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Polycrystalline samples of mixed Yb1-xTbxMnO3 (x = 0, 0.25, 0.50, 0.75 and 1) were prepared by a solid state reaction procedure. Detailed crystal structure studies were performed using X-ray diffraction data obtained at room temperature. The application of the Rietveld method confirmed the reported hexagonal P63cm and orthorhombic Pnma phases for x = 0 (YbMnO3) and x = 1 (TbMnO3), respectively. A single hexagonal phase was also observed for x = 0.25, while in the case of x = 0.50 and x = 0.75 both phases coexist in the produced samples. Crystallographic parameters for the pure compounds are in agreement with those found in the literature. Changes in the lattice parameters, unit-cell volume, polyhedral distortions and tilting observed in the mixed compounds are explained as a function of x. Sharing of Tb3+ and Yb3+ ions between different sites is discussed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889813010546/fs5035sup1.cif
Contains datablocks global, TbMnO3

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0021889813010546/fs5035TbMnO3sup2.rtv
Contains datablock TbMnO3

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889813010546/fs5035sup3.cif
Contains datablocks global, Yb25Tb75, Yb25Tb75_phase_1, Yb25Tb75_phase_2

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0021889813010546/fs5035Yb25Tb75sup4.rtv
Contains datablock Yb25Tb75

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889813010546/fs5035sup5.cif
Contains datablocks global, Yb50Tb50, Yb50Tb50_phase1, Yb50Tb50_phase_2

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0021889813010546/fs5035Yb50Tb50sup6.rtv
Contains datablock Yb50Tb50

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889813010546/fs5035sup7.cif
Contains datablocks global, Yb75Tb25

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0021889813010546/fs5035Yb75Tb25sup8.rtv
Contains datablock Yb75Tb25

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889813010546/fs5035sup9.cif
Contains datablocks global, YbMnO3

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0021889813010546/fs5035YbMnO3sup10.rtv
Contains datablock YbMnO3

Computing details top

Cell refinement: GSAS software; program(s) used to solve structure: GSAS software; program(s) used to refine structure: GSAS software.

(TbMnO3) top
Crystal data top
MnO3TbV = 229.27 (2) Å3
Mr = 261.86Z = 4
Orthorhombic, PnmaCu Kα1, Cu Kα2 radiation, λ = 1.540500, 1.544300 Å
a = 5.8307 (2) ÅT = 295 K
b = 7.4146 (3) Å?, ? × ? × ? mm
c = 5.3031 (2) ÅSpecimen preparation: Prepared at 1773 K and 101 kPa
Data collection top
Rigaku Geigerflex
diffractometer
Data collection mode: reflection
Radiation source: X-ray tubeScan method: step
Specimen mounting: packed powder pellet2θmin = 12.02°, 2θmax = 139.98°, 2θstep = 0.02°
Refinement top
Rp = 0.0896399 data points
Rwp = 0.123Excluded region(s): There were two excluded regions: from 4.02 to 12.00 degrees because there is no relevant information there and from 31.62 to 32.26 degrees where a very small peak from the non reacted rare earth oxide R2O3 was observed
Rexp = 0.094Profile function: CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 0.000 #2(GV) = 6.224 #3(GW) = 7.764 #4(GP) = 0.000 #5(LX) = 0.000 #6(LY) = 25.851 #7(S/L) = 0.0346 #8(H/L) = 0.0273 #9(trns) = -7.62 #10(shft)= 1.6525 #11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00 #14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000 #17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R(F2) = 0.04276
χ2 = 1.716Background function: GSAS Background function number 1 with 10 terms. Shifted Chebyshev function of 1st kind 1: 41.8959 2: -5.30503 3: 8.05638 4: -2.06175 5: -0.870980 6: -1.05595 7: 0.191005 8: 0.163087 9: -8.878920E-0210: -8.072430E-02
Crystal data top
MnO3TbV = 229.27 (2) Å3
Mr = 261.86Z = 4
Orthorhombic, PnmaCu Kα1, Cu Kα2 radiation, λ = 1.540500, 1.544300 Å
a = 5.8307 (2) ÅT = 295 K
b = 7.4146 (3) Å?, ? × ? × ? mm
c = 5.3031 (2) Å
Data collection top
Rigaku Geigerflex
diffractometer
Scan method: step
Specimen mounting: packed powder pellet2θmin = 12.02°, 2θmax = 139.98°, 2θstep = 0.02°
Data collection mode: reflection
Refinement top
Rp = 0.089R(F2) = 0.04276
Rwp = 0.123χ2 = 1.716
Rexp = 0.0946399 data points
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Tb10.08002 (14)0.250.9836 (2)0.0097 (3)*
O10.4638 (14)0.250.1040 (15)0.015 (3)*
O20.3293 (12)0.0521 (9)0.7024 (13)0.029 (2)*
Mn10.00.00.50.0088 (6)*
Geometric parameters (Å, º) top
Tb1—Tb1i3.8269 (4)O1—Mn1xii1.945 (3)
Tb1—Tb1ii3.8269 (4)O1—Mn1xiii1.945 (3)
Tb1—Tb1iii3.8259 (14)O2—Tb12.548 (7)
Tb1—Tb1iv3.8259 (14)O2—Tb1xiv2.577 (6)
Tb1—O1v2.327 (8)O2—Tb1iv2.294 (7)
Tb1—O1iii2.290 (8)O2—Mn12.233 (7)
Tb1—O22.548 (7)O2—Mn1viii1.906 (7)
Tb1—O2vi2.577 (6)Mn1—Tb1xi3.3396 (9)
Tb1—O2vii2.548 (7)Mn1—Tb13.1985 (9)
Tb1—O2viii2.577 (6)Mn1—Tb1xiv3.0725 (7)
Tb1—O2iii2.294 (7)Mn1—Tb1xv3.1985 (9)
Tb1—O2ix2.294 (7)Mn1—Tb1i3.3396 (9)
Tb1—Mn13.1985 (9)Mn1—Tb1iii3.0725 (7)
Tb1—Mn1v3.3396 (9)Mn1—O1xvi1.945 (3)
Tb1—Mn1vi3.0725 (7)Mn1—O1xvii1.945 (3)
Tb1—Mn1vii3.1985 (9)Mn1—O22.233 (7)
Tb1—Mn1x3.3396 (9)Mn1—O2xiii1.906 (7)
Tb1—Mn1viii3.0725 (7)Mn1—O2xv2.233 (7)
O1—Tb1xi2.327 (8)Mn1—O2ix1.906 (7)
O1—Tb1iv2.290 (8)
O1v—Tb1—O1xviii91.29 (19)O2viii—Tb1—O2ix76.6 (3)
O1v—Tb1—O267.2 (2)O2viii—Tb1—Mn1vi110.37 (15)
O1v—Tb1—O2vi71.29 (18)O2viii—Tb1—Mn1viii45.53 (16)
O1v—Tb1—O2vii67.2 (2)O2xix—Tb1—O2ix79.5 (3)
O1v—Tb1—O2viii71.29 (18)O2xx—Tb1—Mn1vi97.70 (17)
O1v—Tb1—O2xix136.94 (19)O2xx—Tb1—Mn1viii154.95 (19)
O1v—Tb1—O2ix136.94 (19)O2xxi—Tb1—Mn1vi154.95 (19)
O1v—Tb1—Mn1vi39.27 (6)O2xxi—Tb1—Mn1viii97.70 (17)
O1v—Tb1—Mn1viii39.27 (6)Mn1vi—Tb1—Mn1viii74.214 (19)
O1xix—Tb1—O2136.7 (2)Tb1xi—O1—Tb1iv123.1 (4)
O1xix—Tb1—O2vi68.33 (18)Tb1xi—O1—Mn1xii91.5 (2)
O1xix—Tb1—O2vii136.7 (2)Tb1xi—O1—Mn1xiii91.5 (2)
O1xix—Tb1—O2viii68.33 (18)Tb1xxii—O1—Mn1xii103.8 (2)
O1xix—Tb1—O2xix102.8 (2)Tb1xxii—O1—Mn1xiii103.8 (2)
O1xix—Tb1—O2ix102.8 (2)Mn1xii—O1—Mn1xiii144.7 (5)
O1xx—Tb1—Mn1vi102.05 (17)Tb1—O2—Tb1xiv151.8 (3)
O1xx—Tb1—Mn1viii102.05 (17)Tb1—O2—Tb1iv104.3 (2)
O2—Tb1—O2vi130.32 (11)Tb1—O2—Mn1viii86.0 (3)
O2—Tb1—O2vii70.4 (3)Tb1xiv—O2—Tb1iv103.4 (3)
O2—Tb1—O2viii69.26 (10)Tb1xiv—O2—Mn1viii95.2 (3)
O2—Tb1—O2xix118.71 (12)Tb1xxii—O2—Mn1viii98.8 (3)
O2—Tb1—O2ix75.13 (15)Tb1xiv—Mn1—Tb1iii180.0
O2—Tb1—Mn1vi84.80 (15)Tb1xiv—Mn1—O1xvi49.2 (2)
O2—Tb1—Mn1viii38.22 (16)Tb1xiv—Mn1—O1iv130.8 (2)
O2vi—Tb1—O2vii69.26 (10)Tb1xiv—Mn1—O2xiii55.8 (2)
O2vi—Tb1—O2viii120.7 (3)Tb1xiv—Mn1—O2ix124.2 (2)
O2vi—Tb1—O2xix76.6 (3)Tb1xviii—Mn1—O1xvi130.8 (2)
O2vi—Tb1—O2ix151.66 (15)Tb1xviii—Mn1—O1iv49.2 (2)
O2vi—Tb1—Mn1vi45.53 (16)Tb1xix—Mn1—O2xiii124.2 (2)
O2vi—Tb1—Mn1viii110.37 (15)Tb1xix—Mn1—O2ix55.8 (2)
O2vii—Tb1—O2viii130.32 (11)O1xvi—Mn1—O1iv180.0
O2vii—Tb1—O2xix75.13 (15)O1xvi—Mn1—O2xiii89.2 (3)
O2vii—Tb1—O2ix118.71 (12)O1xvi—Mn1—O2ix90.9 (3)
O2vii—Tb1—Mn1vi38.22 (16)O1xxiii—Mn1—O2xiii90.9 (3)
O2vii—Tb1—Mn1viii84.80 (15)O1xxiii—Mn1—O2ix89.2 (3)
O2viii—Tb1—O2xix151.66 (15)O2xiii—Mn1—O2ix180.0
Symmetry codes: (i) x, y, z+2; (ii) x, y+1, z+2; (iii) x1/2, y+1/2, z+3/2; (iv) x+1/2, y+1/2, z+3/2; (v) x, y, z+1; (vi) x+1/2, y+1/2, z+1/2; (vii) x, y+1/2, z; (viii) x+1/2, y, z+1/2; (ix) x1/2, y, z+3/2; (x) x, y+1/2, z+1; (xi) x, y, z1; (xii) x+1/2, y+1/2, z1/2; (xiii) x+1/2, y, z1/2; (xiv) x+1/2, y1/2, z1/2; (xv) x, y, z+1; (xvi) x+1/2, y1/2, z+1/2; (xvii) x1/2, y+1/2, z+1/2; (xviii) x+1/2, y+1/2, z+5/2; (xix) x1/2, y+3/2, z+3/2; (xx) x+1/2, y+3/2, z+5/2; (xxi) x+1/2, y, z+5/2; (xxii) x+3/2, y+3/2, z+5/2; (xxiii) x1/2, y+3/2, z+1/2.

Experimental details

Crystal data
Chemical formulaMnO3Tb
Mr261.86
Crystal system, space groupOrthorhombic, Pnma
Temperature (K)295
a, b, c (Å)5.8307 (2), 7.4146 (3), 5.3031 (2)
V3)229.27 (2)
Z4
Radiation typeCu Kα1, Cu Kα2, λ = 1.540500, 1.544300 Å
Specimen shape, size (mm)?, ? × ? × ?
Data collection
DiffractometerRigaku Geigerflex
diffractometer
Specimen mountingPacked powder pellet
Data collection modeReflection
Scan methodStep
2θ values (°)2θmin = 12.02 2θmax = 139.98 2θstep = 0.02
Refinement
R factors and goodness of fitRp = 0.089, Rwp = 0.123, Rexp = 0.094, R(F2) = 0.04276, χ2 = 1.716
No. of data points6399
No. of parameters?
No. of restraints?

Computer programs: GSAS software.

 

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