resulting in a more robust crystallographic structural parameter set as compared to that from individual refinements. As X-ray is not sensitive to the magnetic contribution while neutron is, a good co-refinement would confirm that the diffraction would be of crystallographic rather than magnetic contribution. We also attempted to differentiate the valence of the Mn/Co at the same site using the X-ray diffraction data.

Computing details top

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
(MN0_4CO0_6CR2O4_phase_1) top
Crystal data top
Co0.15Cr0.42Mn0.19OV = 588.0 (2) Å3
Mr = 56.56Z = 32
Cubic, Fd3m Kα1, Kα2 radiation, λ = 1.821324 Å
a = 8.3777 (10) Å?; ?, ?; ? × ?; ? mm
Data collection top
2θmin = 19.802°, 2θmax = 79.802°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full2988 data points
Rp = 0.093Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 263.344 #2(GV) = -287.705 #3(GW) = 165.433 #4(LX) = 0.000 #5(LY) = 3.144 #6(trns) = 0.000 #7(asym) = 20.5532 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.13431 parameters
Rexp = 0.1020 restraints
R(F2) = 0.02849(Δ/σ)max = 0.25
χ2 = 1.322Background function: GSAS Background function number 2 with 4 terms. Cosine Fourier series 1: 66.0807 2: 24.3709 3: 12.7658 4: 4.53611
Crystal data top
Co0.15Cr0.42Mn0.19OV = 588.0 (2) Å3
Mr = 56.56Z = 32
Cubic, Fd3m Kα1, Kα2 radiation, λ = 1.821324 Å
a = 8.3777 (10) Å?; ?, ?; ? × ?; ? mm
Data collection top
2θmin = 19.802°, 2θmax = 79.802°, 2θstep = 0.05°
Refinement top
Rp = 0.0932988 data points
Rwp = 0.13431 parameters
Rexp = 0.1020 restraints
R(F2) = 0.02849(Δ/σ)max = 0.25
χ2 = 1.322
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
O-2_160.26254 (8)0.26254 (8)0.26254 (8)0.0056 (4)*
Cr+3_50.50.50.50.0107 (7)*0.831 (6)
Co+2_50.1250.1250.1250.012 (3)*0.580 (14)
Mn+2_50.1250.1250.1250.019 (4)*0.420 (14)
Mn+3_50.50.50.50.087 (17)*0.169 (6)
Geometric parameters (Å, º) top
O-2_16—Cr+3_52i1.9949 (7)Co+2_59—O-2_161.9958 (12)
O-2_16—Cr+3_52ii1.9949 (7)Co+2_59—O-2_16vii1.9958 (12)
O-2_16—Cr+3_52iii1.9949 (7)Co+2_59—O-2_16viii1.9958 (12)
O-2_16—Co+2_591.9958 (12)Co+2_59—O-2_16ix1.9958 (12)
O-2_16—Mn+2_551.9958 (12)Mn+2_55—O-2_161.9958 (12)
O-2_16—Mn+3_55i1.9949 (7)Mn+2_55—O-2_16vii1.9958 (12)
O-2_16—Mn+3_55ii1.9949 (7)Mn+2_55—O-2_16viii1.9958 (12)
O-2_16—Mn+3_55iii1.9949 (7)Mn+2_55—O-2_16ix1.9958 (12)
Cr+3_52—O-2_16iv1.9949 (7)Mn+3_55—O-2_16iv1.9949 (7)
Cr+3_52—O-2_16v1.9949 (7)Mn+3_55—O-2_16v1.9949 (7)
Cr+3_52—O-2_16vi1.9949 (7)Mn+3_55—O-2_16vi1.9949 (7)
Cr+3_52—O-2_16i1.9949 (7)Mn+3_55—O-2_16i1.9949 (7)
Cr+3_52—O-2_16ii1.9949 (7)Mn+3_55—O-2_16ii1.9949 (7)
Cr+3_52—O-2_16iii1.9949 (7)Mn+3_55—O-2_16iii1.9949 (7)
Cr+3_52—Cr+3_52iv2.9620 (4)Mn+3_55—Cr+3_52iv2.9620 (4)
Cr+3_52—Cr+3_52v2.9620 (3)Mn+3_55—Cr+3_52v2.9620 (3)
Cr+3_52—Cr+3_52vi2.9620 (3)Mn+3_55—Cr+3_52vi2.9620 (3)
Cr+3_52—Cr+3_52i2.9620 (4)Mn+3_55—Cr+3_52i2.9620 (4)
Cr+3_52—Cr+3_52ii2.9620 (3)Mn+3_55—Cr+3_52ii2.9620 (3)
Cr+3_52—Cr+3_52iii2.9620 (3)Mn+3_55—Cr+3_52iii2.9620 (3)
Cr+3_52—Mn+3_55iv2.9620 (4)Mn+3_55—Mn+3_55iv2.9620 (4)
Cr+3_52—Mn+3_55v2.9620 (3)Mn+3_55—Mn+3_55v2.9620 (3)
Cr+3_52—Mn+3_55vi2.9620 (3)Mn+3_55—Mn+3_55vi2.9620 (3)
Cr+3_52—Mn+3_55i2.9620 (4)Mn+3_55—Mn+3_55i2.9620 (4)
Cr+3_52—Mn+3_55ii2.9620 (3)Mn+3_55—Mn+3_55ii2.9620 (3)
Cr+3_52—Mn+3_55iii2.9620 (3)Mn+3_55—Mn+3_55iii2.9620 (3)
Cr+3_52x—O-2_16—Cr+3_52ii95.87 (4)O-2_16v—Cr+3_52—O-2_16xvii180.0
Cr+3_52x—O-2_16—Cr+3_52xi95.87 (4)O-2_16v—Cr+3_52—O-2_16xviii96.19 (4)
Cr+3_52xii—O-2_16—Co+2_59120.99 (3)O-2_16vi—Cr+3_52—O-2_16i96.19 (4)
Cr+3_52xiii—O-2_16—Mn+2_55120.99 (3)O-2_16vi—Cr+3_52—O-2_16xvii96.19 (4)
Cr+3_52xiii—O-2_16—Mn+3_55xiii0.0O-2_16vi—Cr+3_52—O-2_16xviii180.0
Cr+3_52xiii—O-2_16—Mn+3_55xiv95.87 (4)O-2_16i—Cr+3_52—O-2_16xvii83.81 (4)
Cr+3_52xiii—O-2_16—Mn+3_55xv95.87 (4)O-2_16i—Cr+3_52—O-2_16xviii83.81 (4)
Cr+3_52ii—O-2_16—Cr+3_52xi95.87 (4)O-2_16xvii—Cr+3_52—O-2_16xviii83.81 (4)
Cr+3_52xvi—O-2_16—Co+2_59120.99 (3)O-2_16—Co+2_59—O-2_16xix109.471 (5)
Cr+3_52xiv—O-2_16—Mn+2_55120.99 (3)O-2_16—Co+2_59—O-2_16xx109.471 (9)
Cr+3_52xiv—O-2_16—Mn+3_55xiii95.87 (4)O-2_16—Co+2_59—O-2_16xxi109.471 (5)
Cr+3_52xiv—O-2_16—Mn+3_55xiv0.0O-2_16xix—Co+2_59—O-2_16xx109.471 (5)
Cr+3_52xiv—O-2_16—Mn+3_55xv95.87 (4)O-2_16xix—Co+2_59—O-2_16xxi109.471 (9)
Cr+3_52iii—O-2_16—Co+2_59120.99 (3)O-2_16xx—Co+2_59—O-2_16xxi109.471 (5)
Cr+3_52xv—O-2_16—Mn+2_55120.99 (3)O-2_16—Mn+2_55—O-2_16xix109.471 (5)
Cr+3_52xv—O-2_16—Mn+3_55xiii95.87 (4)O-2_16—Mn+2_55—O-2_16xx109.471 (9)
Cr+3_52xv—O-2_16—Mn+3_55xiv95.87 (4)O-2_16—Mn+2_55—O-2_16xxi109.471 (5)
Cr+3_52xv—O-2_16—Mn+3_55xv0.0O-2_16xix—Mn+2_55—O-2_16xx109.471 (5)
Co+2_59—O-2_16—Mn+2_550.0O-2_16xix—Mn+2_55—O-2_16xxi109.471 (9)
Co+2_59—O-2_16—Mn+3_55xiii120.99 (3)O-2_16xx—Mn+2_55—O-2_16xxi109.471 (5)
Co+2_59—O-2_16—Mn+3_55xiv120.99 (3)O-2_16iv—Mn+3_55—O-2_16v83.81 (4)
Co+2_59—O-2_16—Mn+3_55xv120.99 (3)O-2_16iv—Mn+3_55—O-2_16vi83.81 (4)
Mn+2_55—O-2_16—Mn+3_55xiii120.99 (3)O-2_16iv—Mn+3_55—O-2_16i180.0
Mn+2_55—O-2_16—Mn+3_55xiv120.99 (3)O-2_16iv—Mn+3_55—O-2_16xvii96.19 (4)
Mn+2_55—O-2_16—Mn+3_55xv120.99 (3)O-2_16iv—Mn+3_55—O-2_16xviii96.19 (4)
Mn+3_55xiii—O-2_16—Mn+3_55xiv95.87 (4)O-2_16v—Mn+3_55—O-2_16vi83.81 (4)
Mn+3_55xiii—O-2_16—Mn+3_55xv95.87 (4)O-2_16v—Mn+3_55—O-2_16i96.19 (4)
Mn+3_55xiv—O-2_16—Mn+3_55xv95.87 (4)O-2_16v—Mn+3_55—O-2_16xvii180.0
O-2_16iv—Cr+3_52—O-2_16v83.81 (4)O-2_16v—Mn+3_55—O-2_16xviii96.19 (4)
O-2_16iv—Cr+3_52—O-2_16vi83.81 (4)O-2_16vi—Mn+3_55—O-2_16i96.19 (4)
O-2_16iv—Cr+3_52—O-2_16i180.0O-2_16vi—Mn+3_55—O-2_16xvii96.19 (4)
O-2_16iv—Cr+3_52—O-2_16xvii96.19 (4)O-2_16vi—Mn+3_55—O-2_16xviii180.0
O-2_16iv—Cr+3_52—O-2_16xviii96.19 (4)O-2_16i—Mn+3_55—O-2_16xvii83.81 (4)
O-2_16v—Cr+3_52—O-2_16vi83.81 (4)O-2_16i—Mn+3_55—O-2_16xviii83.81 (4)
O-2_16v—Cr+3_52—O-2_16i96.19 (4)O-2_16xvii—Mn+3_55—O-2_16xviii83.81 (4)
Symmetry codes: (i) x+3/4, y+3/4, z; (ii) z, x+3/4, y+3/4; (iii) y+3/4, z, x+3/4; (iv) x+1/4, y+1/4, z+1; (v) z+1, x+1/4, y+1/4; (vi) y+1/4, z+1, x+1/4; (vii) z+1/4, x, y+1/4; (viii) z+1/4, x+1/4, y; (ix) z, x3/4, y3/4; (x) x+7/4, y+3/4, z1; (xi) y+7/4, z1, x+3/4; (xii) x+3/4, y+7/4, z1; (xiii) x+3/4, y+3/4, z1; (xiv) z1, x+3/4, y+3/4; (xv) y+3/4, z1, x+3/4; (xvi) z1, x+7/4, y+3/4; (xvii) z1, x+3/4, y+7/4; (xviii) y+3/4, z1, x+7/4; (xix) z3/4, x2, y3/4; (xx) z3/4, x7/4, y1; (xxi) z1, x3/4, y+1/4.
(MNCO2O4_phase_1) top
Crystal data top
Co0.43Mn0.32OV = 565.31 (19) Å3
Mr = 58.91Z = 32
Cubic, Fd3m Kα1, Kα2 radiation, λ = 1.819625 Å
a = 8.2685 (9) Å?; ?, ?; ? × ?; ? mm
Data collection top
2θmin = 27.827°, 2θmax = 67.827°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3027 data points
Rp = 0.112Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 818.360 #2(GV) = -0.100 #3(GW) = 0.100 #4(LX) = 0.000 #5(LY) = 9.280 #6(trns) = 0.000 #7(asym) = 34.2836 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.14731 parameters
Rexp = 0.1170 restraints
R(F2) = 0.10144(Δ/σ)max = 0.96
χ2 = 1.464Background function: GSAS Background function number 2 with 4 terms. Cosine Fourier series 1: 56.9702 2: 8.51500 3: 6.57185 4: 2.68720
Crystal data top
Co0.43Mn0.32OV = 565.31 (19) Å3
Mr = 58.91Z = 32
Cubic, Fd3m Kα1, Kα2 radiation, λ = 1.819625 Å
a = 8.2685 (9) Å?; ?, ?; ? × ?; ? mm
Data collection top
2θmin = 27.827°, 2θmax = 67.827°, 2θstep = 0.05°
Refinement top
Rp = 0.1123027 data points
Rwp = 0.14731 parameters
Rexp = 0.1170 restraints
R(F2) = 0.10144(Δ/σ)max = 0.96
χ2 = 1.464
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
O-2_160.26242 (14)0.26242 (14)0.26242 (14)0.0173 (9)*
Co+3_50.50.50.50.015 (4)*0.427 (15)
Mn+3_50.50.50.50.021 (3)*0.573 (15)
Mn+2_50.1250.1250.1250.04 (2)*0.143 (27)
Co+2_50.1250.1250.1250.013 (4)*0.857 (27)
Geometric parameters (Å, º) top
O-2_16—Co+3_59i1.9698 (10)Mn+3_55—O-2_16i1.9698 (10)
O-2_16—Co+3_59ii1.9698 (10)Mn+3_55—O-2_16ii1.9698 (10)
O-2_16—Co+3_59iii1.9698 (10)Mn+3_55—O-2_16iii1.9698 (10)
O-2_16—Mn+3_55i1.9698 (10)Mn+3_55—Co+3_59iv2.9234 (3)
O-2_16—Mn+3_55ii1.9698 (10)Mn+3_55—Co+3_59v2.9234 (2)
O-2_16—Mn+3_55iii1.9698 (10)Mn+3_55—Co+3_59vi2.9234 (2)
O-2_16—Mn+2_551.968 (2)Mn+3_55—Co+3_59i2.9234 (3)
O-2_16—Co+2_591.968 (2)Mn+3_55—Co+3_59ii2.9234 (2)
Co+3_59—O-2_16iv1.9698 (10)Mn+3_55—Co+3_59iii2.9234 (2)
Co+3_59—O-2_16v1.9698 (10)Mn+3_55—Mn+3_55iv2.9234 (3)
Co+3_59—O-2_16vi1.9698 (10)Mn+3_55—Mn+3_55v2.9234 (2)
Co+3_59—O-2_16i1.9698 (10)Mn+3_55—Mn+3_55vi2.9234 (2)
Co+3_59—O-2_16ii1.9698 (10)Mn+3_55—Mn+3_55i2.9234 (3)
Co+3_59—O-2_16iii1.9698 (10)Mn+3_55—Mn+3_55ii2.9234 (2)
Co+3_59—Mn+3_55iv2.9234 (3)Mn+3_55—Mn+3_55iii2.9234 (2)
Co+3_59—Mn+3_55v2.9234 (2)Mn+2_55—O-2_161.968 (2)
Co+3_59—Mn+3_55vi2.9234 (2)Mn+2_55—O-2_16vii1.968 (2)
Co+3_59—Mn+3_55i2.9234 (3)Mn+2_55—O-2_16viii1.968 (2)
Co+3_59—Mn+3_55ii2.9234 (2)Mn+2_55—O-2_16ix1.968 (2)
Co+3_59—Mn+3_55iii2.9234 (2)Co+2_59—O-2_161.968 (2)
Mn+3_55—O-2_16iv1.9698 (10)Co+2_59—O-2_16vii1.968 (2)
Mn+3_55—O-2_16v1.9698 (10)Co+2_59—O-2_16viii1.968 (2)
Mn+3_55—O-2_16vi1.9698 (10)Co+2_59—O-2_16ix1.968 (2)
Co+3_59x—O-2_16—Co+3_59ii95.81 (7)O-2_16v—Co+3_59—O-2_16xvii180.0
Co+3_59x—O-2_16—Co+3_59xi95.81 (7)O-2_16v—Co+3_59—O-2_16xviii96.13 (7)
Co+3_59xii—O-2_16—Mn+3_55xii0.0O-2_16vi—Co+3_59—O-2_16i96.13 (7)
Co+3_59xii—O-2_16—Mn+3_55xiii95.81 (7)O-2_16vi—Co+3_59—O-2_16xvii96.13 (7)
Co+3_59xii—O-2_16—Mn+3_55iii95.81 (7)O-2_16vi—Co+3_59—O-2_16xviii180.0
Co+3_59xiv—O-2_16—Mn+2_55121.04 (5)O-2_16i—Co+3_59—O-2_16xvii83.87 (7)
Co+3_59xiv—O-2_16—Co+2_59121.04 (5)O-2_16i—Co+3_59—O-2_16xviii83.87 (7)
Co+3_59ii—O-2_16—Co+3_59xi95.81 (7)O-2_16xvii—Co+3_59—O-2_16xviii83.87 (7)
Co+3_59xiii—O-2_16—Mn+3_55xii95.81 (7)O-2_16iv—Mn+3_55—O-2_16v83.87 (7)
Co+3_59xiii—O-2_16—Mn+3_55xiii0.0O-2_16iv—Mn+3_55—O-2_16vi83.87 (7)
Co+3_59xiii—O-2_16—Mn+3_55iii95.81 (7)O-2_16iv—Mn+3_55—O-2_16i180.0
Co+3_59xv—O-2_16—Mn+2_55121.04 (5)O-2_16iv—Mn+3_55—O-2_16xvii96.13 (7)
Co+3_59xv—O-2_16—Co+2_59121.04 (5)O-2_16iv—Mn+3_55—O-2_16xviii96.13 (7)
Co+3_59iii—O-2_16—Mn+3_55xii95.81 (7)O-2_16v—Mn+3_55—O-2_16vi83.87 (7)
Co+3_59iii—O-2_16—Mn+3_55xiii95.81 (7)O-2_16v—Mn+3_55—O-2_16i96.13 (7)
Co+3_59iii—O-2_16—Mn+3_55iii0.0O-2_16v—Mn+3_55—O-2_16xvii180.0
Co+3_59xvi—O-2_16—Mn+2_55121.04 (5)O-2_16v—Mn+3_55—O-2_16xviii96.13 (7)
Co+3_59xvi—O-2_16—Co+2_59121.04 (5)O-2_16vi—Mn+3_55—O-2_16i96.13 (7)
Mn+3_55xii—O-2_16—Mn+3_55xiii95.81 (7)O-2_16vi—Mn+3_55—O-2_16xvii96.13 (7)
Mn+3_55xii—O-2_16—Mn+3_55iii95.81 (7)O-2_16vi—Mn+3_55—O-2_16xviii180.0
Mn+3_55xiv—O-2_16—Mn+2_55121.04 (5)O-2_16i—Mn+3_55—O-2_16xvii83.87 (7)
Mn+3_55xiv—O-2_16—Co+2_59121.04 (5)O-2_16i—Mn+3_55—O-2_16xviii83.87 (7)
Mn+3_55xiii—O-2_16—Mn+3_55iii95.81 (7)O-2_16xvii—Mn+3_55—O-2_16xviii83.87 (7)
Mn+3_55xv—O-2_16—Mn+2_55121.04 (5)O-2_16—Mn+2_55—O-2_16xix109.471 (4)
Mn+3_55xv—O-2_16—Co+2_59121.04 (5)O-2_16—Mn+2_55—O-2_16xx109.471 (9)
Mn+3_55xvi—O-2_16—Mn+2_55121.04 (5)O-2_16—Mn+2_55—O-2_16xxi109.471 (4)
Mn+3_55xvi—O-2_16—Co+2_59121.04 (5)O-2_16xix—Mn+2_55—O-2_16xx109.471 (4)
Mn+2_55—O-2_16—Co+2_590.0O-2_16xix—Mn+2_55—O-2_16xxi109.471 (9)
O-2_16iv—Co+3_59—O-2_16v83.87 (7)O-2_16xx—Mn+2_55—O-2_16xxi109.471 (4)
O-2_16iv—Co+3_59—O-2_16vi83.87 (7)O-2_16—Co+2_59—O-2_16xix109.471 (4)
O-2_16iv—Co+3_59—O-2_16i180.0O-2_16—Co+2_59—O-2_16xx109.471 (9)
O-2_16iv—Co+3_59—O-2_16xvii96.13 (7)O-2_16—Co+2_59—O-2_16xxi109.471 (4)
O-2_16iv—Co+3_59—O-2_16xviii96.13 (7)O-2_16xix—Co+2_59—O-2_16xx109.471 (4)
O-2_16v—Co+3_59—O-2_16vi83.87 (7)O-2_16xix—Co+2_59—O-2_16xxi109.471 (9)
O-2_16v—Co+3_59—O-2_16i96.13 (7)O-2_16xx—Co+2_59—O-2_16xxi109.471 (4)
Symmetry codes: (i) x+3/4, y+3/4, z; (ii) z, x+3/4, y+3/4; (iii) y+3/4, z, x+3/4; (iv) x+1/4, y+1/4, z+1; (v) z+1, x+1/4, y+1/4; (vi) y+1/4, z+1, x+1/4; (vii) z+1/4, x, y+1/4; (viii) z+1/4, x+1/4, y; (ix) z, x3/4, y3/4; (x) x+7/4, y+3/4, z1; (xi) y+7/4, z1, x+3/4; (xii) x+3/4, y+7/4, z1; (xiii) z1, x+7/4, y+3/4; (xiv) x+3/4, y+3/4, z1; (xv) z1, x+3/4, y+3/4; (xvi) y+3/4, z1, x+3/4; (xvii) z1, x+3/4, y+7/4; (xviii) y+3/4, z1, x+7/4; (xix) z3/4, x2, y3/4; (xx) z3/4, x7/4, y1; (xxi) z1, x3/4, y+1/4.
(MN1_5CO1_5O4_phase_1) top
Crystal data top
Co0.23Mn0.52OV = 301.09 (14) Å3
Mr = 58.12Z = 16
Tetragonal, I41/amd Kα1, Kα2 radiation, λ = 1.82122 Å
a = 5.7184 (10) Å?; ?, ?; ? × ?; ? mm
c = 9.208 (2) Å
Data collection top
2θmin = 27.893°, 2θmax = 67.893°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3100 data points
Rp = 0.106Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 3038.690 #2(GV) = -550.261 #3(GW) = 0.100 #4(LX) = 0.000 #5(LY) = 29.941 #6(trns) = 0.000 #7(asym) = 9.7056 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 3038.690 #2(GV) = -550.261 #3(GW) = 0.100 #4(LX) = 0.000 #5(LY) = 29.941 #6(trns) = 0.000 #7(asym) = 9.7056 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.13735 parameters
Rexp = 0.0960 restraints
R(F2) = 0.13557(Δ/σ)max = 1.25
χ2 = 1.796Background function: GSAS Background function number 2 with 6 terms. Cosine Fourier series 1: 84.6776 2: 10.3679 3: 14.2859 4: 6.45260 5: 3.12375 6: 4.31977
Crystal data top
Co0.23Mn0.52OV = 301.09 (14) Å3
Mr = 58.12Z = 16
Tetragonal, I41/amd Kα1, Kα2 radiation, λ = 1.82122 Å
a = 5.7184 (10) Å?; ?, ?; ? × ?; ? mm
c = 9.208 (2) Å
Data collection top
2θmin = 27.893°, 2θmax = 67.893°, 2θstep = 0.05°
Refinement top
Rp = 0.1063100 data points
Rwp = 0.13735 parameters
Rexp = 0.0960 restraints
R(F2) = 0.13557(Δ/σ)max = 1.25
χ2 = 1.796
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
O-2_160.00.4770 (10)0.2615 (6)0.0100 (15)*
Co+3_50.00.00.50.8 (18)*0.042 (19)
Mn+3_50.00.00.50.005*0.958 (19)
Co+2_50.00.750.1250.005*0.830 (25)
Mn+2_50.00.750.1250.004*0.170 (25)
Geometric parameters (Å, º) top
O-2_16—Co+3_59i1.934 (4)Mn+3_55—O-2_16iv1.934 (4)
O-2_16—Co+3_59ii1.934 (4)Mn+3_55—O-2_16ii1.934 (4)
O-2_16—Co+3_59iii2.200 (6)Mn+3_55—O-2_16iii2.200 (6)
O-2_16—Mn+3_55i1.934 (4)Mn+3_55—O-2_16v1.934 (4)
O-2_16—Mn+3_55ii1.934 (4)Mn+3_55—O-2_16vi2.200 (6)
O-2_16—Mn+3_55iii2.200 (6)Mn+3_55—O-2_16vii1.934 (4)
O-2_16—Co+2_592.004 (5)Mn+3_55—Co+3_59viii2.8592 (5)
O-2_16—Mn+2_552.004 (5)Mn+3_55—Co+3_59iii2.8592 (5)
Co+3_59—O-2_16iv1.934 (4)Mn+3_55—Mn+3_55viii2.8592 (5)
Co+3_59—O-2_16ii1.934 (4)Mn+3_55—Mn+3_55iii2.8592 (5)
Co+3_59—O-2_16iii2.200 (6)Co+2_59—O-2_162.004 (5)
Co+3_59—O-2_16v1.934 (4)Co+2_59—O-2_16ix2.004 (5)
Co+3_59—O-2_16vi2.200 (6)Co+2_59—O-2_16x2.004 (5)
Co+3_59—O-2_16vii1.934 (4)Co+2_59—O-2_16xi2.004 (5)
Co+3_59—Co+3_59viii2.8592 (5)Mn+2_55—O-2_162.004 (5)
Co+3_59—Co+3_59iii2.8592 (5)Mn+2_55—O-2_16ix2.004 (5)
Co+3_59—Mn+3_55viii2.8592 (5)Mn+2_55—O-2_16x2.004 (5)
Co+3_59—Mn+3_55iii2.8592 (5)Mn+2_55—O-2_16xi2.004 (5)
Co+3_59i—O-2_16—Co+3_59xii95.3 (3)O-2_16xiii—Co+3_59—O-2_16xiv180.0
Co+3_59i—O-2_16—Mn+3_55i0.0O-2_16iv—Mn+3_55—O-2_16ii180.0
Co+3_59i—O-2_16—Mn+3_55ii95.3 (3)O-2_16iv—Mn+3_55—O-2_16xiii84.3 (3)
Co+3_59i—O-2_16—Co+2_59119.25 (19)O-2_16iv—Mn+3_55—O-2_16xiv95.7 (3)
Co+3_59i—O-2_16—Mn+2_55119.25 (19)O-2_16ii—Mn+3_55—O-2_16xiii95.7 (3)
Co+3_59ii—O-2_16—Mn+3_55i95.3 (3)O-2_16ii—Mn+3_55—O-2_16xiv84.3 (3)
Co+3_59ii—O-2_16—Mn+3_55ii0.0O-2_16xiii—Mn+3_55—O-2_16xiv180.0
Co+3_59ii—O-2_16—Co+2_59119.25 (19)O-2_16—Co+2_59—O-2_16ix113.15 (18)
Co+3_59xii—O-2_16—Mn+2_55119.25 (19)O-2_16—Co+2_59—O-2_16xv102.4 (3)
Mn+3_55i—O-2_16—Mn+3_55ii95.3 (3)O-2_16—Co+2_59—O-2_16xvi113.15 (18)
Mn+3_55i—O-2_16—Co+2_59119.25 (19)O-2_16ix—Co+2_59—O-2_16xv113.15 (18)
Mn+3_55i—O-2_16—Mn+2_55119.25 (19)O-2_16ix—Co+2_59—O-2_16xvi102.4 (3)
Mn+3_55ii—O-2_16—Co+2_59119.25 (19)O-2_16xv—Co+2_59—O-2_16xvi113.15 (18)
Mn+3_55xii—O-2_16—Mn+2_55119.25 (19)O-2_16—Mn+2_55—O-2_16ix113.15 (18)
Co+2_59—O-2_16—Mn+2_550.0O-2_16—Mn+2_55—O-2_16xv102.4 (3)
O-2_16iv—Co+3_59—O-2_16ii180.0O-2_16—Mn+2_55—O-2_16xvi113.15 (18)
O-2_16iv—Co+3_59—O-2_16xiii84.3 (3)O-2_16ix—Mn+2_55—O-2_16xv113.15 (18)
O-2_16iv—Co+3_59—O-2_16xiv95.7 (3)O-2_16ix—Mn+2_55—O-2_16xvi102.4 (3)
O-2_16ii—Co+3_59—O-2_16xiii95.7 (3)O-2_16xv—Mn+2_55—O-2_16xvi113.15 (18)
O-2_16ii—Co+3_59—O-2_16xiv84.3 (3)
Symmetry codes: (i) y+1/4, x+1/4, z1/4; (ii) y1/4, x+1/4, z+3/4; (iii) x, y+1/2, z; (iv) y+1/4, x1/4, z+1/4; (v) y1/4, x1/4, z+1/4; (vi) x1, y3/2, z; (vii) y3/4, x3/4, z1/4; (viii) x, y1/2, z; (ix) y+3/4, x+3/4, z+1/4; (x) x, y+3/2, z; (xi) y7/4, x1/4, z3/4; (xii) y1/4, x+5/4, z+3/4; (xiii) y5/4, x5/4, z7/4; (xiv) y3/4, x3/4, z+3/4; (xv) x2, y+1/2, z2; (xvi) y7/4, x+3/4, z3/4.
(MN1_5CO1_5O4_phase_2) top
Crystal data top
Co0.33Mn0.42OV = 572.1 (3) Å3
Mr = 58.54Z = 32
Cubic, Fd3m Kα1, Kα2 radiation, λ = 1.82122 Å
a = 8.3015 (13) Å?; ?, ?; ? × ?; ? mm
Data collection top
2θmin = 27.893°, 2θmax = 67.893°, 2θstep = 0.05°
Refinement top
Least-squares matrix: full3100 data points
Rp = 0.106Profile function: CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 3038.690 #2(GV) = -550.261 #3(GW) = 0.100 #4(LX) = 0.000 #5(LY) = 29.941 #6(trns) = 0.000 #7(asym) = 9.7056 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 2 with 18 terms Profile coefficients for Simpson's rule integration of pseudovoigt function C.J. Howard (1982). J. Appl. Cryst.,15,615-620. P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. #1(GU) = 3038.690 #2(GV) = -550.261 #3(GW) = 0.100 #4(LX) = 0.000 #5(LY) = 29.941 #6(trns) = 0.000 #7(asym) = 9.7056 #8(shft) = 0.0000 #9(GP) = 0.000 #10(stec)= 0.00 #11(ptec)= 0.00 #12(sfec)= 0.00 #13(L11) = 0.000 #14(L22) = 0.000 #15(L33) = 0.000 #16(L12) = 0.000 #17(L13) = 0.000 #18(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rwp = 0.13735 parameters
Rexp = 0.0960 restraints
R(F2) = 0.13557(Δ/σ)max = 1.25
χ2 = 1.796Background function: GSAS Background function number 2 with 6 terms. Cosine Fourier series 1: 84.6776 2: 10.3679 3: 14.2859 4: 6.45260 5: 3.12375 6: 4.31977
Crystal data top
Co0.33Mn0.42OV = 572.1 (3) Å3
Mr = 58.54Z = 32
Cubic, Fd3m Kα1, Kα2 radiation, λ = 1.82122 Å
a = 8.3015 (13) Å?; ?, ?; ? × ?; ? mm
Data collection top
2θmin = 27.893°, 2θmax = 67.893°, 2θstep = 0.05°
Refinement top
Rp = 0.1063100 data points
Rwp = 0.13735 parameters
Rexp = 0.0960 restraints
R(F2) = 0.13557(Δ/σ)max = 1.25
χ2 = 1.796
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
O10.2618 (3)0.2618 (3)0.2618 (3)0.0286 (14)*
Co+3BN0.50.50.50.004*0.216 (14)
Mn+3BN0.50.50.50.030 (3)*0.784 (14)
Mn+2AN0.1250.1250.1250.004*0.098 (18)
Co+2AN0.1250.1250.1250.004*0.902 (18)
Geometric parameters (Å, º) top
O1—Co+3BNi1.983 (2)Mn+3BN—O1i1.983 (2)
O1—Co+3BNii1.983 (2)Mn+3BN—O1ii1.983 (2)
O1—Co+3BNiii1.983 (2)Mn+3BN—O1iii1.983 (2)
O1—Mn+3BNi1.983 (2)Mn+3BN—Co+3BNiv2.9350 (4)
O1—Mn+3BNii1.983 (2)Mn+3BN—Co+3BNv2.9350 (3)
O1—Mn+3BNiii1.983 (2)Mn+3BN—Co+3BNvi2.9350 (3)
O1—Mn+2AN1.966 (4)Mn+3BN—Co+3BNi2.9350 (4)
O1—Co+2AN1.966 (4)Mn+3BN—Co+3BNii2.9350 (3)
Co+3BN—O1iv1.983 (2)Mn+3BN—Co+3BNiii2.9350 (3)
Co+3BN—O1v1.983 (2)Mn+3BN—Mn+3BNiv2.9350 (4)
Co+3BN—O1vi1.983 (2)Mn+3BN—Mn+3BNv2.9350 (3)
Co+3BN—O1i1.983 (2)Mn+3BN—Mn+3BNvi2.9350 (3)
Co+3BN—O1ii1.983 (2)Mn+3BN—Mn+3BNi2.9350 (4)
Co+3BN—O1iii1.983 (2)Mn+3BN—Mn+3BNii2.9350 (3)
Co+3BN—Mn+3BNiv2.9350 (4)Mn+3BN—Mn+3BNiii2.9350 (3)
Co+3BN—Mn+3BNv2.9350 (3)Mn+2AN—O11.966 (4)
Co+3BN—Mn+3BNvi2.9350 (3)Mn+2AN—O1vii1.966 (4)
Co+3BN—Mn+3BNi2.9350 (4)Mn+2AN—O1viii1.966 (4)
Co+3BN—Mn+3BNii2.9350 (3)Mn+2AN—O1ix1.966 (4)
Co+3BN—Mn+3BNiii2.9350 (3)Co+2AN—O11.966 (4)
Mn+3BN—O1iv1.983 (2)Co+2AN—O1vii1.966 (4)
Mn+3BN—O1v1.983 (2)Co+2AN—O1viii1.966 (4)
Mn+3BN—O1vi1.983 (2)Co+2AN—O1ix1.966 (4)
Co+3BNx—O1—Co+3BNii95.50 (14)O1v—Co+3BN—O1xvii180.0
Co+3BNx—O1—Co+3BNxi95.50 (14)O1v—Co+3BN—O1xviii95.78 (15)
Co+3BNxii—O1—Mn+3BNxii0.0O1vi—Co+3BN—O1i95.78 (15)
Co+3BNxii—O1—Mn+3BNxiii95.50 (14)O1vi—Co+3BN—O1xvii95.78 (15)
Co+3BNxii—O1—Mn+3BNiii95.50 (14)O1vi—Co+3BN—O1xviii180.0
Co+3BNxiv—O1—Mn+2AN121.27 (10)O1i—Co+3BN—O1xvii84.22 (15)
Co+3BNxiv—O1—Co+2AN121.27 (10)O1i—Co+3BN—O1xviii84.22 (15)
Co+3BNii—O1—Co+3BNxi95.50 (14)O1xvii—Co+3BN—O1xviii84.22 (15)
Co+3BNxiii—O1—Mn+3BNxii95.50 (14)O1iv—Mn+3BN—O1v84.22 (15)
Co+3BNxiii—O1—Mn+3BNxiii0.0O1iv—Mn+3BN—O1vi84.22 (15)
Co+3BNxiii—O1—Mn+3BNiii95.50 (14)O1iv—Mn+3BN—O1i180.0
Co+3BNxv—O1—Mn+2AN121.27 (10)O1iv—Mn+3BN—O1xvii95.78 (15)
Co+3BNxv—O1—Co+2AN121.27 (10)O1iv—Mn+3BN—O1xviii95.78 (15)
Co+3BNiii—O1—Mn+3BNxii95.50 (14)O1v—Mn+3BN—O1vi84.22 (15)
Co+3BNiii—O1—Mn+3BNxiii95.50 (14)O1v—Mn+3BN—O1i95.78 (15)
Co+3BNiii—O1—Mn+3BNiii0.0O1v—Mn+3BN—O1xvii180.0
Co+3BNxvi—O1—Mn+2AN121.27 (10)O1v—Mn+3BN—O1xviii95.78 (15)
Co+3BNxvi—O1—Co+2AN121.27 (10)O1vi—Mn+3BN—O1i95.78 (15)
Mn+3BNxii—O1—Mn+3BNxiii95.50 (14)O1vi—Mn+3BN—O1xvii95.78 (15)
Mn+3BNxii—O1—Mn+3BNiii95.50 (14)O1vi—Mn+3BN—O1xviii180.0
Mn+3BNxiv—O1—Mn+2AN121.27 (10)O1i—Mn+3BN—O1xvii84.22 (15)
Mn+3BNxiv—O1—Co+2AN121.27 (10)O1i—Mn+3BN—O1xviii84.22 (15)
Mn+3BNxiii—O1—Mn+3BNiii95.50 (14)O1xvii—Mn+3BN—O1xviii84.22 (15)
Mn+3BNxv—O1—Mn+2AN121.27 (10)O1—Mn+2AN—O1xix109.471 (6)
Mn+3BNxv—O1—Co+2AN121.27 (10)O1—Mn+2AN—O1xx109.471 (12)
Mn+3BNxvi—O1—Mn+2AN121.27 (10)O1—Mn+2AN—O1xxi109.471 (6)
Mn+3BNxvi—O1—Co+2AN121.27 (10)O1xix—Mn+2AN—O1xx109.471 (6)
Mn+2AN—O1—Co+2AN0.0O1xix—Mn+2AN—O1xxi109.471 (12)
O1iv—Co+3BN—O1v84.22 (15)O1xx—Mn+2AN—O1xxi109.471 (6)
O1iv—Co+3BN—O1vi84.22 (15)O1—Co+2AN—O1xix109.471 (6)
O1iv—Co+3BN—O1i180.0O1—Co+2AN—O1xx109.471 (12)
O1iv—Co+3BN—O1xvii95.78 (15)O1—Co+2AN—O1xxi109.471 (6)
O1iv—Co+3BN—O1xviii95.78 (15)O1xix—Co+2AN—O1xx109.471 (6)
O1v—Co+3BN—O1vi84.22 (15)O1xix—Co+2AN—O1xxi109.471 (12)
O1v—Co+3BN—O1i95.78 (15)O1xx—Co+2AN—O1xxi109.471 (6)
Symmetry codes: (i) x+3/4, y+3/4, z; (ii) z, x+3/4, y+3/4; (iii) y+3/4, z, x+3/4; (iv) x+1/4, y+1/4, z+1; (v) z+1, x+1/4, y+1/4; (vi) y+1/4, z+1, x+1/4; (vii) z+1/4, x, y+1/4; (viii) z+1/4, x+1/4, y; (ix) z, x3/4, y3/4; (x) x+7/4, y+3/4, z1; (xi) y+7/4, z1, x+3/4; (xii) x+3/4, y+7/4, z1; (xiii) z1, x+7/4, y+3/4; (xiv) x+3/4, y+3/4, z1; (xv) z1, x+3/4, y+3/4; (xvi) y+3/4, z1, x+3/4; (xvii) z1, x+3/4, y+7/4; (xviii) y+3/4, z1, x+7/4; (xix) z3/4, x2, y3/4; (xx) z3/4, x7/4, y1; (xxi) z1, x3/4, y+1/4.

Experimental details

(MN0_4CO0_6CR2O4_phase_1)(MNCO2O4_phase_1)(MN1_5CO1_5O4_phase_1)(MN1_5CO1_5O4_phase_2)
Crystal data
Chemical formulaCo0.15Cr0.42Mn0.19OCo0.43Mn0.32OCo0.23Mn0.52OCo0.33Mn0.42O
Mr56.5658.9158.1258.54
Crystal system, space groupCubic, Fd3mCubic, Fd3mTetragonal, I41/amdCubic, Fd3m
Temperature (K)????
a, b, c (Å)8.3777 (10), 8.3777, 8.37778.2685 (9), 8.2685, 8.26855.7184 (10), 5.7184, 9.208 (2)8.3015 (13), 8.3015, 8.3015
α, β, γ (°)90, 90, 9090, 90, 9090, 90, 9090, 90, 90
V3)588.0 (2)565.31 (19)301.09 (14)572.1 (3)
Z32321632
Radiation type Kα1, Kα2, λ = 1.821324 Å Kα1, Kα2, λ = 1.819625 Å Kα1, Kα2, λ = 1.82122 Å Kα1, Kα2, λ = 1.82122 Å
Specimen shape, size (mm)?; ?, ?; ? × ?; ??; ?, ?; ? × ?; ??; ?, ?; ? × ?; ??; ?, ?; ? × ?; ?
Data collection
Diffractometer?; ??; ??; ??; ?
Specimen mounting?; ??; ??; ??; ?
Data collection mode?; ??; ??; ??; ?
Scan method?; ??; ??; ??; ?
2θ values (°)2θmin = 19.802 2θmax = 79.802 2θstep = 0.052θmin = 27.827 2θmax = 67.827 2θstep = 0.052θmin = 27.893 2θmax = 67.893 2θstep = 0.052θmin = 27.893 2θmax = 67.893 2θstep = 0.05
Refinement
R factors and goodness of fitRp = 0.093, Rwp = 0.134, Rexp = 0.102, R(F2) = 0.02849, χ2 = 1.322Rp = 0.112, Rwp = 0.147, Rexp = 0.117, R(F2) = 0.10144, χ2 = 1.464Rp = 0.106, Rwp = 0.137, Rexp = 0.096, R(F2) = 0.13557, χ2 = 1.796Rp = 0.106, Rwp = 0.137, Rexp = 0.096, R(F2) = 0.13557, χ2 = 1.796
No. of data points2988302731003100
No. of parameters31313535
(Δ/σ)max0.250.961.251.25

Computer programs: GSAS.

 

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