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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
| 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 |
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$_1$.
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.
(MN0_4CO0_6CR2O4_phase_1)
top
Crystal data top
Co0.15Cr0.42Mn0.19O | V = 588.0 (2) Å3 |
Mr = 56.56 | Z = 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: full | 2988 data points |
Rp = 0.093 | Profile 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 = 0.134 | 31 parameters |
Rexp = 0.102 | 0 restraints |
R(F2) = 0.02849 | (Δ/σ)max = 0.25 |
χ2 = 1.322 | Background 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
Co0.15Cr0.42Mn0.19O | V = 588.0 (2) Å3 |
Mr = 56.56 | Z = 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 = 0.093 | 2988 data points |
Rwp = 0.134 | 31 parameters |
Rexp = 0.102 | 0 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
O-2_16 | 0.26254 (8) | 0.26254 (8) | 0.26254 (8) | 0.0056 (4)* | |
Cr+3_5 | 0.5 | 0.5 | 0.5 | 0.0107 (7)* | 0.831 (6) |
Co+2_5 | 0.125 | 0.125 | 0.125 | 0.012 (3)* | 0.580 (14) |
Mn+2_5 | 0.125 | 0.125 | 0.125 | 0.019 (4)* | 0.420 (14) |
Mn+3_5 | 0.5 | 0.5 | 0.5 | 0.087 (17)* | 0.169 (6) |
Geometric parameters (Å, º) top
O-2_16—Cr+3_52i | 1.9949 (7) | Co+2_59—O-2_16 | 1.9958 (12) |
O-2_16—Cr+3_52ii | 1.9949 (7) | Co+2_59—O-2_16vii | 1.9958 (12) |
O-2_16—Cr+3_52iii | 1.9949 (7) | Co+2_59—O-2_16viii | 1.9958 (12) |
O-2_16—Co+2_59 | 1.9958 (12) | Co+2_59—O-2_16ix | 1.9958 (12) |
O-2_16—Mn+2_55 | 1.9958 (12) | Mn+2_55—O-2_16 | 1.9958 (12) |
O-2_16—Mn+3_55i | 1.9949 (7) | Mn+2_55—O-2_16vii | 1.9958 (12) |
O-2_16—Mn+3_55ii | 1.9949 (7) | Mn+2_55—O-2_16viii | 1.9958 (12) |
O-2_16—Mn+3_55iii | 1.9949 (7) | Mn+2_55—O-2_16ix | 1.9958 (12) |
Cr+3_52—O-2_16iv | 1.9949 (7) | Mn+3_55—O-2_16iv | 1.9949 (7) |
Cr+3_52—O-2_16v | 1.9949 (7) | Mn+3_55—O-2_16v | 1.9949 (7) |
Cr+3_52—O-2_16vi | 1.9949 (7) | Mn+3_55—O-2_16vi | 1.9949 (7) |
Cr+3_52—O-2_16i | 1.9949 (7) | Mn+3_55—O-2_16i | 1.9949 (7) |
Cr+3_52—O-2_16ii | 1.9949 (7) | Mn+3_55—O-2_16ii | 1.9949 (7) |
Cr+3_52—O-2_16iii | 1.9949 (7) | Mn+3_55—O-2_16iii | 1.9949 (7) |
Cr+3_52—Cr+3_52iv | 2.9620 (4) | Mn+3_55—Cr+3_52iv | 2.9620 (4) |
Cr+3_52—Cr+3_52v | 2.9620 (3) | Mn+3_55—Cr+3_52v | 2.9620 (3) |
Cr+3_52—Cr+3_52vi | 2.9620 (3) | Mn+3_55—Cr+3_52vi | 2.9620 (3) |
Cr+3_52—Cr+3_52i | 2.9620 (4) | Mn+3_55—Cr+3_52i | 2.9620 (4) |
Cr+3_52—Cr+3_52ii | 2.9620 (3) | Mn+3_55—Cr+3_52ii | 2.9620 (3) |
Cr+3_52—Cr+3_52iii | 2.9620 (3) | Mn+3_55—Cr+3_52iii | 2.9620 (3) |
Cr+3_52—Mn+3_55iv | 2.9620 (4) | Mn+3_55—Mn+3_55iv | 2.9620 (4) |
Cr+3_52—Mn+3_55v | 2.9620 (3) | Mn+3_55—Mn+3_55v | 2.9620 (3) |
Cr+3_52—Mn+3_55vi | 2.9620 (3) | Mn+3_55—Mn+3_55vi | 2.9620 (3) |
Cr+3_52—Mn+3_55i | 2.9620 (4) | Mn+3_55—Mn+3_55i | 2.9620 (4) |
Cr+3_52—Mn+3_55ii | 2.9620 (3) | Mn+3_55—Mn+3_55ii | 2.9620 (3) |
Cr+3_52—Mn+3_55iii | 2.9620 (3) | Mn+3_55—Mn+3_55iii | 2.9620 (3) |
| | | |
Cr+3_52x—O-2_16—Cr+3_52ii | 95.87 (4) | O-2_16v—Cr+3_52—O-2_16xvii | 180.0 |
Cr+3_52x—O-2_16—Cr+3_52xi | 95.87 (4) | O-2_16v—Cr+3_52—O-2_16xviii | 96.19 (4) |
Cr+3_52xii—O-2_16—Co+2_59 | 120.99 (3) | O-2_16vi—Cr+3_52—O-2_16i | 96.19 (4) |
Cr+3_52xiii—O-2_16—Mn+2_55 | 120.99 (3) | O-2_16vi—Cr+3_52—O-2_16xvii | 96.19 (4) |
Cr+3_52xiii—O-2_16—Mn+3_55xiii | 0.0 | O-2_16vi—Cr+3_52—O-2_16xviii | 180.0 |
Cr+3_52xiii—O-2_16—Mn+3_55xiv | 95.87 (4) | O-2_16i—Cr+3_52—O-2_16xvii | 83.81 (4) |
Cr+3_52xiii—O-2_16—Mn+3_55xv | 95.87 (4) | O-2_16i—Cr+3_52—O-2_16xviii | 83.81 (4) |
Cr+3_52ii—O-2_16—Cr+3_52xi | 95.87 (4) | O-2_16xvii—Cr+3_52—O-2_16xviii | 83.81 (4) |
Cr+3_52xvi—O-2_16—Co+2_59 | 120.99 (3) | O-2_16—Co+2_59—O-2_16xix | 109.471 (5) |
Cr+3_52xiv—O-2_16—Mn+2_55 | 120.99 (3) | O-2_16—Co+2_59—O-2_16xx | 109.471 (9) |
Cr+3_52xiv—O-2_16—Mn+3_55xiii | 95.87 (4) | O-2_16—Co+2_59—O-2_16xxi | 109.471 (5) |
Cr+3_52xiv—O-2_16—Mn+3_55xiv | 0.0 | O-2_16xix—Co+2_59—O-2_16xx | 109.471 (5) |
Cr+3_52xiv—O-2_16—Mn+3_55xv | 95.87 (4) | O-2_16xix—Co+2_59—O-2_16xxi | 109.471 (9) |
Cr+3_52iii—O-2_16—Co+2_59 | 120.99 (3) | O-2_16xx—Co+2_59—O-2_16xxi | 109.471 (5) |
Cr+3_52xv—O-2_16—Mn+2_55 | 120.99 (3) | O-2_16—Mn+2_55—O-2_16xix | 109.471 (5) |
Cr+3_52xv—O-2_16—Mn+3_55xiii | 95.87 (4) | O-2_16—Mn+2_55—O-2_16xx | 109.471 (9) |
Cr+3_52xv—O-2_16—Mn+3_55xiv | 95.87 (4) | O-2_16—Mn+2_55—O-2_16xxi | 109.471 (5) |
Cr+3_52xv—O-2_16—Mn+3_55xv | 0.0 | O-2_16xix—Mn+2_55—O-2_16xx | 109.471 (5) |
Co+2_59—O-2_16—Mn+2_55 | 0.0 | O-2_16xix—Mn+2_55—O-2_16xxi | 109.471 (9) |
Co+2_59—O-2_16—Mn+3_55xiii | 120.99 (3) | O-2_16xx—Mn+2_55—O-2_16xxi | 109.471 (5) |
Co+2_59—O-2_16—Mn+3_55xiv | 120.99 (3) | O-2_16iv—Mn+3_55—O-2_16v | 83.81 (4) |
Co+2_59—O-2_16—Mn+3_55xv | 120.99 (3) | O-2_16iv—Mn+3_55—O-2_16vi | 83.81 (4) |
Mn+2_55—O-2_16—Mn+3_55xiii | 120.99 (3) | O-2_16iv—Mn+3_55—O-2_16i | 180.0 |
Mn+2_55—O-2_16—Mn+3_55xiv | 120.99 (3) | O-2_16iv—Mn+3_55—O-2_16xvii | 96.19 (4) |
Mn+2_55—O-2_16—Mn+3_55xv | 120.99 (3) | O-2_16iv—Mn+3_55—O-2_16xviii | 96.19 (4) |
Mn+3_55xiii—O-2_16—Mn+3_55xiv | 95.87 (4) | O-2_16v—Mn+3_55—O-2_16vi | 83.81 (4) |
Mn+3_55xiii—O-2_16—Mn+3_55xv | 95.87 (4) | O-2_16v—Mn+3_55—O-2_16i | 96.19 (4) |
Mn+3_55xiv—O-2_16—Mn+3_55xv | 95.87 (4) | O-2_16v—Mn+3_55—O-2_16xvii | 180.0 |
O-2_16iv—Cr+3_52—O-2_16v | 83.81 (4) | O-2_16v—Mn+3_55—O-2_16xviii | 96.19 (4) |
O-2_16iv—Cr+3_52—O-2_16vi | 83.81 (4) | O-2_16vi—Mn+3_55—O-2_16i | 96.19 (4) |
O-2_16iv—Cr+3_52—O-2_16i | 180.0 | O-2_16vi—Mn+3_55—O-2_16xvii | 96.19 (4) |
O-2_16iv—Cr+3_52—O-2_16xvii | 96.19 (4) | O-2_16vi—Mn+3_55—O-2_16xviii | 180.0 |
O-2_16iv—Cr+3_52—O-2_16xviii | 96.19 (4) | O-2_16i—Mn+3_55—O-2_16xvii | 83.81 (4) |
O-2_16v—Cr+3_52—O-2_16vi | 83.81 (4) | O-2_16i—Mn+3_55—O-2_16xviii | 83.81 (4) |
O-2_16v—Cr+3_52—O-2_16i | 96.19 (4) | O-2_16xvii—Mn+3_55—O-2_16xviii | 83.81 (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, −x−3/4, −y−3/4; (x) −x+7/4, −y+3/4, z−1; (xi) −y+7/4, z−1, −x+3/4; (xii) −x+3/4, −y+7/4, z−1; (xiii) −x+3/4, −y+3/4, z−1; (xiv) z−1, −x+3/4, −y+3/4; (xv) −y+3/4, z−1, −x+3/4; (xvi) z−1, −x+7/4, −y+3/4; (xvii) z−1, −x+3/4, −y+7/4; (xviii) −y+3/4, z−1, −x+7/4; (xix) −z−3/4, x−2, −y−3/4; (xx) −z−3/4, −x−7/4, y−1; (xxi) z−1, −x−3/4, −y+1/4. |
Crystal data top
Co0.43Mn0.32O | V = 565.31 (19) Å3 |
Mr = 58.91 | Z = 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: full | 3027 data points |
Rp = 0.112 | Profile 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 = 0.147 | 31 parameters |
Rexp = 0.117 | 0 restraints |
R(F2) = 0.10144 | (Δ/σ)max = 0.96 |
χ2 = 1.464 | Background 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
Co0.43Mn0.32O | V = 565.31 (19) Å3 |
Mr = 58.91 | Z = 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 = 0.112 | 3027 data points |
Rwp = 0.147 | 31 parameters |
Rexp = 0.117 | 0 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
O-2_16 | 0.26242 (14) | 0.26242 (14) | 0.26242 (14) | 0.0173 (9)* | |
Co+3_5 | 0.5 | 0.5 | 0.5 | 0.015 (4)* | 0.427 (15) |
Mn+3_5 | 0.5 | 0.5 | 0.5 | 0.021 (3)* | 0.573 (15) |
Mn+2_5 | 0.125 | 0.125 | 0.125 | 0.04 (2)* | 0.143 (27) |
Co+2_5 | 0.125 | 0.125 | 0.125 | 0.013 (4)* | 0.857 (27) |
Geometric parameters (Å, º) top
O-2_16—Co+3_59i | 1.9698 (10) | Mn+3_55—O-2_16i | 1.9698 (10) |
O-2_16—Co+3_59ii | 1.9698 (10) | Mn+3_55—O-2_16ii | 1.9698 (10) |
O-2_16—Co+3_59iii | 1.9698 (10) | Mn+3_55—O-2_16iii | 1.9698 (10) |
O-2_16—Mn+3_55i | 1.9698 (10) | Mn+3_55—Co+3_59iv | 2.9234 (3) |
O-2_16—Mn+3_55ii | 1.9698 (10) | Mn+3_55—Co+3_59v | 2.9234 (2) |
O-2_16—Mn+3_55iii | 1.9698 (10) | Mn+3_55—Co+3_59vi | 2.9234 (2) |
O-2_16—Mn+2_55 | 1.968 (2) | Mn+3_55—Co+3_59i | 2.9234 (3) |
O-2_16—Co+2_59 | 1.968 (2) | Mn+3_55—Co+3_59ii | 2.9234 (2) |
Co+3_59—O-2_16iv | 1.9698 (10) | Mn+3_55—Co+3_59iii | 2.9234 (2) |
Co+3_59—O-2_16v | 1.9698 (10) | Mn+3_55—Mn+3_55iv | 2.9234 (3) |
Co+3_59—O-2_16vi | 1.9698 (10) | Mn+3_55—Mn+3_55v | 2.9234 (2) |
Co+3_59—O-2_16i | 1.9698 (10) | Mn+3_55—Mn+3_55vi | 2.9234 (2) |
Co+3_59—O-2_16ii | 1.9698 (10) | Mn+3_55—Mn+3_55i | 2.9234 (3) |
Co+3_59—O-2_16iii | 1.9698 (10) | Mn+3_55—Mn+3_55ii | 2.9234 (2) |
Co+3_59—Mn+3_55iv | 2.9234 (3) | Mn+3_55—Mn+3_55iii | 2.9234 (2) |
Co+3_59—Mn+3_55v | 2.9234 (2) | Mn+2_55—O-2_16 | 1.968 (2) |
Co+3_59—Mn+3_55vi | 2.9234 (2) | Mn+2_55—O-2_16vii | 1.968 (2) |
Co+3_59—Mn+3_55i | 2.9234 (3) | Mn+2_55—O-2_16viii | 1.968 (2) |
Co+3_59—Mn+3_55ii | 2.9234 (2) | Mn+2_55—O-2_16ix | 1.968 (2) |
Co+3_59—Mn+3_55iii | 2.9234 (2) | Co+2_59—O-2_16 | 1.968 (2) |
Mn+3_55—O-2_16iv | 1.9698 (10) | Co+2_59—O-2_16vii | 1.968 (2) |
Mn+3_55—O-2_16v | 1.9698 (10) | Co+2_59—O-2_16viii | 1.968 (2) |
Mn+3_55—O-2_16vi | 1.9698 (10) | Co+2_59—O-2_16ix | 1.968 (2) |
| | | |
Co+3_59x—O-2_16—Co+3_59ii | 95.81 (7) | O-2_16v—Co+3_59—O-2_16xvii | 180.0 |
Co+3_59x—O-2_16—Co+3_59xi | 95.81 (7) | O-2_16v—Co+3_59—O-2_16xviii | 96.13 (7) |
Co+3_59xii—O-2_16—Mn+3_55xii | 0.0 | O-2_16vi—Co+3_59—O-2_16i | 96.13 (7) |
Co+3_59xii—O-2_16—Mn+3_55xiii | 95.81 (7) | O-2_16vi—Co+3_59—O-2_16xvii | 96.13 (7) |
Co+3_59xii—O-2_16—Mn+3_55iii | 95.81 (7) | O-2_16vi—Co+3_59—O-2_16xviii | 180.0 |
Co+3_59xiv—O-2_16—Mn+2_55 | 121.04 (5) | O-2_16i—Co+3_59—O-2_16xvii | 83.87 (7) |
Co+3_59xiv—O-2_16—Co+2_59 | 121.04 (5) | O-2_16i—Co+3_59—O-2_16xviii | 83.87 (7) |
Co+3_59ii—O-2_16—Co+3_59xi | 95.81 (7) | O-2_16xvii—Co+3_59—O-2_16xviii | 83.87 (7) |
Co+3_59xiii—O-2_16—Mn+3_55xii | 95.81 (7) | O-2_16iv—Mn+3_55—O-2_16v | 83.87 (7) |
Co+3_59xiii—O-2_16—Mn+3_55xiii | 0.0 | O-2_16iv—Mn+3_55—O-2_16vi | 83.87 (7) |
Co+3_59xiii—O-2_16—Mn+3_55iii | 95.81 (7) | O-2_16iv—Mn+3_55—O-2_16i | 180.0 |
Co+3_59xv—O-2_16—Mn+2_55 | 121.04 (5) | O-2_16iv—Mn+3_55—O-2_16xvii | 96.13 (7) |
Co+3_59xv—O-2_16—Co+2_59 | 121.04 (5) | O-2_16iv—Mn+3_55—O-2_16xviii | 96.13 (7) |
Co+3_59iii—O-2_16—Mn+3_55xii | 95.81 (7) | O-2_16v—Mn+3_55—O-2_16vi | 83.87 (7) |
Co+3_59iii—O-2_16—Mn+3_55xiii | 95.81 (7) | O-2_16v—Mn+3_55—O-2_16i | 96.13 (7) |
Co+3_59iii—O-2_16—Mn+3_55iii | 0.0 | O-2_16v—Mn+3_55—O-2_16xvii | 180.0 |
Co+3_59xvi—O-2_16—Mn+2_55 | 121.04 (5) | O-2_16v—Mn+3_55—O-2_16xviii | 96.13 (7) |
Co+3_59xvi—O-2_16—Co+2_59 | 121.04 (5) | O-2_16vi—Mn+3_55—O-2_16i | 96.13 (7) |
Mn+3_55xii—O-2_16—Mn+3_55xiii | 95.81 (7) | O-2_16vi—Mn+3_55—O-2_16xvii | 96.13 (7) |
Mn+3_55xii—O-2_16—Mn+3_55iii | 95.81 (7) | O-2_16vi—Mn+3_55—O-2_16xviii | 180.0 |
Mn+3_55xiv—O-2_16—Mn+2_55 | 121.04 (5) | O-2_16i—Mn+3_55—O-2_16xvii | 83.87 (7) |
Mn+3_55xiv—O-2_16—Co+2_59 | 121.04 (5) | O-2_16i—Mn+3_55—O-2_16xviii | 83.87 (7) |
Mn+3_55xiii—O-2_16—Mn+3_55iii | 95.81 (7) | O-2_16xvii—Mn+3_55—O-2_16xviii | 83.87 (7) |
Mn+3_55xv—O-2_16—Mn+2_55 | 121.04 (5) | O-2_16—Mn+2_55—O-2_16xix | 109.471 (4) |
Mn+3_55xv—O-2_16—Co+2_59 | 121.04 (5) | O-2_16—Mn+2_55—O-2_16xx | 109.471 (9) |
Mn+3_55xvi—O-2_16—Mn+2_55 | 121.04 (5) | O-2_16—Mn+2_55—O-2_16xxi | 109.471 (4) |
Mn+3_55xvi—O-2_16—Co+2_59 | 121.04 (5) | O-2_16xix—Mn+2_55—O-2_16xx | 109.471 (4) |
Mn+2_55—O-2_16—Co+2_59 | 0.0 | O-2_16xix—Mn+2_55—O-2_16xxi | 109.471 (9) |
O-2_16iv—Co+3_59—O-2_16v | 83.87 (7) | O-2_16xx—Mn+2_55—O-2_16xxi | 109.471 (4) |
O-2_16iv—Co+3_59—O-2_16vi | 83.87 (7) | O-2_16—Co+2_59—O-2_16xix | 109.471 (4) |
O-2_16iv—Co+3_59—O-2_16i | 180.0 | O-2_16—Co+2_59—O-2_16xx | 109.471 (9) |
O-2_16iv—Co+3_59—O-2_16xvii | 96.13 (7) | O-2_16—Co+2_59—O-2_16xxi | 109.471 (4) |
O-2_16iv—Co+3_59—O-2_16xviii | 96.13 (7) | O-2_16xix—Co+2_59—O-2_16xx | 109.471 (4) |
O-2_16v—Co+3_59—O-2_16vi | 83.87 (7) | O-2_16xix—Co+2_59—O-2_16xxi | 109.471 (9) |
O-2_16v—Co+3_59—O-2_16i | 96.13 (7) | O-2_16xx—Co+2_59—O-2_16xxi | 109.471 (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, −x−3/4, −y−3/4; (x) −x+7/4, −y+3/4, z−1; (xi) −y+7/4, z−1, −x+3/4; (xii) −x+3/4, −y+7/4, z−1; (xiii) z−1, −x+7/4, −y+3/4; (xiv) −x+3/4, −y+3/4, z−1; (xv) z−1, −x+3/4, −y+3/4; (xvi) −y+3/4, z−1, −x+3/4; (xvii) z−1, −x+3/4, −y+7/4; (xviii) −y+3/4, z−1, −x+7/4; (xix) −z−3/4, x−2, −y−3/4; (xx) −z−3/4, −x−7/4, y−1; (xxi) z−1, −x−3/4, −y+1/4. |
(MN1_5CO1_5O4_phase_1)
top
Crystal data top
Co0.23Mn0.52O | V = 301.09 (14) Å3 |
Mr = 58.12 | Z = 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: full | 3100 data points |
Rp = 0.106 | Profile 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 = 0.137 | 35 parameters |
Rexp = 0.096 | 0 restraints |
R(F2) = 0.13557 | (Δ/σ)max = 1.25 |
χ2 = 1.796 | Background 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
Co0.23Mn0.52O | V = 301.09 (14) Å3 |
Mr = 58.12 | Z = 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 = 0.106 | 3100 data points |
Rwp = 0.137 | 35 parameters |
Rexp = 0.096 | 0 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
O-2_16 | 0.0 | 0.4770 (10) | 0.2615 (6) | 0.0100 (15)* | |
Co+3_5 | 0.0 | 0.0 | 0.5 | 0.8 (18)* | 0.042 (19) |
Mn+3_5 | 0.0 | 0.0 | 0.5 | 0.005* | 0.958 (19) |
Co+2_5 | 0.0 | 0.75 | 0.125 | 0.005* | 0.830 (25) |
Mn+2_5 | 0.0 | 0.75 | 0.125 | 0.004* | 0.170 (25) |
Geometric parameters (Å, º) top
O-2_16—Co+3_59i | 1.934 (4) | Mn+3_55—O-2_16iv | 1.934 (4) |
O-2_16—Co+3_59ii | 1.934 (4) | Mn+3_55—O-2_16ii | 1.934 (4) |
O-2_16—Co+3_59iii | 2.200 (6) | Mn+3_55—O-2_16iii | 2.200 (6) |
O-2_16—Mn+3_55i | 1.934 (4) | Mn+3_55—O-2_16v | 1.934 (4) |
O-2_16—Mn+3_55ii | 1.934 (4) | Mn+3_55—O-2_16vi | 2.200 (6) |
O-2_16—Mn+3_55iii | 2.200 (6) | Mn+3_55—O-2_16vii | 1.934 (4) |
O-2_16—Co+2_59 | 2.004 (5) | Mn+3_55—Co+3_59viii | 2.8592 (5) |
O-2_16—Mn+2_55 | 2.004 (5) | Mn+3_55—Co+3_59iii | 2.8592 (5) |
Co+3_59—O-2_16iv | 1.934 (4) | Mn+3_55—Mn+3_55viii | 2.8592 (5) |
Co+3_59—O-2_16ii | 1.934 (4) | Mn+3_55—Mn+3_55iii | 2.8592 (5) |
Co+3_59—O-2_16iii | 2.200 (6) | Co+2_59—O-2_16 | 2.004 (5) |
Co+3_59—O-2_16v | 1.934 (4) | Co+2_59—O-2_16ix | 2.004 (5) |
Co+3_59—O-2_16vi | 2.200 (6) | Co+2_59—O-2_16x | 2.004 (5) |
Co+3_59—O-2_16vii | 1.934 (4) | Co+2_59—O-2_16xi | 2.004 (5) |
Co+3_59—Co+3_59viii | 2.8592 (5) | Mn+2_55—O-2_16 | 2.004 (5) |
Co+3_59—Co+3_59iii | 2.8592 (5) | Mn+2_55—O-2_16ix | 2.004 (5) |
Co+3_59—Mn+3_55viii | 2.8592 (5) | Mn+2_55—O-2_16x | 2.004 (5) |
Co+3_59—Mn+3_55iii | 2.8592 (5) | Mn+2_55—O-2_16xi | 2.004 (5) |
| | | |
Co+3_59i—O-2_16—Co+3_59xii | 95.3 (3) | O-2_16xiii—Co+3_59—O-2_16xiv | 180.0 |
Co+3_59i—O-2_16—Mn+3_55i | 0.0 | O-2_16iv—Mn+3_55—O-2_16ii | 180.0 |
Co+3_59i—O-2_16—Mn+3_55ii | 95.3 (3) | O-2_16iv—Mn+3_55—O-2_16xiii | 84.3 (3) |
Co+3_59i—O-2_16—Co+2_59 | 119.25 (19) | O-2_16iv—Mn+3_55—O-2_16xiv | 95.7 (3) |
Co+3_59i—O-2_16—Mn+2_55 | 119.25 (19) | O-2_16ii—Mn+3_55—O-2_16xiii | 95.7 (3) |
Co+3_59ii—O-2_16—Mn+3_55i | 95.3 (3) | O-2_16ii—Mn+3_55—O-2_16xiv | 84.3 (3) |
Co+3_59ii—O-2_16—Mn+3_55ii | 0.0 | O-2_16xiii—Mn+3_55—O-2_16xiv | 180.0 |
Co+3_59ii—O-2_16—Co+2_59 | 119.25 (19) | O-2_16—Co+2_59—O-2_16ix | 113.15 (18) |
Co+3_59xii—O-2_16—Mn+2_55 | 119.25 (19) | O-2_16—Co+2_59—O-2_16xv | 102.4 (3) |
Mn+3_55i—O-2_16—Mn+3_55ii | 95.3 (3) | O-2_16—Co+2_59—O-2_16xvi | 113.15 (18) |
Mn+3_55i—O-2_16—Co+2_59 | 119.25 (19) | O-2_16ix—Co+2_59—O-2_16xv | 113.15 (18) |
Mn+3_55i—O-2_16—Mn+2_55 | 119.25 (19) | O-2_16ix—Co+2_59—O-2_16xvi | 102.4 (3) |
Mn+3_55ii—O-2_16—Co+2_59 | 119.25 (19) | O-2_16xv—Co+2_59—O-2_16xvi | 113.15 (18) |
Mn+3_55xii—O-2_16—Mn+2_55 | 119.25 (19) | O-2_16—Mn+2_55—O-2_16ix | 113.15 (18) |
Co+2_59—O-2_16—Mn+2_55 | 0.0 | O-2_16—Mn+2_55—O-2_16xv | 102.4 (3) |
O-2_16iv—Co+3_59—O-2_16ii | 180.0 | O-2_16—Mn+2_55—O-2_16xvi | 113.15 (18) |
O-2_16iv—Co+3_59—O-2_16xiii | 84.3 (3) | O-2_16ix—Mn+2_55—O-2_16xv | 113.15 (18) |
O-2_16iv—Co+3_59—O-2_16xiv | 95.7 (3) | O-2_16ix—Mn+2_55—O-2_16xvi | 102.4 (3) |
O-2_16ii—Co+3_59—O-2_16xiii | 95.7 (3) | O-2_16xv—Mn+2_55—O-2_16xvi | 113.15 (18) |
O-2_16ii—Co+3_59—O-2_16xiv | 84.3 (3) | | |
Symmetry codes: (i) y+1/4, −x+1/4, z−1/4; (ii) y−1/4, −x+1/4, −z+3/4; (iii) −x, −y+1/2, z; (iv) −y+1/4, x−1/4, z+1/4; (v) y−1/4, −x−1/4, z+1/4; (vi) x−1, y−3/2, −z; (vii) −y−3/4, x−3/4, −z−1/4; (viii) −x, −y−1/2, z; (ix) −y+3/4, x+3/4, −z+1/4; (x) −x, −y+3/2, z; (xi) y−7/4, −x−1/4, −z−3/4; (xii) y−1/4, −x+5/4, −z+3/4; (xiii) y−5/4, −x−5/4, z−7/4; (xiv) −y−3/4, x−3/4, −z+3/4; (xv) −x−2, −y+1/2, z−2; (xvi) y−7/4, −x+3/4, −z−3/4. |
(MN1_5CO1_5O4_phase_2)
top
Crystal data top
Co0.33Mn0.42O | V = 572.1 (3) Å3 |
Mr = 58.54 | Z = 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: full | 3100 data points |
Rp = 0.106 | Profile 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 = 0.137 | 35 parameters |
Rexp = 0.096 | 0 restraints |
R(F2) = 0.13557 | (Δ/σ)max = 1.25 |
χ2 = 1.796 | Background 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
Co0.33Mn0.42O | V = 572.1 (3) Å3 |
Mr = 58.54 | Z = 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 = 0.106 | 3100 data points |
Rwp = 0.137 | 35 parameters |
Rexp = 0.096 | 0 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
O1 | 0.2618 (3) | 0.2618 (3) | 0.2618 (3) | 0.0286 (14)* | |
Co+3BN | 0.5 | 0.5 | 0.5 | 0.004* | 0.216 (14) |
Mn+3BN | 0.5 | 0.5 | 0.5 | 0.030 (3)* | 0.784 (14) |
Mn+2AN | 0.125 | 0.125 | 0.125 | 0.004* | 0.098 (18) |
Co+2AN | 0.125 | 0.125 | 0.125 | 0.004* | 0.902 (18) |
Geometric parameters (Å, º) top
O1—Co+3BNi | 1.983 (2) | Mn+3BN—O1i | 1.983 (2) |
O1—Co+3BNii | 1.983 (2) | Mn+3BN—O1ii | 1.983 (2) |
O1—Co+3BNiii | 1.983 (2) | Mn+3BN—O1iii | 1.983 (2) |
O1—Mn+3BNi | 1.983 (2) | Mn+3BN—Co+3BNiv | 2.9350 (4) |
O1—Mn+3BNii | 1.983 (2) | Mn+3BN—Co+3BNv | 2.9350 (3) |
O1—Mn+3BNiii | 1.983 (2) | Mn+3BN—Co+3BNvi | 2.9350 (3) |
O1—Mn+2AN | 1.966 (4) | Mn+3BN—Co+3BNi | 2.9350 (4) |
O1—Co+2AN | 1.966 (4) | Mn+3BN—Co+3BNii | 2.9350 (3) |
Co+3BN—O1iv | 1.983 (2) | Mn+3BN—Co+3BNiii | 2.9350 (3) |
Co+3BN—O1v | 1.983 (2) | Mn+3BN—Mn+3BNiv | 2.9350 (4) |
Co+3BN—O1vi | 1.983 (2) | Mn+3BN—Mn+3BNv | 2.9350 (3) |
Co+3BN—O1i | 1.983 (2) | Mn+3BN—Mn+3BNvi | 2.9350 (3) |
Co+3BN—O1ii | 1.983 (2) | Mn+3BN—Mn+3BNi | 2.9350 (4) |
Co+3BN—O1iii | 1.983 (2) | Mn+3BN—Mn+3BNii | 2.9350 (3) |
Co+3BN—Mn+3BNiv | 2.9350 (4) | Mn+3BN—Mn+3BNiii | 2.9350 (3) |
Co+3BN—Mn+3BNv | 2.9350 (3) | Mn+2AN—O1 | 1.966 (4) |
Co+3BN—Mn+3BNvi | 2.9350 (3) | Mn+2AN—O1vii | 1.966 (4) |
Co+3BN—Mn+3BNi | 2.9350 (4) | Mn+2AN—O1viii | 1.966 (4) |
Co+3BN—Mn+3BNii | 2.9350 (3) | Mn+2AN—O1ix | 1.966 (4) |
Co+3BN—Mn+3BNiii | 2.9350 (3) | Co+2AN—O1 | 1.966 (4) |
Mn+3BN—O1iv | 1.983 (2) | Co+2AN—O1vii | 1.966 (4) |
Mn+3BN—O1v | 1.983 (2) | Co+2AN—O1viii | 1.966 (4) |
Mn+3BN—O1vi | 1.983 (2) | Co+2AN—O1ix | 1.966 (4) |
| | | |
Co+3BNx—O1—Co+3BNii | 95.50 (14) | O1v—Co+3BN—O1xvii | 180.0 |
Co+3BNx—O1—Co+3BNxi | 95.50 (14) | O1v—Co+3BN—O1xviii | 95.78 (15) |
Co+3BNxii—O1—Mn+3BNxii | 0.0 | O1vi—Co+3BN—O1i | 95.78 (15) |
Co+3BNxii—O1—Mn+3BNxiii | 95.50 (14) | O1vi—Co+3BN—O1xvii | 95.78 (15) |
Co+3BNxii—O1—Mn+3BNiii | 95.50 (14) | O1vi—Co+3BN—O1xviii | 180.0 |
Co+3BNxiv—O1—Mn+2AN | 121.27 (10) | O1i—Co+3BN—O1xvii | 84.22 (15) |
Co+3BNxiv—O1—Co+2AN | 121.27 (10) | O1i—Co+3BN—O1xviii | 84.22 (15) |
Co+3BNii—O1—Co+3BNxi | 95.50 (14) | O1xvii—Co+3BN—O1xviii | 84.22 (15) |
Co+3BNxiii—O1—Mn+3BNxii | 95.50 (14) | O1iv—Mn+3BN—O1v | 84.22 (15) |
Co+3BNxiii—O1—Mn+3BNxiii | 0.0 | O1iv—Mn+3BN—O1vi | 84.22 (15) |
Co+3BNxiii—O1—Mn+3BNiii | 95.50 (14) | O1iv—Mn+3BN—O1i | 180.0 |
Co+3BNxv—O1—Mn+2AN | 121.27 (10) | O1iv—Mn+3BN—O1xvii | 95.78 (15) |
Co+3BNxv—O1—Co+2AN | 121.27 (10) | O1iv—Mn+3BN—O1xviii | 95.78 (15) |
Co+3BNiii—O1—Mn+3BNxii | 95.50 (14) | O1v—Mn+3BN—O1vi | 84.22 (15) |
Co+3BNiii—O1—Mn+3BNxiii | 95.50 (14) | O1v—Mn+3BN—O1i | 95.78 (15) |
Co+3BNiii—O1—Mn+3BNiii | 0.0 | O1v—Mn+3BN—O1xvii | 180.0 |
Co+3BNxvi—O1—Mn+2AN | 121.27 (10) | O1v—Mn+3BN—O1xviii | 95.78 (15) |
Co+3BNxvi—O1—Co+2AN | 121.27 (10) | O1vi—Mn+3BN—O1i | 95.78 (15) |
Mn+3BNxii—O1—Mn+3BNxiii | 95.50 (14) | O1vi—Mn+3BN—O1xvii | 95.78 (15) |
Mn+3BNxii—O1—Mn+3BNiii | 95.50 (14) | O1vi—Mn+3BN—O1xviii | 180.0 |
Mn+3BNxiv—O1—Mn+2AN | 121.27 (10) | O1i—Mn+3BN—O1xvii | 84.22 (15) |
Mn+3BNxiv—O1—Co+2AN | 121.27 (10) | O1i—Mn+3BN—O1xviii | 84.22 (15) |
Mn+3BNxiii—O1—Mn+3BNiii | 95.50 (14) | O1xvii—Mn+3BN—O1xviii | 84.22 (15) |
Mn+3BNxv—O1—Mn+2AN | 121.27 (10) | O1—Mn+2AN—O1xix | 109.471 (6) |
Mn+3BNxv—O1—Co+2AN | 121.27 (10) | O1—Mn+2AN—O1xx | 109.471 (12) |
Mn+3BNxvi—O1—Mn+2AN | 121.27 (10) | O1—Mn+2AN—O1xxi | 109.471 (6) |
Mn+3BNxvi—O1—Co+2AN | 121.27 (10) | O1xix—Mn+2AN—O1xx | 109.471 (6) |
Mn+2AN—O1—Co+2AN | 0.0 | O1xix—Mn+2AN—O1xxi | 109.471 (12) |
O1iv—Co+3BN—O1v | 84.22 (15) | O1xx—Mn+2AN—O1xxi | 109.471 (6) |
O1iv—Co+3BN—O1vi | 84.22 (15) | O1—Co+2AN—O1xix | 109.471 (6) |
O1iv—Co+3BN—O1i | 180.0 | O1—Co+2AN—O1xx | 109.471 (12) |
O1iv—Co+3BN—O1xvii | 95.78 (15) | O1—Co+2AN—O1xxi | 109.471 (6) |
O1iv—Co+3BN—O1xviii | 95.78 (15) | O1xix—Co+2AN—O1xx | 109.471 (6) |
O1v—Co+3BN—O1vi | 84.22 (15) | O1xix—Co+2AN—O1xxi | 109.471 (12) |
O1v—Co+3BN—O1i | 95.78 (15) | O1xx—Co+2AN—O1xxi | 109.471 (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, −x−3/4, −y−3/4; (x) −x+7/4, −y+3/4, z−1; (xi) −y+7/4, z−1, −x+3/4; (xii) −x+3/4, −y+7/4, z−1; (xiii) z−1, −x+7/4, −y+3/4; (xiv) −x+3/4, −y+3/4, z−1; (xv) z−1, −x+3/4, −y+3/4; (xvi) −y+3/4, z−1, −x+3/4; (xvii) z−1, −x+3/4, −y+7/4; (xviii) −y+3/4, z−1, −x+7/4; (xix) −z−3/4, x−2, −y−3/4; (xx) −z−3/4, −x−7/4, y−1; (xxi) z−1, −x−3/4, −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 formula | Co0.15Cr0.42Mn0.19O | Co0.43Mn0.32O | Co0.23Mn0.52O | Co0.33Mn0.42O |
Mr | 56.56 | 58.91 | 58.12 | 58.54 |
Crystal system, space group | Cubic, Fd3m | Cubic, Fd3m | Tetragonal, I41/amd | Cubic, Fd3m |
Temperature (K) | ? | ? | ? | ? |
a, b, c (Å) | 8.3777 (10), 8.3777, 8.3777 | 8.2685 (9), 8.2685, 8.2685 | 5.7184 (10), 5.7184, 9.208 (2) | 8.3015 (13), 8.3015, 8.3015 |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 588.0 (2) | 565.31 (19) | 301.09 (14) | 572.1 (3) |
Z | 32 | 32 | 16 | 32 |
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 = 0.05 | 2θmin = 27.827 2θmax = 67.827 2θstep = 0.05 | 2θmin = 27.893 2θmax = 67.893 2θstep = 0.05 | 2θmin = 27.893 2θmax = 67.893 2θstep = 0.05 |
|
Refinement |
R factors and goodness of fit | Rp = 0.093, Rwp = 0.134, Rexp = 0.102, R(F2) = 0.02849, χ2 = 1.322 | Rp = 0.112, Rwp = 0.147, Rexp = 0.117, R(F2) = 0.10144, χ2 = 1.464 | Rp = 0.106, Rwp = 0.137, Rexp = 0.096, R(F2) = 0.13557, χ2 = 1.796 | Rp = 0.106, Rwp = 0.137, Rexp = 0.096, R(F2) = 0.13557, χ2 = 1.796 |
No. of data points | 2988 | 3027 | 3100 | 3100 |
No. of parameters | 31 | 31 | 35 | 35 |
(Δ/σ)max | 0.25 | 0.96 | 1.25 | 1.25 |
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