X-ray powder diffraction beamline at D10B of LNLS: application to the Ba2FeReO6 double perovskite

Ferreira, F.F.; Granado, E.; Carvalho, W. Jr; Kycia, S.W.; Bruno, D.; Droppa, R. Jr

doi:10.1107/S0909049505039208

X-ray powder diffraction beamline at D10B of LNLS: application to the Ba₂FeReO₆ double perovskite

F. F. Ferreira, E. Granado, W. Carvalho Jr, S. W. Kycia, D. Bruno and R. Droppa Jr

A new beamline, fully dedicated to X-ray powder diffraction (XPD) measurements, has been installed after the exit port B of the bending magnet D10 at the Brazilian Synchrotron Light Laboratory (LNLS) and commissioned. The technical characteristics of the beamline are described and some performance indicators are listed, such as the incoming photon flux and the angular/energy resolutions obtainable under typical experimental conditions. The results of a Rietveld refinement for a standard sample of Y₂O₃ using high-resolution data are shown. The refined parameters match those found in the literature, within experimental error. High-resolution XPD measurements on Ba₂FeReO₆ demonstrate a slight departure from the ideal cubic double-perovskite structure at low temperatures, not detected by previous powder diffraction experiments. The onset of the structural transition coincides with the ferrimagnetic ordering temperature, T_c ≃ 315 K. Subtle structural features, such as those reported here for Ba₂FeReO₆, as well as the determination and/or refinement of complex crystal structures in polycrystalline samples are ideal candidate problems to be investigated on this beamline.

Keywords: X-ray powder diffraction; high resolution; structural phase transitions; energy resolution; Rietveld refinement; LNLS.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0909049505039208/ml5212sup1.cif Contains datablocks I, II, III, global, T14KBST_phase_2, T14KBST_phase_3, T400KBST_phase_1, T400KBST_phase_2, T14KBST_p_01, T400KBST_p_01, T14KBST_overall, T400KBST_overall
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0909049505039208/ml5212Isup2.rtv Contains datablock I
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0909049505039208/ml5212IIsup3.rtv Contains datablock II
	Rietveld powder data file (CIF format) https://doi.org/10.1107/S0909049505039208/ml5212IIIsup4.rtv Contains datablock III
	Structure factor file (CIF format) https://doi.org/10.1107/S0909049505039208/ml5212Isup5.hkl Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S0909049505039208/ml5212IIsup6.hkl Contains datablock II
	Structure factor file (CIF format) https://doi.org/10.1107/S0909049505039208/ml5212IIIsup7.hkl Contains datablock III

Computing details top

Data collection: SPEC (Certified Scientific Software, 1992) for (I). Data reduction: POWF 2.11 (Virginia Tech, 2001-2003) for (I). For all compounds, program(s) used to solve structure: GSAS (Larson & Von Dreele, 2001). Program(s) used to refine structure: GSAS for (I).

Figures top

(T14KBST_phase_2) iron oxide top

Crystal data top

Fe₃O₄	Z = 8
M_r = 231.54	Synchrotron radiation, λ = 1.377285 Å
Cubic, Fd3m	T = 14 K
Hall symbol: F d -3 m	Particle morphology: powder
a = 8.3814 (5) Å	flat_sheet, 20 × 10 mm
V = 588.78 (10) Å³

Data collection top

Huber 4+2 circle diffractometer	Data collection mode: reflection
Radiation source: synchrotron, LNLS D10B-XPD beamline	Scan method: step
Si 111 monochromator	2θ_min = 15.003°, 2θ_max = 150.193°, 2θ_step = 0.01°
Specimen mounting: copper sample holder

Refinement top

Least-squares matrix: full	13520 data points
R_p = 0.168	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) = 0.000 #2(GV) = 0.000 #3(GW) = 0.000 #4(LX) = 0.000 #5(LY) = 19.847 #6(trns) = 0.000 #7(asym) = 0.0000 #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 0.0010 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) = 8.917 #2(GV) = 4.299 #3(GW) = -0.168 #4(LX) = 0.000 #5(LY) = 7.306 #6(trns) = 0.000 #7(asym) = 0.0000 #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 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.267	24 parameters
R_exp = 0.195	0 restraints
R(F²) = 0.18130	(Δ/σ)_max = 0.02
χ² = 1.904	Background function: GSAS Background function number 2 with 10 terms. Cosine Fourier series 1: 1.69071 2: -2.03612 3: -3.99352 4: -3.60868 5: -3.03652 6: -2.11781 7: -1.58570 8: -1.02935 9: -0.776166 10: -0.281473

Crystal data top

Fe₃O₄	Z = 8
M_r = 231.54	Synchrotron radiation, λ = 1.377285 Å
Cubic, Fd3m	T = 14 K
a = 8.3814 (5) Å	flat_sheet, 20 × 10 mm
V = 588.78 (10) Å³

Data collection top

Huber 4+2 circle diffractometer	Scan method: step
Specimen mounting: copper sample holder	2θ_min = 15.003°, 2θ_max = 150.193°, 2θ_step = 0.01°
Data collection mode: reflection

Refinement top

R_p = 0.168	χ² = 1.904
R_wp = 0.267	13520 data points
R_exp = 0.195	24 parameters
R(F²) = 0.18130	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe1	0.125	0.125	0.125	−0.001 (4)*
Fe2	0.5	0.5	0.5	−0.001 (4)*
O	0.2583	0.2583	0.2583	−0.001 (4)*

Geometric parameters (Å, º) top

Fe1—O	1.9351 (1)	Fe2—O^vii	2.0282 (1)
Fe1—Oⁱ	1.9351 (1)	Fe2—O^viii	2.0282 (1)
Fe1—Oⁱⁱ	1.9351 (1)	Fe2—O^ix	2.0282 (1)
Fe1—Oⁱⁱⁱ	1.9351 (1)	O—Fe1	1.9351 (1)
Fe2—O^iv	2.0282 (1)	O—Fe2^vii	2.0282 (1)
Fe2—O^v	2.0282 (1)	O—Fe2^viii	2.0282 (1)
Fe2—O^vi	2.0282 (1)	O—Fe2^ix	2.0282 (1)

O—Fe1—O^x	109.471 (2)	O^v—Fe2—O^ix	93.9965
O—Fe1—O^xi	109.471 (4)	O^vi—Fe2—O^xiii	93.9965
O—Fe1—O^xii	109.471 (2)	O^vi—Fe2—O^xiv	93.9965
O^x—Fe1—O^xi	109.471 (2)	O^vi—Fe2—O^ix	179.9802
O^x—Fe1—O^xii	109.471 (4)	O^xiii—Fe2—O^xiv	86.0035
O^xi—Fe1—O^xii	109.471 (2)	O^xiii—Fe2—O^ix	86.0035
O^iv—Fe2—O^v	86.0035	O^xiv—Fe2—O^ix	86.0035
O^iv—Fe2—O^vi	86.0035	Fe1—O—Fe2^xv	122.484 (2)
O^iv—Fe2—O^xiii	179.9802	Fe1—O—Fe2^viii	122.4840 (12)
O^iv—Fe2—O^xiv	93.9965	Fe1—O—Fe2^xvi	122.4840 (12)
O^iv—Fe2—O^ix	93.9965	Fe2^xv—O—Fe2^viii	93.8613
O^v—Fe2—O^vi	86.0035	Fe2^xv—O—Fe2^xvi	93.8613
O^v—Fe2—O^xiii	93.9965	Fe2^viii—O—Fe2^xvi	93.8613
O^v—Fe2—O^xiv	179.9802

Symmetry codes: (i) −z+1/4, x, −y+1/4; (ii) −z+1/4, −x+1/4, y; (iii) z, −x−3/4, −y−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) −x+3/4, −y+3/4, z; (viii) z, −x+3/4, −y+3/4; (ix) −y+3/4, z, −x+3/4; (x) −z−3/4, x−1, −y−7/4; (xi) −z−3/4, −x−3/4, y−2; (xii) z−1, −x+1/4, −y−3/4; (xiii) −x+3/4, −y+7/4, z−1; (xiv) z−1, −x+7/4, −y+3/4; (xv) −x+7/4, −y+3/4, z−1; (xvi) −y+7/4, z−1, −x+3/4.

(T14KBST_phase_3) top

Crystal data top

Ba₂FeReO₆	V = 259.11 (1) Å³
M_r = 306.36	Z = 4
Tetragonal, I4/mmm	Synchrotron radiation, λ = 1.377285 Å
Hall symbol: I 4/m m m	T = 14 K
a = 5.68278 (2) Å	Particle morphology: powder
c = 8.02337 (5) Å	flat_sheet, 20 × 10 mm

Data collection top

Huber 4+2 circle diffractometer	Data collection mode: reflection
Radiation source: synchrotron, LNLS D10B-XPD beamline	Scan method: step
Si 111 monochromator	2θ_min = 15.003°, 2θ_max = 150.193°, 2θ_step = 0.01°
Specimen mounting: copper sample holder

Refinement top

Least-squares matrix: full	13520 data points
R_p = 0.168	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) = 0.000 #2(GV) = 0.000 #3(GW) = 0.000 #4(LX) = 0.000 #5(LY) = 19.847 #6(trns) = 0.000 #7(asym) = 0.0000 #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 0.0010 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) = 8.917 #2(GV) = 4.299 #3(GW) = -0.168 #4(LX) = 0.000 #5(LY) = 7.306 #6(trns) = 0.000 #7(asym) = 0.0000 #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 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.267	24 parameters
R_exp = 0.195	0 restraints
R(F²) = 0.18130	(Δ/σ)_max = 0.02
χ² = 1.904	Background function: GSAS Background function number 2 with 10 terms. Cosine Fourier series 1: 1.69071 2: -2.03612 3: -3.99352 4: -3.60868 5: -3.03652 6: -2.11781 7: -1.58570 8: -1.02935 9: -0.776166 10: -0.281473

Crystal data top

Ba₂FeReO₆	V = 259.11 (1) Å³
M_r = 306.36	Z = 4
Tetragonal, I4/mmm	Synchrotron radiation, λ = 1.377285 Å
a = 5.68278 (2) Å	T = 14 K
c = 8.02337 (5) Å	flat_sheet, 20 × 10 mm

Data collection top

Huber 4+2 circle diffractometer	Scan method: step
Specimen mounting: copper sample holder	2θ_min = 15.003°, 2θ_max = 150.193°, 2θ_step = 0.01°
Data collection mode: reflection

Refinement top

R_p = 0.168	χ² = 1.904
R_wp = 0.267	13520 data points
R_exp = 0.195	24 parameters
R(F²) = 0.18130	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
FE1	0.0	0.0	0.0	0.00840 (17)*	0.9646
RE2	0.0	0.0	0.5	0.00840 (17)*	0.9646
BA3	0.5	0.0	0.25	0.00325 (16)*
O4	0.2570 (13)	0.2570 (13)	0.0	0.0011 (10)*
O5	0.0	0.0	0.255 (2)	0.0011 (10)*
FE6	0.0	0.0	0.5	0.00840 (17)*	0.0354
RE7	0.0	0.0	0.0	0.00840 (17)*	0.0354

Geometric parameters (Å, º) top

FE1—BA3ⁱ	3.4781 (1)	BA3—O5^xxviii	2.8417 (2)
FE1—BA3	3.4781 (1)	BA3—FE6	3.4781 (1)
FE1—BA3ⁱⁱ	3.4781 (1)	BA3—FE6^xviii	3.4781 (1)
FE1—BA3ⁱⁱⁱ	3.4781 (1)	BA3—FE6^xxi	3.4781 (1)
FE1—BA3^iv	3.4781 (1)	BA3—FE6^xxii	3.4781 (1)
FE1—BA3^v	3.4781 (1)	BA3—RE7	3.4781 (1)
FE1—BA3^vi	3.4781 (1)	BA3—RE7^xviii	3.4781 (1)
FE1—BA3^vii	3.4781 (1)	BA3—RE7^xix	3.4781 (1)
FE1—O4	2.065 (11)	BA3—RE7^xx	3.4781 (1)
FE1—O4ⁱⁱⁱ	2.065 (11)	O4—FE1	2.065 (11)
FE1—O4^viii	2.065 (11)	O4—RE2^xxii	1.953 (11)
FE1—O4^ix	2.065 (11)	O4—BA3	2.8396 (2)
FE1—O5	2.044 (17)	O4—BA3ⁱⁱⁱ	2.8396 (2)
FE1—O5^iv	2.044 (17)	O4—BA3^v	2.8396 (2)
RE2—BA3ⁱ	3.4781 (1)	O4—BA3^vii	2.8396 (2)
RE2—BA3	3.4781 (1)	O4—FE6^xxii	1.953 (11)
RE2—BA3ⁱⁱ	3.4781 (1)	O4—RE7	2.065 (11)
RE2—BA3ⁱⁱⁱ	3.4781 (1)	O5—FE1	2.044 (17)
RE2—BA3^x	3.4781 (1)	O5—RE2	1.968 (17)
RE2—BA3^xi	3.4781 (1)	O5—BA3ⁱ	2.8417 (2)
RE2—BA3^xii	3.4781 (1)	O5—BA3	2.8417 (2)
RE2—BA3^xiii	3.4781 (1)	O5—BA3ⁱⁱ	2.8417 (2)
RE2—O4^xiv	1.953 (11)	O5—BA3ⁱⁱⁱ	2.8417 (2)
RE2—O4^xv	1.953 (11)	O5—FE6	1.968 (17)
RE2—O4^xvi	1.953 (11)	O5—RE7	2.044 (17)
RE2—O4^xvii	1.953 (11)	FE6—BA3ⁱ	3.4781 (1)
RE2—O5	1.968 (17)	FE6—BA3	3.4781 (1)
RE2—O5^x	1.968 (17)	FE6—BA3ⁱⁱ	3.4781 (1)
BA3—FE1	3.4781 (1)	FE6—BA3ⁱⁱⁱ	3.4781 (1)
BA3—FE1^xviii	3.4781 (1)	FE6—BA3^x	3.4781 (1)
BA3—FE1^xix	3.4781 (1)	FE6—BA3^xi	3.4781 (1)
BA3—FE1^xx	3.4781 (1)	FE6—BA3^xii	3.4781 (1)
BA3—RE2	3.4781 (1)	FE6—BA3^xiii	3.4781 (1)
BA3—RE2^xviii	3.4781 (1)	FE6—O4^xiv	1.953 (11)
BA3—RE2^xxi	3.4781 (1)	FE6—O4^xv	1.953 (11)
BA3—RE2^xxii	3.4781 (1)	FE6—O4^xvi	1.953 (11)
BA3—BA3ⁱⁱ	4.0183 (1)	FE6—O4^xvii	1.953 (11)
BA3—BA3ⁱⁱⁱ	4.0183 (1)	FE6—O5	1.968 (17)
BA3—BA3^xxiii	4.0183 (1)	FE6—O5^x	1.968 (17)
BA3—BA3^xxiv	4.0183 (1)	RE7—BA3ⁱ	3.4781 (1)
BA3—BA3^v	4.0117 (1)	RE7—BA3	3.4781 (1)
BA3—BA3^xi	4.0117 (1)	RE7—BA3ⁱⁱ	3.4781 (1)
BA3—O4	2.8396 (2)	RE7—BA3ⁱⁱⁱ	3.4781 (1)
BA3—O4^xxiv	2.8396 (2)	RE7—BA3^iv	3.4781 (1)
BA3—O4^xxv	2.8396 (2)	RE7—BA3^v	3.4781 (1)
BA3—O4^ix	2.8396 (2)	RE7—BA3^vi	3.4781 (1)
BA3—O4^xix	2.8396 (2)	RE7—BA3^vii	3.4781 (1)
BA3—O4^xv	2.8396 (2)	RE7—O4	2.065 (11)
BA3—O4^xvi	2.8396 (2)	RE7—O4ⁱⁱⁱ	2.065 (11)
BA3—O4^xxvi	2.8396 (2)	RE7—O4^viii	2.065 (11)
BA3—O5	2.8417 (2)	RE7—O4^ix	2.065 (11)
BA3—O5^xviii	2.8417 (2)	RE7—O5	2.044 (17)
BA3—O5^xxvii	2.8417 (2)	RE7—O5^iv	2.044 (17)

BA3ⁱ—FE1—BA3	109.5606 (4)	BA3ⁱⁱ—BA3—O5^xviii	134.995 (5)
BA3ⁱ—FE1—BA3ⁱⁱ	70.5734 (2)	BA3ⁱⁱ—BA3—O5^xxvii	45.005 (5)
BA3ⁱ—FE1—BA3ⁱⁱⁱ	70.5734 (2)	BA3ⁱⁱⁱ—BA3—BA3^xxiii	180.0
BA3ⁱ—FE1—BA3^iv	70.4394 (4)	BA3ⁱⁱⁱ—BA3—BA3^xxiv	90.0
BA3ⁱ—FE1—BA3^v	180.0	BA3ⁱⁱⁱ—BA3—BA3^v	90.0
BA3ⁱ—FE1—BA3^vi	109.4265 (2)	BA3ⁱⁱⁱ—BA3—BA3^xi	90.0
BA3ⁱ—FE1—BA3^vii	109.4265 (2)	BA3ⁱⁱⁱ—BA3—O4	44.964 (4)
BA3ⁱ—FE1—O4	125.2867 (1)	BA3ⁱⁱⁱ—BA3—O4^xxiv	88.9 (2)
BA3ⁱ—FE1—O4ⁱⁱⁱ	54.7133 (1)	BA3ⁱⁱⁱ—BA3—O4^xxv	135.036 (4)
BA3ⁱ—FE1—O4^viii	54.7133 (1)	BA3ⁱⁱⁱ—BA3—O4^ix	91.1 (2)
BA3ⁱ—FE1—O4^ix	125.2867 (1)	BA3ⁱⁱⁱ—BA3—O4^xix	135.036 (4)
BA3ⁱ—FE1—O5	54.7803 (2)	BA3ⁱⁱⁱ—BA3—O4^xv	88.9 (2)
BA3ⁱ—FE1—O5^iv	125.2197 (2)	BA3ⁱⁱⁱ—BA3—O4^xvi	44.964 (4)
BA3—FE1—BA3ⁱⁱ	70.5734 (2)	BA3ⁱⁱⁱ—BA3—O4^xxvi	91.1 (2)
BA3—FE1—BA3ⁱⁱⁱ	70.5734 (2)	BA3ⁱⁱⁱ—BA3—O5	45.005 (5)
BA3—FE1—BA3^iv	180.0	BA3ⁱⁱⁱ—BA3—O5^xviii	134.995 (5)
BA3—FE1—BA3^v	70.4394 (4)	BA3ⁱⁱⁱ—BA3—O5^xxvii	134.995 (5)
BA3—FE1—BA3^vi	109.4266 (2)	BA3^xxiii—BA3—BA3^xxiv	90.0
BA3—FE1—BA3^vii	109.4265 (2)	BA3^xxiii—BA3—BA3^v	90.0
BA3—FE1—O4	54.7133 (1)	BA3^xxiii—BA3—BA3^xi	90.0
BA3—FE1—O4ⁱⁱⁱ	125.2867 (1)	BA3^xxiii—BA3—O4	135.036 (4)
BA3—FE1—O4^viii	125.2867 (1)	BA3^xxiii—BA3—O4^xxiv	91.1 (2)
BA3—FE1—O4^ix	54.7133 (1)	BA3^xxiii—BA3—O4^xxv	44.964 (4)
BA3—FE1—O5	54.7803 (2)	BA3^xxiii—BA3—O4^ix	88.9 (2)
BA3—FE1—O5^iv	125.2197 (2)	BA3^xxiii—BA3—O4^xix	44.964 (4)
BA3ⁱⁱ—FE1—BA3ⁱⁱⁱ	109.5606 (4)	BA3^xxiii—BA3—O4^xv	91.1 (2)
BA3ⁱⁱ—FE1—BA3^iv	109.4265 (2)	BA3^xxiii—BA3—O4^xvi	135.036 (4)
BA3ⁱⁱ—FE1—BA3^v	109.4265 (2)	BA3^xxiii—BA3—O4^xxvi	88.9 (2)
BA3ⁱⁱ—FE1—BA3^vi	70.4394 (4)	BA3^xxiii—BA3—O5	134.995 (5)
BA3ⁱⁱ—FE1—BA3^vii	180.0	BA3^xxiii—BA3—O5^xviii	45.005 (5)
BA3ⁱⁱ—FE1—O4	125.2867 (1)	BA3^xxiii—BA3—O5^xxvii	45.005 (5)
BA3ⁱⁱ—FE1—O4ⁱⁱⁱ	125.2867 (1)	BA3^xxiv—BA3—BA3^v	90.0
BA3ⁱⁱ—FE1—O4^viii	54.7133 (1)	BA3^xxiv—BA3—BA3^xi	90.0
BA3ⁱⁱ—FE1—O4^ix	54.7133 (1)	BA3^xxiv—BA3—O4	88.9 (2)
BA3ⁱⁱ—FE1—O5	54.7803 (2)	BA3^xxiv—BA3—O4^xxiv	44.964 (4)
BA3ⁱⁱ—FE1—O5^iv	125.2197 (2)	BA3^xxiv—BA3—O4^xxv	91.1 (2)
BA3ⁱⁱⁱ—FE1—BA3^iv	109.4266 (2)	BA3^xxiv—BA3—O4^ix	135.036 (4)
BA3ⁱⁱⁱ—FE1—BA3^v	109.4265 (2)	BA3^xxiv—BA3—O4^xix	88.9 (2)
BA3ⁱⁱⁱ—FE1—BA3^vi	180.0	BA3^xxiv—BA3—O4^xv	135.036 (4)
BA3ⁱⁱⁱ—FE1—BA3^vii	70.4394 (4)	BA3^xxiv—BA3—O4^xvi	91.1 (2)
BA3ⁱⁱⁱ—FE1—O4	54.7133 (1)	BA3^xxiv—BA3—O4^xxvi	44.964 (4)
BA3ⁱⁱⁱ—FE1—O4ⁱⁱⁱ	54.7133 (1)	BA3^xxiv—BA3—O5	134.995 (5)
BA3ⁱⁱⁱ—FE1—O4^viii	125.2867 (1)	BA3^xxiv—BA3—O5^xviii	45.005 (5)
BA3ⁱⁱⁱ—FE1—O4^ix	125.2867 (1)	BA3^xxiv—BA3—O5^xxvii	134.995 (5)
BA3ⁱⁱⁱ—FE1—O5	54.7803 (2)	BA3^v—BA3—BA3^xi	180.0
BA3ⁱⁱⁱ—FE1—O5^iv	125.2197 (2)	BA3^v—BA3—O4	45.058 (4)
BA3^iv—FE1—BA3^v	109.5606 (4)	BA3^v—BA3—O4^xxiv	45.058 (4)
BA3^iv—FE1—BA3^vi	70.5734 (2)	BA3^v—BA3—O4^xxv	45.058 (4)
BA3^iv—FE1—BA3^vii	70.5734 (2)	BA3^v—BA3—O4^ix	45.058 (4)
BA3^iv—FE1—O4	125.2867 (1)	BA3^v—BA3—O4^xix	134.941 (4)
BA3^iv—FE1—O4ⁱⁱⁱ	54.7133 (1)	BA3^v—BA3—O4^xv	134.941 (4)
BA3^iv—FE1—O4^viii	54.7133 (1)	BA3^v—BA3—O4^xvi	134.941 (4)
BA3^iv—FE1—O4^ix	125.2867 (1)	BA3^v—BA3—O4^xxvi	134.941 (4)
BA3^iv—FE1—O5	125.2197 (2)	BA3^v—BA3—O5	90.8 (3)
BA3^iv—FE1—O5^iv	54.7803 (2)	BA3^v—BA3—O5^xviii	90.8 (3)
BA3^v—FE1—BA3^vi	70.5734 (2)	BA3^v—BA3—O5^xxvii	89.2 (3)
BA3^v—FE1—BA3^vii	70.5734 (2)	BA3^xi—BA3—O4	134.941 (4)
BA3^v—FE1—O4	54.7133 (1)	BA3^xi—BA3—O4^xxiv	134.941 (4)
BA3^v—FE1—O4ⁱⁱⁱ	125.2867 (1)	BA3^xi—BA3—O4^xxv	134.941 (4)
BA3^v—FE1—O4^viii	125.2867 (1)	BA3^xi—BA3—O4^ix	134.941 (4)
BA3^v—FE1—O4^ix	54.7133 (1)	BA3^xi—BA3—O4^xix	45.058 (4)
BA3^v—FE1—O5	125.2197 (2)	BA3^xi—BA3—O4^xv	45.058 (4)
BA3^v—FE1—O5^iv	54.7803 (2)	BA3^xi—BA3—O4^xvi	45.058 (4)
BA3^vi—FE1—BA3^vii	109.5606 (4)	BA3^xi—BA3—O4^xxvi	45.058 (4)
BA3^vi—FE1—O4	125.2867 (1)	BA3^xi—BA3—O5	89.2 (3)
BA3^vi—FE1—O4ⁱⁱⁱ	125.2867 (1)	BA3^xi—BA3—O5^xviii	89.2 (3)
BA3^vi—FE1—O4^viii	54.7133 (1)	BA3^xi—BA3—O5^xxvii	90.8 (3)
BA3^vi—FE1—O4^ix	54.7133 (1)	O4—BA3—O4^xxiv	58.2 (4)
BA3^vi—FE1—O5	125.2197 (2)	O4—BA3—O4^xxv	90.117 (8)
BA3^vi—FE1—O5^iv	54.7803 (2)	O4—BA3—O4^ix	61.9 (4)
BA3^vii—FE1—O4	54.7133 (1)	O4—BA3—O4^xix	177.7 (4)
BA3^vii—FE1—O4ⁱⁱⁱ	54.7133 (1)	O4—BA3—O4^xv	119.932 (5)
BA3^vii—FE1—O4^viii	125.2867 (1)	O4—BA3—O4^xvi	89.927 (9)
BA3^vii—FE1—O4^ix	125.2867 (1)	O4—BA3—O4^xxvi	119.932 (5)
BA3^vii—FE1—O5	125.2197 (2)	O4—BA3—O5	61.5 (3)
BA3^vii—FE1—O5^iv	54.7803 (2)	O4—BA3—O5^xviii	119.7 (4)
O4—FE1—O4ⁱⁱⁱ	90.0	O4—BA3—O5^xxvii	120.3 (4)
O4—FE1—O4^viii	179.9802	O4^xxiv—BA3—O4^xxv	61.9 (4)
O4—FE1—O4^ix	90.0	O4^xxiv—BA3—O4^ix	90.117 (8)
O4—FE1—O5	90.0	O4^xxiv—BA3—O4^xix	119.932 (5)
O4—FE1—O5^iv	90.0	O4^xxiv—BA3—O4^xv	177.7 (4)
O4ⁱⁱⁱ—FE1—O4^viii	90.0	O4^xxiv—BA3—O4^xvi	119.932 (5)
O4ⁱⁱⁱ—FE1—O4^ix	179.972	O4^xxiv—BA3—O4^xxvi	89.927 (9)
O4ⁱⁱⁱ—FE1—O5	90.0	O4^xxiv—BA3—O5	119.7 (4)
O4ⁱⁱⁱ—FE1—O5^iv	90.0	O4^xxiv—BA3—O5^xviii	61.5 (3)
O4^viii—FE1—O4^ix	90.0	O4^xxiv—BA3—O5^xxvii	120.3 (4)
O4^viii—FE1—O5	90.0	O4^xxv—BA3—O4^ix	58.2 (4)
O4^viii—FE1—O5^iv	90.0	O4^xxv—BA3—O4^xix	89.927 (9)
O4^ix—FE1—O5	90.0	O4^xxv—BA3—O4^xv	119.932 (5)
O4^ix—FE1—O5^iv	90.0	O4^xxv—BA3—O4^xvi	177.7 (4)
O5—FE1—O5^iv	180.0	O4^xxv—BA3—O4^xxvi	119.932 (5)
BA3ⁱ—RE2—BA3	109.5606 (4)	O4^xxv—BA3—O5	119.7 (4)
BA3ⁱ—RE2—BA3ⁱⁱ	70.5734 (2)	O4^xxv—BA3—O5^xviii	61.5 (3)
BA3ⁱ—RE2—BA3ⁱⁱⁱ	70.5734 (2)	O4^xxv—BA3—O5^xxvii	58.4 (3)
BA3ⁱ—RE2—BA3^x	70.4394 (4)	O4^ix—BA3—O4^xix	119.932 (5)
BA3ⁱ—RE2—BA3^xi	180.0	O4^ix—BA3—O4^xv	89.927 (9)
BA3ⁱ—RE2—BA3^xii	109.4265 (2)	O4^ix—BA3—O4^xvi	119.932 (5)
BA3ⁱ—RE2—BA3^xiii	109.4266 (2)	O4^ix—BA3—O4^xxvi	177.7 (4)
BA3ⁱ—RE2—O4^xiv	54.7133 (1)	O4^ix—BA3—O5	61.5 (3)
BA3ⁱ—RE2—O4^xv	125.2867 (1)	O4^ix—BA3—O5^xviii	119.7 (4)
BA3ⁱ—RE2—O4^xvi	125.2867 (1)	O4^ix—BA3—O5^xxvii	58.4 (3)
BA3ⁱ—RE2—O4^xvii	54.7133 (1)	O4^xix—BA3—O4^xv	61.9 (4)
BA3ⁱ—RE2—O5	54.7803 (2)	O4^xix—BA3—O4^xvi	90.117 (8)
BA3ⁱ—RE2—O5^x	125.2197 (2)	O4^xix—BA3—O4^xxvi	58.2 (4)
BA3—RE2—BA3ⁱⁱ	70.5734 (2)	O4^xix—BA3—O5	120.3 (4)
BA3—RE2—BA3ⁱⁱⁱ	70.5734 (2)	O4^xix—BA3—O5^xviii	58.4 (3)
BA3—RE2—BA3^x	180.0	O4^xix—BA3—O5^xxvii	61.5 (3)
BA3—RE2—BA3^xi	70.4394 (4)	O4^xv—BA3—O4^xvi	58.2 (4)
BA3—RE2—BA3^xii	109.4265 (2)	O4^xv—BA3—O4^xxvi	90.117 (8)
BA3—RE2—BA3^xiii	109.4265 (2)	O4^xv—BA3—O5	58.4 (3)
BA3—RE2—O4^xiv	125.2867 (1)	O4^xv—BA3—O5^xviii	120.3 (4)
BA3—RE2—O4^xv	54.7133 (1)	O4^xv—BA3—O5^xxvii	61.5 (3)
BA3—RE2—O4^xvi	54.7133 (1)	O4^xvi—BA3—O4^xxvi	61.9 (4)
BA3—RE2—O4^xvii	125.2867 (1)	O4^xvi—BA3—O5	58.4 (3)
BA3—RE2—O5	54.7803 (2)	O4^xvi—BA3—O5^xviii	120.3 (4)
BA3—RE2—O5^x	125.2197 (2)	O4^xvi—BA3—O5^xxvii	119.7 (4)
BA3ⁱⁱ—RE2—BA3ⁱⁱⁱ	109.5606 (4)	O4^xxvi—BA3—O5	120.3 (4)
BA3ⁱⁱ—RE2—BA3^x	109.4265 (2)	O4^xxvi—BA3—O5^xviii	58.4 (3)
BA3ⁱⁱ—RE2—BA3^xi	109.4266 (2)	O4^xxvi—BA3—O5^xxvii	119.7 (4)
BA3ⁱⁱ—RE2—BA3^xii	70.4394 (4)	O5—BA3—O5^xviii	178.5 (7)
BA3ⁱⁱ—RE2—BA3^xiii	180.0	O5—BA3—O5^xxvii	90.010 (9)
BA3ⁱⁱ—RE2—O4^xiv	54.7133 (1)	O5^xviii—BA3—O5^xxvii	90.010 (9)
BA3ⁱⁱ—RE2—O4^xv	54.7133 (1)	FE1—O4—RE2^xxii	180.0
BA3ⁱⁱ—RE2—O4^xvi	125.2867 (1)	FE1—O4—BA3	88.9 (2)
BA3ⁱⁱ—RE2—O4^xvii	125.2867 (1)	FE1—O4—BA3ⁱⁱⁱ	88.9 (2)
BA3ⁱⁱ—RE2—O5	54.7803 (2)	FE1—O4—BA3^v	88.9 (2)
BA3ⁱⁱ—RE2—O5^x	125.2197 (2)	FE1—O4—BA3^vii	88.9 (2)
BA3ⁱⁱⁱ—RE2—BA3^x	109.4265 (2)	FE1—O4—FE6^xxii	180.0
BA3ⁱⁱⁱ—RE2—BA3^xi	109.4265 (2)	FE1—O4—RE7	0.0
BA3ⁱⁱⁱ—RE2—BA3^xii	180.0	RE2^xxii—O4—BA3	91.1 (2)
BA3ⁱⁱⁱ—RE2—BA3^xiii	70.4394 (4)	RE2^xxii—O4—BA3ⁱⁱⁱ	91.1 (2)
BA3ⁱⁱⁱ—RE2—O4^xiv	125.2867 (1)	RE2^xxii—O4—BA3^v	91.1 (2)
BA3ⁱⁱⁱ—RE2—O4^xv	125.2867 (1)	RE2^xxii—O4—BA3^vii	91.1 (2)
BA3ⁱⁱⁱ—RE2—O4^xvi	54.7133 (1)	RE2^xxii—O4—FE6^xxii	0.0
BA3ⁱⁱⁱ—RE2—O4^xvii	54.7133 (1)	RE2^xxii—O4—RE7	180.0
BA3ⁱⁱⁱ—RE2—O5	54.7803 (2)	BA3—O4—BA3ⁱⁱⁱ	90.073 (9)
BA3ⁱⁱⁱ—RE2—O5^x	125.2197 (2)	BA3—O4—BA3^v	89.883 (8)
BA3^x—RE2—BA3^xi	109.5606 (4)	BA3—O4—BA3^vii	177.7 (4)
BA3^x—RE2—BA3^xii	70.5734 (2)	BA3—O4—FE6^xxii	91.1 (2)
BA3^x—RE2—BA3^xiii	70.5734 (2)	BA3—O4—RE7	88.9 (2)
BA3^x—RE2—O4^xiv	54.7133 (1)	BA3ⁱⁱⁱ—O4—BA3^v	177.7 (4)
BA3^x—RE2—O4^xv	125.2867 (1)	BA3ⁱⁱⁱ—O4—BA3^vii	89.883 (8)
BA3^x—RE2—O4^xvi	125.2867 (1)	BA3ⁱⁱⁱ—O4—FE6^xxii	91.1 (2)
BA3^x—RE2—O4^xvii	54.7133 (1)	BA3ⁱⁱⁱ—O4—RE7	88.9 (2)
BA3^x—RE2—O5	125.2197 (2)	BA3^v—O4—BA3^vii	90.073 (9)
BA3^x—RE2—O5^x	54.7803 (2)	BA3^v—O4—FE6^xxii	91.1 (2)
BA3^xi—RE2—BA3^xii	70.5734 (2)	BA3^v—O4—RE7	88.9 (2)
BA3^xi—RE2—BA3^xiii	70.5734 (2)	BA3^vii—O4—FE6^xxii	91.1 (2)
BA3^xi—RE2—O4^xiv	125.2867 (1)	BA3^vii—O4—RE7	88.9 (2)
BA3^xi—RE2—O4^xv	54.7133 (1)	FE6^xxii—O4—RE7	180.0
BA3^xi—RE2—O4^xvi	54.7133 (1)	FE1—O5—RE2	180.0
BA3^xi—RE2—O4^xvii	125.2867 (1)	FE1—O5—BA3ⁱ	89.2 (3)
BA3^xi—RE2—O5	125.2197 (2)	FE1—O5—BA3	89.2 (3)
BA3^xi—RE2—O5^x	54.7803 (2)	FE1—O5—BA3ⁱⁱ	89.2 (3)
BA3^xii—RE2—BA3^xiii	109.5606 (4)	FE1—O5—BA3ⁱⁱⁱ	89.2 (3)
BA3^xii—RE2—O4^xiv	54.7133 (1)	FE1—O5—FE6	180.0
BA3^xii—RE2—O4^xv	54.7133 (1)	FE1—O5—RE7	0.0
BA3^xii—RE2—O4^xvi	125.2867 (1)	RE2—O5—BA3ⁱ	90.8 (3)
BA3^xii—RE2—O4^xvii	125.2867 (1)	RE2—O5—BA3	90.8 (3)
BA3^xii—RE2—O5	125.2197 (2)	RE2—O5—BA3ⁱⁱ	90.8 (3)
BA3^xii—RE2—O5^x	54.7803 (2)	RE2—O5—BA3ⁱⁱⁱ	90.8 (3)
BA3^xiii—RE2—O4^xiv	125.2867 (1)	RE2—O5—FE6	0.0
BA3^xiii—RE2—O4^xv	125.2867 (1)	RE2—O5—RE7	180.0
BA3^xiii—RE2—O4^xvi	54.7133 (1)	BA3ⁱ—O5—BA3	178.5 (7)
BA3^xiii—RE2—O4^xvii	54.7133 (1)	BA3ⁱ—O5—BA3ⁱⁱ	89.990 (9)
BA3^xiii—RE2—O5	125.2197 (2)	BA3ⁱ—O5—BA3ⁱⁱⁱ	89.990 (9)
BA3^xiii—RE2—O5^x	54.7803 (2)	BA3ⁱ—O5—FE6	90.8 (3)
O4^xiv—RE2—O4^xv	90.0	BA3ⁱ—O5—RE7	89.2 (3)
O4^xiv—RE2—O4^xvi	180.0	BA3—O5—BA3ⁱⁱ	89.990 (9)
O4^xiv—RE2—O4^xvii	90.0	BA3—O5—BA3ⁱⁱⁱ	89.990 (9)
O4^xiv—RE2—O5	90.0	BA3—O5—FE6	90.8 (3)
O4^xiv—RE2—O5^x	90.0	BA3—O5—RE7	89.2 (3)
O4^xv—RE2—O4^xvi	90.0	BA3ⁱⁱ—O5—BA3ⁱⁱⁱ	178.5 (7)
O4^xv—RE2—O4^xvii	180.0	BA3ⁱⁱ—O5—FE6	90.8 (3)
O4^xv—RE2—O5	90.0	BA3ⁱⁱ—O5—RE7	89.2 (3)
O4^xv—RE2—O5^x	90.0	BA3ⁱⁱⁱ—O5—FE6	90.8 (3)
O4^xvi—RE2—O4^xvii	90.0	BA3ⁱⁱⁱ—O5—RE7	89.2 (3)
O4^xvi—RE2—O5	90.0	FE6—O5—RE7	180.0
O4^xvi—RE2—O5^x	90.0	BA3ⁱ—FE6—BA3	109.5606 (4)
O4^xvii—RE2—O5	90.0	BA3ⁱ—FE6—BA3ⁱⁱ	70.5734 (2)
O4^xvii—RE2—O5^x	90.0	BA3ⁱ—FE6—BA3ⁱⁱⁱ	70.5734 (2)
O5—RE2—O5^x	180.0	BA3ⁱ—FE6—BA3^x	70.4394 (4)
FE1—BA3—FE1^xviii	109.5606 (4)	BA3ⁱ—FE6—BA3^xi	180.0
FE1—BA3—FE1^xix	109.4265 (2)	BA3ⁱ—FE6—BA3^xii	109.4265 (2)
FE1—BA3—FE1^xx	109.4266 (2)	BA3ⁱ—FE6—BA3^xiii	109.4266 (2)
FE1—BA3—RE2	70.4394 (4)	BA3ⁱ—FE6—O4^xiv	54.7133 (1)
FE1—BA3—RE2^xviii	180.0	BA3ⁱ—FE6—O4^xv	125.2867 (1)
FE1—BA3—RE2^xxi	70.5734 (2)	BA3ⁱ—FE6—O4^xvi	125.2867 (1)
FE1—BA3—RE2^xxii	70.5734 (2)	BA3ⁱ—FE6—O4^xvii	54.7133 (1)
FE1—BA3—BA3ⁱⁱ	54.7133 (1)	BA3ⁱ—FE6—O5	54.7803 (2)
FE1—BA3—BA3ⁱⁱⁱ	54.7133 (1)	BA3ⁱ—FE6—O5^x	125.2197 (2)
FE1—BA3—BA3^xxiii	125.2867 (1)	BA3—FE6—BA3ⁱⁱ	70.5734 (2)
FE1—BA3—BA3^xxiv	125.2867 (1)	BA3—FE6—BA3ⁱⁱⁱ	70.5734 (2)
FE1—BA3—BA3^v	54.7803 (2)	BA3—FE6—BA3^x	180.0
FE1—BA3—BA3^xi	125.2197 (2)	BA3—FE6—BA3^xi	70.4394 (4)
FE1—BA3—O4	36.4 (2)	BA3—FE6—BA3^xii	109.4265 (2)
FE1—BA3—O4^xxiv	89.43 (12)	BA3—FE6—BA3^xiii	109.4265 (2)
FE1—BA3—O4^xxv	89.43 (12)	BA3—FE6—O4^xiv	125.2867 (1)
FE1—BA3—O4^ix	36.4 (2)	BA3—FE6—O4^xv	54.7133 (1)
FE1—BA3—O4^xix	145.8 (2)	BA3—FE6—O4^xvi	54.7133 (1)
FE1—BA3—O4^xv	89.27 (12)	BA3—FE6—O4^xvii	125.2867 (1)
FE1—BA3—O4^xvi	89.27 (12)	BA3—FE6—O5	54.7803 (2)
FE1—BA3—O4^xxvi	145.8 (2)	BA3—FE6—O5^x	125.2197 (2)
FE1—BA3—O5	36.0 (3)	BA3ⁱⁱ—FE6—BA3ⁱⁱⁱ	109.5606 (4)
FE1—BA3—O5^xviii	145.6 (3)	BA3ⁱⁱ—FE6—BA3^x	109.4265 (2)
FE1—BA3—O5^xxvii	89.6 (2)	BA3ⁱⁱ—FE6—BA3^xi	109.4266 (2)
FE1^xviii—BA3—FE1^xix	109.4265 (2)	BA3ⁱⁱ—FE6—BA3^xii	70.4394 (4)
FE1^xviii—BA3—FE1^xx	109.4265 (2)	BA3ⁱⁱ—FE6—BA3^xiii	180.0
FE1^xviii—BA3—RE2	180.0	BA3ⁱⁱ—FE6—O4^xiv	54.7133 (1)
FE1^xviii—BA3—RE2^xviii	70.4394 (4)	BA3ⁱⁱ—FE6—O4^xv	54.7133 (1)
FE1^xviii—BA3—RE2^xxi	70.5734 (2)	BA3ⁱⁱ—FE6—O4^xvi	125.2867 (1)
FE1^xviii—BA3—RE2^xxii	70.5734 (2)	BA3ⁱⁱ—FE6—O4^xvii	125.2867 (1)
FE1^xviii—BA3—BA3ⁱⁱ	125.2867 (1)	BA3ⁱⁱ—FE6—O5	54.7803 (2)
FE1^xviii—BA3—BA3ⁱⁱⁱ	125.2867 (1)	BA3ⁱⁱ—FE6—O5^x	125.2197 (2)
FE1^xviii—BA3—BA3^xxiii	54.7133 (1)	BA3ⁱⁱⁱ—FE6—BA3^x	109.4265 (2)
FE1^xviii—BA3—BA3^xxiv	54.7133 (1)	BA3ⁱⁱⁱ—FE6—BA3^xi	109.4265 (2)
FE1^xviii—BA3—BA3^v	54.7803 (2)	BA3ⁱⁱⁱ—FE6—BA3^xii	180.0
FE1^xviii—BA3—BA3^xi	125.2197 (2)	BA3ⁱⁱⁱ—FE6—BA3^xiii	70.4394 (4)
FE1^xviii—BA3—O4	89.43 (12)	BA3ⁱⁱⁱ—FE6—O4^xiv	125.2867 (1)
FE1^xviii—BA3—O4^xxiv	36.4 (2)	BA3ⁱⁱⁱ—FE6—O4^xv	125.2867 (1)
FE1^xviii—BA3—O4^xxv	36.4 (2)	BA3ⁱⁱⁱ—FE6—O4^xvi	54.7133 (1)
FE1^xviii—BA3—O4^ix	89.43 (12)	BA3ⁱⁱⁱ—FE6—O4^xvii	54.7133 (1)
FE1^xviii—BA3—O4^xix	89.27 (12)	BA3ⁱⁱⁱ—FE6—O5	54.7803 (2)
FE1^xviii—BA3—O4^xv	145.8 (2)	BA3ⁱⁱⁱ—FE6—O5^x	125.2197 (2)
FE1^xviii—BA3—O4^xvi	145.8 (2)	BA3^x—FE6—BA3^xi	109.5606 (4)
FE1^xviii—BA3—O4^xxvi	89.27 (12)	BA3^x—FE6—BA3^xii	70.5734 (2)
FE1^xviii—BA3—O5	145.6 (3)	BA3^x—FE6—BA3^xiii	70.5734 (2)
FE1^xviii—BA3—O5^xviii	36.0 (3)	BA3^x—FE6—O4^xiv	54.7133 (1)
FE1^xviii—BA3—O5^xxvii	89.6 (2)	BA3^x—FE6—O4^xv	125.2867 (1)
FE1^xix—BA3—FE1^xx	109.5606 (4)	BA3^x—FE6—O4^xvi	125.2867 (1)
FE1^xix—BA3—RE2	70.5734 (2)	BA3^x—FE6—O4^xvii	54.7133 (1)
FE1^xix—BA3—RE2^xviii	70.5734 (2)	BA3^x—FE6—O5	125.2197 (2)
FE1^xix—BA3—RE2^xxi	70.4394 (4)	BA3^x—FE6—O5^x	54.7803 (2)
FE1^xix—BA3—RE2^xxii	180.0	BA3^xi—FE6—BA3^xii	70.5734 (2)
FE1^xix—BA3—BA3ⁱⁱ	54.7133 (1)	BA3^xi—FE6—BA3^xiii	70.5734 (2)
FE1^xix—BA3—BA3ⁱⁱⁱ	125.2867 (1)	BA3^xi—FE6—O4^xiv	125.2867 (1)
FE1^xix—BA3—BA3^xxiii	54.7133 (1)	BA3^xi—FE6—O4^xv	54.7133 (1)
FE1^xix—BA3—BA3^xxiv	125.2867 (1)	BA3^xi—FE6—O4^xvi	54.7133 (1)
FE1^xix—BA3—BA3^v	125.2197 (2)	BA3^xi—FE6—O4^xvii	125.2867 (1)
FE1^xix—BA3—BA3^xi	54.7803 (2)	BA3^xi—FE6—O5	125.2197 (2)
FE1^xix—BA3—O4	145.8 (2)	BA3^xi—FE6—O5^x	54.7803 (2)
FE1^xix—BA3—O4^xxiv	145.8 (2)	BA3^xii—FE6—BA3^xiii	109.5606 (4)
FE1^xix—BA3—O4^xxv	89.27 (12)	BA3^xii—FE6—O4^xiv	54.7133 (1)
FE1^xix—BA3—O4^ix	89.27 (12)	BA3^xii—FE6—O4^xv	54.7133 (1)
FE1^xix—BA3—O4^xix	36.4 (2)	BA3^xii—FE6—O4^xvi	125.2867 (1)
FE1^xix—BA3—O4^xv	36.4 (2)	BA3^xii—FE6—O4^xvii	125.2867 (1)
FE1^xix—BA3—O4^xvi	89.43 (12)	BA3^xii—FE6—O5	125.2197 (2)
FE1^xix—BA3—O4^xxvi	89.43 (12)	BA3^xii—FE6—O5^x	54.7803 (2)
FE1^xix—BA3—O5	89.6 (2)	BA3^xiii—FE6—O4^xiv	125.2867 (1)
FE1^xix—BA3—O5^xviii	89.6 (2)	BA3^xiii—FE6—O4^xv	125.2867 (1)
FE1^xix—BA3—O5^xxvii	36.0 (3)	BA3^xiii—FE6—O4^xvi	54.7133 (1)
FE1^xx—BA3—RE2	70.5734 (2)	BA3^xiii—FE6—O4^xvii	54.7133 (1)
FE1^xx—BA3—RE2^xviii	70.5734 (2)	BA3^xiii—FE6—O5	125.2197 (2)
FE1^xx—BA3—RE2^xxi	180.0	BA3^xiii—FE6—O5^x	54.7803 (2)
FE1^xx—BA3—RE2^xxii	70.4394 (4)	O4^xiv—FE6—O4^xv	90.0
FE1^xx—BA3—BA3ⁱⁱ	125.2867 (1)	O4^xiv—FE6—O4^xvi	180.0
FE1^xx—BA3—BA3ⁱⁱⁱ	54.7133 (1)	O4^xiv—FE6—O4^xvii	90.0
FE1^xx—BA3—BA3^xxiii	125.2867 (1)	O4^xiv—FE6—O5	90.0
FE1^xx—BA3—BA3^xxiv	54.7133 (1)	O4^xiv—FE6—O5^x	90.0
FE1^xx—BA3—BA3^v	125.2197 (2)	O4^xv—FE6—O4^xvi	90.0
FE1^xx—BA3—BA3^xi	54.7803 (2)	O4^xv—FE6—O4^xvii	180.0
FE1^xx—BA3—O4	89.27 (12)	O4^xv—FE6—O5	90.0
FE1^xx—BA3—O4^xxiv	89.27 (12)	O4^xv—FE6—O5^x	90.0
FE1^xx—BA3—O4^xxv	145.8 (2)	O4^xvi—FE6—O4^xvii	90.0
FE1^xx—BA3—O4^ix	145.8 (2)	O4^xvi—FE6—O5	90.0
FE1^xx—BA3—O4^xix	89.43 (12)	O4^xvi—FE6—O5^x	90.0
FE1^xx—BA3—O4^xv	89.43 (12)	O4^xvii—FE6—O5	90.0
FE1^xx—BA3—O4^xvi	36.4 (2)	O4^xvii—FE6—O5^x	90.0
FE1^xx—BA3—O4^xxvi	36.4 (2)	O5—FE6—O5^x	180.0
FE1^xx—BA3—O5	89.6 (2)	BA3ⁱ—RE7—BA3	109.5606 (4)
FE1^xx—BA3—O5^xviii	89.6 (2)	BA3ⁱ—RE7—BA3ⁱⁱ	70.5734 (2)
FE1^xx—BA3—O5^xxvii	145.6 (3)	BA3ⁱ—RE7—BA3ⁱⁱⁱ	70.5734 (2)
RE2—BA3—RE2^xviii	109.5606 (4)	BA3ⁱ—RE7—BA3^iv	70.4394 (4)
RE2—BA3—RE2^xxi	109.4265 (2)	BA3ⁱ—RE7—BA3^v	180.0
RE2—BA3—RE2^xxii	109.4265 (2)	BA3ⁱ—RE7—BA3^vi	109.4265 (2)
RE2—BA3—BA3ⁱⁱ	54.7133 (1)	BA3ⁱ—RE7—BA3^vii	109.4265 (2)
RE2—BA3—BA3ⁱⁱⁱ	54.7133 (1)	BA3ⁱ—RE7—O4	125.2867 (1)
RE2—BA3—BA3^xxiii	125.2867 (1)	BA3ⁱ—RE7—O4ⁱⁱⁱ	54.7133 (1)
RE2—BA3—BA3^xxiv	125.2867 (1)	BA3ⁱ—RE7—O4^viii	54.7133 (1)
RE2—BA3—BA3^v	125.2197 (2)	BA3ⁱ—RE7—O4^ix	125.2867 (1)
RE2—BA3—BA3^xi	54.7803 (2)	BA3ⁱ—RE7—O5	54.7803 (2)
RE2—BA3—O4	90.57 (12)	BA3ⁱ—RE7—O5^iv	125.2197 (2)
RE2—BA3—O4^xxiv	143.6 (2)	BA3—RE7—BA3ⁱⁱ	70.5734 (2)
RE2—BA3—O4^xxv	143.6 (2)	BA3—RE7—BA3ⁱⁱⁱ	70.5734 (2)
RE2—BA3—O4^ix	90.57 (12)	BA3—RE7—BA3^iv	180.0
RE2—BA3—O4^xix	90.73 (12)	BA3—RE7—BA3^v	70.4394 (4)
RE2—BA3—O4^xv	34.2 (2)	BA3—RE7—BA3^vi	109.4266 (2)
RE2—BA3—O4^xvi	34.2 (2)	BA3—RE7—BA3^vii	109.4265 (2)
RE2—BA3—O4^xxvi	90.73 (12)	BA3—RE7—O4	54.7133 (1)
RE2—BA3—O5	34.5 (3)	BA3—RE7—O4ⁱⁱⁱ	125.2867 (1)
RE2—BA3—O5^xviii	144.0 (3)	BA3—RE7—O4^viii	125.2867 (1)
RE2—BA3—O5^xxvii	90.4 (2)	BA3—RE7—O4^ix	54.7133 (1)
RE2^xviii—BA3—RE2^xxi	109.4266 (2)	BA3—RE7—O5	54.7803 (2)
RE2^xviii—BA3—RE2^xxii	109.4265 (2)	BA3—RE7—O5^iv	125.2197 (2)
RE2^xviii—BA3—BA3ⁱⁱ	125.2867 (1)	BA3ⁱⁱ—RE7—BA3ⁱⁱⁱ	109.5606 (4)
RE2^xviii—BA3—BA3ⁱⁱⁱ	125.2867 (1)	BA3ⁱⁱ—RE7—BA3^iv	109.4265 (2)
RE2^xviii—BA3—BA3^xxiii	54.7133 (1)	BA3ⁱⁱ—RE7—BA3^v	109.4265 (2)
RE2^xviii—BA3—BA3^xxiv	54.7133 (1)	BA3ⁱⁱ—RE7—BA3^vi	70.4394 (4)
RE2^xviii—BA3—BA3^v	125.2197 (2)	BA3ⁱⁱ—RE7—BA3^vii	180.0
RE2^xviii—BA3—BA3^xi	54.7803 (2)	BA3ⁱⁱ—RE7—O4	125.2867 (1)
RE2^xviii—BA3—O4	143.6 (2)	BA3ⁱⁱ—RE7—O4ⁱⁱⁱ	125.2867 (1)
RE2^xviii—BA3—O4^xxiv	90.57 (12)	BA3ⁱⁱ—RE7—O4^viii	54.7133 (1)
RE2^xviii—BA3—O4^xxv	90.57 (12)	BA3ⁱⁱ—RE7—O4^ix	54.7133 (1)
RE2^xviii—BA3—O4^ix	143.6 (2)	BA3ⁱⁱ—RE7—O5	54.7803 (2)
RE2^xviii—BA3—O4^xix	34.2 (2)	BA3ⁱⁱ—RE7—O5^iv	125.2197 (2)
RE2^xviii—BA3—O4^xv	90.73 (12)	BA3ⁱⁱⁱ—RE7—BA3^iv	109.4266 (2)
RE2^xviii—BA3—O4^xvi	90.73 (12)	BA3ⁱⁱⁱ—RE7—BA3^v	109.4265 (2)
RE2^xviii—BA3—O4^xxvi	34.2 (2)	BA3ⁱⁱⁱ—RE7—BA3^vi	180.0
RE2^xviii—BA3—O5	144.0 (3)	BA3ⁱⁱⁱ—RE7—BA3^vii	70.4394 (4)
RE2^xviii—BA3—O5^xviii	34.5 (3)	BA3ⁱⁱⁱ—RE7—O4	54.7133 (1)
RE2^xviii—BA3—O5^xxvii	90.4 (2)	BA3ⁱⁱⁱ—RE7—O4ⁱⁱⁱ	54.7133 (1)
RE2^xxi—BA3—RE2^xxii	109.5606 (4)	BA3ⁱⁱⁱ—RE7—O4^viii	125.2867 (1)
RE2^xxi—BA3—BA3ⁱⁱ	54.7133 (1)	BA3ⁱⁱⁱ—RE7—O4^ix	125.2867 (1)
RE2^xxi—BA3—BA3ⁱⁱⁱ	125.2867 (1)	BA3ⁱⁱⁱ—RE7—O5	54.7803 (2)
RE2^xxi—BA3—BA3^xxiii	54.7133 (1)	BA3ⁱⁱⁱ—RE7—O5^iv	125.2197 (2)
RE2^xxi—BA3—BA3^xxiv	125.2867 (1)	BA3^iv—RE7—BA3^v	109.5606 (4)
RE2^xxi—BA3—BA3^v	54.7803 (2)	BA3^iv—RE7—BA3^vi	70.5734 (2)
RE2^xxi—BA3—BA3^xi	125.2197 (2)	BA3^iv—RE7—BA3^vii	70.5734 (2)
RE2^xxi—BA3—O4	90.73 (12)	BA3^iv—RE7—O4	125.2867 (1)
RE2^xxi—BA3—O4^xxiv	90.73 (12)	BA3^iv—RE7—O4ⁱⁱⁱ	54.7133 (1)
RE2^xxi—BA3—O4^xxv	34.2 (2)	BA3^iv—RE7—O4^viii	54.7133 (1)
RE2^xxi—BA3—O4^ix	34.2 (2)	BA3^iv—RE7—O4^ix	125.2867 (1)
RE2^xxi—BA3—O4^xix	90.57 (12)	BA3^iv—RE7—O5	125.2197 (2)
RE2^xxi—BA3—O4^xv	90.57 (12)	BA3^iv—RE7—O5^iv	54.7803 (2)
RE2^xxi—BA3—O4^xvi	143.6 (2)	BA3^v—RE7—BA3^vi	70.5734 (2)
RE2^xxi—BA3—O4^xxvi	143.6 (2)	BA3^v—RE7—BA3^vii	70.5734 (2)
RE2^xxi—BA3—O5	90.4 (2)	BA3^v—RE7—O4	54.7133 (1)
RE2^xxi—BA3—O5^xviii	90.4 (2)	BA3^v—RE7—O4ⁱⁱⁱ	125.2867 (1)
RE2^xxi—BA3—O5^xxvii	34.5 (3)	BA3^v—RE7—O4^viii	125.2867 (1)
RE2^xxii—BA3—BA3ⁱⁱ	125.2867 (1)	BA3^v—RE7—O4^ix	54.7133 (1)
RE2^xxii—BA3—BA3ⁱⁱⁱ	54.7133 (1)	BA3^v—RE7—O5	125.2197 (2)
RE2^xxii—BA3—BA3^xxiii	125.2867 (1)	BA3^v—RE7—O5^iv	54.7803 (2)
RE2^xxii—BA3—BA3^xxiv	54.7133 (1)	BA3^vi—RE7—BA3^vii	109.5606 (4)
RE2^xxii—BA3—BA3^v	54.7803 (2)	BA3^vi—RE7—O4	125.2867 (1)
RE2^xxii—BA3—BA3^xi	125.2197 (2)	BA3^vi—RE7—O4ⁱⁱⁱ	125.2867 (1)
RE2^xxii—BA3—O4	34.2 (2)	BA3^vi—RE7—O4^viii	54.7133 (1)
RE2^xxii—BA3—O4^xxiv	34.2 (2)	BA3^vi—RE7—O4^ix	54.7133 (1)
RE2^xxii—BA3—O4^xxv	90.73 (12)	BA3^vi—RE7—O5	125.2197 (2)
RE2^xxii—BA3—O4^ix	90.73 (12)	BA3^vi—RE7—O5^iv	54.7803 (2)
RE2^xxii—BA3—O4^xix	143.6 (2)	BA3^vii—RE7—O4	54.7133 (1)
RE2^xxii—BA3—O4^xv	143.6 (2)	BA3^vii—RE7—O4ⁱⁱⁱ	54.7133 (1)
RE2^xxii—BA3—O4^xvi	90.57 (12)	BA3^vii—RE7—O4^viii	125.2867 (1)
RE2^xxii—BA3—O4^xxvi	90.57 (12)	BA3^vii—RE7—O4^ix	125.2867 (1)
RE2^xxii—BA3—O5	90.4 (2)	BA3^vii—RE7—O5	125.2197 (2)
RE2^xxii—BA3—O5^xviii	90.4 (2)	BA3^vii—RE7—O5^iv	54.7803 (2)
RE2^xxii—BA3—O5^xxvii	144.0 (3)	O4—RE7—O4ⁱⁱⁱ	90.0
BA3ⁱⁱ—BA3—BA3ⁱⁱⁱ	90.0	O4—RE7—O4^viii	179.9802
BA3ⁱⁱ—BA3—BA3^xxiii	90.0	O4—RE7—O4^ix	90.0
BA3ⁱⁱ—BA3—BA3^xxiv	180.0	O4—RE7—O5	90.0
BA3ⁱⁱ—BA3—BA3^v	90.0	O4—RE7—O5^iv	90.0
BA3ⁱⁱ—BA3—BA3^xi	90.0	O4ⁱⁱⁱ—RE7—O4^viii	90.0
BA3ⁱⁱ—BA3—O4	91.1 (2)	O4ⁱⁱⁱ—RE7—O4^ix	179.972
BA3ⁱⁱ—BA3—O4^xxiv	135.036 (4)	O4ⁱⁱⁱ—RE7—O5	90.0
BA3ⁱⁱ—BA3—O4^xxv	88.9 (2)	O4ⁱⁱⁱ—RE7—O5^iv	90.0
BA3ⁱⁱ—BA3—O4^ix	44.964 (4)	O4^viii—RE7—O4^ix	90.0
BA3ⁱⁱ—BA3—O4^xix	91.1 (2)	O4^viii—RE7—O5	90.0
BA3ⁱⁱ—BA3—O4^xv	44.964 (4)	O4^viii—RE7—O5^iv	90.0
BA3ⁱⁱ—BA3—O4^xvi	88.9 (2)	O4^ix—RE7—O5	90.0
BA3ⁱⁱ—BA3—O4^xxvi	135.036 (4)	O4^ix—RE7—O5^iv	90.0
BA3ⁱⁱ—BA3—O5	45.005 (5)	O5—RE7—O5^iv	180.0

Symmetry codes: (i) x−1, y, z; (ii) −y, x−1, z; (iii) −y, x, z; (iv) −x, −y, −z; (v) −x+1, −y, −z; (vi) y, −x, −z; (vii) y, −x+1, −z; (viii) −x, −y, z; (ix) y, −x, z; (x) −x, −y, −z+1; (xi) −x+1, −y, −z+1; (xii) y, −x, −z+1; (xiii) y, −x+1, −z+1; (xiv) x−1/2, y−1/2, z+1/2; (xv) −y+1/2, x−1/2, z+1/2; (xvi) −x+1/2, −y+1/2, z+1/2; (xvii) y−1/2, −x+1/2, z+1/2; (xviii) x+1, y, z; (xix) x+1/2, y−1/2, z+1/2; (xx) x+1/2, y+1/2, z+1/2; (xxi) x+1/2, y−1/2, z−1/2; (xxii) x+1/2, y+1/2, z−1/2; (xxiii) −y+1, x−1, z; (xxiv) −y+1, x, z; (xxv) −x+1, −y, z; (xxvi) y+1/2, −x+1/2, z+1/2; (xxvii) −x−1/2, −y−3/2, −z−1/2; (xxviii) −x−1/2, −y−1/2, −z−1/2.

(T400KBST_phase_1) top

Crystal data top

Ba2FeReO₆	Z = 8
M_r = 306.36	? radiation, λ = 1.377287 Å
Cubic, Fm3m	T = 400 K
Hall symbol: F m 3 m	Particle morphology: powder
a = 8.063327 (13) Å	flat_sheet, 20 × 10 mm
V = 524.26 (1) Å³

Data collection top

Huber 4+2 circle diffractometer	Data collection mode: reflection
Radiation source: synchrotron, LNLS D10B-XPD beamline	Scan method: step
Si 111 monochromator	2θ_min = 15.003°, 2θ_max = 150.193°, 2θ_step = 0.01°
Specimen mounting: copper sample holder

Refinement top

Least-squares matrix: full	13520 data points
R_p = 0.149	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) = 1.637 #2(GV) = 2.828 #3(GW) = 0.012 #4(LX) = 0.000 #5(LY) = 8.663 #6(trns) = 0.000 #7(asym) = 0.0000 #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 0.0010 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) = 0.000 #2(GV) = 0.000 #3(GW) = 0.000 #4(LX) = 0.000 #5(LY) = 12.919 #6(trns) = 0.000 #7(asym) = 0.0000 #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 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.221	25 parameters
R_exp = 0.170	0 restraints
R(F²) = 0.12564	(Δ/σ)_max = 0.02
χ² = 1.690	Background function: GSAS Background function number 2 with 10 terms. Cosine Fourier series 1: 5.36654 2: 1.01816 3: -5.78612 4: -0.425017 5: -3.39798 6: -0.251197 7: -1.97797 8: 0.272396 9: -0.804030 10: 0.197454

Crystal data top

Ba2FeReO₆	Z = 8
M_r = 306.36	? radiation, λ = 1.377287 Å
Cubic, Fm3m	T = 400 K
a = 8.063327 (13) Å	flat_sheet, 20 × 10 mm
V = 524.26 (1) Å³

Data collection top

Huber 4+2 circle diffractometer	Scan method: step
Specimen mounting: copper sample holder	2θ_min = 15.003°, 2θ_max = 150.193°, 2θ_step = 0.01°
Data collection mode: reflection

Refinement top

R_p = 0.149	χ² = 1.690
R_wp = 0.221	13520 data points
R_exp = 0.170	25 parameters
R(F²) = 0.12564	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ba	0.25	0.25	0.25	0.0073 (2)*
Fe	0.0	0.0	0.0	0.0101 (2)*	0.9646
Re	0.5	0.0	0.0	0.0101 (2)*	0.9646
RE5	0.0	0.0	0.0	0.0100 (2)*	0.0354
FE6	0.5	0.0	0.0	0.0100 (2)*	0.0354
O7	0.2608 (9)	0.0	0.0	0.0091 (12)*

Geometric parameters (Å, º) top

Ba—Fe	3.4915	Re—O7	1.929 (8)
Ba—Feⁱ	3.4915	Re—O7^xxvii	1.929 (8)
Ba—Feⁱⁱ	3.4915	Re—O7^xxviii	1.929 (8)
Ba—Feⁱⁱⁱ	3.4915	Re—O7^ix	1.929 (8)
Ba—Re	3.4915	Re—O7^xxix	1.929 (8)
Ba—Re^iv	3.4915	Re—O7^xiii	1.929 (8)
Ba—Re^v	3.4915	RE5—Ba	3.4915
Ba—Reⁱ	3.4915	RE5—Ba^xiv	3.4915
Ba—RE5	3.4915	RE5—Ba^xv	3.4915
Ba—RE5ⁱ	3.4915	RE5—Ba^xvi	3.4915
Ba—RE5ⁱⁱ	3.4915	RE5—Ba^xvii	3.4915
Ba—RE5ⁱⁱⁱ	3.4915	RE5—Ba^xviii	3.4915
Ba—FE6	3.4915	RE5—Ba^xix	3.4915
Ba—FE6^iv	3.4915	RE5—Ba^xx	3.4915
Ba—FE6^v	3.4915	RE5—O7	2.103 (8)
Ba—FE6ⁱ	3.4915	RE5—O7^iv	2.103 (8)
Ba—O7	2.8521 (2)	RE5—O7^v	2.103 (8)
Ba—O7^iv	2.8521 (2)	RE5—O7^xix	2.103 (8)
Ba—O7^v	2.8521 (2)	RE5—O7^xxi	2.103 (8)
Ba—O7ⁱ	2.8521 (2)	RE5—O7^xxii	2.103 (8)
Ba—O7^vi	2.8521 (2)	FE6—Ba	3.4915
Ba—O7^vii	2.8521 (2)	FE6—Ba^xiv	3.4915
Ba—O7^viii	2.8521 (2)	FE6—Ba^xxiii	3.4915
Ba—O7^ix	2.8521 (2)	FE6—Ba^xvi	3.4915
Ba—O7^x	2.8521 (2)	FE6—Ba^xxiv	3.4915
Ba—O7^xi	2.8521 (2)	FE6—Ba^xxv	3.4915
Ba—O7^xii	2.8521 (2)	FE6—Ba^xix	3.4915
Ba—O7^xiii	2.8521 (2)	FE6—Ba^xxvi	3.4915
Fe—Ba	3.4915	FE6—O7	1.929 (8)
Fe—Ba^xiv	3.4915	FE6—O7^xxvii	1.929 (8)
Fe—Ba^xv	3.4915	FE6—O7^xxviii	1.929 (8)
Fe—Ba^xvi	3.4915	FE6—O7^ix	1.929 (8)
Fe—Ba^xvii	3.4915	FE6—O7^xxix	1.929 (8)
Fe—Ba^xviii	3.4915	FE6—O7^xiii	1.929 (8)
Fe—Ba^xix	3.4915	O7—Ba	2.8521 (2)
Fe—Ba^xx	3.4915	O7—Ba^xiv	2.8521 (2)
Fe—O7	2.103 (8)	O7—Ba^xvi	2.8521 (2)
Fe—O7^iv	2.103 (8)	O7—Ba^xix	2.8521 (2)
Fe—O7^v	2.103 (8)	O7—Fe	2.103 (8)
Fe—O7^xix	2.103 (8)	O7—Re	1.929 (8)
Fe—O7^xxi	2.103 (8)	O7—RE5	2.103 (8)
Fe—O7^xxii	2.103 (8)	O7—FE6	1.929 (8)
Re—Ba	3.4915	O7—O7^iv	2.974 (11)
Re—Ba^xiv	3.4915	O7—O7^v	2.974 (11)
Re—Ba^xxiii	3.4915	O7—O7^xix	2.974 (11)
Re—Ba^xvi	3.4915	O7—O7^xxii	2.974 (11)
Re—Ba^xxiv	3.4915	O7—O7^xxviii	2.728 (11)
Re—Ba^xxv	3.4915	O7—O7^ix	2.728 (11)
Re—Ba^xix	3.4915	O7—O7^xxix	2.728 (11)
Re—Ba^xxvi	3.4915	O7—O7^xiii	2.728 (11)

O7—Fe—O7^iv	90.0	O7—RE5—O7^xxi	180.0
O7—Fe—O7^v	90.0	O7—RE5—O7^xxii	90.0
O7—Fe—O7^xix	90.0	O7^iv—RE5—O7^v	90.0
O7—Fe—O7^xxi	180.0	O7^iv—RE5—O7^xix	90.0
O7—Fe—O7^xxii	90.0	O7^iv—RE5—O7^xxi	90.0
O7^iv—Fe—O7^v	90.0	O7^iv—RE5—O7^xxii	180.0
O7^iv—Fe—O7^xix	90.0	O7^v—RE5—O7^xix	180.0
O7^iv—Fe—O7^xxi	90.0	O7^v—RE5—O7^xxi	90.0
O7^iv—Fe—O7^xxii	180.0	O7^v—RE5—O7^xxii	90.0
O7^v—Fe—O7^xix	180.0	O7^xix—RE5—O7^xxi	90.0
O7^v—Fe—O7^xxi	90.0	O7^xix—RE5—O7^xxii	90.0
O7^v—Fe—O7^xxii	90.0	O7^xxi—RE5—O7^xxii	90.0
O7^xix—Fe—O7^xxi	90.0	O7—FE6—O7^xxvii	179.9604
O7^xix—Fe—O7^xxii	90.0	O7—FE6—O7^xxviii	90.0
O7^xxi—Fe—O7^xxii	90.0	O7—FE6—O7^ix	90.0
O7—Re—O7^xxvii	179.9604	O7—FE6—O7^xxix	90.0
O7—Re—O7^xxviii	90.0	O7—FE6—O7^xiii	90.0
O7—Re—O7^ix	90.0	O7^xxvii—FE6—O7^xxviii	90.0
O7—Re—O7^xxix	90.0	O7^xxvii—FE6—O7^ix	90.0
O7—Re—O7^xiii	90.0	O7^xxvii—FE6—O7^xxix	90.0
O7^xxvii—Re—O7^xxviii	90.0	O7^xxvii—FE6—O7^xiii	90.0
O7^xxvii—Re—O7^ix	90.0	O7^xxviii—FE6—O7^ix	180.0
O7^xxvii—Re—O7^xxix	90.0	O7^xxviii—FE6—O7^xxix	90.0
O7^xxvii—Re—O7^xiii	90.0	O7^xxviii—FE6—O7^xiii	90.0
O7^xxviii—Re—O7^ix	180.0	O7^ix—FE6—O7^xxix	90.0
O7^xxviii—Re—O7^xxix	90.0	O7^ix—FE6—O7^xiii	90.0
O7^xxviii—Re—O7^xiii	90.0	O7^xxix—FE6—O7^xiii	180.0
O7^ix—Re—O7^xxix	90.0	Fe—O7—Re	180.0
O7^ix—Re—O7^xiii	90.0	Fe—O7—RE5	0.0
O7^xxix—Re—O7^xiii	180.0	Fe—O7—FE6	180.0
O7—RE5—O7^iv	90.0	Re—O7—RE5	180.0
O7—RE5—O7^v	90.0	Re—O7—FE6	0.0
O7—RE5—O7^xix	90.0	RE5—O7—FE6	180.0

Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x+1/2, y, z+1/2; (iii) x+1/2, y+1/2, z; (iv) z, x, y; (v) y, z, x; (vi) y, −z+1/2, −x+1/2; (vii) −z, −x+1/2, y+1/2; (viii) z+1/2, x, y+1/2; (ix) y+1/2, −z, −x+1/2; (x) −x+1/2, y, −z+1/2; (xi) y+1/2, z+1/2, x; (xii) −x+1/2, y+1/2, −z; (xiii) −z+1/2, −x+1/2, y; (xiv) x, y, −z; (xv) −z, x, y; (xvi) y, −z, x; (xvii) −z, x, −y; (xviii) −y, −z, x; (xix) y, −z, −x; (xx) −x, −y, −z; (xxi) −x, y, −z; (xxii) −z, −x, y; (xxiii) −z+1, x, y; (xxiv) −z+1, x, −y; (xxv) −y+1, −z, x; (xxvi) −x+1, −y, −z; (xxvii) −x+1, y, −z; (xxviii) y+1/2, z, x−1/2; (xxix) z+1/2, x−1/2, y.

(T400KBST_phase_2) iron oxide top

Crystal data top

Fe₃O₄	Z = 8
M_r = 231.54	? radiation, λ = 1.377287 Å
Cubic, Fd3m	T = 400 K
Hall symbol: F d -3 m	Particle morphology: powder
a = 8.3985 (5) Å	flat_sheet, 20 × 10 mm
V = 592.38 (10) Å³

Data collection top

Huber 4+2 circle diffractometer	Data collection mode: reflection
Radiation source: synchrotron, LNLS D10B-XPD beamline	Scan method: step
Si 111 monochromator	2θ_min = 15.003°, 2θ_max = 150.193°, 2θ_step = 0.01°
Specimen mounting: copper sample holder

Refinement top

Least-squares matrix: full	13520 data points
R_p = 0.149	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) = 1.637 #2(GV) = 2.828 #3(GW) = 0.012 #4(LX) = 0.000 #5(LY) = 8.663 #6(trns) = 0.000 #7(asym) = 0.0000 #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 0.0010 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) = 0.000 #2(GV) = 0.000 #3(GW) = 0.000 #4(LX) = 0.000 #5(LY) = 12.919 #6(trns) = 0.000 #7(asym) = 0.0000 #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 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0
R_wp = 0.221	25 parameters
R_exp = 0.170	0 restraints
R(F²) = 0.12564	(Δ/σ)_max = 0.02
χ² = 1.690	Background function: GSAS Background function number 2 with 10 terms. Cosine Fourier series 1: 5.36654 2: 1.01816 3: -5.78612 4: -0.425017 5: -3.39798 6: -0.251197 7: -1.97797 8: 0.272396 9: -0.804030 10: 0.197454

Crystal data top

Fe₃O₄	Z = 8
M_r = 231.54	? radiation, λ = 1.377287 Å
Cubic, Fd3m	T = 400 K
a = 8.3985 (5) Å	flat_sheet, 20 × 10 mm
V = 592.38 (10) Å³

Data collection top

Huber 4+2 circle diffractometer	Scan method: step
Specimen mounting: copper sample holder	2θ_min = 15.003°, 2θ_max = 150.193°, 2θ_step = 0.01°
Data collection mode: reflection

Refinement top

R_p = 0.149	χ² = 1.690
R_wp = 0.221	13520 data points
R_exp = 0.170	25 parameters
R(F²) = 0.12564	0 restraints

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe1	0.125	0.125	0.125	−0.016 (4)*
Fe2	0.5	0.5	0.5	−0.016 (4)*
O	0.246 (10)	0.246 (10)	0.246 (10)	−0.016 (4)*

Geometric parameters (Å, º) top

Fe1—O	1.76 (15)	Fe2—O^vii	2.14 (9)
Fe1—Oⁱ	1.76 (15)	Fe2—O^viii	2.14 (9)
Fe1—Oⁱⁱ	1.76 (15)	Fe2—O^ix	2.14 (9)
Fe1—Oⁱⁱⁱ	1.76 (15)	O—Fe1	1.76 (15)
Fe2—O^iv	2.14 (9)	O—Fe2^vii	2.14 (9)
Fe2—O^v	2.14 (9)	O—Fe2^viii	2.14 (9)
Fe2—O^vi	2.14 (9)	O—Fe2^ix	2.14 (9)

O—Fe1—O^x	109.471 (2)	O^v—Fe2—O^ix	88 (4)
O—Fe1—O^xi	109.471 (4)	O^vi—Fe2—O^xiii	88 (4)
O—Fe1—O^xii	109.471 (2)	O^vi—Fe2—O^xiv	88 (4)
O^x—Fe1—O^xi	109.471 (2)	O^vi—Fe2—O^ix	179.9557
O^x—Fe1—O^xii	109.471 (4)	O^xiii—Fe2—O^xiv	92 (4)
O^xi—Fe1—O^xii	109.471 (2)	O^xiii—Fe2—O^ix	92 (4)
O^iv—Fe2—O^v	92 (4)	O^xiv—Fe2—O^ix	92 (4)
O^iv—Fe2—O^vi	92 (4)	Fe1—O—Fe2^xv	127 (3)
O^iv—Fe2—O^xiii	179.9557	Fe1—O—Fe2^viii	127 (3)
O^iv—Fe2—O^xiv	88 (4)	Fe1—O—Fe2^xvi	127 (3)
O^iv—Fe2—O^ix	88 (4)	Fe2^xv—O—Fe2^viii	88 (5)
O^v—Fe2—O^vi	92 (4)	Fe2^xv—O—Fe2^xvi	88 (5)
O^v—Fe2—O^xiii	88 (4)	Fe2^viii—O—Fe2^xvi	88 (5)
O^v—Fe2—O^xiv	179.9557

Experimental details

	(T14KBST_phase_2)	(T14KBST_phase_3)	(T400KBST_phase_1)	(T400KBST_phase_2)
Crystal data
Chemical formula	Fe₃O₄	Ba₂FeReO₆	Ba2FeReO₆	Fe₃O₄
M_r	231.54	306.36	306.36	231.54
Crystal system, space group	Cubic, Fd3m	Tetragonal, I4/mmm	Cubic, Fm3m	Cubic, Fd3m
Temperature (K)	14	14	400	400
a, b, c (Å)	8.3814 (5), 8.3814, 8.3814	5.68278 (2), 5.682775, 8.02337 (5)	8.063327 (13), 8.063327, 8.063327	8.3985 (5), 8.3985, 8.3985
α, β, γ (°)	90, 90, 90	90, 90, 90	90, 90, 90	90, 90, 90
V (Å³)	588.78 (10)	259.11 (1)	524.26 (1)	592.38 (10)
Z	8	4	8	8
Radiation type	Synchrotron, λ = 1.377285 Å	Synchrotron, λ = 1.377285 Å	?, λ = 1.377287 Å	?, λ = 1.377287 Å
Specimen shape, size (mm)	Flat_sheet, 20 × 10	Flat_sheet, 20 × 10	Flat_sheet, 20 × 10	Flat_sheet, 20 × 10

Data collection
Diffractometer	Huber 4+2 circle diffractometer	Huber 4+2 circle diffractometer	Huber 4+2 circle diffractometer	Huber 4+2 circle diffractometer
Specimen mounting	Copper sample holder	Copper sample holder	Copper sample holder	Copper sample holder
Data collection mode	Reflection	Reflection	Reflection	Reflection
Scan method	Step	Step	Step	Step
2θ values (°)	2θ_min = 15.003 2θ_max = 150.193 2θ_step = 0.01	2θ_min = 15.003 2θ_max = 150.193 2θ_step = 0.01	2θ_min = 15.003 2θ_max = 150.193 2θ_step = 0.01	2θ_min = 15.003 2θ_max = 150.193 2θ_step = 0.01

Refinement
R factors and goodness of fit	R_p = 0.168, R_wp = 0.267, R_exp = 0.195, R(F²) = 0.18130, χ² = 1.904	R_p = 0.168, R_wp = 0.267, R_exp = 0.195, R(F²) = 0.18130, χ² = 1.904	R_p = 0.149, R_wp = 0.221, R_exp = 0.170, R(F²) = 0.12564, χ² = 1.690	R_p = 0.149, R_wp = 0.221, R_exp = 0.170, R(F²) = 0.12564, χ² = 1.690
No. of data points	13520	13520	13520	13520
No. of parameters	24	24	25	25

Computer programs: SPEC (Certified Scientific Software, 1992), POWF 2.11 (Virginia Tech, 2001-2003), GSAS (Larson & Von Dreele, 2001), GSAS.

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