Compound characterization data — Perween et al., 2026

Ba₂In₀.₅Sb₀.₅O₄ and Ba₂In₀.₅Sb₀.₅O₄ + xPVDF fluorination series
Krypton physisorption, BET surface area, 77 K	Ba₂In₀.₅Sb₀.₅O₄: 1.2 m² g⁻¹; x = 2.0: 0.9 m² g⁻¹; x = 1.5: 0.9 m² g⁻¹; x = 1.1: 0.5 m² g⁻¹; x = 1.05: 1.0 m² g⁻¹; x = 1.0: 0.9 m² g⁻¹; x = 0.75: 0.6 m² g⁻¹; x = 0.5: 0.8 m² g⁻¹; x = 0.25: 0.9 m² g⁻¹
RT-PXRD Rietveld refinement, Ba₂In₀.₅Sb₀.₅O₄	Ba₂In₀.₅Sb₀.₅O₄ 100.000 wt.%, I4/mmm (139), a = 4.16513(4) Å, c = 13.29977(17) Å, V = 230.729(5) Å³
RT-PXRD Rietveld refinement, xPVDF = 0.25	RP #1 53.3(2) wt.%, a = 4.16518(6) Å, c = 13.3174(5) Å, V = 231.040(11) Å³; RP #2 6.38(12) wt.%, a = 4.1602(3) Å, c = 13.6573(16) Å, V = 236.37(4) Å³; RP #3 21.57(18) wt.%, a = 4.15238(12) Å, c = 14.483(4) Å, V = 249.72(7) Å³; RP #4 1.97(9) wt.%, a = 3.9174(6) Å, c = 15.258(5) Å, V = 234.16(11) Å³; BaF₂ 0.68(7) wt.%, Fm3̅m (225), a = 6.1973(5) Å, V = 238.02(6) Å³; BaCO₃ 6.3(2) wt.%, Pmcn (62), a = 5.2964(13) Å, b = 8.914(2) Å, c = 6.4568(17) Å, V = 304.88(14) Å³; BaIn₀.₅Sb₀.₅O₃ 9.83(17) wt.%, Pm3̅m (221), a = 4.1470(4) Å, V = 71.319(18) Å³
RT-PXRD Rietveld refinement, xPVDF = 0.50	RP #1 46.6(3) wt.%, a = 4.1500(2) Å, c = 13.280(11) Å, V = 228.71(19) Å³; RP #2 4.00(10) wt.%, a = 4.1500(11) Å, c = 13.758(5) Å, V = 236.94(16) Å³; RP #3 36.9(3) wt.%, a = 4.14877(15) Å, c = 14.6627(8) Å, V = 252.38(2) Å³; RP #4 2.06(10) wt.%, a = 3.9062(11) Å, c = 15.817(11) Å, V = 241.3(2) Å³; BaF₂ 1.97(9) wt.%, Fm3̅m (225), a = 6.1992(4) Å, V = 238.24(5) Å³; BaCO₃ 6.26(19) wt.%, Pmcn (62), a = 5.3072(11) Å, b = 8.901(2) Å, c = 6.4541(14) Å, V = 304.92(11) Å³; BaIn₀.₅Sb₀.₅O₃ 2.2(2) wt.%, Pm3̅m (221), a = 4.1465(5) Å, V = 71.29(3) Å³
RT-PXRD Rietveld refinement, xPVDF = 0.75	RP #1 37.9(3) wt.%, a = 4.15000(19) Å, c = 13.308(19) Å, V = 229.2(3) Å³; RP #2 2.51(9) wt.%, a = 4.1415(15) Å, c = 13.824(8) Å, V = 237.1(2) Å³; RP #3 26.9(2) wt.%, a = 4.1415(2) Å, c = 14.7863(11) Å, V = 253.61(3) Å³; RP #4 8.82(14) wt.%, a = 4.1090(4) Å, c = 16.208(3) Å, V = 273.65(8) Å³; RP #5 4.71(15) wt.%, a = 4.0938(9) Å, c = 16.575(7) Å, V = 277.79(17) Å³; RP #6 4.23(13) wt.%, a = 4.0905(10) Å, c = 17.001(8) Å, V = 284.46(19) Å³; RP #7 3.25(11) wt.%, a = 4.0673(9) Å, c = 17.573(9) Å, V = 290.7(2) Å³; BaF₂ 3.43(8) wt.%, Fm3̅m (225), a = 6.2063(2) Å, V = 239.05(3) Å³; BaCO₃ 6.62(15) wt.%, Pmcn (62), a = 5.3020(9) Å, b = 8.9130(17) Å, c = 6.4654(12) Å, V = 305.53(10) Å³; BaIn₀.₅Sb₀.₅O₃ 1.58(15) wt.%, Pm3̅m (221), a = 4.1198(5) Å, V = 69.92(3) Å³
RT-PXRD Rietveld refinement, xPVDF = 1.0	RP #1 3.53(11) wt.%, a = 4.150(2) Å, c = 13.290(10) Å, V = 228.9(3) Å³; RP #2 5.59(12) wt.%, a = 4.1479(16) Å, c = 13.853(7) Å, V = 238.3(2) Å³; RP #3 9.54(16) wt.%, a = 4.1391(8) Å, c = 14.784(5) Å, V = 253.27(13) Å³; RP #4 25.3(6) wt.%, a = 4.1008(4) Å, c = 16.270(3) Å, V = 273.61(8) Å³; RP #5 23.7(6) wt.%, a = 4.0871(5) Å, c = 16.465(3) Å, V = 275.03(9) Å³; RP #6 10.4(5) wt.%, a = 4.0778(11) Å, c = 17.011(9) Å, V = 282.9(2) Å³; RP #7 7.1(4) wt.%, a = 4.0522(10) Å, c = 17.344(10) Å, V = 284.8(2) Å³; BaF₂ 3.90(9) wt.%, Fm3̅m (225), a = 6.2039(3) Å, V = 238.78(3) Å³; BaCO₃ 6.66(16) wt.%, Pmcn (62), a = 5.3046(9) Å, b = 8.9043(16) Å, c = 6.4578(12) Å, V = 305.02(10) Å³; BaIn₀.₅Sb₀.₅O₃ 4.23(14) wt.%, Pm3̅m (221), a = 4.1332(3) Å, V = 70.606(14) Å³
RT-PXRD Rietveld refinement, xPVDF = 1.05	RP #1 2.46(10) wt.%, a = 4.150(2) Å, c = 13.282(11) Å, V = 228.8(3) Å³; RP #2 4.63(10) wt.%, a = 4.1406(16) Å, c = 13.871(7) Å, V = 237.8(2) Å³; RP #3 7.34(12) wt.%, a = 4.1367(9) Å, c = 14.756(5) Å, V = 252.51(14) Å³; RP #4 20.0(4) wt.%, a = 4.0999(4) Å, c = 16.243(3) Å, V = 273.03(8) Å³; RP #5 20.9(4) wt.%, a = 4.0798(4) Å, c = 16.464(3) Å, V = 274.04(7) Å³; RP #6 13.3(4) wt.%, a = 4.0637(6) Å, c = 17.056(6) Å, V = 281.67(13) Å³; RP #7 12.5(3) wt.%, a = 4.0320(6) Å, c = 17.411(5) Å, V = 283.05(11) Å³; BaF₂ 4.47(8) wt.%, Fm3̅m (225), a = 6.20184(18) Å, V = 238.54(2) Å³; BaCO₃ 8.03(15) wt.%, Pmcn (62), a = 5.2998(7) Å, b = 8.9101(13) Å, c = 6.4531(9) Å, V = 304.73(7) Å³; BaIn₀.₅Sb₀.₅O₃ 6.4(2) wt.%, Pm3̅m (221), a = 4.1211(5) Å, V = 69.99(3) Å³
RT-PXRD Rietveld refinement, xPVDF = 1.10	RP #1 3.21(12) wt.%, a = 4.150(2) Å, c = 13.294(11) Å, V = 229.0(3) Å³; RP #2 4.76(12) wt.%, a = 4.1432(18) Å, c = 13.839(8) Å, V = 237.6(3) Å³; RP #3 6.68(13) wt.%, a = 4.1365(11) Å, c = 14.738(6) Å, V = 252.17(17) Å³; RP #4 16.4(4) wt.%, a = 4.1016(5) Å, c = 16.233(4) Å, V = 273.10(10) Å³; RP #5 24.8(4) wt.%, a = 4.0795(4) Å, c = 16.463(3) Å, V = 273.99(7) Å³; RP #6 12.8(4) wt.%, a = 4.0585(6) Å, c = 17.083(7) Å, V = 281.39(15) Å³; RP #7 13.3(3) wt.%, a = 4.0279(7) Å, c = 17.449(5) Å, V = 283.09(12) Å³; BaF₂ 4.29(10) wt.%, Fm3̅m (225), a = 6.2020(2) Å, V = 238.56(3) Å³; BaCO₃ 6.95(16) wt.%, Pmcn (62), a = 5.3032(9) Å, b = 8.9082(16) Å, c = 6.4506(11) Å, V = 304.74(9) Å³; BaIn₀.₅Sb₀.₅O₃ 6.8(3) wt.%, Pm3̅m (221), a = 4.1302(5) Å, V = 70.46(3) Å³
RT-PXRD Rietveld refinement, xPVDF = 1.20	RP #1 3.4(2) wt.%, a = 4.150(4) Å, c = 13.30(2) Å, V = 229.1(6) Å³; RP #2 4.3(2) wt.%, a = 4.135(4) Å, c = 13.91(2) Å, V = 237.9(6) Å³; RP #3 4.2(2) wt.%, a = 4.118(4) Å, c = 15.04(2) Å, V = 254.9(6) Å³; RP #4 19.5(7) wt.%, a = 4.0971(11) Å, c = 16.231(8) Å, V = 272.5(2) Å³; RP #5 24.3(8) wt.%, a = 4.0683(9) Å, c = 16.533(7) Å, V = 273.64(17) Å³; RP #6 18.1(8) wt.%, a = 4.0337(12) Å, c = 17.233(15) Å, V = 280.4(3) Å³; RP #7 20.8(8) wt.%, a = 4.0125(10) Å, c = 17.558(9) Å, V = 282.69(19) Å³; BaF₂ 5.4(2) wt.%, Fm3̅m (225), a = 6.1989(8) Å, V = 238.20(9) Å³
RT-PXRD Rietveld refinement, xPVDF = 1.50	RP #1 2.36(10) wt.%, a = 4.137(2) Å, c = 13.310(11) Å, V = 227.8(3) Å³; RP #2 2.65(10) wt.%, a = 4.128(2) Å, c = 13.893(10) Å, V = 236.7(3) Å³; RP #3 3.76(10) wt.%, a = 4.1120(12) Å, c = 15.483(8) Å, V = 261.8(2) Å³; RP #4 13.8(3) wt.%, a = 4.0691(4) Å, c = 16.423(3) Å, V = 271.93(8) Å³; RP #5 14.6(3) wt.%, a = 4.0469(4) Å, c = 16.628(3) Å, V = 272.32(8) Å³; RP #6 26.7(3) wt.%, a = 4.0107(3) Å, c = 17.417(3) Å, V = 280.18(6) Å³; RP #7 27.1(3) wt.%, a = 4.0009(3) Å, c = 17.6634(18) Å, V = 282.75(5) Å³; BaF₂ 8.98(12) wt.%, Fm3̅m (225), a = 6.20100(13) Å, V = 238.443(15) Å³
RT-PXRD Rietveld refinement, xPVDF = 2.0	Tetragonal RP phase 87.59(11) wt.%, I4/mmm (139), a = 4.08633(9) Å, c = 16.8480(7) Å, V = 281.330(16) Å³; BaF₂ 12.41(11) wt.%, Fm3̅m (225), a = 6.20020(15) Å, V = 238.351(17) Å³
RT-PXRD Rietveld refinement reliability, Rp; Rwp; Rexp; χ²	Ba₂In₀.₅Sb₀.₅O₄: 4.28 %; 6.12 %; 2.04 %; 3.00; xPVDF = 0.25: 3.23 %; 4.38 %; 3.95 %; 1.11; 0.50: 4.36 %; 6.34 %; 3.78 %; 1.68; 0.75: 3.61 %; 5.16 %; 3.48 %; 1.48; 1.0: 2.89 %; 3.89 %; 3.50 %; 1.11; 1.05: 2.74 %; 3.67 %; 3.49 %; 1.05; 1.10: 2.55 %; 3.45 %; 3.57 %; 0.96; 1.20: 2.55 %; 3.32 %; 3.80 %; 0.87; 1.50: 2.47 %; 3.41 %; 3.61 %; 0.94; 2.0: 3.89 %; 5.24 %; 3.78 %; 1.39
Mole-fraction-weighted PXRD lattice evolution, parent oxide to xPVDF = 2.0	a: 4.165 to 4.086 Å, ~1.90 % contraction; c: 13.30 to 16.848 Å, ~26.68 % increase; unit-cell volume: 230.729 to 281.309 Å³, ~21.92 % expansion
In situ PXRD and mass spectrometry, Ba₂In₀.₅Sb₀.₅O₄ + PVDF under flowing air	The RP (103) reflection shifted toward lower Q values upon heating to 370 °C; transient tetragonal RP phases appeared and disappeared successively. H₂O was observed at m/z 18 and CO₂ at m/z 44; CO₂ release began around ~250 °C and coincided with the appearance of fluorinated tetragonal RP phases
Coupled PXRD–PND Rietveld refinement, Ba₂In₀.₅Sb₀.₅O₂F₄	Tetragonal I4/mmm (139), a = 4.08776(7) Å, c = 16.8327(6) Å, V = 281.270(14) Å³; Rexp = 2.43 %, Rwp = 2.45 %, Rp = 1.73 %, GOF = 1.01
Coupled PXRD–PND refined crystallographic parameters, Ba₂In₀.₅Sb₀.₅O₂F₄	Ba1: 4e, x = 0, y = 0, z = 0.34707(7), occupancy 1, Bₑq = 0.93(6) Å²; In1: 2a, x = 0, y = 0, z = 0, occupancy 0.5, Bₑq = 1.76(7) Å²; Sb1: 2a, x = 0, y = 0, z = 0, occupancy 0.5, Bₑq = 1.76(7) Å²; O1: 4c, x = 0, y = 1/2, z = 0, occupancy 1.000(9), Bₑq = 2.32(5) Å²; F1: 4e, x = 0, y = 0, z = 0.1153(2), occupancy 1.000(6), Bₑq = 2.32(5) Å²; F2: 4d, x = 1/2, y = 0, z = 1/4, occupancy 1.000(8), Bₑq = 2.32(5) Å²
PXRD refined crystallographic parameters, Ba₂In₀.₅Sb₀.₅O₄	Tetragonal I4/mmm (139), a = 4.16510(4) Å, c = 13.2998(2) Å, V = 230.725(6) Å³; Ba1: 4e, x = 0, y = 0, z = 0.35421(4), occupancy 1, Bₑq = 0.30(2) Å²; In1: 2a, x = 0, y = 0, z = 0, occupancy 0.5, Bₑq = 0.30(2) Å²; Sb1: 2a, x = 0, y = 0, z = 0, occupancy 0.5, Bₑq = 0.30(2) Å²; O1: 4c, x = 0, y = 1/2, z = 0, occupancy 1, Bₑq = 0.30(2) Å²; O2: 4e, x = 0, y = 0, z = 0.1602(4), occupancy 1, Bₑq = 0.30(2) Å²; Rexp = 2.04 %, Rwp = 6.12 %, Rp = 4.28 %, GOF = 3.00
PXRD and coupled PXRD–PND refined interatomic distances, parent oxide; oxyfluoride	Ba–apical anion: 2.5809 Å (1×) and 2.9514 Å (4×); 2.960(1) Å (4×). Ba–interstitial F: —; 2.615(1) Å (4×). Ba–equatorial O: 2.8454 Å (4×); —. In/Sb–equatorial O: 2.0826 Å (4×); 2.0445(1) Å (4×). In/Sb–apical O/F: 2.1302 Å (2×); 1.937(4) Å (2×)
Bond-valence-sum and global-instability-index analysis, Ba₂In₀.₅Sb₀.₅O₂F₄	C1, equatorial O, apical F, interstitial F: GII 0.3902; C2, equatorial F, apical O, interstitial F: 0.4188; C3, equatorial F, apical F, interstitial O: 0.4690
Bond-valence parameters, R₀; b	Ba–O: 2.285 Å; 0.37 Å. Ba–F: 2.188 Å; 0.37 Å. In–O: 1.902 Å; 0.37 Å. In–F: 1.792 Å; 0.37 Å. Sb–O: 1.912 Å; 0.37 Å. Sb–F: 1.797 Å; 0.37 Å
Bond-valence sums, C1, formal valence; calculated BVS; deviation; weighted deviation	Ba: +2; 2.0271; 0.0271; 0.0015. In: +3; 4.0715; 1.0715; 0.5741. Sb: +5; 4.1645; −0.8355; 0.3491. Equatorial O: −2; 1.6485; −0.3515; 0.2470. Apical F: −1; 1.1761; 0.1761; 0.0620. Interstitial F: −1; 1.2614; 0.2614; 0.1367
Bond-valence sums, C2, formal valence; calculated BVS; deviation; weighted deviation	Ba: +2; 2.1138; 0.1138; 0.0259. In: +3; 3.8391; 0.8391; 0.3520. Sb: +5; 3.9164; −1.0836; 0.5871. Equatorial F: −1; 1.2248; 0.2248; 0.1010. Apical O: −2; 1.5665; −0.4335; 0.3758. Interstitial F: −1; 1.2614; 0.2614; 0.1367
Bond-valence sums, C3, formal valence; calculated BVS; deviation; weighted deviation	Ba: +2; 2.3431; 0.3431; 0.2355. In: +3; 3.3716; 0.3716; 0.0691. Sb: +5; 3.4175; −1.5825; 1.2521. Equatorial F: −1; 1.2248; 0.2248; 0.1010. Apical F: −1; 1.1761; 0.1761; 0.0620. Interstitial O: −2; 1.6395; −0.3605; 0.2599
XPS, parent oxide and fully fluorinated oxyfluoride	In 3d and Ba 3d remained at essentially constant binding energy, with no observable chemical shift or additional spectral components. Sb 3d3/2 showed no distinct additional low-binding-energy feature attributable to a substantial Sb³⁺ contribution. The oxyfluoride F 1s spectrum consisted of a single unresolved peak centered at approximately 685–686 eV; a BaF₂ contribution could not be excluded
In K-edge XANES	Ba₂In₀.₅Sb₀.₅O₄: 27944.0 eV; Ba₂In₀.₅Sb₀.₅O₃F₂: 27943.2 eV; a shift of 2.6 eV was observed between Ba₂In₀.₅Sb₀.₅O₃F₂ and Ba₂In₀.₅Sb₀.₅O₂F₄
Sb K-edge XANES	Ba₂In₀.₅Sb₀.₅O₃F₂: 30496.8 eV; Ba₂In₀.₅Sb₀.₅O₂F₄: 30496.0 eV; no variation in oxidation state was detected
UV–Vis diffuse-reflectance spectroscopy	Fluorinated materials showed broader absorption at lower photon energies while the principal absorption maximum remained at approximately 4.82 eV (257 nm); no clear dependence on fluorination degree was evident
Photoluminescence, 260 nm excitation	xPVDF = 0.75, 1.1, and 2.0 showed increased intensity between 330 and 390 nm; the other fluorinated samples showed a shoulder in this range; no clear dependence on fluorination degree was observed
Photoluminescence excitation, emission at 425–435 nm	Comparable excitation features occurred at approximately 350–380 nm for all samples
Photoluminescence, approximately 370–380 nm excitation	All materials showed local emission maxima around 430 and 470 nm; xPVDF = 1.5 and 2.0 had more intense emission at 430 nm than at 470 nm, while the other samples had higher emission at 470 nm; x = 0.25 showed a similar intensity ratio to x = 1.5 and 2.0