An accurate X-ray diffraction study of (Y0.95Bi0.05)Fe3(BO3)4 single crystals in the temperature range 90–500 K was performed on a laboratory diffractometer and used synchrotron radiation. It was established that the crystal undergoes a diffuse structural phase transition in the temperature range 350–380 K. The complexity of localization of such a transition over temperature was overcome by means of special analysis of systematic extinction reflections by symmetry. The transition temperature can be considered to be Tstr ≃ 370 K. The crystal has a trigonal structure in the space group P3121 at temperatures of 90–370 K, and it has a trigonal structure in the space group R32 at 375–500 K. There is one type of chain formed by the FeO6 octahedra along the c axis in the R32 phase. When going into the P3121 phase, two types of nonequivalent chains arise, in which Fe atoms are separated from the Y atoms by a different distance. Upon lowering the temperature from 500 to 90 K, a distortion of the Y(Bi)O6, FeO6, B(2,3)O3 coordination polyhedra is observed. The distances between atoms in helical Fe chains and Fe—O—Fe angles change non-uniformly. A sharp jump in the equivalent isotropic displacement parameters of O1 and O2 atoms within the Fe—Fe chains and fluctuations of the equivalent isotropic displacement parameters of B2 and B3 atoms were observed in the region of structural transition as well as noticeable elongation of O1, O2, B2, B3, Fe1, Fe2 atomic displacement ellipsoids. It was established that the helices of electron density formed by Fe, O1 and O2 atoms may be structural elements determining chirality, optical activity and multiferroicity of rare-earth iron borates. Compression and stretching of these helices account for the symmetry change and for the manifestation of a number of properties, whose geometry is controlled by an indirect exchange interaction between iron cations that compete with the thermal motion of atoms in the structure. Structural analysis detected these changes as variations of a number of structural characteristics in the c unit-cell direction, that is, the direction of the helices. Structural results for the local surrounding of the atoms in (Y0.95Bi0.05)Fe3(BO3)4 were confirmed by EXAFS and Mössbauer spectroscopies.
Supporting information
| Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520618002962/xk5046sup1.cif Contains datablocks global, I, II, III, IV, V, VI, VII, VIII, IX, X, XI, XII, XIII, XIV |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046Isup2.hkl Contains datablock I |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046IIsup3.hkl Contains datablock II |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046IIIsup4.hkl Contains datablock III |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046IVsup5.hkl Contains datablock IV |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046Vsup6.hkl Contains datablock V |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046VIsup7.hkl Contains datablock VI |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046VIIsup8.hkl Contains datablock VII |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046VIIIsup9.hkl Contains datablock VIII |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046IXsup10.hkl Contains datablock IX |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046Xsup11.hkl Contains datablock X |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046XIsup12.hkl Contains datablock XI |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046XIIsup13.hkl Contains datablock XII |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046XIIIsup14.hkl Contains datablock XIII |
| Structure factor file (CIF format) https://doi.org/10.1107/S2052520618002962/xk5046XIVsup15.hkl Contains datablock XIV |
| Portable Document Format (PDF) file https://doi.org/10.1107/S2052520618002962/xk5046sup16.pdf Supplementary material |
CCDC references: 1824825; 1824826; 1824827; 1824828; 1824829; 1824830; 1824831; 1824832; 1824833; 1824834; 1824835; 1824836; 1824837; 1824838
Crystal data top
B4Bi0.056Fe3O12Y0.944 | Dx = 4.197 Mg m−3 |
Mr = 498.4 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3121 | Cell parameters from 22254 reflections |
Hall symbol: P 31 2" | θ = 5.6–73.8° |
a = 9.5161 (1) Å | µ = 13.61 mm−1 |
c = 7.5441 (1) Å | T = 90 K |
V = 591.64 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 8103 independent reflections |
Radiation source: X-ray tube | 5808 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.2°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −22→24 |
Tmin = 0.190, Tmax = 0.280 | l = −19→20 |
60809 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.018 | (Δ/σ)max = 0.044 |
wR(F2) = 0.014 | Δρmax = 0.82 e Å−3 |
S = 0.98 | Δρmin = −1.51 e Å−3 |
8103 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
97 parameters | Extinction coefficient: 380 (20) |
0 restraints | Absolute structure: 3680 of Friedel pairs used in the refinement |
5 constraints | Absolute structure parameter: 0.5101 (10) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | −0.334977 (14) | −0.334977 (14) | 0 | 0.00312 (2) | 0.9440 (6) |
Bi1 | −0.334977 (14) | −0.334977 (14) | 0 | 0.00312 (2) | 0.0560 (6) |
Fe1 | 0.115612 (17) | 0.115612 (17) | 0 | 0.00247 (3) | |
Fe2 | −0.212182 (14) | −0.548629 (14) | 0.345015 (9) | 0.00255 (2) | |
O1 | 0 | −0.07764 (8) | 0.166667 | 0.00509 (16) | |
O2 | −0.58124 (7) | −0.27714 (7) | 0.12609 (6) | 0.00510 (12) | |
O3 | −0.12126 (8) | −0.30394 (8) | −0.17733 (8) | 0.00469 (15) | |
O4 | −0.14768 (8) | −0.36289 (8) | 0.18531 (8) | 0.00460 (15) | |
O5 | 0.47521 (8) | 0.14564 (8) | −0.15710 (8) | 0.00417 (14) | |
O6 | 0.18725 (10) | 0 | −0.166667 | 0.00439 (19) | |
O7 | −0.52470 (8) | −0.53358 (8) | −0.18552 (7) | 0.00476 (14) | |
B1 | 0.3317 (2) | 0 | −0.166667 | 0.0034 (2) | |
B2 | −0.44831 (11) | −0.12451 (11) | 0.15124 (10) | 0.0042 (2) | |
B3 | 0 | −0.22186 (15) | 0.166667 | 0.0040 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00311 (2) | 0.00311 (2) | 0.00318 (2) | 0.00159 (3) | −0.000100 (12) | 0.000100 (12) |
Bi1 | 0.00311 (2) | 0.00311 (2) | 0.00318 (2) | 0.00159 (3) | −0.000100 (12) | 0.000100 (12) |
Fe1 | 0.00237 (3) | 0.00237 (3) | 0.00275 (3) | 0.00124 (4) | −0.000033 (18) | 0.000033 (18) |
Fe2 | 0.00239 (3) | 0.00236 (3) | 0.00296 (2) | 0.00123 (3) | 0.00008 (2) | 0.00007 (2) |
O1 | 0.0061 (3) | 0.00325 (16) | 0.0069 (2) | 0.00303 (13) | 0.00247 (17) | 0.00124 (9) |
O2 | 0.00338 (15) | 0.00421 (14) | 0.00636 (13) | 0.00088 (13) | −0.00092 (12) | 0.00112 (10) |
O3 | 0.0053 (2) | 0.00310 (18) | 0.00562 (16) | 0.00209 (15) | 0.00074 (13) | 0.00065 (12) |
O4 | 0.00429 (19) | 0.00366 (18) | 0.00497 (15) | 0.00133 (16) | −0.00011 (12) | 0.00047 (12) |
O5 | 0.00305 (17) | 0.00337 (17) | 0.00503 (18) | 0.00081 (13) | −0.00036 (12) | 0.00043 (12) |
O6 | 0.0036 (2) | 0.0047 (3) | 0.0052 (2) | 0.00236 (15) | −0.00055 (10) | −0.0011 (2) |
O7 | 0.00404 (17) | 0.00541 (18) | 0.00558 (15) | 0.00291 (15) | −0.00032 (12) | −0.00080 (12) |
B1 | 0.0032 (2) | 0.0025 (4) | 0.00443 (19) | 0.0013 (2) | 0.00004 (17) | 0.0001 (3) |
B2 | 0.0035 (3) | 0.0040 (3) | 0.0046 (3) | 0.0014 (2) | 0.00011 (17) | 0.00052 (16) |
B3 | 0.0040 (5) | 0.0034 (3) | 0.0049 (3) | 0.0020 (2) | 0.0002 (3) | 0.00010 (16) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Fe1—O3iv | 1.9648 (7) |
Y1—O3 | 2.3265 (7) | Fe1—O6 | 2.0015 (6) |
Y1—O3i | 2.3265 (7) | Fe1—O6iii | 2.0015 (6) |
Y1—O4 | 2.3823 (8) | Fe2—O2v | 2.0592 (5) |
Y1—O4i | 2.3823 (8) | Fe2—O2vi | 2.0381 (5) |
Y1—O7 | 2.3191 (5) | Fe2—O4 | 1.9666 (7) |
Y1—O7i | 2.3191 (5) | Fe2—O5vii | 2.0248 (10) |
Bi1—O3 | 2.3265 (7) | Fe2—O5viii | 2.0143 (10) |
Bi1—O3i | 2.3265 (7) | Fe2—O7ix | 1.9836 (9) |
Bi1—O4 | 2.3823 (8) | O1—B3 | 1.3724 (16) |
Bi1—O4i | 2.3823 (8) | O2—B2 | 1.3814 (9) |
Bi1—O7 | 2.3191 (5) | O3—B2i | 1.3728 (15) |
Bi1—O7i | 2.3191 (5) | O4—B3 | 1.3820 (8) |
Fe1—O1 | 2.0371 (5) | O5—B1 | 1.3778 (11) |
Fe1—O1ii | 2.0371 (5) | O6—B1 | 1.375 (2) |
Fe1—O3iii | 1.9648 (7) | O7—B2x | 1.3639 (18) |
| | | |
Bi1—Y1—O3 | 0 | O6—Fe1—O6iii | 168.00 (2) |
Bi1—Y1—O3i | 0 | O2v—Fe2—O2vi | 86.35 (3) |
Bi1—Y1—O4 | 0 | O2v—Fe2—O4 | 168.13 (4) |
Bi1—Y1—O4i | 0 | O2v—Fe2—O5vii | 96.78 (3) |
Bi1—Y1—O7 | 0 | O2v—Fe2—O5viii | 75.63 (3) |
Bi1—Y1—O7i | 0 | O2v—Fe2—O7ix | 81.91 (3) |
O3—Y1—O3i | 119.93 (2) | O2vi—Fe2—O4 | 93.78 (3) |
O3—Y1—O4 | 72.32 (2) | O2vi—Fe2—O5vii | 75.87 (3) |
O3—Y1—O4i | 89.14 (3) | O2vi—Fe2—O5viii | 92.37 (3) |
O3—Y1—O7 | 91.80 (2) | O2vi—Fe2—O7ix | 160.34 (4) |
O3—Y1—O7i | 140.02 (3) | O4—Fe2—O5vii | 94.75 (3) |
O3i—Y1—O4 | 89.14 (3) | O4—Fe2—O5viii | 92.51 (3) |
O3i—Y1—O4i | 72.32 (2) | O4—Fe2—O7ix | 100.94 (3) |
O3i—Y1—O7 | 140.02 (3) | O5vii—Fe2—O5viii | 166.54 (2) |
O3i—Y1—O7i | 91.80 (2) | O5vii—Fe2—O7ix | 89.87 (3) |
O4—Y1—O4i | 142.88 (2) | O5viii—Fe2—O7ix | 99.87 (3) |
O4—Y1—O7 | 125.75 (3) | Fe1—O1—Fe1iii | 101.50 (4) |
O4—Y1—O7i | 85.58 (2) | Fe1—O1—B3 | 129.249 (18) |
O4i—Y1—O7 | 85.58 (2) | Fe1iii—O1—B3 | 129.249 (18) |
O4i—Y1—O7i | 125.75 (3) | Fe2xi—O2—Fe2xii | 102.50 (2) |
O7—Y1—O7i | 74.361 (19) | Fe2xi—O2—B2 | 121.86 (5) |
Y1—Bi1—O3 | 0 | Fe2xii—O2—B2 | 127.63 (7) |
Y1—Bi1—O3i | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O4 | 0 | Y1—O3—Fe1ii | 122.53 (4) |
Y1—Bi1—O4i | 0 | Y1—O3—B2i | 102.10 (5) |
Y1—Bi1—O7 | 0 | Bi1—O3—Fe1ii | 122.53 (4) |
Y1—Bi1—O7i | 0 | Bi1—O3—B2i | 102.10 (5) |
O3—Bi1—O3i | 119.93 (2) | Fe1ii—O3—B2i | 135.06 (6) |
O3—Bi1—O4 | 72.32 (2) | Y1—O4—Bi1 | 0.0 (5) |
O3—Bi1—O4i | 89.14 (3) | Y1—O4—Fe2 | 123.03 (3) |
O3—Bi1—O7 | 91.80 (2) | Y1—O4—B3 | 106.63 (5) |
O3—Bi1—O7i | 140.02 (3) | Bi1—O4—Fe2 | 123.03 (3) |
O3i—Bi1—O4 | 89.14 (3) | Bi1—O4—B3 | 106.63 (5) |
O3i—Bi1—O4i | 72.32 (2) | Fe2—O4—B3 | 130.10 (6) |
O3i—Bi1—O7 | 140.02 (3) | Fe2xiii—O5—Fe2xiv | 104.59 (2) |
O3i—Bi1—O7i | 91.80 (2) | Fe2xiii—O5—B1 | 126.66 (6) |
O4—Bi1—O4i | 142.88 (2) | Fe2xiv—O5—B1 | 128.66 (6) |
O4—Bi1—O7 | 125.75 (3) | Fe1—O6—Fe1ii | 104.03 (4) |
O4—Bi1—O7i | 85.58 (2) | Fe1—O6—B1 | 127.98 (2) |
O4i—Bi1—O7 | 85.58 (2) | Fe1ii—O6—B1 | 127.98 (2) |
O4i—Bi1—O7i | 125.75 (3) | Y1—O7—Bi1 | 0.0 (5) |
O7—Bi1—O7i | 74.361 (19) | Y1—O7—Fe2xv | 116.58 (4) |
O1—Fe1—O1ii | 87.661 (5) | Y1—O7—B2x | 115.76 (6) |
O1—Fe1—O3iii | 85.22 (2) | Bi1—O7—Fe2xv | 116.58 (4) |
O1—Fe1—O3iv | 167.32 (4) | Bi1—O7—B2x | 115.76 (6) |
O1—Fe1—O6 | 94.024 (19) | Fe2xv—O7—B2x | 127.60 (5) |
O1—Fe1—O6iii | 77.23 (3) | O5—B1—O5iv | 121.55 (15) |
O1ii—Fe1—O3iii | 167.32 (4) | O5—B1—O6 | 119.22 (8) |
O1ii—Fe1—O3iv | 85.22 (2) | O5iv—B1—O6 | 119.22 (8) |
O1ii—Fe1—O6 | 77.23 (3) | O2—B2—O3i | 115.04 (10) |
O1ii—Fe1—O6iii | 94.024 (19) | O2—B2—O7xvi | 120.04 (9) |
O3iii—Fe1—O3iv | 103.59 (4) | O3i—B2—O7xvi | 124.92 (7) |
O3iii—Fe1—O6 | 92.80 (4) | O1—B3—O4 | 117.56 (6) |
O3iii—Fe1—O6iii | 94.62 (3) | O1—B3—O4xvii | 117.56 (6) |
O3iv—Fe1—O6 | 94.62 (3) | O4—B3—O4xvii | 124.87 (12) |
O3iv—Fe1—O6iii | 92.80 (4) | | |
Symmetry codes: (i) y, x, −z; (ii) −x+y, −x, z−1/3; (iii) −y, x−y, z+1/3; (iv) x−y, −y, −z−1/3; (v) x−y, −y−1, −z+2/3; (vi) −x−1, −x+y−1, −z+1/3; (vii) −y, x−y−1, z+1/3; (viii) −x+y, −x, z+2/3; (ix) −x+y, −x−1, z+2/3; (x) −x+y−1, −x−1, z−1/3; (xi) x−y−1, −y−1, −z+2/3; (xii) −x−1, −x+y, −z+1/3; (xiii) −y, x−y, z−2/3; (xiv) −x+y+1, −x, z−1/3; (xv) −y−1, x−y−1, z−2/3; (xvi) −y−1, x−y, z+1/3; (xvii) −x, −x+y, −z+1/3. |
Crystal data top
B4Bi0.053Fe3O12Y0.947 | Dx = 4.187 Mg m−3 |
Mr = 498 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3121 | Cell parameters from 12858 reflections |
Hall symbol: P 31 2" | θ = 5.6–73.5° |
a = 9.5191 (1) Å | µ = 13.54 mm−1 |
c = 7.5517 (1) Å | T = 295 K |
V = 592.61 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 8029 independent reflections |
Radiation source: X-ray tube | 3847 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.053 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.3°, θmin = 4.3° |
ω scans | h = −22→23 |
Absorption correction: for a sphere Jana2006 | k = −24→22 |
Tmin = 0.191, Tmax = 0.281 | l = −20→19 |
56649 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.020 | (Δ/σ)max = 0.041 |
wR(F2) = 0.014 | Δρmax = 0.48 e Å−3 |
S = 0.67 | Δρmin = −1.10 e Å−3 |
8029 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
97 parameters | Extinction coefficient: 389 (15) |
0 restraints | Absolute structure: 3613 of Friedel pairs used in the refinement |
5 constraints | Absolute structure parameter: 0.5060 (12) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | −0.33419 (2) | −0.33419 (2) | 0 | 0.00719 (4) | 0.9465 (6) |
Bi1 | −0.33419 (2) | −0.33419 (2) | 0 | 0.00719 (4) | 0.0535 (6) |
Fe1 | 0.11583 (3) | 0.11583 (3) | 0 | 0.00491 (5) | |
Fe2 | −0.21289 (2) | −0.54889 (2) | 0.342977 (13) | 0.00496 (3) | |
O1 | 0 | −0.07736 (12) | 0.166667 | 0.0093 (3) | |
O2 | −0.58264 (10) | −0.27350 (9) | 0.13282 (9) | 0.00976 (19) | |
O3 | −0.12094 (11) | −0.30444 (11) | −0.17811 (10) | 0.0079 (2) | |
O4 | −0.14739 (11) | −0.36208 (11) | 0.18440 (11) | 0.0078 (2) | |
O5 | 0.47568 (10) | 0.14531 (11) | −0.15878 (12) | 0.0067 (2) | |
O6 | 0.18772 (14) | 0 | −0.166667 | 0.0073 (3) | |
O7 | −0.52356 (11) | −0.53560 (12) | −0.18471 (10) | 0.0084 (2) | |
B1 | 0.3321 (3) | 0 | −0.166667 | 0.0050 (3) | |
B2 | −0.44816 (16) | −0.12229 (15) | 0.15413 (14) | 0.0063 (3) | |
B3 | 0 | −0.2213 (2) | 0.166667 | 0.0065 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00742 (4) | 0.00742 (4) | 0.00689 (3) | 0.00382 (6) | −0.00023 (2) | 0.00023 (2) |
Bi1 | 0.00742 (4) | 0.00742 (4) | 0.00689 (3) | 0.00382 (6) | −0.00023 (2) | 0.00023 (2) |
Fe1 | 0.00469 (5) | 0.00469 (5) | 0.00542 (4) | 0.00240 (7) | −0.00003 (3) | 0.00003 (3) |
Fe2 | 0.00459 (4) | 0.00463 (4) | 0.00572 (3) | 0.00234 (4) | 0.00008 (3) | 0.00018 (3) |
O1 | 0.0108 (5) | 0.0057 (3) | 0.0131 (4) | 0.0054 (2) | 0.0057 (3) | 0.00283 (15) |
O2 | 0.0065 (2) | 0.0059 (2) | 0.0135 (2) | 0.0006 (2) | −0.0031 (2) | 0.00268 (17) |
O3 | 0.0096 (3) | 0.0054 (3) | 0.0086 (2) | 0.0037 (2) | 0.0018 (2) | 0.00179 (19) |
O4 | 0.0069 (3) | 0.0061 (3) | 0.0089 (2) | 0.0020 (2) | −0.0003 (2) | 0.0012 (2) |
O5 | 0.0047 (3) | 0.0055 (3) | 0.0082 (3) | 0.0012 (2) | −0.00057 (19) | 0.00100 (19) |
O6 | 0.0053 (3) | 0.0087 (5) | 0.0090 (4) | 0.0044 (3) | −0.00150 (17) | −0.0030 (3) |
O7 | 0.0070 (3) | 0.0104 (3) | 0.0094 (2) | 0.0055 (3) | −0.00068 (19) | −0.00189 (19) |
B1 | 0.0043 (3) | 0.0051 (6) | 0.0061 (2) | 0.0025 (3) | 0.0001 (3) | 0.0002 (5) |
B2 | 0.0055 (4) | 0.0056 (4) | 0.0063 (4) | 0.0016 (3) | 0.0001 (2) | 0.0008 (2) |
B3 | 0.0061 (7) | 0.0054 (4) | 0.0081 (5) | 0.0031 (4) | −0.0001 (5) | 0.0000 (2) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Fe1—O3iv | 1.9636 (9) |
Y1—O3 | 2.3314 (10) | Fe1—O6 | 2.0057 (8) |
Y1—O3i | 2.3314 (10) | Fe1—O6iii | 2.0057 (8) |
Y1—O4 | 2.3756 (11) | Fe2—O2v | 2.0559 (7) |
Y1—O4i | 2.3756 (11) | Fe2—O2vi | 2.0351 (7) |
Y1—O7 | 2.3269 (8) | Fe2—O4 | 1.9688 (9) |
Y1—O7i | 2.3269 (8) | Fe2—O5vii | 2.0228 (13) |
Bi1—O3 | 2.3314 (10) | Fe2—O5viii | 2.0165 (13) |
Bi1—O3i | 2.3314 (10) | Fe2—O7ix | 1.9784 (13) |
Bi1—O4 | 2.3756 (11) | O1—B3 | 1.370 (2) |
Bi1—O4i | 2.3756 (11) | O2—B2 | 1.3762 (12) |
Bi1—O7 | 2.3269 (8) | O3—B2i | 1.374 (2) |
Bi1—O7i | 2.3269 (8) | O4—B3 | 1.3793 (12) |
Fe1—O1 | 2.0381 (7) | O5—B1 | 1.3762 (15) |
Fe1—O1ii | 2.0381 (7) | O6—B1 | 1.375 (3) |
Fe1—O3iii | 1.9636 (9) | O7—B2x | 1.363 (2) |
| | | |
Bi1—Y1—O3 | 0 | O6—Fe1—O6iii | 168.03 (3) |
Bi1—Y1—O3i | 0 | O2v—Fe2—O2vi | 86.53 (4) |
Bi1—Y1—O4 | 0 | O2v—Fe2—O4 | 168.21 (5) |
Bi1—Y1—O4i | 0 | O2v—Fe2—O5vii | 96.38 (4) |
Bi1—Y1—O7 | 0 | O2v—Fe2—O5viii | 75.82 (4) |
Bi1—Y1—O7i | 0 | O2v—Fe2—O7ix | 82.55 (4) |
O3—Y1—O3i | 120.51 (3) | O2vi—Fe2—O4 | 92.52 (4) |
O3—Y1—O4 | 72.35 (3) | O2vi—Fe2—O5vii | 76.15 (4) |
O3—Y1—O4i | 89.27 (4) | O2vi—Fe2—O5viii | 92.55 (4) |
O3—Y1—O7 | 91.32 (3) | O2vi—Fe2—O7ix | 161.55 (5) |
O3—Y1—O7i | 140.36 (4) | O4—Fe2—O5vii | 94.80 (5) |
O3i—Y1—O4 | 89.27 (4) | O4—Fe2—O5viii | 92.49 (4) |
O3i—Y1—O4i | 72.35 (3) | O4—Fe2—O7ix | 101.15 (4) |
O3i—Y1—O7 | 140.36 (4) | O5vii—Fe2—O5viii | 166.78 (3) |
O3i—Y1—O7i | 91.32 (3) | O5vii—Fe2—O7ix | 90.30 (5) |
O4—Y1—O4i | 142.87 (3) | O5viii—Fe2—O7ix | 99.10 (5) |
O4—Y1—O7 | 125.04 (4) | Fe1—O1—Fe1iii | 101.63 (5) |
O4—Y1—O7i | 86.27 (3) | Fe1—O1—B3 | 129.18 (3) |
O4i—Y1—O7 | 86.27 (3) | Fe1iii—O1—B3 | 129.18 (3) |
O4i—Y1—O7i | 125.04 (4) | Fe2xi—O2—Fe2xii | 102.61 (3) |
O7—Y1—O7i | 73.88 (3) | Fe2xi—O2—B2 | 123.30 (7) |
Y1—Bi1—O3 | 0 | Fe2xii—O2—B2 | 128.40 (9) |
Y1—Bi1—O3i | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O4 | 0 | Y1—O3—Fe1ii | 122.16 (6) |
Y1—Bi1—O4i | 0 | Y1—O3—B2i | 103.24 (7) |
Y1—Bi1—O7 | 0 | Bi1—O3—Fe1ii | 122.16 (6) |
Y1—Bi1—O7i | 0 | Bi1—O3—B2i | 103.24 (7) |
O3—Bi1—O3i | 120.51 (3) | Fe1ii—O3—B2i | 134.31 (9) |
O3—Bi1—O4 | 72.35 (3) | Y1—O4—Bi1 | 0.0 (5) |
O3—Bi1—O4i | 89.27 (4) | Y1—O4—Fe2 | 122.74 (4) |
O3—Bi1—O7 | 91.32 (3) | Y1—O4—B3 | 106.80 (8) |
O3—Bi1—O7i | 140.36 (4) | Bi1—O4—Fe2 | 122.74 (4) |
O3i—Bi1—O4 | 89.27 (4) | Bi1—O4—B3 | 106.80 (8) |
O3i—Bi1—O4i | 72.35 (3) | Fe2—O4—B3 | 130.21 (8) |
O3i—Bi1—O7 | 140.36 (4) | Fe2xiii—O5—Fe2xiv | 104.45 (3) |
O3i—Bi1—O7i | 91.32 (3) | Fe2xiii—O5—B1 | 126.91 (8) |
O4—Bi1—O4i | 142.87 (3) | Fe2xiv—O5—B1 | 128.57 (9) |
O4—Bi1—O7 | 125.04 (4) | Fe1—O6—Fe1ii | 103.94 (6) |
O4—Bi1—O7i | 86.27 (3) | Fe1—O6—B1 | 128.03 (3) |
O4i—Bi1—O7 | 86.27 (3) | Fe1ii—O6—B1 | 128.03 (3) |
O4i—Bi1—O7i | 125.04 (4) | Y1—O7—Bi1 | 0.0 (5) |
O7—Bi1—O7i | 73.88 (3) | Y1—O7—Fe2xv | 117.47 (5) |
O1—Fe1—O1ii | 87.621 (7) | Y1—O7—B2x | 114.37 (8) |
O1—Fe1—O3iii | 85.46 (3) | Bi1—O7—Fe2xv | 117.47 (5) |
O1—Fe1—O3iv | 167.36 (5) | Bi1—O7—B2x | 114.37 (8) |
O1—Fe1—O6 | 94.06 (3) | Fe2xv—O7—B2x | 128.14 (7) |
O1—Fe1—O6iii | 77.21 (4) | O5—B1—O5iv | 121.3 (2) |
O1ii—Fe1—O3iii | 167.36 (5) | O5—B1—O6 | 119.36 (11) |
O1ii—Fe1—O3iv | 85.46 (3) | O5iv—B1—O6 | 119.36 (11) |
O1ii—Fe1—O6 | 77.21 (4) | O2—B2—O3i | 115.24 (13) |
O1ii—Fe1—O6iii | 94.06 (3) | O2—B2—O7xvi | 119.67 (13) |
O3iii—Fe1—O3iv | 103.19 (5) | O3i—B2—O7xvi | 125.08 (9) |
O3iii—Fe1—O6 | 92.73 (5) | O1—B3—O4 | 117.59 (9) |
O3iii—Fe1—O6iii | 94.70 (4) | O1—B3—O4xvii | 117.59 (9) |
O3iv—Fe1—O6 | 94.70 (4) | O4—B3—O4xvii | 124.82 (16) |
O3iv—Fe1—O6iii | 92.73 (5) | | |
Symmetry codes: (i) y, x, −z; (ii) −x+y, −x, z−1/3; (iii) −y, x−y, z+1/3; (iv) x−y, −y, −z−1/3; (v) x−y, −y−1, −z+2/3; (vi) −x−1, −x+y−1, −z+1/3; (vii) −y, x−y−1, z+1/3; (viii) −x+y, −x, z+2/3; (ix) −x+y, −x−1, z+2/3; (x) −x+y−1, −x−1, z−1/3; (xi) x−y−1, −y−1, −z+2/3; (xii) −x−1, −x+y, −z+1/3; (xiii) −y, x−y, z−2/3; (xiv) −x+y+1, −x, z−1/3; (xv) −y−1, x−y−1, z−2/3; (xvi) −y−1, x−y, z+1/3; (xvii) −x, −x+y, −z+1/3. |
Crystal data top
B4Bi0.054Fe3O12Y0.946 | Dx = 4.178 Mg m−3 |
Mr = 498.2 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3121 | Cell parameters from 11559 reflections |
Hall symbol: P 31 2" | θ = 5.6–73.4° |
a = 9.5261 (1) Å | µ = 13.52 mm−1 |
c = 7.5589 (1) Å | T = 350 K |
V = 594.05 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 8053 independent reflections |
Radiation source: X-ray tube | 3210 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.053 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.1°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −22→24 |
Tmin = 0.192, Tmax = 0.281 | l = −19→20 |
54572 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.020 | (Δ/σ)max = 0.040 |
wR(F2) = 0.016 | Δρmax = 0.44 e Å−3 |
S = 0.70 | Δρmin = −0.77 e Å−3 |
8053 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
97 parameters | Extinction coefficient: 366 (15) |
0 restraints | Absolute structure: 3632 of Friedel pairs used in the refinement |
5 constraints | Absolute structure parameter: 0.5096 (14) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | −0.33378 (3) | −0.33378 (3) | 0 | 0.00876 (5) | 0.9461 (6) |
Bi1 | −0.33378 (3) | −0.33378 (3) | 0 | 0.00876 (5) | 0.0539 (6) |
Fe1 | 0.11597 (3) | 0.11597 (3) | 0 | 0.00581 (6) | |
Fe2 | −0.21329 (3) | −0.54902 (3) | 0.341404 (17) | 0.00594 (5) | |
O1 | 0 | −0.07723 (17) | 0.166667 | 0.0126 (4) | |
O2 | −0.58390 (13) | −0.27090 (12) | 0.13856 (11) | 0.0124 (3) | |
O3 | −0.12077 (15) | −0.30496 (14) | −0.17855 (13) | 0.0093 (3) | |
O4 | −0.14735 (15) | −0.36137 (14) | 0.18353 (14) | 0.0094 (3) | |
O5 | 0.47619 (13) | 0.14517 (13) | −0.16043 (17) | 0.0080 (3) | |
O6 | 0.18827 (19) | 0 | −0.166667 | 0.0085 (4) | |
O7 | −0.52254 (15) | −0.53718 (15) | −0.18363 (13) | 0.0097 (3) | |
B1 | 0.3337 (4) | 0 | −0.166667 | 0.0056 (5) | |
B2 | −0.4476 (2) | −0.1209 (2) | 0.1564 (2) | 0.0068 (4) | |
B3 | 0 | −0.2203 (3) | 0.166667 | 0.0082 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00900 (5) | 0.00900 (5) | 0.00835 (4) | 0.00455 (8) | −0.00031 (3) | 0.00031 (3) |
Bi1 | 0.00900 (5) | 0.00900 (5) | 0.00835 (4) | 0.00455 (8) | −0.00031 (3) | 0.00031 (3) |
Fe1 | 0.00560 (7) | 0.00560 (7) | 0.00646 (5) | 0.00298 (10) | 0.00003 (4) | −0.00003 (4) |
Fe2 | 0.00551 (6) | 0.00532 (6) | 0.00690 (4) | 0.00264 (5) | −0.00001 (4) | 0.00024 (4) |
O1 | 0.0153 (7) | 0.0075 (4) | 0.0174 (5) | 0.0077 (4) | 0.0081 (5) | 0.0041 (2) |
O2 | 0.0068 (3) | 0.0072 (3) | 0.0182 (4) | −0.0003 (3) | −0.0047 (3) | 0.0051 (2) |
O3 | 0.0117 (5) | 0.0047 (3) | 0.0109 (3) | 0.0038 (3) | 0.0021 (3) | 0.0016 (3) |
O4 | 0.0089 (5) | 0.0085 (4) | 0.0098 (3) | 0.0037 (4) | 0.0001 (3) | 0.0017 (3) |
O5 | 0.0052 (4) | 0.0051 (4) | 0.0109 (3) | 0.0004 (2) | −0.0003 (3) | 0.0018 (3) |
O6 | 0.0081 (5) | 0.0086 (7) | 0.0090 (5) | 0.0043 (3) | −0.0016 (2) | −0.0032 (4) |
O7 | 0.0072 (4) | 0.0123 (4) | 0.0109 (3) | 0.0060 (3) | −0.0007 (3) | −0.0021 (3) |
B1 | 0.0050 (5) | 0.0041 (8) | 0.0075 (3) | 0.0020 (4) | 0.0004 (4) | 0.0008 (7) |
B2 | 0.0052 (5) | 0.0060 (5) | 0.0083 (5) | 0.0020 (4) | 0.0009 (3) | 0.0007 (3) |
B3 | 0.0097 (11) | 0.0079 (7) | 0.0076 (7) | 0.0048 (5) | −0.0003 (7) | −0.0002 (3) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Fe1—O3iv | 1.9653 (12) |
Y1—O3 | 2.3361 (14) | Fe1—O6 | 2.0107 (11) |
Y1—O3i | 2.3361 (14) | Fe1—O6iii | 2.0107 (11) |
Y1—O4 | 2.3695 (15) | Fe2—O2v | 2.0512 (9) |
Y1—O4i | 2.3695 (15) | Fe2—O2vi | 2.0370 (10) |
Y1—O7 | 2.3303 (10) | Fe2—O4 | 1.9726 (12) |
Y1—O7i | 2.3303 (10) | Fe2—O5vii | 2.0225 (17) |
Bi1—O3 | 2.3361 (14) | Fe2—O5viii | 2.0174 (17) |
Bi1—O3i | 2.3361 (14) | Fe2—O7ix | 1.9753 (17) |
Bi1—O4 | 2.3695 (15) | O1—B3 | 1.363 (3) |
Bi1—O4i | 2.3695 (15) | O2—B2 | 1.3751 (16) |
Bi1—O7 | 2.3303 (10) | O3—B2i | 1.368 (3) |
Bi1—O7i | 2.3303 (10) | O4—B3 | 1.3805 (16) |
Fe1—O1 | 2.0400 (10) | O5—B1 | 1.371 (2) |
Fe1—O1ii | 2.0400 (10) | O6—B1 | 1.385 (4) |
Fe1—O3iii | 1.9653 (12) | O7—B2x | 1.370 (3) |
| | | |
Bi1—Y1—O3 | 0 | O6—Fe1—O6iii | 168.12 (4) |
Bi1—Y1—O3i | 0 | O2v—Fe2—O2vi | 86.65 (5) |
Bi1—Y1—O4 | 0 | O2v—Fe2—O4 | 168.12 (7) |
Bi1—Y1—O4i | 0 | O2v—Fe2—O5vii | 96.08 (6) |
Bi1—Y1—O7 | 0 | O2v—Fe2—O5viii | 76.00 (6) |
Bi1—Y1—O7i | 0 | O2v—Fe2—O7ix | 83.04 (5) |
O3—Y1—O3i | 120.91 (4) | O2vi—Fe2—O4 | 91.44 (5) |
O3—Y1—O4 | 72.31 (4) | O2vi—Fe2—O5vii | 76.20 (5) |
O3—Y1—O4i | 89.37 (5) | O2vi—Fe2—O5viii | 92.69 (6) |
O3—Y1—O7 | 91.00 (4) | O2vi—Fe2—O7ix | 162.46 (7) |
O3—Y1—O7i | 140.63 (6) | O4—Fe2—O5vii | 94.84 (6) |
O3i—Y1—O4 | 89.37 (5) | O4—Fe2—O5viii | 92.40 (6) |
O3i—Y1—O4i | 72.31 (4) | O4—Fe2—O7ix | 101.48 (5) |
O3i—Y1—O7 | 140.63 (6) | O5vii—Fe2—O5viii | 166.87 (4) |
O3i—Y1—O7i | 91.00 (4) | O5vii—Fe2—O7ix | 90.78 (6) |
O4—Y1—O4i | 142.76 (4) | O5viii—Fe2—O7ix | 98.51 (6) |
O4—Y1—O7 | 124.48 (5) | Fe1—O1—Fe1iii | 101.69 (7) |
O4—Y1—O7i | 86.89 (4) | Fe1—O1—B3 | 129.15 (4) |
O4i—Y1—O7 | 86.89 (4) | Fe1iii—O1—B3 | 129.15 (4) |
O4i—Y1—O7i | 124.48 (5) | Fe2xi—O2—Fe2xii | 102.71 (4) |
O7—Y1—O7i | 73.44 (4) | Fe2xi—O2—B2 | 124.43 (9) |
Y1—Bi1—O3 | 0 | Fe2xii—O2—B2 | 128.91 (11) |
Y1—Bi1—O3i | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O4 | 0 | Y1—O3—Fe1ii | 121.86 (8) |
Y1—Bi1—O4i | 0 | Y1—O3—B2i | 104.07 (9) |
Y1—Bi1—O7 | 0 | Bi1—O3—Fe1ii | 121.86 (8) |
Y1—Bi1—O7i | 0 | Bi1—O3—B2i | 104.07 (9) |
O3—Bi1—O3i | 120.91 (4) | Fe1ii—O3—B2i | 133.78 (11) |
O3—Bi1—O4 | 72.31 (4) | Y1—O4—Bi1 | 0.0 (5) |
O3—Bi1—O4i | 89.37 (5) | Y1—O4—Fe2 | 122.54 (5) |
O3—Bi1—O7 | 91.00 (4) | Y1—O4—B3 | 106.96 (10) |
O3—Bi1—O7i | 140.63 (6) | Bi1—O4—Fe2 | 122.54 (5) |
O3i—Bi1—O4 | 89.37 (5) | Bi1—O4—B3 | 106.96 (10) |
O3i—Bi1—O4i | 72.31 (4) | Fe2—O4—B3 | 130.24 (11) |
O3i—Bi1—O7 | 140.63 (6) | Fe2xiii—O5—Fe2xiv | 104.44 (4) |
O3i—Bi1—O7i | 91.00 (4) | Fe2xiii—O5—B1 | 127.44 (11) |
O4—Bi1—O4i | 142.76 (4) | Fe2xiv—O5—B1 | 128.08 (12) |
O4—Bi1—O7 | 124.48 (5) | Fe1—O6—Fe1ii | 103.77 (8) |
O4—Bi1—O7i | 86.89 (4) | Fe1—O6—B1 | 128.12 (4) |
O4i—Bi1—O7 | 86.89 (4) | Fe1ii—O6—B1 | 128.12 (4) |
O4i—Bi1—O7i | 124.48 (5) | Y1—O7—Bi1 | 0.0 (5) |
O7—Bi1—O7i | 73.44 (4) | Y1—O7—Fe2xv | 118.24 (7) |
O1—Fe1—O1ii | 87.584 (9) | Y1—O7—B2x | 113.47 (11) |
O1—Fe1—O3iii | 85.64 (4) | Bi1—O7—Fe2xv | 118.24 (7) |
O1—Fe1—O3iv | 167.41 (7) | Bi1—O7—B2x | 113.47 (11) |
O1—Fe1—O6 | 94.07 (4) | Fe2xv—O7—B2x | 128.29 (9) |
O1—Fe1—O6iii | 77.27 (5) | O5—B1—O5iv | 121.9 (3) |
O1ii—Fe1—O3iii | 167.41 (7) | O5—B1—O6 | 119.06 (15) |
O1ii—Fe1—O3iv | 85.64 (4) | O5iv—B1—O6 | 119.06 (15) |
O1ii—Fe1—O6 | 77.27 (5) | O2—B2—O3i | 115.73 (17) |
O1ii—Fe1—O6iii | 94.07 (4) | O2—B2—O7xvi | 119.06 (17) |
O3iii—Fe1—O3iv | 102.88 (6) | O3i—B2—O7xvi | 125.22 (12) |
O3iii—Fe1—O6 | 92.63 (7) | O1—B3—O4 | 117.70 (12) |
O3iii—Fe1—O6iii | 94.77 (5) | O1—B3—O4xvii | 117.70 (12) |
O3iv—Fe1—O6 | 94.77 (5) | O4—B3—O4xvii | 124.6 (2) |
O3iv—Fe1—O6iii | 92.63 (7) | | |
Symmetry codes: (i) y, x, −z; (ii) −x+y, −x, z−1/3; (iii) −y, x−y, z+1/3; (iv) x−y, −y, −z−1/3; (v) x−y, −y−1, −z+2/3; (vi) −x−1, −x+y−1, −z+1/3; (vii) −y, x−y−1, z+1/3; (viii) −x+y, −x, z+2/3; (ix) −x+y, −x−1, z+2/3; (x) −x+y−1, −x−1, z−1/3; (xi) x−y−1, −y−1, −z+2/3; (xii) −x−1, −x+y, −z+1/3; (xiii) −y, x−y, z−2/3; (xiv) −x+y+1, −x, z−1/3; (xv) −y−1, x−y−1, z−2/3; (xvi) −y−1, x−y, z+1/3; (xvii) −x, −x+y, −z+1/3. |
Crystal data top
B4Bi0.05Fe3O12Y0.95 | Dx = 4.181 Mg m−3 |
Mr = 497.7 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3121 | Cell parameters from 11179 reflections |
Hall symbol: P 31 2" | θ = 5.6–73.5° |
a = 9.5194 (1) Å | µ = 13.49 mm−1 |
c = 7.5552 (1) Å | T = 360 K |
V = 592.92 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 8140 independent reflections |
Radiation source: X-ray tube | 3080 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.055 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.4°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −22→24 |
Tmin = 0.191, Tmax = 0.281 | l = −19→20 |
61236 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.018 | (Δ/σ)max = 0.043 |
wR(F2) = 0.015 | Δρmax = 0.34 e Å−3 |
S = 0.67 | Δρmin = −0.74 e Å−3 |
8140 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
97 parameters | Extinction coefficient: 435 (14) |
0 restraints | Absolute structure: 3695 of Friedel pairs used in the refinement |
5 constraints | Absolute structure parameter: 0.5073 (13) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | −0.33370 (3) | −0.33370 (3) | 0 | 0.00868 (5) | 0.9500 (6) |
Bi1 | −0.33370 (3) | −0.33370 (3) | 0 | 0.00868 (5) | 0.0500 (6) |
Fe1 | 0.11610 (3) | 0.11610 (3) | 0 | 0.00581 (7) | |
Fe2 | −0.21357 (3) | −0.54906 (3) | 0.340715 (18) | 0.00600 (5) | |
O1 | 0 | −0.07702 (17) | 0.166667 | 0.0128 (4) | |
O2 | −0.58498 (13) | −0.27020 (12) | 0.14086 (12) | 0.0130 (3) | |
O3 | −0.12100 (15) | −0.30520 (15) | −0.17866 (13) | 0.0096 (3) | |
O4 | −0.14739 (15) | −0.36118 (14) | 0.18327 (14) | 0.0089 (3) | |
O5 | 0.47613 (14) | 0.14497 (14) | −0.16114 (19) | 0.0085 (3) | |
O6 | 0.18823 (18) | 0 | −0.166667 | 0.0077 (4) | |
O7 | −0.52255 (15) | −0.53795 (16) | −0.18316 (13) | 0.0097 (3) | |
B1 | 0.3326 (4) | 0 | −0.166667 | 0.0060 (5) | |
B2 | −0.4476 (2) | −0.1204 (2) | 0.1574 (2) | 0.0078 (4) | |
B3 | 0 | −0.2202 (3) | 0.166667 | 0.0067 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00897 (5) | 0.00897 (5) | 0.00826 (4) | 0.00461 (9) | −0.00028 (3) | 0.00028 (3) |
Bi1 | 0.00897 (5) | 0.00897 (5) | 0.00826 (4) | 0.00461 (9) | −0.00028 (3) | 0.00028 (3) |
Fe1 | 0.00559 (7) | 0.00559 (7) | 0.00641 (5) | 0.00293 (10) | −0.00001 (4) | 0.00001 (4) |
Fe2 | 0.00559 (6) | 0.00532 (6) | 0.00703 (4) | 0.00268 (6) | 0.00006 (5) | 0.00022 (4) |
O1 | 0.0158 (7) | 0.0076 (4) | 0.0178 (5) | 0.0079 (4) | 0.0094 (5) | 0.0047 (2) |
O2 | 0.0073 (3) | 0.0077 (3) | 0.0186 (4) | −0.0002 (3) | −0.0047 (3) | 0.0052 (2) |
O3 | 0.0117 (5) | 0.0061 (4) | 0.0106 (3) | 0.0042 (4) | 0.0019 (3) | 0.0020 (3) |
O4 | 0.0079 (5) | 0.0070 (4) | 0.0097 (3) | 0.0021 (3) | −0.0007 (3) | 0.0013 (3) |
O5 | 0.0057 (4) | 0.0063 (4) | 0.0109 (3) | 0.0011 (3) | −0.0013 (3) | 0.0014 (3) |
O6 | 0.0059 (5) | 0.0085 (7) | 0.0095 (5) | 0.0042 (3) | −0.0011 (2) | −0.0023 (5) |
O7 | 0.0071 (4) | 0.0119 (4) | 0.0113 (3) | 0.0056 (3) | −0.0005 (3) | −0.0022 (3) |
B1 | 0.0048 (4) | 0.0074 (9) | 0.0068 (3) | 0.0037 (5) | 0.0000 (4) | 0.0000 (8) |
B2 | 0.0062 (5) | 0.0070 (5) | 0.0079 (5) | 0.0015 (4) | −0.0001 (3) | 0.0011 (3) |
B3 | 0.0045 (8) | 0.0061 (6) | 0.0088 (7) | 0.0023 (4) | −0.0001 (6) | −0.0001 (3) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Fe1—O3iv | 1.9645 (13) |
Y1—O3 | 2.3337 (14) | Fe1—O6 | 2.0093 (11) |
Y1—O3i | 2.3337 (14) | Fe1—O6iii | 2.0093 (11) |
Y1—O4 | 2.3654 (15) | Fe2—O2v | 2.0460 (9) |
Y1—O4i | 2.3654 (15) | Fe2—O2vi | 2.0314 (10) |
Y1—O7 | 2.3306 (10) | Fe2—O4 | 1.9708 (12) |
Y1—O7i | 2.3306 (10) | Fe2—O5vii | 2.0229 (18) |
Bi1—O3 | 2.3337 (14) | Fe2—O5viii | 2.0157 (18) |
Bi1—O3i | 2.3337 (14) | Fe2—O7ix | 1.9752 (18) |
Bi1—O4 | 2.3654 (15) | O1—B3 | 1.363 (3) |
Bi1—O4i | 2.3654 (15) | O2—B2 | 1.3760 (17) |
Bi1—O7 | 2.3306 (10) | O3—B2i | 1.368 (3) |
Bi1—O7i | 2.3306 (10) | O4—B3 | 1.3793 (16) |
Fe1—O1 | 2.0384 (11) | O5—B1 | 1.374 (2) |
Fe1—O1ii | 2.0384 (11) | O6—B1 | 1.374 (4) |
Fe1—O3iii | 1.9645 (13) | O7—B2x | 1.368 (3) |
| | | |
Bi1—Y1—O3 | 0 | O6—Fe1—O6iii | 168.04 (4) |
Bi1—Y1—O3i | 0 | O2v—Fe2—O2vi | 86.73 (5) |
Bi1—Y1—O4 | 0 | O2v—Fe2—O4 | 167.99 (7) |
Bi1—Y1—O4i | 0 | O2v—Fe2—O5vii | 96.04 (6) |
Bi1—Y1—O7 | 0 | O2v—Fe2—O5viii | 76.01 (6) |
Bi1—Y1—O7i | 0 | O2v—Fe2—O7ix | 83.33 (5) |
O3—Y1—O3i | 121.06 (4) | O2vi—Fe2—O4 | 91.01 (5) |
O3—Y1—O4 | 72.33 (4) | O2vi—Fe2—O5vii | 76.18 (6) |
O3—Y1—O4i | 89.37 (5) | O2vi—Fe2—O5viii | 92.91 (6) |
O3—Y1—O7 | 90.92 (4) | O2vi—Fe2—O7ix | 162.83 (7) |
O3—Y1—O7i | 140.70 (6) | O4—Fe2—O5vii | 94.87 (6) |
O3i—Y1—O4 | 89.37 (5) | O4—Fe2—O5viii | 92.34 (6) |
O3i—Y1—O4i | 72.33 (4) | O4—Fe2—O7ix | 101.52 (5) |
O3i—Y1—O7 | 140.70 (6) | O5vii—Fe2—O5viii | 167.00 (5) |
O3i—Y1—O7i | 90.92 (4) | O5vii—Fe2—O7ix | 90.95 (7) |
O4—Y1—O4i | 142.72 (4) | O5viii—Fe2—O7ix | 98.21 (7) |
O4—Y1—O7 | 124.30 (5) | Fe1—O1—Fe1iii | 101.78 (7) |
O4—Y1—O7i | 87.11 (5) | Fe1—O1—B3 | 129.11 (4) |
O4i—Y1—O7 | 87.11 (5) | Fe1iii—O1—B3 | 129.11 (4) |
O4i—Y1—O7i | 124.30 (5) | Fe2xi—O2—Fe2xii | 102.93 (4) |
O7—Y1—O7i | 73.20 (4) | Fe2xi—O2—B2 | 124.73 (10) |
Y1—Bi1—O3 | 0 | Fe2xii—O2—B2 | 129.01 (12) |
Y1—Bi1—O3i | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O4 | 0 | Y1—O3—Fe1ii | 121.85 (8) |
Y1—Bi1—O4i | 0 | Y1—O3—B2i | 104.47 (9) |
Y1—Bi1—O7 | 0 | Bi1—O3—Fe1ii | 121.85 (8) |
Y1—Bi1—O7i | 0 | Bi1—O3—B2i | 104.47 (9) |
O3—Bi1—O3i | 121.06 (4) | Fe1ii—O3—B2i | 133.40 (12) |
O3—Bi1—O4 | 72.33 (4) | Y1—O4—Bi1 | 0.0 (5) |
O3—Bi1—O4i | 89.37 (5) | Y1—O4—Fe2 | 122.45 (5) |
O3—Bi1—O7 | 90.92 (4) | Y1—O4—B3 | 107.06 (10) |
O3—Bi1—O7i | 140.70 (6) | Bi1—O4—Fe2 | 122.45 (5) |
O3i—Bi1—O4 | 89.37 (5) | Bi1—O4—B3 | 107.06 (10) |
O3i—Bi1—O4i | 72.33 (4) | Fe2—O4—B3 | 130.24 (11) |
O3i—Bi1—O7 | 140.70 (6) | Fe2xiii—O5—Fe2xiv | 104.33 (4) |
O3i—Bi1—O7i | 90.92 (4) | Fe2xiii—O5—B1 | 127.39 (12) |
O4—Bi1—O4i | 142.72 (4) | Fe2xiv—O5—B1 | 128.26 (12) |
O4—Bi1—O7 | 124.30 (5) | Fe1—O6—Fe1ii | 103.84 (8) |
O4—Bi1—O7i | 87.11 (5) | Fe1—O6—B1 | 128.08 (4) |
O4i—Bi1—O7 | 87.11 (5) | Fe1ii—O6—B1 | 128.08 (4) |
O4i—Bi1—O7i | 124.30 (5) | Y1—O7—Bi1 | 0.0 (5) |
O7—Bi1—O7i | 73.20 (4) | Y1—O7—Fe2xv | 118.40 (7) |
O1—Fe1—O1ii | 87.551 (10) | Y1—O7—B2x | 113.06 (11) |
O1—Fe1—O3iii | 85.66 (4) | Bi1—O7—Fe2xv | 118.40 (7) |
O1—Fe1—O3iv | 167.31 (7) | Bi1—O7—B2x | 113.06 (11) |
O1—Fe1—O6 | 94.09 (4) | Fe2xv—O7—B2x | 128.53 (10) |
O1—Fe1—O6iii | 77.19 (5) | O5—B1—O5iv | 121.0 (3) |
O1ii—Fe1—O3iii | 167.31 (7) | O5—B1—O6 | 119.48 (15) |
O1ii—Fe1—O3iv | 85.66 (4) | O5iv—B1—O6 | 119.48 (15) |
O1ii—Fe1—O6 | 77.19 (5) | O2—B2—O3i | 115.89 (18) |
O1ii—Fe1—O6iii | 94.09 (4) | O2—B2—O7xvi | 118.91 (18) |
O3iii—Fe1—O3iv | 102.91 (6) | O3i—B2—O7xvi | 125.19 (13) |
O3iii—Fe1—O6 | 92.61 (7) | O1—B3—O4 | 117.67 (12) |
O3iii—Fe1—O6iii | 94.83 (5) | O1—B3—O4xvii | 117.67 (12) |
O3iv—Fe1—O6 | 94.83 (5) | O4—B3—O4xvii | 124.7 (2) |
O3iv—Fe1—O6iii | 92.61 (7) | | |
Symmetry codes: (i) y, x, −z; (ii) −x+y, −x, z−1/3; (iii) −y, x−y, z+1/3; (iv) x−y, −y, −z−1/3; (v) x−y, −y−1, −z+2/3; (vi) −x−1, −x+y−1, −z+1/3; (vii) −y, x−y−1, z+1/3; (viii) −x+y, −x, z+2/3; (ix) −x+y, −x−1, z+2/3; (x) −x+y−1, −x−1, z−1/3; (xi) x−y−1, −y−1, −z+2/3; (xii) −x−1, −x+y, −z+1/3; (xiii) −y, x−y, z−2/3; (xiv) −x+y+1, −x, z−1/3; (xv) −y−1, x−y−1, z−2/3; (xvi) −y−1, x−y, z+1/3; (xvii) −x, −x+y, −z+1/3. |
Crystal data top
B4Bi0.05Fe3O12Y0.95 | Dx = 4.172 Mg m−3 |
Mr = 497.7 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3121 | Cell parameters from 11133 reflections |
Hall symbol: P 31 2" | θ = 5.6–73.1° |
a = 9.5259 (1) Å | µ = 13.46 mm−1 |
c = 7.5624 (1) Å | T = 365 K |
V = 594.30 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 8038 independent reflections |
Radiation source: X-ray tube | 2927 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.048 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.2°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −22→24 |
Tmin = 0.192, Tmax = 0.281 | l = −20→20 |
53278 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.018 | (Δ/σ)max = 0.047 |
wR(F2) = 0.015 | Δρmax = 0.45 e Å−3 |
S = 0.68 | Δρmin = −0.59 e Å−3 |
8038 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
97 parameters | Extinction coefficient: 433 (13) |
0 restraints | Absolute structure: 3618 of Friedel pairs used in the refinement |
5 constraints | Absolute structure parameter: 0.5085 (13) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | −0.33359 (3) | −0.33359 (3) | 0 | 0.00891 (5) | 0.9501 (6) |
Bi1 | −0.33359 (3) | −0.33359 (3) | 0 | 0.00891 (5) | 0.0499 (6) |
Fe1 | 0.11604 (4) | 0.11604 (4) | 0 | 0.00585 (7) | |
Fe2 | −0.21355 (3) | −0.54914 (3) | 0.34025 (2) | 0.00604 (5) | |
O1 | 0 | −0.07680 (18) | 0.166667 | 0.0132 (5) | |
O2 | −0.58496 (14) | −0.26910 (13) | 0.14251 (13) | 0.0131 (3) | |
O3 | −0.12086 (16) | −0.30530 (15) | −0.17888 (14) | 0.0095 (4) | |
O4 | −0.14716 (16) | −0.36028 (15) | 0.18318 (15) | 0.0092 (4) | |
O5 | 0.47697 (14) | 0.14511 (15) | −0.1619 (2) | 0.0089 (3) | |
O6 | 0.1891 (2) | 0 | −0.166667 | 0.0079 (4) | |
O7 | −0.52225 (17) | −0.53846 (17) | −0.18315 (15) | 0.0106 (4) | |
B1 | 0.3345 (4) | 0 | −0.166667 | 0.0060 (5) | |
B2 | −0.4473 (2) | −0.1198 (2) | 0.1576 (2) | 0.0059 (4) | |
B3 | 0 | −0.2198 (3) | 0.166667 | 0.0109 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00932 (5) | 0.00932 (5) | 0.00842 (4) | 0.00490 (9) | −0.00031 (3) | 0.00031 (3) |
Bi1 | 0.00932 (5) | 0.00932 (5) | 0.00842 (4) | 0.00490 (9) | −0.00031 (3) | 0.00031 (3) |
Fe1 | 0.00556 (7) | 0.00556 (7) | 0.00657 (6) | 0.00289 (10) | 0.00014 (5) | −0.00014 (5) |
Fe2 | 0.00557 (7) | 0.00545 (6) | 0.00704 (4) | 0.00270 (6) | −0.00005 (5) | 0.00032 (5) |
O1 | 0.0175 (8) | 0.0074 (4) | 0.0179 (5) | 0.0088 (4) | 0.0086 (5) | 0.0043 (2) |
O2 | 0.0077 (3) | 0.0071 (3) | 0.0197 (4) | 0.0002 (3) | −0.0052 (3) | 0.0053 (2) |
O3 | 0.0126 (5) | 0.0056 (4) | 0.0109 (4) | 0.0049 (4) | 0.0023 (3) | 0.0024 (3) |
O4 | 0.0081 (5) | 0.0087 (4) | 0.0100 (4) | 0.0036 (4) | −0.0004 (3) | 0.0016 (3) |
O5 | 0.0049 (4) | 0.0064 (4) | 0.0110 (4) | −0.0004 (3) | −0.0003 (3) | 0.0024 (3) |
O6 | 0.0080 (5) | 0.0048 (6) | 0.0099 (6) | 0.0024 (3) | −0.0015 (2) | −0.0031 (4) |
O7 | 0.0086 (4) | 0.0132 (5) | 0.0117 (4) | 0.0067 (4) | −0.0009 (3) | −0.0024 (3) |
B1 | 0.0071 (5) | 0.0018 (7) | 0.0074 (3) | 0.0009 (4) | 0.0016 (3) | 0.0032 (7) |
B2 | 0.0035 (5) | 0.0060 (5) | 0.0087 (5) | 0.0029 (4) | 0.0004 (3) | 0.0002 (3) |
B3 | 0.0171 (13) | 0.0102 (8) | 0.0076 (7) | 0.0085 (7) | 0.0024 (8) | 0.0012 (4) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Fe1—O3iv | 1.9659 (13) |
Y1—O3 | 2.3373 (15) | Fe1—O6 | 2.0157 (12) |
Y1—O3i | 2.3373 (15) | Fe1—O6iii | 2.0157 (12) |
Y1—O4 | 2.3641 (16) | Fe2—O2v | 2.0481 (10) |
Y1—O4i | 2.3641 (16) | Fe2—O2vi | 2.0362 (11) |
Y1—O7 | 2.3344 (11) | Fe2—O4 | 1.9773 (13) |
Y1—O7i | 2.3344 (11) | Fe2—O5vii | 2.0196 (19) |
Bi1—O3 | 2.3373 (15) | Fe2—O5viii | 2.0164 (19) |
Bi1—O3i | 2.3373 (15) | Fe2—O7ix | 1.9727 (19) |
Bi1—O4 | 2.3641 (16) | O1—B3 | 1.362 (3) |
Bi1—O4i | 2.3641 (16) | O2—B2 | 1.3751 (16) |
Bi1—O7 | 2.3344 (11) | O3—B2i | 1.368 (3) |
Bi1—O7i | 2.3344 (11) | O4—B3 | 1.3768 (18) |
Fe1—O1 | 2.0382 (11) | O5—B1 | 1.370 (2) |
Fe1—O1ii | 2.0382 (11) | O6—B1 | 1.386 (4) |
Fe1—O3iii | 1.9659 (13) | O7—B2x | 1.369 (3) |
| | | |
Bi1—Y1—O3 | 0 | O6—Fe1—O6iii | 168.33 (4) |
Bi1—Y1—O3i | 0 | O2v—Fe2—O2vi | 86.74 (5) |
Bi1—Y1—O4 | 0 | O2v—Fe2—O4 | 167.86 (7) |
Bi1—Y1—O4i | 0 | O2v—Fe2—O5vii | 96.05 (6) |
Bi1—Y1—O7 | 0 | O2v—Fe2—O5viii | 76.02 (6) |
Bi1—Y1—O7i | 0 | O2v—Fe2—O7ix | 83.52 (6) |
O3—Y1—O3i | 121.17 (4) | O2vi—Fe2—O4 | 90.74 (5) |
O3—Y1—O4 | 72.36 (5) | O2vi—Fe2—O5vii | 76.21 (6) |
O3—Y1—O4i | 89.25 (5) | O2vi—Fe2—O5viii | 92.68 (6) |
O3—Y1—O7 | 90.78 (5) | O2vi—Fe2—O7ix | 163.20 (8) |
O3—Y1—O7i | 140.81 (6) | O4—Fe2—O5vii | 94.87 (7) |
O3i—Y1—O4 | 89.25 (5) | O4—Fe2—O5viii | 92.27 (6) |
O3i—Y1—O4i | 72.36 (5) | O4—Fe2—O7ix | 101.54 (5) |
O3i—Y1—O7 | 140.81 (6) | O5vii—Fe2—O5viii | 166.84 (5) |
O3i—Y1—O7i | 90.78 (5) | O5vii—Fe2—O7ix | 91.21 (7) |
O4—Y1—O4i | 142.45 (4) | O5viii—Fe2—O7ix | 98.18 (7) |
O4—Y1—O7 | 124.30 (6) | Fe1—O1—Fe1iii | 101.88 (8) |
O4—Y1—O7i | 87.33 (5) | Fe1—O1—B3 | 129.06 (4) |
O4i—Y1—O7 | 87.33 (5) | Fe1iii—O1—B3 | 129.06 (4) |
O4i—Y1—O7i | 124.30 (6) | Fe2xi—O2—Fe2xii | 102.80 (4) |
O7—Y1—O7i | 73.18 (4) | Fe2xi—O2—B2 | 125.19 (10) |
Y1—Bi1—O3 | 0 | Fe2xii—O2—B2 | 129.11 (12) |
Y1—Bi1—O3i | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O4 | 0 | Y1—O3—Fe1ii | 121.74 (9) |
Y1—Bi1—O4i | 0 | Y1—O3—B2i | 104.66 (9) |
Y1—Bi1—O7 | 0 | Bi1—O3—Fe1ii | 121.74 (9) |
Y1—Bi1—O7i | 0 | Bi1—O3—B2i | 104.66 (9) |
O3—Bi1—O3i | 121.17 (4) | Fe1ii—O3—B2i | 133.34 (12) |
O3—Bi1—O4 | 72.36 (5) | Y1—O4—Bi1 | 0.0 (5) |
O3—Bi1—O4i | 89.25 (5) | Y1—O4—Fe2 | 122.29 (6) |
O3—Bi1—O7 | 90.78 (5) | Y1—O4—B3 | 107.27 (11) |
O3—Bi1—O7i | 140.81 (6) | Bi1—O4—Fe2 | 122.29 (6) |
O3i—Bi1—O4 | 89.25 (5) | Bi1—O4—B3 | 107.27 (11) |
O3i—Bi1—O4i | 72.36 (5) | Fe2—O4—B3 | 130.23 (12) |
O3i—Bi1—O7 | 140.81 (6) | Fe2xiii—O5—Fe2xiv | 104.53 (4) |
O3i—Bi1—O7i | 90.78 (5) | Fe2xiii—O5—B1 | 127.70 (13) |
O4—Bi1—O4i | 142.45 (4) | Fe2xiv—O5—B1 | 127.75 (13) |
O4—Bi1—O7 | 124.30 (6) | Fe1—O6—Fe1ii | 103.48 (9) |
O4—Bi1—O7i | 87.33 (5) | Fe1—O6—B1 | 128.26 (4) |
O4i—Bi1—O7 | 87.33 (5) | Fe1ii—O6—B1 | 128.26 (4) |
O4i—Bi1—O7i | 124.30 (6) | Y1—O7—Bi1 | 0.0 (5) |
O7—Bi1—O7i | 73.18 (4) | Y1—O7—Fe2xv | 118.61 (8) |
O1—Fe1—O1ii | 87.596 (10) | Y1—O7—B2x | 112.82 (11) |
O1—Fe1—O3iii | 85.73 (4) | Bi1—O7—Fe2xv | 118.61 (8) |
O1—Fe1—O3iv | 167.34 (7) | Bi1—O7—B2x | 112.82 (11) |
O1—Fe1—O6 | 94.17 (4) | Fe2xv—O7—B2x | 128.56 (10) |
O1—Fe1—O6iii | 77.32 (6) | O5—B1—O5iv | 121.9 (3) |
O1ii—Fe1—O3iii | 167.34 (7) | O5—B1—O6 | 119.07 (16) |
O1ii—Fe1—O3iv | 85.73 (4) | O5iv—B1—O6 | 119.07 (16) |
O1ii—Fe1—O6 | 77.32 (6) | O2—B2—O3i | 115.91 (18) |
O1ii—Fe1—O6iii | 94.17 (4) | O2—B2—O7xvi | 118.77 (17) |
O3iii—Fe1—O3iv | 102.74 (7) | O3i—B2—O7xvi | 125.33 (13) |
O3iii—Fe1—O6 | 92.44 (7) | O1—B3—O4 | 117.57 (13) |
O3iii—Fe1—O6iii | 94.84 (5) | O1—B3—O4xvii | 117.57 (14) |
O3iv—Fe1—O6 | 94.84 (5) | O4—B3—O4xvii | 124.9 (2) |
O3iv—Fe1—O6iii | 92.44 (7) | | |
Symmetry codes: (i) y, x, −z; (ii) −x+y, −x, z−1/3; (iii) −y, x−y, z+1/3; (iv) x−y, −y, −z−1/3; (v) x−y, −y−1, −z+2/3; (vi) −x−1, −x+y−1, −z+1/3; (vii) −y, x−y−1, z+1/3; (viii) −x+y, −x, z+2/3; (ix) −x+y, −x−1, z+2/3; (x) −x+y−1, −x−1, z−1/3; (xi) x−y−1, −y−1, −z+2/3; (xii) −x−1, −x+y, −z+1/3; (xiii) −y, x−y, z−2/3; (xiv) −x+y+1, −x, z−1/3; (xv) −y−1, x−y−1, z−2/3; (xvi) −y−1, x−y, z+1/3; (xvii) −x, −x+y, −z+1/3. |
Crystal data top
B4Bi0.053Fe3O12Y0.947 | Dx = 4.179 Mg m−3 |
Mr = 498 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3121 | Cell parameters from 10914 reflections |
Hall symbol: P 31 2" | θ = 5.6–73.2° |
a = 9.5245 (1) Å | µ = 13.52 mm−1 |
c = 7.5570 (1) Å | T = 370 K |
V = 593.70 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 8144 independent reflections |
Radiation source: X-ray tube | 2644 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.055 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.3°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −22→24 |
Tmin = 0.191, Tmax = 0.281 | l = −19→20 |
61266 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.048 |
wR(F2) = 0.014 | Δρmax = 0.33 e Å−3 |
S = 0.61 | Δρmin = −0.81 e Å−3 |
8144 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
97 parameters | Extinction coefficient: 395 (13) |
0 restraints | Absolute structure: 3696 of Friedel pairs used in the refinement |
5 constraints | Absolute structure parameter: 0.5076 (12) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | −0.33349 (4) | −0.33349 (4) | 0 | 0.00917 (6) | 0.9466 (5) |
Bi1 | −0.33349 (4) | −0.33349 (4) | 0 | 0.00917 (6) | 0.0534 (5) |
Fe1 | 0.11638 (4) | 0.11638 (4) | 0 | 0.00598 (8) | |
Fe2 | −0.21410 (3) | −0.54914 (3) | 0.33866 (2) | 0.00621 (6) | |
O1 | 0 | −0.0764 (2) | 0.166667 | 0.0150 (6) | |
O2 | −0.58716 (17) | −0.26671 (15) | 0.14828 (17) | 0.0163 (3) | |
O3 | −0.12111 (18) | −0.30599 (17) | −0.17949 (16) | 0.0094 (4) | |
O4 | −0.14694 (19) | −0.35997 (17) | 0.18259 (17) | 0.0098 (4) | |
O5 | 0.47692 (16) | 0.14502 (16) | −0.1627 (2) | 0.0086 (3) | |
O6 | 0.1889 (2) | 0 | −0.166667 | 0.0078 (5) | |
O7 | −0.52173 (19) | −0.53972 (19) | −0.18261 (16) | 0.0102 (4) | |
B1 | 0.3332 (4) | 0 | −0.166667 | 0.0061 (5) | |
B2 | −0.4477 (2) | −0.1191 (3) | 0.1602 (3) | 0.0084 (5) | |
B3 | 0 | −0.2198 (3) | 0.166667 | 0.0064 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00948 (6) | 0.00948 (6) | 0.00864 (3) | 0.00481 (10) | −0.00025 (4) | 0.00025 (4) |
Bi1 | 0.00948 (6) | 0.00948 (6) | 0.00864 (3) | 0.00481 (10) | −0.00025 (4) | 0.00025 (4) |
Fe1 | 0.00582 (9) | 0.00582 (9) | 0.00659 (6) | 0.00312 (12) | −0.00002 (5) | 0.00002 (5) |
Fe2 | 0.00576 (8) | 0.00524 (7) | 0.00745 (4) | 0.00261 (6) | 0.00007 (6) | 0.00012 (5) |
O1 | 0.0206 (11) | 0.0087 (5) | 0.0197 (6) | 0.0103 (5) | 0.0128 (6) | 0.0064 (3) |
O2 | 0.0084 (4) | 0.0083 (4) | 0.0255 (6) | −0.0009 (3) | −0.0066 (4) | 0.0078 (3) |
O3 | 0.0122 (6) | 0.0044 (4) | 0.0118 (4) | 0.0043 (4) | 0.0026 (4) | 0.0022 (3) |
O4 | 0.0093 (6) | 0.0089 (5) | 0.0100 (4) | 0.0035 (4) | −0.0002 (4) | 0.0015 (3) |
O5 | 0.0044 (5) | 0.0059 (5) | 0.0119 (4) | −0.0002 (3) | −0.0013 (3) | 0.0023 (3) |
O6 | 0.0075 (6) | 0.0069 (7) | 0.0089 (6) | 0.0035 (4) | −0.0004 (2) | −0.0009 (5) |
O7 | 0.0081 (5) | 0.0124 (5) | 0.0109 (4) | 0.0059 (4) | −0.0006 (3) | −0.0023 (3) |
B1 | 0.0030 (3) | 0.0104 (10) | 0.0073 (3) | 0.0052 (5) | −0.0009 (4) | −0.0018 (8) |
B2 | 0.0071 (7) | 0.0069 (6) | 0.0085 (6) | 0.0014 (5) | 0.0000 (4) | 0.0019 (4) |
B3 | 0.0026 (8) | 0.0057 (8) | 0.0098 (9) | 0.0013 (4) | −0.0013 (6) | −0.0007 (3) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Fe1—O3iv | 1.9648 (15) |
Y1—O3 | 2.3389 (17) | Fe1—O6 | 2.0143 (14) |
Y1—O3i | 2.3389 (17) | Fe1—O6iii | 2.0143 (14) |
Y1—O4 | 2.3607 (19) | Fe2—O2v | 2.0422 (12) |
Y1—O4i | 2.3607 (19) | Fe2—O2vi | 2.0303 (13) |
Y1—O7 | 2.3356 (13) | Fe2—O4 | 1.9732 (15) |
Y1—O7i | 2.3356 (13) | Fe2—O5vii | 2.018 (2) |
Bi1—O3 | 2.3389 (17) | Fe2—O5viii | 2.016 (2) |
Bi1—O3i | 2.3389 (17) | Fe2—O7ix | 1.973 (2) |
Bi1—O4 | 2.3607 (19) | O1—B3 | 1.366 (4) |
Bi1—O4i | 2.3607 (19) | O2—B2 | 1.372 (2) |
Bi1—O7 | 2.3356 (13) | O3—B2i | 1.367 (3) |
Bi1—O7i | 2.3356 (13) | O4—B3 | 1.3737 (19) |
Fe1—O1 | 2.0373 (13) | O5—B1 | 1.375 (2) |
Fe1—O1ii | 2.0373 (13) | O6—B1 | 1.375 (4) |
Fe1—O3iii | 1.9648 (15) | O7—B2x | 1.371 (4) |
| | | |
Bi1—Y1—O3 | 0 | O6—Fe1—O6iii | 168.10 (5) |
Bi1—Y1—O3i | 0 | O2v—Fe2—O2vi | 86.82 (6) |
Bi1—Y1—O4 | 0 | O2v—Fe2—O4 | 167.65 (9) |
Bi1—Y1—O4i | 0 | O2v—Fe2—O5vii | 95.57 (8) |
Bi1—Y1—O7 | 0 | O2v—Fe2—O5viii | 76.06 (7) |
Bi1—Y1—O7i | 0 | O2v—Fe2—O7ix | 84.35 (7) |
O3—Y1—O3i | 121.53 (5) | O2vi—Fe2—O4 | 89.68 (7) |
O3—Y1—O4 | 72.30 (5) | O2vi—Fe2—O5vii | 76.28 (7) |
O3—Y1—O4i | 89.35 (6) | O2vi—Fe2—O5viii | 93.18 (8) |
O3—Y1—O7 | 90.50 (5) | O2vi—Fe2—O7ix | 164.04 (9) |
O3—Y1—O7i | 140.98 (7) | O4—Fe2—O5vii | 95.09 (8) |
O3i—Y1—O4 | 89.35 (6) | O4—Fe2—O5viii | 92.33 (7) |
O3i—Y1—O4i | 72.30 (5) | O4—Fe2—O7ix | 101.61 (6) |
O3i—Y1—O7 | 140.98 (7) | O5vii—Fe2—O5viii | 167.04 (5) |
O3i—Y1—O7i | 90.50 (5) | O5vii—Fe2—O7ix | 91.36 (8) |
O4—Y1—O4i | 142.32 (4) | O5viii—Fe2—O7ix | 97.55 (8) |
O4—Y1—O7 | 123.90 (7) | Fe1—O1—Fe1iii | 102.03 (9) |
O4—Y1—O7i | 87.80 (6) | Fe1—O1—B3 | 128.99 (5) |
O4i—Y1—O7 | 87.80 (6) | Fe1iii—O1—B3 | 128.99 (5) |
O4i—Y1—O7i | 123.90 (7) | Fe2xi—O2—Fe2xii | 103.01 (5) |
O7—Y1—O7i | 72.92 (4) | Fe2xi—O2—B2 | 125.90 (13) |
Y1—Bi1—O3 | 0 | Fe2xii—O2—B2 | 129.48 (15) |
Y1—Bi1—O3i | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O4 | 0 | Y1—O3—Fe1ii | 121.57 (9) |
Y1—Bi1—O4i | 0 | Y1—O3—B2i | 105.42 (11) |
Y1—Bi1—O7 | 0 | Bi1—O3—Fe1ii | 121.57 (9) |
Y1—Bi1—O7i | 0 | Bi1—O3—B2i | 105.42 (11) |
O3—Bi1—O3i | 121.53 (5) | Fe1ii—O3—B2i | 132.76 (14) |
O3—Bi1—O4 | 72.30 (5) | Y1—O4—Bi1 | 0.0 (5) |
O3—Bi1—O4i | 89.35 (6) | Y1—O4—Fe2 | 121.95 (7) |
O3—Bi1—O7 | 90.50 (5) | Y1—O4—B3 | 107.49 (12) |
O3—Bi1—O7i | 140.98 (7) | Bi1—O4—Fe2 | 121.95 (7) |
O3i—Bi1—O4 | 89.35 (6) | Bi1—O4—B3 | 107.49 (12) |
O3i—Bi1—O4i | 72.30 (5) | Fe2—O4—B3 | 130.34 (14) |
O3i—Bi1—O7 | 140.98 (7) | Fe2xiii—O5—Fe2xiv | 104.38 (5) |
O3i—Bi1—O7i | 90.50 (5) | Fe2xiii—O5—B1 | 127.54 (14) |
O4—Bi1—O4i | 142.32 (4) | Fe2xiv—O5—B1 | 128.06 (14) |
O4—Bi1—O7 | 123.90 (7) | Fe1—O6—Fe1ii | 103.66 (10) |
O4—Bi1—O7i | 87.80 (6) | Fe1—O6—B1 | 128.17 (5) |
O4i—Bi1—O7 | 87.80 (6) | Fe1ii—O6—B1 | 128.17 (5) |
O4i—Bi1—O7i | 123.90 (7) | Y1—O7—Bi1 | 0.0 (5) |
O7—Bi1—O7i | 72.92 (4) | Y1—O7—Fe2xv | 119.13 (9) |
O1—Fe1—O1ii | 87.459 (12) | Y1—O7—B2x | 111.71 (13) |
O1—Fe1—O3iii | 85.93 (5) | Bi1—O7—Fe2xv | 119.13 (9) |
O1—Fe1—O3iv | 167.19 (8) | Bi1—O7—B2x | 111.71 (13) |
O1—Fe1—O6 | 94.15 (5) | Fe2xv—O7—B2x | 129.14 (12) |
O1—Fe1—O6iii | 77.16 (6) | O5—B1—O5iv | 120.9 (3) |
O1ii—Fe1—O3iii | 167.19 (8) | O5—B1—O6 | 119.54 (15) |
O1ii—Fe1—O3iv | 85.93 (5) | O5iv—B1—O6 | 119.54 (15) |
O1ii—Fe1—O6 | 77.16 (6) | O2—B2—O3i | 116.7 (2) |
O1ii—Fe1—O6iii | 94.15 (5) | O2—B2—O7xvi | 118.1 (2) |
O3iii—Fe1—O3iv | 102.54 (8) | O3i—B2—O7xvi | 125.15 (15) |
O3iii—Fe1—O6 | 92.38 (8) | O1—B3—O4 | 117.55 (15) |
O3iii—Fe1—O6iii | 95.06 (6) | O1—B3—O4xvii | 117.55 (15) |
O3iv—Fe1—O6 | 95.06 (6) | O4—B3—O4xvii | 124.9 (3) |
O3iv—Fe1—O6iii | 92.38 (8) | | |
Symmetry codes: (i) y, x, −z; (ii) −x+y, −x, z−1/3; (iii) −y, x−y, z+1/3; (iv) x−y, −y, −z−1/3; (v) x−y, −y−1, −z+2/3; (vi) −x−1, −x+y−1, −z+1/3; (vii) −y, x−y−1, z+1/3; (viii) −x+y, −x, z+2/3; (ix) −x+y, −x−1, z+2/3; (x) −x+y−1, −x−1, z−1/3; (xi) x−y−1, −y−1, −z+2/3; (xii) −x−1, −x+y, −z+1/3; (xiii) −y, x−y, z−2/3; (xiv) −x+y+1, −x, z−1/3; (xv) −y−1, x−y−1, z−2/3; (xvi) −y−1, x−y, z+1/3; (xvii) −x, −x+y, −z+1/3. |
Crystal data top
B4Bi0.05Fe3O12Y0.95 | Dx = 4.171 Mg m−3 |
Mr = 497.7 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R32 | Cell parameters from 10855 reflections |
Hall symbol: R 3 2" | θ = 5.6–73.8° |
a = 9.5272 (1) Å | µ = 13.46 mm−1 |
c = 7.5618 (1) Å | T = 375 K |
V = 594.41 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 2723 independent reflections |
Radiation source: X-ray tube | 2418 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.038 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.1°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −22→24 |
Tmin = 0.192, Tmax = 0.281 | l = −20→20 |
20360 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.038 |
wR(F2) = 0.012 | Δρmax = 0.29 e Å−3 |
S = 0.99 | Δρmin = −0.60 e Å−3 |
2723 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
37 parameters | Extinction coefficient: 425 (19) |
0 restraints | Absolute structure: 1231 of Friedel pairs used in the refinement |
2 constraints | Absolute structure parameter: 0.5094 (19) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | 0 | 0 | 0 | 0.00933 (3) | 0.9501 (8) |
Bi1 | 0 | 0 | 0 | 0.00933 (3) | 0.0499 (8) |
Fe1 | 0.215713 (12) | 0.333333 | 0.333333 | 0.00650 (2) | |
O1 | 0.14428 (6) | 0.14428 (6) | 0.5 | 0.00866 (13) | |
O2 | 0.40771 (7) | 0.40771 (7) | 0.5 | 0.01954 (18) | |
O3 | 0.02437 (6) | 0.21081 (6) | 0.18126 (6) | 0.01026 (13) | |
B1 | 0 | 0 | 0.5 | 0.0060 (2) | |
B2 | 0.55123 (8) | 0.55123 (8) | 0.5 | 0.0082 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00962 (4) | 0.00962 (4) | 0.00874 (5) | 0.00481 (2) | 0 | 0 |
Bi1 | 0.00962 (4) | 0.00962 (4) | 0.00874 (5) | 0.00481 (2) | 0 | 0 |
Fe1 | 0.00580 (3) | 0.00581 (3) | 0.00791 (3) | 0.002904 (17) | 0.000105 (14) | 0.00021 (3) |
O1 | 0.00626 (13) | 0.00626 (13) | 0.0112 (2) | 0.00140 (15) | −0.00148 (8) | 0.00148 (8) |
O2 | 0.00962 (16) | 0.00962 (16) | 0.0303 (4) | −0.00199 (19) | −0.00954 (14) | 0.00954 (14) |
O3 | 0.00817 (14) | 0.01255 (17) | 0.01116 (15) | 0.00601 (13) | −0.00209 (11) | −0.00235 (12) |
B1 | 0.0055 (3) | 0.0055 (3) | 0.0069 (4) | 0.00277 (14) | 0 | 0 |
B2 | 0.0067 (2) | 0.0067 (2) | 0.0103 (2) | 0.0026 (3) | −0.00099 (18) | 0.00099 (18) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Bi1—O3iv | 2.3452 (5) |
Y1—O3 | 2.3452 (6) | Bi1—O3v | 2.3452 (7) |
Y1—O3i | 2.3452 (5) | Fe1—O1 | 2.0174 (4) |
Y1—O3ii | 2.3452 (7) | Fe1—O1vi | 2.0174 (4) |
Y1—O3iii | 2.3452 (6) | Fe1—O2 | 2.0348 (5) |
Y1—O3iv | 2.3452 (5) | Fe1—O2vi | 2.0348 (8) |
Y1—O3v | 2.3452 (7) | Fe1—O3 | 1.9698 (4) |
Bi1—O3 | 2.3452 (6) | Fe1—O3vii | 1.9698 (7) |
Bi1—O3i | 2.3452 (5) | O1—B1 | 1.3746 (4) |
Bi1—O3ii | 2.3452 (7) | O2—B2 | 1.3673 (7) |
Bi1—O3iii | 2.3452 (6) | O3—B2viii | 1.3714 (11) |
| | | |
Bi1—Y1—O3 | 0 | O3ii—Bi1—O3v | 141.560 (15) |
Bi1—Y1—O3i | 0 | O3iii—Bi1—O3iv | 89.29 (2) |
Bi1—Y1—O3ii | 0 | O3iii—Bi1—O3v | 89.29 (2) |
Bi1—Y1—O3iii | 0 | O3iv—Bi1—O3v | 89.29 (2) |
Bi1—Y1—O3iv | 0 | O1—Fe1—O1vi | 167.48 (3) |
Bi1—Y1—O3v | 0 | O1—Fe1—O2 | 76.538 (19) |
O3—Y1—O3i | 89.29 (2) | O1—Fe1—O2vi | 94.28 (2) |
O3—Y1—O3ii | 89.29 (2) | O1—Fe1—O3 | 92.092 (18) |
O3—Y1—O3iii | 122.930 (15) | O1—Fe1—O3vii | 95.78 (2) |
O3—Y1—O3iv | 141.56 (2) | O1vi—Fe1—O2 | 94.28 (2) |
O3—Y1—O3v | 72.41 (2) | O1vi—Fe1—O2vi | 76.54 (3) |
O3i—Y1—O3ii | 89.29 (2) | O1vi—Fe1—O3 | 95.78 (2) |
O3i—Y1—O3iii | 141.56 (2) | O1vi—Fe1—O3vii | 92.09 (2) |
O3i—Y1—O3iv | 72.414 (17) | O2—Fe1—O2vi | 87.09 (3) |
O3i—Y1—O3v | 122.93 (2) | O2—Fe1—O3 | 166.51 (3) |
O3ii—Y1—O3iii | 72.41 (2) | O2—Fe1—O3vii | 86.54 (3) |
O3ii—Y1—O3iv | 122.93 (2) | O2vi—Fe1—O3 | 86.54 (3) |
O3ii—Y1—O3v | 141.560 (15) | O2vi—Fe1—O3vii | 166.51 (2) |
O3iii—Y1—O3iv | 89.29 (2) | O3—Fe1—O3vii | 102.03 (3) |
O3iii—Y1—O3v | 89.29 (2) | Fe1—O1—Fe1ix | 104.086 (19) |
O3iv—Y1—O3v | 89.29 (2) | Fe1—O1—B1 | 127.96 (3) |
Y1—Bi1—O3 | 0 | Fe1ix—O1—B1 | 127.96 (3) |
Y1—Bi1—O3i | 0 | Fe1—O2—Fe1ix | 102.84 (2) |
Y1—Bi1—O3ii | 0 | Fe1—O2—B2 | 128.58 (4) |
Y1—Bi1—O3iii | 0 | Fe1ix—O2—B2 | 128.58 (4) |
Y1—Bi1—O3iv | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O3v | 0 | Y1—O3—Fe1 | 120.98 (3) |
O3—Bi1—O3i | 89.29 (2) | Y1—O3—B2viii | 108.21 (3) |
O3—Bi1—O3ii | 89.29 (2) | Bi1—O3—Fe1 | 120.98 (3) |
O3—Bi1—O3iii | 122.930 (15) | Bi1—O3—B2viii | 108.21 (3) |
O3—Bi1—O3iv | 141.56 (2) | Fe1—O3—B2viii | 130.66 (4) |
O3—Bi1—O3v | 72.41 (2) | O1—B1—O1i | 120.00 (4) |
O3i—Bi1—O3ii | 89.29 (2) | O1—B1—O1ii | 120.00 (4) |
O3i—Bi1—O3iii | 141.56 (2) | O1i—B1—O1ii | 120.00 (4) |
O3i—Bi1—O3iv | 72.414 (17) | O2—B2—O3x | 117.45 (7) |
O3i—Bi1—O3v | 122.93 (2) | O2—B2—O3xi | 117.45 (7) |
O3ii—Bi1—O3iii | 72.41 (2) | O3x—B2—O3xi | 125.10 (5) |
O3ii—Bi1—O3iv | 122.93 (2) | | |
Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) y, x, −z; (iv) x−y, −y, −z; (v) −x, −x+y, −z; (vi) −x+y+1/3, −x+2/3, z−1/3; (vii) x−y+1/3, −y+2/3, −z+2/3; (viii) x−2/3, y−1/3, z−1/3; (ix) −y+2/3, x−y+1/3, z+1/3; (x) x+2/3, y+1/3, z+1/3; (xi) y+1/3, x+2/3, −z+2/3. |
Crystal data top
B4Bi0.051Fe3O12Y0.949 | Dx = 4.176 Mg m−3 |
Mr = 497.8 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R32 | Cell parameters from 10955 reflections |
Hall symbol: R 3 2" | θ = 5.6–73.5° |
a = 9.5265 (1) Å | µ = 13.48 mm−1 |
c = 7.5561 (1) Å | T = 380 K |
V = 593.88 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 2715 independent reflections |
Radiation source: X-ray tube | 2406 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.3°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −22→23 |
Tmin = 0.191, Tmax = 0.281 | l = −19→20 |
20394 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.034 |
wR(F2) = 0.012 | Δρmax = 0.30 e Å−3 |
S = 0.91 | Δρmin = −0.88 e Å−3 |
2715 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
37 parameters | Extinction coefficient: 420 (20) |
0 restraints | Absolute structure: 1228 of Friedel pairs used in the refinement |
2 constraints | Absolute structure parameter: 0.5071 (18) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | 0 | 0 | 0 | 0.00947 (3) | 0.9491 (9) |
Bi1 | 0 | 0 | 0 | 0.00947 (3) | 0.0509 (9) |
Fe1 | 0.215741 (11) | 0.333333 | 0.333333 | 0.00645 (2) | |
O1 | 0.14424 (6) | 0.14424 (6) | 0.5 | 0.00873 (12) | |
O2 | 0.40782 (7) | 0.40782 (7) | 0.5 | 0.01852 (16) | |
O3 | 0.02447 (5) | 0.21077 (6) | 0.18150 (6) | 0.01030 (12) | |
B1 | 0 | 0 | 0.5 | 0.0060 (2) | |
B2 | 0.55137 (8) | 0.55137 (8) | 0.5 | 0.0080 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00978 (4) | 0.00978 (4) | 0.00884 (5) | 0.00489 (2) | 0 | 0 |
Bi1 | 0.00978 (4) | 0.00978 (4) | 0.00884 (5) | 0.00489 (2) | 0 | 0 |
Fe1 | 0.00582 (2) | 0.00585 (3) | 0.00770 (3) | 0.002926 (16) | 0.000064 (13) | 0.00013 (3) |
O1 | 0.00616 (12) | 0.00616 (12) | 0.01144 (18) | 0.00126 (14) | −0.00147 (7) | 0.00147 (7) |
O2 | 0.00927 (15) | 0.00927 (15) | 0.0287 (3) | −0.00164 (17) | −0.00868 (13) | 0.00868 (13) |
O3 | 0.00810 (13) | 0.01288 (17) | 0.01094 (13) | 0.00601 (12) | −0.00220 (10) | −0.00238 (11) |
B1 | 0.0053 (3) | 0.0053 (3) | 0.0075 (4) | 0.00265 (13) | 0 | 0 |
B2 | 0.00621 (19) | 0.00621 (19) | 0.0100 (2) | 0.0019 (3) | −0.00061 (16) | 0.00061 (16) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Bi1—O3iv | 2.3449 (4) |
Y1—O3 | 2.3449 (5) | Bi1—O3v | 2.3449 (7) |
Y1—O3i | 2.3449 (4) | Fe1—O1 | 2.0169 (4) |
Y1—O3ii | 2.3449 (7) | Fe1—O1vi | 2.0169 (4) |
Y1—O3iii | 2.3449 (5) | Fe1—O2 | 2.0345 (5) |
Y1—O3iv | 2.3449 (4) | Fe1—O2vi | 2.0345 (8) |
Y1—O3v | 2.3449 (7) | Fe1—O3 | 1.9678 (4) |
Bi1—O3 | 2.3449 (5) | Fe1—O3vii | 1.9678 (7) |
Bi1—O3i | 2.3449 (4) | O1—B1 | 1.3741 (4) |
Bi1—O3ii | 2.3449 (7) | O2—B2 | 1.3676 (7) |
Bi1—O3iii | 2.3449 (5) | O3—B2viii | 1.3720 (10) |
| | | |
Bi1—Y1—O3 | 0 | O3ii—Bi1—O3v | 141.619 (14) |
Bi1—Y1—O3i | 0 | O3iii—Bi1—O3iv | 89.251 (19) |
Bi1—Y1—O3ii | 0 | O3iii—Bi1—O3v | 89.251 (19) |
Bi1—Y1—O3iii | 0 | O3iv—Bi1—O3v | 89.251 (19) |
Bi1—Y1—O3iv | 0 | O1—Fe1—O1vi | 167.50 (3) |
Bi1—Y1—O3v | 0 | O1—Fe1—O2 | 76.597 (17) |
O3—Y1—O3i | 89.251 (19) | O1—Fe1—O2vi | 94.24 (2) |
O3—Y1—O3ii | 89.251 (19) | O1—Fe1—O3 | 92.010 (17) |
O3—Y1—O3iii | 122.910 (14) | O1—Fe1—O3vii | 95.85 (2) |
O3—Y1—O3iv | 141.62 (2) | O1vi—Fe1—O2 | 94.24 (2) |
O3—Y1—O3v | 72.478 (19) | O1vi—Fe1—O2vi | 76.60 (2) |
O3i—Y1—O3ii | 89.251 (19) | O1vi—Fe1—O3 | 95.850 (19) |
O3i—Y1—O3iii | 141.62 (2) | O1vi—Fe1—O3vii | 92.01 (2) |
O3i—Y1—O3iv | 72.478 (16) | O2—Fe1—O2vi | 87.06 (2) |
O3i—Y1—O3v | 122.91 (2) | O2—Fe1—O3 | 166.49 (3) |
O3ii—Y1—O3iii | 72.478 (19) | O2—Fe1—O3vii | 86.57 (3) |
O3ii—Y1—O3iv | 122.91 (2) | O2vi—Fe1—O3 | 86.57 (2) |
O3ii—Y1—O3v | 141.619 (14) | O2vi—Fe1—O3vii | 166.491 (19) |
O3iii—Y1—O3iv | 89.251 (19) | O3—Fe1—O3vii | 102.01 (3) |
O3iii—Y1—O3v | 89.251 (19) | Fe1—O1—Fe1ix | 104.034 (18) |
O3iv—Y1—O3v | 89.251 (19) | Fe1—O1—B1 | 127.98 (3) |
Y1—Bi1—O3 | 0 | Fe1ix—O1—B1 | 127.98 (3) |
Y1—Bi1—O3i | 0 | Fe1—O2—Fe1ix | 102.77 (2) |
Y1—Bi1—O3ii | 0 | Fe1—O2—B2 | 128.61 (4) |
Y1—Bi1—O3iii | 0 | Fe1ix—O2—B2 | 128.61 (4) |
Y1—Bi1—O3iv | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O3v | 0 | Y1—O3—Fe1 | 121.01 (3) |
O3—Bi1—O3i | 89.251 (19) | Y1—O3—B2viii | 108.18 (3) |
O3—Bi1—O3ii | 89.251 (19) | Bi1—O3—Fe1 | 121.01 (3) |
O3—Bi1—O3iii | 122.910 (14) | Bi1—O3—B2viii | 108.18 (3) |
O3—Bi1—O3iv | 141.62 (2) | Fe1—O3—B2viii | 130.67 (4) |
O3—Bi1—O3v | 72.478 (19) | O1—B1—O1i | 120.00 (4) |
O3i—Bi1—O3ii | 89.251 (19) | O1—B1—O1ii | 120.00 (4) |
O3i—Bi1—O3iii | 141.62 (2) | O1i—B1—O1ii | 120.00 (4) |
O3i—Bi1—O3iv | 72.478 (16) | O2—B2—O3x | 117.39 (7) |
O3i—Bi1—O3v | 122.91 (2) | O2—B2—O3xi | 117.39 (7) |
O3ii—Bi1—O3iii | 72.478 (19) | O3x—B2—O3xi | 125.23 (5) |
O3ii—Bi1—O3iv | 122.91 (2) | | |
Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) y, x, −z; (iv) x−y, −y, −z; (v) −x, −x+y, −z; (vi) −x+y+1/3, −x+2/3, z−1/3; (vii) x−y+1/3, −y+2/3, −z+2/3; (viii) x−2/3, y−1/3, z−1/3; (ix) −y+2/3, x−y+1/3, z+1/3; (x) x+2/3, y+1/3, z+1/3; (xi) y+1/3, x+2/3, −z+2/3. |
Crystal data top
B4Bi0.053Fe3O12Y0.947 | Dx = 4.169 Mg m−3 |
Mr = 498 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R32 | Cell parameters from 10417 reflections |
Hall symbol: R 3 2" | θ = 5.6–73.8° |
a = 9.5321 (1) Å | µ = 13.49 mm−1 |
c = 7.5627 (1) Å | T = 430 K |
V = 595.09 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 705 | |
Data collection top
Oxford Diffraction CCD diffractometer | 2724 independent reflections |
Radiation source: X-ray tube | 2356 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.041 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.2°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −22→24 |
Tmin = 0.186, Tmax = 0.276 | l = −19→20 |
20455 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.017 | (Δ/σ)max = 0.042 |
wR(F2) = 0.014 | Δρmax = 0.34 e Å−3 |
S = 1.01 | Δρmin = −0.58 e Å−3 |
2724 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
37 parameters | Extinction coefficient: 440 (20) |
0 restraints | Absolute structure: 1232 of Friedel pairs used in the refinement |
2 constraints | Absolute structure parameter: 0.503 (2) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | 0 | 0 | 0 | 0.01074 (4) | 0.9512 (9) |
Bi1 | 0 | 0 | 0 | 0.01074 (4) | 0.0488 (9) |
Fe1 | 0.215782 (13) | 0.333333 | 0.333333 | 0.00717 (2) | |
O1 | 0.14419 (7) | 0.14419 (7) | 0.5 | 0.00945 (13) | |
O2 | 0.40784 (7) | 0.40784 (7) | 0.5 | 0.01789 (17) | |
O3 | 0.02465 (6) | 0.21099 (6) | 0.18114 (6) | 0.01120 (13) | |
B1 | 0 | 0 | 0.5 | 0.0065 (2) | |
B2 | 0.55151 (8) | 0.55151 (8) | 0.5 | 0.0087 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.01111 (4) | 0.01111 (4) | 0.00999 (6) | 0.00556 (2) | 0 | 0 |
Bi1 | 0.01111 (4) | 0.01111 (4) | 0.00999 (6) | 0.00556 (2) | 0 | 0 |
Fe1 | 0.00655 (3) | 0.00664 (4) | 0.00836 (3) | 0.003320 (18) | −0.000016 (15) | −0.00003 (3) |
O1 | 0.00676 (14) | 0.00676 (14) | 0.0123 (2) | 0.00147 (16) | −0.00153 (8) | 0.00153 (8) |
O2 | 0.00960 (17) | 0.00960 (17) | 0.0265 (3) | −0.00116 (19) | −0.00771 (13) | 0.00771 (13) |
O3 | 0.00850 (15) | 0.01418 (19) | 0.01181 (15) | 0.00634 (14) | −0.00221 (11) | −0.00236 (13) |
B1 | 0.0057 (3) | 0.0057 (3) | 0.0083 (5) | 0.00284 (15) | 0 | 0 |
B2 | 0.0071 (2) | 0.0071 (2) | 0.0104 (2) | 0.0022 (4) | −0.00036 (18) | 0.00036 (18) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Bi1—O3iv | 2.3461 (5) |
Y1—O3 | 2.3461 (6) | Bi1—O3v | 2.3461 (8) |
Y1—O3i | 2.3461 (5) | Fe1—O1 | 2.0186 (5) |
Y1—O3ii | 2.3461 (8) | Fe1—O1vi | 2.0186 (4) |
Y1—O3iii | 2.3461 (6) | Fe1—O2 | 2.0358 (5) |
Y1—O3iv | 2.3461 (5) | Fe1—O2vi | 2.0358 (8) |
Y1—O3v | 2.3461 (8) | Fe1—O3 | 1.9696 (5) |
Bi1—O3 | 2.3461 (6) | Fe1—O3vii | 1.9696 (7) |
Bi1—O3i | 2.3461 (5) | O1—B1 | 1.3744 (4) |
Bi1—O3ii | 2.3461 (8) | O2—B2 | 1.3694 (7) |
Bi1—O3iii | 2.3461 (6) | O3—B2viii | 1.3725 (11) |
| | | |
Bi1—Y1—O3 | 0 | O3ii—Bi1—O3v | 141.646 (16) |
Bi1—Y1—O3i | 0 | O3iii—Bi1—O3iv | 89.35 (2) |
Bi1—Y1—O3ii | 0 | O3iii—Bi1—O3v | 89.35 (2) |
Bi1—Y1—O3iii | 0 | O3iv—Bi1—O3v | 89.35 (2) |
Bi1—Y1—O3iv | 0 | O1—Fe1—O1vi | 167.54 (3) |
Bi1—Y1—O3v | 0 | O1—Fe1—O2 | 76.611 (19) |
O3—Y1—O3i | 89.35 (2) | O1—Fe1—O2vi | 94.26 (2) |
O3—Y1—O3ii | 89.35 (2) | O1—Fe1—O3 | 92.092 (19) |
O3—Y1—O3iii | 122.801 (16) | O1—Fe1—O3vii | 95.74 (2) |
O3—Y1—O3iv | 141.65 (3) | O1vi—Fe1—O2 | 94.26 (2) |
O3—Y1—O3v | 72.36 (2) | O1vi—Fe1—O2vi | 76.61 (3) |
O3i—Y1—O3ii | 89.35 (2) | O1vi—Fe1—O3 | 95.74 (2) |
O3i—Y1—O3iii | 141.65 (3) | O1vi—Fe1—O3vii | 92.09 (3) |
O3i—Y1—O3iv | 72.359 (18) | O2—Fe1—O2vi | 87.09 (3) |
O3i—Y1—O3v | 122.80 (2) | O2—Fe1—O3 | 166.56 (3) |
O3ii—Y1—O3iii | 72.36 (2) | O2—Fe1—O3vii | 86.51 (3) |
O3ii—Y1—O3iv | 122.80 (2) | O2vi—Fe1—O3 | 86.51 (3) |
O3ii—Y1—O3v | 141.646 (16) | O2vi—Fe1—O3vii | 166.56 (2) |
O3iii—Y1—O3iv | 89.35 (2) | O3—Fe1—O3vii | 102.05 (3) |
O3iii—Y1—O3v | 89.35 (2) | Fe1—O1—Fe1ix | 104.00 (2) |
O3iv—Y1—O3v | 89.35 (2) | Fe1—O1—B1 | 128.00 (3) |
Y1—Bi1—O3 | 0 | Fe1ix—O1—B1 | 128.00 (3) |
Y1—Bi1—O3i | 0 | Fe1—O2—Fe1ix | 102.77 (2) |
Y1—Bi1—O3ii | 0 | Fe1—O2—B2 | 128.61 (4) |
Y1—Bi1—O3iii | 0 | Fe1ix—O2—B2 | 128.61 (4) |
Y1—Bi1—O3iv | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O3v | 0 | Y1—O3—Fe1 | 121.02 (3) |
O3—Bi1—O3i | 89.35 (2) | Y1—O3—B2viii | 108.22 (3) |
O3—Bi1—O3ii | 89.35 (2) | Bi1—O3—Fe1 | 121.02 (3) |
O3—Bi1—O3iii | 122.801 (16) | Bi1—O3—B2viii | 108.22 (3) |
O3—Bi1—O3iv | 141.65 (3) | Fe1—O3—B2viii | 130.61 (4) |
O3—Bi1—O3v | 72.36 (2) | O1—B1—O1i | 120.00 (4) |
O3i—Bi1—O3ii | 89.35 (2) | O1—B1—O1ii | 120.00 (4) |
O3i—Bi1—O3iii | 141.65 (3) | O1i—B1—O1ii | 120.00 (4) |
O3i—Bi1—O3iv | 72.359 (18) | O2—B2—O3x | 117.42 (8) |
O3i—Bi1—O3v | 122.80 (2) | O2—B2—O3xi | 117.42 (8) |
O3ii—Bi1—O3iii | 72.36 (2) | O3x—B2—O3xi | 125.16 (5) |
O3ii—Bi1—O3iv | 122.80 (2) | | |
Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) y, x, −z; (iv) x−y, −y, −z; (v) −x, −x+y, −z; (vi) −x+y+1/3, −x+2/3, z−1/3; (vii) x−y+1/3, −y+2/3, −z+2/3; (viii) x−2/3, y−1/3, z−1/3; (ix) −y+2/3, x−y+1/3, z+1/3; (x) x+2/3, y+1/3, z+1/3; (xi) y+1/3, x+2/3, −z+2/3. |
Crystal data top
B4Bi0.054Fe3O12Y0.946 | Dx = 4.156 Mg m−3 |
Mr = 498.2 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R32 | Cell parameters from 9316 reflections |
Hall symbol: R 3 2" | θ = 5.6–73.7° |
a = 9.5394 (1) Å | µ = 13.46 mm−1 |
c = 7.5765 (1) Å | T = 500 K |
V = 597.09 (2) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Oxford Diffraction CCD diffractometer | 2727 independent reflections |
Radiation source: X-ray tube | 2231 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.044 |
Detector resolution: 16.0628 pixels mm-1 | θmax = 74.2°, θmin = 4.3° |
ω scans | h = −24→22 |
Absorption correction: for a sphere Jana2006 | k = −25→25 |
Tmin = 0.193, Tmax = 0.282 | l = −20→19 |
20271 measured reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000001F2) |
R[F2 > 2σ(F2)] = 0.019 | (Δ/σ)max = 0.043 |
wR(F2) = 0.014 | Δρmax = 0.45 e Å−3 |
S = 0.97 | Δρmin = −0.89 e Å−3 |
2727 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
37 parameters | Extinction coefficient: 390 (20) |
0 restraints | Absolute structure: 1236 of Friedel pairs used in the refinement |
2 constraints | Absolute structure parameter: 0.509 (2) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | 0 | 0 | 0 | 0.01223 (4) | 0.9457 (9) |
Bi1 | 0 | 0 | 0 | 0.01223 (4) | 0.0543 (9) |
Fe1 | 0.215770 (14) | 0.333333 | 0.333333 | 0.00782 (3) | |
O1 | 0.14409 (7) | 0.14409 (7) | 0.5 | 0.01035 (15) | |
O2 | 0.40800 (8) | 0.40800 (8) | 0.5 | 0.0194 (2) | |
O3 | 0.02456 (7) | 0.21096 (7) | 0.18123 (7) | 0.01246 (15) | |
B1 | 0 | 0 | 0.5 | 0.0075 (3) | |
B2 | 0.55141 (9) | 0.55141 (9) | 0.5 | 0.0093 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.01274 (5) | 0.01274 (5) | 0.01120 (6) | 0.00637 (3) | 0 | 0 |
Bi1 | 0.01274 (5) | 0.01274 (5) | 0.01120 (6) | 0.00637 (3) | 0 | 0 |
Fe1 | 0.00719 (3) | 0.00727 (4) | 0.00903 (4) | 0.00363 (2) | −0.000006 (17) | −0.00001 (3) |
O1 | 0.00726 (16) | 0.00726 (16) | 0.0135 (2) | 0.00135 (18) | −0.00161 (9) | 0.00161 (9) |
O2 | 0.01027 (19) | 0.01027 (19) | 0.0292 (4) | −0.0012 (2) | −0.00838 (15) | 0.00838 (15) |
O3 | 0.00921 (17) | 0.0154 (2) | 0.01366 (17) | 0.00683 (16) | −0.00254 (13) | −0.00283 (15) |
B1 | 0.0069 (3) | 0.0069 (3) | 0.0086 (5) | 0.00345 (17) | 0 | 0 |
B2 | 0.0076 (2) | 0.0076 (2) | 0.0109 (3) | 0.0025 (4) | −0.0007 (2) | 0.0007 (2) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Bi1—O3iv | 2.3492 (5) |
Y1—O3 | 2.3492 (6) | Bi1—O3v | 2.3492 (8) |
Y1—O3i | 2.3492 (5) | Fe1—O1 | 2.0215 (5) |
Y1—O3ii | 2.3492 (8) | Fe1—O1vi | 2.0215 (4) |
Y1—O3iii | 2.3492 (6) | Fe1—O2 | 2.0392 (5) |
Y1—O3iv | 2.3492 (5) | Fe1—O2vi | 2.0392 (9) |
Y1—O3v | 2.3492 (8) | Fe1—O3 | 1.9719 (5) |
Bi1—O3 | 2.3492 (6) | Fe1—O3vii | 1.9719 (8) |
Bi1—O3i | 2.3492 (5) | O1—B1 | 1.3746 (5) |
Bi1—O3ii | 2.3492 (8) | O2—B2 | 1.3681 (8) |
Bi1—O3iii | 2.3492 (6) | O3—B2viii | 1.3734 (12) |
| | | |
Bi1—Y1—O3 | 0 | O3ii—Bi1—O3v | 141.634 (17) |
Bi1—Y1—O3i | 0 | O3iii—Bi1—O3iv | 89.28 (2) |
Bi1—Y1—O3ii | 0 | O3iii—Bi1—O3v | 89.28 (2) |
Bi1—Y1—O3iii | 0 | O3iv—Bi1—O3v | 89.28 (2) |
Bi1—Y1—O3iv | 0 | O1—Fe1—O1vi | 167.57 (4) |
Bi1—Y1—O3v | 0 | O1—Fe1—O2 | 76.63 (2) |
O3—Y1—O3i | 89.28 (2) | O1—Fe1—O2vi | 94.27 (3) |
O3—Y1—O3ii | 89.28 (2) | O1—Fe1—O3 | 92.10 (2) |
O3—Y1—O3iii | 122.866 (17) | O1—Fe1—O3vii | 95.71 (2) |
O3—Y1—O3iv | 141.63 (3) | O1vi—Fe1—O2 | 94.27 (2) |
O3—Y1—O3v | 72.44 (2) | O1vi—Fe1—O2vi | 76.63 (3) |
O3i—Y1—O3ii | 89.28 (2) | O1vi—Fe1—O3 | 95.71 (2) |
O3i—Y1—O3iii | 141.63 (3) | O1vi—Fe1—O3vii | 92.10 (3) |
O3i—Y1—O3iv | 72.436 (19) | O2—Fe1—O2vi | 87.13 (3) |
O3i—Y1—O3v | 122.87 (3) | O2—Fe1—O3 | 166.59 (3) |
O3ii—Y1—O3iii | 72.44 (2) | O2—Fe1—O3vii | 86.49 (3) |
O3ii—Y1—O3iv | 122.87 (3) | O2vi—Fe1—O3 | 86.49 (3) |
O3ii—Y1—O3v | 141.634 (17) | O2vi—Fe1—O3vii | 166.59 (2) |
O3iii—Y1—O3iv | 89.28 (2) | O3—Fe1—O3vii | 102.05 (3) |
O3iii—Y1—O3v | 89.28 (2) | Fe1—O1—Fe1ix | 104.01 (2) |
O3iv—Y1—O3v | 89.28 (2) | Fe1—O1—B1 | 128.00 (3) |
Y1—Bi1—O3 | 0 | Fe1ix—O1—B1 | 128.00 (3) |
Y1—Bi1—O3i | 0 | Fe1—O2—Fe1ix | 102.74 (2) |
Y1—Bi1—O3ii | 0 | Fe1—O2—B2 | 128.63 (4) |
Y1—Bi1—O3iii | 0 | Fe1ix—O2—B2 | 128.63 (4) |
Y1—Bi1—O3iv | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O3v | 0 | Y1—O3—Fe1 | 121.02 (4) |
O3—Bi1—O3i | 89.28 (2) | Y1—O3—B2viii | 108.18 (3) |
O3—Bi1—O3ii | 89.28 (2) | Bi1—O3—Fe1 | 121.02 (4) |
O3—Bi1—O3iii | 122.866 (17) | Bi1—O3—B2viii | 108.18 (3) |
O3—Bi1—O3iv | 141.63 (3) | Fe1—O3—B2viii | 130.64 (5) |
O3—Bi1—O3v | 72.44 (2) | O1—B1—O1i | 120.00 (5) |
O3i—Bi1—O3ii | 89.28 (2) | O1—B1—O1ii | 120.00 (5) |
O3i—Bi1—O3iii | 141.63 (3) | O1i—B1—O1ii | 120.00 (5) |
O3i—Bi1—O3iv | 72.436 (19) | O2—B2—O3x | 117.44 (8) |
O3i—Bi1—O3v | 122.87 (3) | O2—B2—O3xi | 117.44 (8) |
O3ii—Bi1—O3iii | 72.44 (2) | O3x—B2—O3xi | 125.12 (5) |
O3ii—Bi1—O3iv | 122.87 (3) | | |
Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) y, x, −z; (iv) x−y, −y, −z; (v) −x, −x+y, −z; (vi) −x+y+1/3, −x+2/3, z−1/3; (vii) x−y+1/3, −y+2/3, −z+2/3; (viii) x−2/3, y−1/3, z−1/3; (ix) −y+2/3, x−y+1/3, z+1/3; (x) x+2/3, y+1/3, z+1/3; (xi) y+1/3, x+2/3, −z+2/3. |
Crystal data top
B4Bi0.05Fe3O12Y0.95 | Dx = 4.196 Mg m−3 |
Mr = 497.7 | Synchrotron radiation, λ = 0.6742 Å |
Trigonal, P3121 | Cell parameters from 4657 reflections |
Hall symbol: P 31 2" | θ = 2.4–32.0° |
a = 9.5131 (1) Å | µ = 11.67 mm−1 |
c = 7.5396 (1) Å | T = 90 K |
V = 590.91 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Multipurpose diffractometer PILATUS@SNBL | 1494 reflections with I > 3σ(I) |
Double-crystal Si(111) monochromator | Rint = 0.042 |
φ scans | θmax = 32°, θmin = 2.4° |
Absorption correction: for a sphere Jana2006 | h = −12→12 |
Tmin = 0.246, Tmax = 0.269 | k = −14→14 |
5121 measured reflections | l = −11→11 |
1505 independent reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000225F2) |
R[F2 > 2σ(F2)] = 0.022 | (Δ/σ)max = 0.048 |
wR(F2) = 0.030 | Δρmax = 0.41 e Å−3 |
S = 1.32 | Δρmin = −0.40 e Å−3 |
1505 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
97 parameters | Extinction coefficient: 420 (160) |
0 restraints | Absolute structure: 646 of Friedel pairs used in the refinement |
2 constraints | Absolute structure parameter: 0.505 (7) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | −0.334925 (10) | −0.334925 (10) | 0 | 0.00465 (15) | 0.950 (3) |
Bi1 | −0.334925 (10) | −0.334925 (10) | 0 | 0.0000 (10)* | 0.050 (3) |
Fe1 | 0.11573 (5) | 0.11573 (5) | 0 | 0.00323 (10) | |
Fe2 | −0.21222 (5) | −0.54853 (5) | 0.34475 (3) | 0.00340 (9) | |
O1 | 0 | −0.07774 (13) | 0.166667 | 0.0073 (3) | |
O2 | −0.58142 (11) | −0.27690 (10) | 0.12612 (13) | 0.0068 (3) | |
O3 | −0.1213 (2) | −0.30357 (19) | −0.1772 (2) | 0.0061 (4) | |
O4 | −0.1479 (2) | −0.36306 (19) | 0.1851 (2) | 0.0061 (4) | |
O5 | 0.4755 (2) | 0.1458 (2) | −0.15741 (11) | 0.0056 (4) | |
O6 | 0.1873 (3) | 0 | −0.166667 | 0.0055 (5) | |
O7 | −0.5246 (2) | −0.5336 (2) | −0.1851 (2) | 0.0069 (4) | |
B1 | 0.33168 (13) | 0 | −0.166667 | 0.0044 (10) | |
B2 | −0.4489 (3) | −0.1247 (3) | 0.15208 (17) | 0.0049 (5) | |
B3 | 0 | −0.2216 (3) | 0.166667 | 0.0051 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00350 (18) | 0.00350 (18) | 0.0071 (3) | 0.00184 (10) | −0.000157 (19) | 0.000157 (19) |
Fe1 | 0.00234 (12) | 0.00234 (12) | 0.00513 (15) | 0.00124 (11) | −0.00001 (5) | 0.00001 (5) |
Fe2 | 0.00233 (12) | 0.00234 (12) | 0.00556 (12) | 0.00120 (10) | 0.00013 (6) | 0.00011 (6) |
O1 | 0.0071 (5) | 0.0045 (3) | 0.0111 (5) | 0.0036 (2) | 0.0022 (4) | 0.0011 (2) |
O2 | 0.0048 (3) | 0.0043 (3) | 0.0099 (4) | 0.0011 (3) | −0.0007 (3) | 0.0009 (3) |
O3 | 0.0060 (5) | 0.0038 (4) | 0.0087 (5) | 0.0025 (4) | 0.0004 (4) | −0.0001 (4) |
O4 | 0.0046 (5) | 0.0043 (4) | 0.0085 (5) | 0.0016 (4) | −0.0005 (4) | 0.0005 (4) |
O5 | 0.0044 (5) | 0.0040 (5) | 0.0081 (5) | 0.0020 (5) | −0.0010 (3) | 0.0010 (3) |
O6 | 0.0042 (5) | 0.0040 (8) | 0.0081 (7) | 0.0020 (4) | −0.0013 (3) | −0.0026 (6) |
O7 | 0.0047 (5) | 0.0068 (5) | 0.0093 (5) | 0.0029 (4) | 0.0001 (4) | −0.0009 (4) |
B1 | 0.0048 (11) | 0.0053 (12) | 0.0033 (17) | 0.0027 (6) | 0.0004 (2) | 0.0007 (4) |
B2 | 0.0044 (6) | 0.0047 (6) | 0.0067 (5) | 0.0031 (6) | 0.0001 (5) | 0.0007 (5) |
B3 | 0.0024 (8) | 0.0059 (7) | 0.0058 (7) | 0.0012 (4) | −0.0010 (7) | −0.0005 (4) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Fe1—O3iv | 1.9618 (18) |
Y1—O3 | 2.3232 (19) | Fe1—O6 | 2.0010 (16) |
Y1—O3i | 2.3232 (19) | Fe1—O6iii | 2.0010 (16) |
Y1—O4 | 2.379 (2) | Fe2—O2v | 2.0616 (9) |
Y1—O4i | 2.379 (2) | Fe2—O2vi | 2.0345 (9) |
Y1—O7 | 2.3162 (15) | Fe2—O4 | 1.9638 (18) |
Y1—O7i | 2.3162 (15) | Fe2—O5vii | 2.023 (3) |
Bi1—O3 | 2.3232 (19) | Fe2—O5viii | 2.011 (3) |
Bi1—O3i | 2.3232 (19) | Fe2—O7ix | 1.985 (2) |
Bi1—O4 | 2.379 (2) | O1—B3 | 1.368 (3) |
Bi1—O4i | 2.379 (2) | O2—B2 | 1.378 (2) |
Bi1—O7 | 2.3162 (15) | O3—B2i | 1.379 (4) |
Bi1—O7i | 2.3162 (15) | O4—B3 | 1.385 (2) |
Fe1—O1 | 2.0377 (9) | O5—B1 | 1.3799 (18) |
Fe1—O1ii | 2.0377 (9) | O6—B1 | 1.374 (3) |
Fe1—O3iii | 1.9618 (18) | O7—B2x | 1.364 (4) |
| | | |
Bi1—Y1—O3 | 0 | O6—Fe1—O6iii | 167.94 (6) |
Bi1—Y1—O3i | 0 | O2v—Fe2—O2vi | 86.30 (4) |
Bi1—Y1—O4 | 0 | O2v—Fe2—O4 | 168.09 (8) |
Bi1—Y1—O4i | 0 | O2v—Fe2—O5vii | 96.80 (8) |
Bi1—Y1—O7 | 0 | O2v—Fe2—O5viii | 75.53 (7) |
Bi1—Y1—O7i | 0 | O2v—Fe2—O7ix | 81.83 (6) |
O3—Y1—O3i | 119.79 (5) | O2vi—Fe2—O4 | 93.73 (6) |
O3—Y1—O4 | 72.33 (6) | O2vi—Fe2—O5vii | 75.88 (7) |
O3—Y1—O4i | 89.13 (7) | O2vi—Fe2—O5viii | 92.27 (8) |
O3—Y1—O7 | 91.88 (6) | O2vi—Fe2—O7ix | 160.34 (9) |
O3—Y1—O7i | 140.11 (8) | O4—Fe2—O5vii | 94.74 (9) |
O3i—Y1—O4 | 89.13 (7) | O4—Fe2—O5viii | 92.58 (9) |
O3i—Y1—O4i | 72.33 (6) | O4—Fe2—O7ix | 101.10 (7) |
O3i—Y1—O7 | 140.11 (8) | O5vii—Fe2—O5viii | 166.43 (8) |
O3i—Y1—O7i | 91.88 (6) | O5vii—Fe2—O7ix | 89.98 (9) |
O4—Y1—O4i | 142.96 (5) | O5viii—Fe2—O7ix | 99.80 (10) |
O4—Y1—O7 | 125.64 (7) | Fe1—O1—Fe1iii | 101.45 (6) |
O4—Y1—O7i | 85.64 (6) | Fe1—O1—B3 | 129.28 (3) |
O4i—Y1—O7 | 85.64 (6) | Fe1iii—O1—B3 | 129.28 (3) |
O4i—Y1—O7i | 125.64 (7) | Fe2xi—O2—Fe2xii | 102.49 (4) |
O7—Y1—O7i | 74.21 (6) | Fe2xi—O2—B2 | 121.60 (9) |
Y1—Bi1—O3 | 0 | Fe2xii—O2—B2 | 127.82 (14) |
Y1—Bi1—O3i | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O4 | 0 | Y1—O3—Fe1ii | 122.71 (11) |
Y1—Bi1—O4i | 0 | Y1—O3—B2i | 102.21 (12) |
Y1—Bi1—O7 | 0 | Bi1—O3—Fe1ii | 122.71 (11) |
Y1—Bi1—O7i | 0 | Bi1—O3—B2i | 102.21 (12) |
O3—Bi1—O3i | 119.79 (5) | Fe1ii—O3—B2i | 134.72 (15) |
O3—Bi1—O4 | 72.33 (6) | Y1—O4—Bi1 | 0.0 (5) |
O3—Bi1—O4i | 89.13 (7) | Y1—O4—Fe2 | 123.10 (8) |
O3—Bi1—O7 | 91.88 (6) | Y1—O4—B3 | 106.59 (13) |
O3—Bi1—O7i | 140.11 (8) | Bi1—O4—Fe2 | 123.10 (8) |
O3i—Bi1—O4 | 89.13 (7) | Bi1—O4—B3 | 106.59 (13) |
O3i—Bi1—O4i | 72.33 (6) | Fe2—O4—B3 | 130.05 (15) |
O3i—Bi1—O7 | 140.11 (8) | Fe2xiii—O5—Fe2xiv | 104.70 (8) |
O3i—Bi1—O7i | 91.88 (6) | Fe2xiii—O5—B1 | 126.63 (12) |
O4—Bi1—O4i | 142.96 (5) | Fe2xiv—O5—B1 | 128.58 (13) |
O4—Bi1—O7 | 125.64 (7) | Fe1—O6—Fe1ii | 104.06 (11) |
O4—Bi1—O7i | 85.64 (6) | Fe1—O6—B1 | 127.97 (6) |
O4i—Bi1—O7 | 85.64 (6) | Fe1ii—O6—B1 | 127.97 (6) |
O4i—Bi1—O7i | 125.64 (7) | Y1—O7—Bi1 | 0.0 (5) |
O7—Bi1—O7i | 74.21 (6) | Y1—O7—Fe2xv | 116.70 (10) |
O1—Fe1—O1ii | 87.600 (14) | Y1—O7—B2x | 115.50 (14) |
O1—Fe1—O3iii | 85.12 (6) | Bi1—O7—Fe2xv | 116.70 (10) |
O1—Fe1—O3iv | 167.24 (9) | Bi1—O7—B2x | 115.50 (14) |
O1—Fe1—O6 | 93.96 (4) | Fe2xv—O7—B2x | 127.75 (13) |
O1—Fe1—O6iii | 77.25 (6) | O5—B1—O5iv | 121.43 (19) |
O1ii—Fe1—O3iii | 167.24 (9) | O5—B1—O6 | 119.28 (13) |
O1ii—Fe1—O3iv | 85.12 (6) | O5iv—B1—O6 | 119.28 (13) |
O1ii—Fe1—O6 | 77.25 (6) | O2—B2—O3i | 115.1 (2) |
O1ii—Fe1—O6iii | 93.96 (4) | O2—B2—O7xvi | 120.2 (2) |
O3iii—Fe1—O3iv | 103.84 (9) | O3i—B2—O7xvi | 124.68 (17) |
O3iii—Fe1—O6 | 92.80 (9) | O1—B3—O4 | 117.63 (15) |
O3iii—Fe1—O6iii | 94.63 (7) | O1—B3—O4xvii | 117.63 (15) |
O3iv—Fe1—O6 | 94.63 (7) | O4—B3—O4xvii | 124.7 (3) |
O3iv—Fe1—O6iii | 92.80 (9) | | |
Symmetry codes: (i) y, x, −z; (ii) −x+y, −x, z−1/3; (iii) −y, x−y, z+1/3; (iv) x−y, −y, −z−1/3; (v) x−y, −y−1, −z+2/3; (vi) −x−1, −x+y−1, −z+1/3; (vii) −y, x−y−1, z+1/3; (viii) −x+y, −x, z+2/3; (ix) −x+y, −x−1, z+2/3; (x) −x+y−1, −x−1, z−1/3; (xi) x−y−1, −y−1, −z+2/3; (xii) −x−1, −x+y, −z+1/3; (xiii) −y, x−y, z−2/3; (xiv) −x+y+1, −x, z−1/3; (xv) −y−1, x−y−1, z−2/3; (xvi) −y−1, x−y, z+1/3; (xvii) −x, −x+y, −z+1/3. |
Crystal data top
B4Bi0.058Fe3O12Y0.942 | Dx = 4.188 Mg m−3 |
Mr = 498.6 | Synchrotron radiation, λ = 0.6742 Å |
Trigonal, P3121 | Cell parameters from 4313 reflections |
Hall symbol: P 31 2" | θ = 3.5–32.1° |
a = 9.5217 (1) Å | µ = 11.72 mm−1 |
c = 7.5547 (1) Å | T = 295 K |
V = 593.17 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Multipurpose diffractometer PILATUS@SNBL | 1496 reflections with I > 3σ(I) |
Double-crystal Si(111) monochromator | Rint = 0.016 |
φ scans | θmax = 32.1°, θmin = 2.3° |
Absorption correction: for a sphere Jana2006 | h = −14→14 |
Tmin = 0.247, Tmax = 0.270 | k = −12→12 |
5271 measured reflections | l = −11→11 |
1512 independent reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000225F2) |
R[F2 > 2σ(F2)] = 0.013 | (Δ/σ)max = 0.047 |
wR(F2) = 0.021 | Δρmax = 0.28 e Å−3 |
S = 1.10 | Δρmin = −0.35 e Å−3 |
1512 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
97 parameters | Extinction coefficient: 280 (110) |
0 restraints | Absolute structure: 649 of Friedel pairs used in the refinement |
2 constraints | Absolute structure parameter: 0.504 (5) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | −0.334151 (6) | −0.334151 (6) | 0 | 0.00990 (16) | 0.942 (3) |
Bi1 | −0.334151 (6) | −0.334151 (6) | 0 | 0.0000 (6)* | 0.058 (3) |
Fe1 | 0.11595 (3) | 0.11595 (3) | 0 | 0.00586 (7) | |
Fe2 | −0.21292 (3) | −0.54877 (3) | 0.342846 (18) | 0.00602 (6) | |
O1 | 0 | −0.07737 (10) | 0.166667 | 0.0121 (2) | |
O2 | −0.58296 (8) | −0.27365 (8) | 0.13276 (9) | 0.01180 (19) | |
O3 | −0.12122 (14) | −0.30446 (14) | −0.17833 (15) | 0.0098 (3) | |
O4 | −0.14758 (15) | −0.36213 (14) | 0.18430 (15) | 0.0095 (3) | |
O5 | 0.47538 (15) | 0.14533 (15) | −0.15873 (7) | 0.0088 (3) | |
O6 | 0.18770 (16) | 0 | −0.166667 | 0.0088 (4) | |
O7 | −0.52353 (15) | −0.53550 (14) | −0.18444 (15) | 0.0102 (3) | |
B1 | 0.33185 (8) | 0 | −0.166667 | 0.0056 (6) | |
B2 | −0.44852 (19) | −0.12273 (19) | 0.15441 (11) | 0.0075 (3) | |
B3 | 0 | −0.2213 (2) | 0.166667 | 0.0073 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.0095 (2) | 0.0095 (2) | 0.0110 (2) | 0.00490 (10) | −0.000330 (12) | 0.000330 (12) |
Fe1 | 0.00527 (8) | 0.00527 (8) | 0.00714 (9) | 0.00270 (7) | −0.00005 (3) | 0.00005 (3) |
Fe2 | 0.00529 (8) | 0.00522 (8) | 0.00750 (8) | 0.00259 (6) | 0.00011 (4) | 0.00008 (4) |
O1 | 0.0135 (4) | 0.0077 (2) | 0.0170 (3) | 0.00674 (18) | 0.0062 (3) | 0.00310 (13) |
O2 | 0.0082 (2) | 0.0072 (2) | 0.0166 (2) | 0.0013 (2) | −0.0032 (2) | 0.0026 (2) |
O3 | 0.0119 (4) | 0.0066 (3) | 0.0114 (3) | 0.0048 (3) | 0.0019 (3) | 0.0012 (2) |
O4 | 0.0081 (3) | 0.0071 (3) | 0.0106 (3) | 0.0018 (3) | −0.0010 (3) | 0.0009 (2) |
O5 | 0.0057 (3) | 0.0060 (4) | 0.0117 (4) | 0.0007 (4) | −0.0013 (2) | 0.0012 (2) |
O6 | 0.0059 (4) | 0.0103 (6) | 0.0117 (5) | 0.0052 (3) | −0.00147 (19) | −0.0029 (4) |
O7 | 0.0085 (3) | 0.0127 (4) | 0.0113 (3) | 0.0068 (3) | −0.0008 (2) | −0.0020 (3) |
B1 | 0.0049 (7) | 0.0052 (7) | 0.0067 (11) | 0.0026 (4) | 0.00005 (13) | 0.0001 (3) |
B2 | 0.0061 (4) | 0.0070 (4) | 0.0093 (4) | 0.0033 (4) | 0.0000 (3) | 0.0008 (3) |
B3 | 0.0056 (5) | 0.0072 (4) | 0.0085 (5) | 0.0028 (3) | 0.0001 (5) | 0.0001 (2) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Fe1—O3iv | 1.9631 (12) |
Y1—O3 | 2.3308 (13) | Fe1—O6 | 2.0063 (10) |
Y1—O3i | 2.3308 (13) | Fe1—O6iii | 2.0063 (10) |
Y1—O4 | 2.3746 (15) | Fe2—O2v | 2.0574 (7) |
Y1—O4i | 2.3746 (15) | Fe2—O2vi | 2.0329 (7) |
Y1—O7 | 2.3263 (10) | Fe2—O4 | 1.9683 (12) |
Y1—O7i | 2.3263 (10) | Fe2—O5vii | 2.0257 (18) |
Bi1—O3 | 2.3308 (13) | Fe2—O5viii | 2.0167 (18) |
Bi1—O3i | 2.3308 (13) | Fe2—O7ix | 1.9815 (17) |
Bi1—O4 | 2.3746 (15) | O1—B3 | 1.371 (2) |
Bi1—O4i | 2.3746 (15) | O2—B2 | 1.3750 (14) |
Bi1—O7 | 2.3263 (10) | O3—B2i | 1.376 (2) |
Bi1—O7i | 2.3263 (10) | O4—B3 | 1.3805 (13) |
Fe1—O1 | 2.0397 (6) | O5—B1 | 1.3766 (11) |
Fe1—O1ii | 2.0397 (6) | O6—B1 | 1.3726 (17) |
Fe1—O3iii | 1.9631 (12) | O7—B2x | 1.366 (3) |
| | | |
Bi1—Y1—O3 | 0 | O6—Fe1—O6iii | 167.96 (4) |
Bi1—Y1—O3i | 0 | O2v—Fe2—O2vi | 86.52 (3) |
Bi1—Y1—O4 | 0 | O2v—Fe2—O4 | 168.14 (6) |
Bi1—Y1—O4i | 0 | O2v—Fe2—O5vii | 96.33 (5) |
Bi1—Y1—O7 | 0 | O2v—Fe2—O5viii | 75.77 (5) |
Bi1—Y1—O7i | 0 | O2v—Fe2—O7ix | 82.48 (4) |
O3—Y1—O3i | 120.58 (4) | O2vi—Fe2—O4 | 92.52 (4) |
O3—Y1—O4 | 72.44 (4) | O2vi—Fe2—O5vii | 76.12 (4) |
O3—Y1—O4i | 89.23 (5) | O2vi—Fe2—O5viii | 92.68 (5) |
O3—Y1—O7 | 91.29 (4) | O2vi—Fe2—O7ix | 161.46 (6) |
O3—Y1—O7i | 140.36 (5) | O4—Fe2—O5vii | 94.90 (6) |
O3i—Y1—O4 | 89.23 (5) | O4—Fe2—O5viii | 92.49 (6) |
O3i—Y1—O4i | 72.44 (4) | O4—Fe2—O7ix | 101.26 (5) |
O3i—Y1—O7 | 140.36 (5) | O5vii—Fe2—O5viii | 166.81 (5) |
O3i—Y1—O7i | 91.29 (4) | O5vii—Fe2—O7ix | 90.27 (6) |
O4—Y1—O4i | 142.92 (3) | O5viii—Fe2—O7ix | 98.99 (6) |
O4—Y1—O7 | 125.02 (5) | Fe1—O1—Fe1iii | 101.63 (4) |
O4—Y1—O7i | 86.25 (4) | Fe1—O1—B3 | 129.18 (2) |
O4i—Y1—O7 | 86.25 (4) | Fe1iii—O1—B3 | 129.18 (2) |
O4i—Y1—O7i | 125.02 (5) | Fe2xi—O2—Fe2xii | 102.70 (3) |
O7—Y1—O7i | 73.81 (4) | Fe2xi—O2—B2 | 123.12 (7) |
Y1—Bi1—O3 | 0 | Fe2xii—O2—B2 | 128.48 (10) |
Y1—Bi1—O3i | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O4 | 0 | Y1—O3—Fe1ii | 122.26 (8) |
Y1—Bi1—O4i | 0 | Y1—O3—B2i | 103.19 (8) |
Y1—Bi1—O7 | 0 | Bi1—O3—Fe1ii | 122.26 (8) |
Y1—Bi1—O7i | 0 | Bi1—O3—B2i | 103.19 (8) |
O3—Bi1—O3i | 120.58 (4) | Fe1ii—O3—B2i | 134.26 (11) |
O3—Bi1—O4 | 72.44 (4) | Y1—O4—Bi1 | 0.0 (5) |
O3—Bi1—O4i | 89.23 (5) | Y1—O4—Fe2 | 122.80 (5) |
O3—Bi1—O7 | 91.29 (4) | Y1—O4—B3 | 106.85 (9) |
O3—Bi1—O7i | 140.36 (5) | Bi1—O4—Fe2 | 122.80 (5) |
O3i—Bi1—O4 | 89.23 (5) | Bi1—O4—B3 | 106.85 (9) |
O3i—Bi1—O4i | 72.44 (4) | Fe2—O4—B3 | 130.11 (10) |
O3i—Bi1—O7 | 140.36 (5) | Fe2xiii—O5—Fe2xiv | 104.42 (5) |
O3i—Bi1—O7i | 91.29 (4) | Fe2xiii—O5—B1 | 126.91 (7) |
O4—Bi1—O4i | 142.92 (3) | Fe2xiv—O5—B1 | 128.60 (8) |
O4—Bi1—O7 | 125.02 (5) | Fe1—O6—Fe1ii | 104.00 (7) |
O4—Bi1—O7i | 86.25 (4) | Fe1—O6—B1 | 128.00 (3) |
O4i—Bi1—O7 | 86.25 (4) | Fe1ii—O6—B1 | 128.00 (4) |
O4i—Bi1—O7i | 125.02 (5) | Y1—O7—Bi1 | 0.0 (5) |
O7—Bi1—O7i | 73.81 (4) | Y1—O7—Fe2xv | 117.52 (7) |
O1—Fe1—O1ii | 87.584 (9) | Y1—O7—B2x | 114.32 (10) |
O1—Fe1—O3iii | 85.43 (4) | Bi1—O7—Fe2xv | 117.52 (7) |
O1—Fe1—O3iv | 167.25 (6) | Bi1—O7—B2x | 114.32 (10) |
O1—Fe1—O6 | 94.04 (3) | Fe2xv—O7—B2x | 128.15 (9) |
O1—Fe1—O6iii | 77.18 (4) | O5—B1—O5iv | 121.30 (12) |
O1ii—Fe1—O3iii | 167.25 (6) | O5—B1—O6 | 119.35 (8) |
O1ii—Fe1—O3iv | 85.43 (4) | O5iv—B1—O6 | 119.35 (8) |
O1ii—Fe1—O6 | 77.18 (4) | O2—B2—O3i | 115.39 (16) |
O1ii—Fe1—O6iii | 94.04 (3) | O2—B2—O7xvi | 119.68 (15) |
O3iii—Fe1—O3iv | 103.31 (6) | O3i—B2—O7xvi | 124.93 (12) |
O3iii—Fe1—O6 | 92.67 (6) | O1—B3—O4 | 117.52 (10) |
O3iii—Fe1—O6iii | 94.79 (5) | O1—B3—O4xvii | 117.52 (10) |
O3iv—Fe1—O6 | 94.79 (5) | O4—B3—O4xvii | 124.95 (17) |
O3iv—Fe1—O6iii | 92.67 (6) | | |
Symmetry codes: (i) y, x, −z; (ii) −x+y, −x, z−1/3; (iii) −y, x−y, z+1/3; (iv) x−y, −y, −z−1/3; (v) x−y, −y−1, −z+2/3; (vi) −x−1, −x+y−1, −z+1/3; (vii) −y, x−y−1, z+1/3; (viii) −x+y, −x, z+2/3; (ix) −x+y, −x−1, z+2/3; (x) −x+y−1, −x−1, z−1/3; (xi) x−y−1, −y−1, −z+2/3; (xii) −x−1, −x+y, −z+1/3; (xiii) −y, x−y, z−2/3; (xiv) −x+y+1, −x, z−1/3; (xv) −y−1, x−y−1, z−2/3; (xvi) −y−1, x−y, z+1/3; (xvii) −x, −x+y, −z+1/3. |
Crystal data top
B4Bi0.047Fe3O12Y0.953 | Dx = 4.168 Mg m−3 |
Mr = 497.3 | Synchrotron radiation, λ = 0.6742 Å |
Trigonal, R32 | Cell parameters from 1599 reflections |
Hall symbol: R 3 2" | θ = 3.5–31.9° |
a = 9.5282 (1) Å | µ = 11.56 mm−1 |
c = 7.5609 (1) Å | T = 380 K |
V = 594.46 (1) Å3 | Sphere, light-green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Multipurpose diffractometer PILATUS@SNBL | 508 reflections with I > 3σ(I) |
Double-crystal Si(111) monochromator | Rint = 0.015 |
φ scans | θmax = 31.9°, θmin = 3.5° |
Absorption correction: for a sphere Jana2006 | h = −14→14 |
Tmin = 0.214, Tmax = 0.240 | k = −13→13 |
1747 measured reflections | l = −11→11 |
508 independent reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000225F2) |
R[F2 > 2σ(F2)] = 0.012 | (Δ/σ)max = 0.048 |
wR(F2) = 0.017 | Δρmax = 0.27 e Å−3 |
S = 1.09 | Δρmin = −0.25 e Å−3 |
508 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
37 parameters | Extinction coefficient: 340 (130) |
0 restraints | Absolute structure: 218 of Friedel pairs used in the refinement |
2 constraints | Absolute structure parameter: 0.504 (6) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | 0 | 0 | 0 | 0.01075 (8) | 0.953 (3) |
Bi1 | 0 | 0 | 0 | 0.01075 (8) | 0.047 (3) |
Fe1 | 0.21577 (3) | 0.333333 | 0.333333 | 0.00807 (11) | |
O1 | 0.14417 (15) | 0.14417 (15) | 0.5 | 0.0100 (4) | |
O2 | 0.40767 (19) | 0.40767 (19) | 0.5 | 0.0193 (5) | |
O3 | 0.02451 (14) | 0.21076 (14) | 0.18101 (15) | 0.0121 (4) | |
B1 | 0 | 0 | 0.5 | 0.0092 (7) | |
B2 | 0.5513 (2) | 0.5513 (2) | 0.5 | 0.0097 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.01149 (10) | 0.01149 (10) | 0.00928 (13) | 0.00574 (5) | 0 | 0 |
Bi1 | 0.01149 (10) | 0.01149 (10) | 0.00928 (13) | 0.00574 (5) | 0 | 0 |
Fe1 | 0.00776 (14) | 0.00776 (14) | 0.00868 (17) | 0.00388 (7) | 0.00001 (3) | 0.00002 (6) |
O1 | 0.0082 (4) | 0.0082 (4) | 0.0109 (5) | 0.0022 (4) | −0.0013 (2) | 0.0013 (2) |
O2 | 0.0117 (5) | 0.0117 (5) | 0.0274 (9) | 0.0006 (6) | −0.0079 (3) | 0.0079 (3) |
O3 | 0.0099 (4) | 0.0159 (5) | 0.0114 (4) | 0.0072 (4) | −0.0022 (3) | −0.0032 (4) |
B1 | 0.0099 (8) | 0.0099 (8) | 0.0078 (12) | 0.0049 (4) | 0 | 0 |
B2 | 0.0084 (6) | 0.0084 (6) | 0.0109 (7) | 0.0031 (7) | −0.0014 (3) | 0.0014 (3) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Bi1—O3iv | 2.3433 (11) |
Y1—O3 | 2.3433 (13) | Bi1—O3v | 2.3433 (18) |
Y1—O3i | 2.3433 (11) | Fe1—O1 | 2.0180 (10) |
Y1—O3ii | 2.3433 (18) | Fe1—O1vi | 2.0180 (9) |
Y1—O3iii | 2.3433 (13) | Fe1—O2 | 2.0341 (14) |
Y1—O3iv | 2.3433 (11) | Fe1—O2vi | 2.034 (2) |
Y1—O3v | 2.3433 (18) | Fe1—O3 | 1.9706 (11) |
Bi1—O3 | 2.3433 (13) | Fe1—O3vii | 1.9706 (17) |
Bi1—O3i | 2.3433 (11) | O1—B1 | 1.3737 (10) |
Bi1—O3ii | 2.3433 (18) | O2—B2 | 1.3690 (19) |
Bi1—O3iii | 2.3433 (13) | O3—B2viii | 1.372 (3) |
| | | |
Bi1—Y1—O3 | 0 | O3ii—Bi1—O3v | 141.61 (4) |
Bi1—Y1—O3i | 0 | O3iii—Bi1—O3iv | 89.33 (5) |
Bi1—Y1—O3ii | 0 | O3iii—Bi1—O3v | 89.33 (5) |
Bi1—Y1—O3iii | 0 | O3iv—Bi1—O3v | 89.33 (5) |
Bi1—Y1—O3iv | 0 | O1—Fe1—O1vi | 167.54 (8) |
Bi1—Y1—O3v | 0 | O1—Fe1—O2 | 76.57 (5) |
O3—Y1—O3i | 89.33 (5) | O1—Fe1—O2vi | 94.30 (6) |
O3—Y1—O3ii | 89.33 (5) | O1—Fe1—O3 | 92.07 (4) |
O3—Y1—O3iii | 122.85 (4) | O1—Fe1—O3vii | 95.75 (5) |
O3—Y1—O3iv | 141.61 (6) | O1vi—Fe1—O2 | 94.30 (5) |
O3—Y1—O3v | 72.37 (5) | O1vi—Fe1—O2vi | 76.57 (7) |
O3i—Y1—O3ii | 89.33 (5) | O1vi—Fe1—O3 | 95.75 (5) |
O3i—Y1—O3iii | 141.61 (6) | O1vi—Fe1—O3vii | 92.07 (6) |
O3i—Y1—O3iv | 72.37 (4) | O2—Fe1—O2vi | 87.10 (7) |
O3i—Y1—O3v | 122.85 (6) | O2—Fe1—O3 | 166.49 (7) |
O3ii—Y1—O3iii | 72.37 (5) | O2—Fe1—O3vii | 86.48 (7) |
O3ii—Y1—O3iv | 122.85 (6) | O2vi—Fe1—O3 | 86.48 (7) |
O3ii—Y1—O3v | 141.61 (4) | O2vi—Fe1—O3vii | 166.49 (5) |
O3iii—Y1—O3iv | 89.33 (5) | O3—Fe1—O3vii | 102.13 (7) |
O3iii—Y1—O3v | 89.33 (5) | Fe1—O1—Fe1ix | 104.01 (5) |
O3iv—Y1—O3v | 89.33 (5) | Fe1—O1—B1 | 128.00 (7) |
Y1—Bi1—O3 | 0 | Fe1ix—O1—B1 | 128.00 (7) |
Y1—Bi1—O3i | 0 | Fe1—O2—Fe1ix | 102.85 (6) |
Y1—Bi1—O3ii | 0 | Fe1—O2—B2 | 128.57 (10) |
Y1—Bi1—O3iii | 0 | Fe1ix—O2—B2 | 128.57 (10) |
Y1—Bi1—O3iv | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O3v | 0 | Y1—O3—Fe1 | 121.04 (8) |
O3—Bi1—O3i | 89.33 (5) | Y1—O3—B2viii | 108.28 (8) |
O3—Bi1—O3ii | 89.33 (5) | Bi1—O3—Fe1 | 121.04 (8) |
O3—Bi1—O3iii | 122.85 (4) | Bi1—O3—B2viii | 108.28 (8) |
O3—Bi1—O3iv | 141.61 (6) | Fe1—O3—B2viii | 130.52 (10) |
O3—Bi1—O3v | 72.37 (5) | O1—B1—O1i | 120.00 (10) |
O3i—Bi1—O3ii | 89.33 (5) | O1—B1—O1ii | 120.00 (10) |
O3i—Bi1—O3iii | 141.61 (6) | O1i—B1—O1ii | 120.00 (10) |
O3i—Bi1—O3iv | 72.37 (4) | O2—B2—O3x | 117.40 (18) |
O3i—Bi1—O3v | 122.85 (6) | O2—B2—O3xi | 117.40 (18) |
O3ii—Bi1—O3iii | 72.37 (5) | O3x—B2—O3xi | 125.20 (12) |
O3ii—Bi1—O3iv | 122.85 (6) | | |
Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) y, x, −z; (iv) x−y, −y, −z; (v) −x, −x+y, −z; (vi) −x+y+1/3, −x+2/3, z−1/3; (vii) x−y+1/3, −y+2/3, −z+2/3; (viii) x−2/3, y−1/3, z−1/3; (ix) −y+2/3, x−y+1/3, z+1/3; (x) x+2/3, y+1/3, z+1/3; (xi) y+1/3, x+2/3, −z+2/3. |
Crystal data top
B4Bi0.042Fe3O12Y0.958 | Dx = 4.161 Mg m−3 |
Mr = 496.7 | Synchrotron radiation, λ = 0.6742 Å |
Trigonal, R32 | Cell parameters from 1242 reflections |
Hall symbol: R 3 2" | θ = 3.5–32.1° |
a = 9.5254 (1) Å | µ = 11.49 mm−1 |
c = 7.5674 (1) Å | T = 500 K |
V = 594.63 (1) Å3 | Sphere, light green |
Z = 3 | 0.09 mm (radius) |
F(000) = 706 | |
Data collection top
Multipurpose diffractometer PILATUS@SNBL | 510 reflections with I > 3σ(I) |
Double-crystal Si(111) monochromator | Rint = 0.012 |
φ scans | θmax = 32.1°, θmin = 3.5° |
Absorption correction: for a sphere Jana2006 | h = −13→13 |
Tmin = 0.248, Tmax = 0.271 | k = −12→12 |
1759 measured reflections | l = −11→11 |
510 independent reflections | |
Refinement top
Refinement on F | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.000225F2) |
R[F2 > 2σ(F2)] = 0.010 | (Δ/σ)max = 0.050 |
wR(F2) = 0.016 | Δρmax = 0.15 e Å−3 |
S = 1.03 | Δρmin = −0.15 e Å−3 |
510 reflections | Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974) |
37 parameters | Extinction coefficient: 400 (120) |
0 restraints | Absolute structure: 218 of Friedel pairs used in the refinement |
2 constraints | Absolute structure parameter: 0.508 (5) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Y1 | 0 | 0 | 0 | 0.01299 (8) | 0.958 (3) |
Bi1 | 0 | 0 | 0 | 0.01299 (8) | 0.042 (3) |
Fe1 | 0.21571 (3) | 0.333333 | 0.333333 | 0.00936 (10) | |
O1 | 0.14402 (13) | 0.14402 (13) | 0.5 | 0.0115 (3) | |
O2 | 0.40810 (17) | 0.40810 (17) | 0.5 | 0.0201 (5) | |
O3 | 0.02463 (13) | 0.21113 (13) | 0.18111 (14) | 0.0143 (3) | |
B1 | 0 | 0 | 0.5 | 0.0092 (6) | |
B2 | 0.55116 (18) | 0.55116 (18) | 0.5 | 0.0104 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.01345 (10) | 0.01345 (10) | 0.01207 (12) | 0.00673 (5) | 0 | 0 |
Bi1 | 0.01345 (10) | 0.01345 (10) | 0.01207 (12) | 0.00673 (5) | 0 | 0 |
Fe1 | 0.00885 (13) | 0.00894 (13) | 0.01034 (16) | 0.00447 (7) | −0.00004 (3) | −0.00008 (6) |
O1 | 0.0092 (4) | 0.0092 (4) | 0.0138 (5) | 0.0028 (4) | −0.0017 (2) | 0.0017 (2) |
O2 | 0.0123 (4) | 0.0123 (4) | 0.0282 (8) | 0.0006 (6) | −0.0079 (3) | 0.0079 (3) |
O3 | 0.0112 (4) | 0.0178 (5) | 0.0147 (4) | 0.0078 (3) | −0.0029 (3) | −0.0035 (3) |
B1 | 0.0095 (7) | 0.0095 (7) | 0.0087 (11) | 0.0047 (4) | 0 | 0 |
B2 | 0.0090 (5) | 0.0090 (5) | 0.0118 (7) | 0.0034 (6) | −0.0011 (3) | 0.0011 (3) |
Geometric parameters (Å, º) top
Y1—Bi1 | 0 | Bi1—O3iv | 2.3465 (10) |
Y1—O3 | 2.3465 (12) | Bi1—O3v | 2.3465 (17) |
Y1—O3i | 2.3465 (10) | Fe1—O1 | 2.0193 (9) |
Y1—O3ii | 2.3465 (17) | Fe1—O1vi | 2.0193 (8) |
Y1—O3iii | 2.3465 (12) | Fe1—O2 | 2.0374 (12) |
Y1—O3iv | 2.3465 (10) | Fe1—O2vi | 2.037 (2) |
Y1—O3v | 2.3465 (17) | Fe1—O3 | 1.9688 (10) |
Bi1—O3 | 2.3465 (12) | Fe1—O3vii | 1.9688 (16) |
Bi1—O3i | 2.3465 (10) | O1—B1 | 1.3718 (9) |
Bi1—O3ii | 2.3465 (17) | O2—B2 | 1.3628 (17) |
Bi1—O3iii | 2.3465 (12) | O3—B2viii | 1.372 (2) |
| | | |
Bi1—Y1—O3 | 0 | O3ii—Bi1—O3v | 141.64 (3) |
Bi1—Y1—O3i | 0 | O3iii—Bi1—O3iv | 89.33 (5) |
Bi1—Y1—O3ii | 0 | O3iii—Bi1—O3v | 89.33 (5) |
Bi1—Y1—O3iii | 0 | O3iv—Bi1—O3v | 89.33 (5) |
Bi1—Y1—O3iv | 0 | O1—Fe1—O1vi | 167.56 (7) |
Bi1—Y1—O3v | 0 | O1—Fe1—O2 | 76.64 (4) |
O3—Y1—O3i | 89.33 (5) | O1—Fe1—O2vi | 94.25 (5) |
O3—Y1—O3ii | 89.33 (5) | O1—Fe1—O3 | 92.15 (4) |
O3—Y1—O3iii | 122.82 (4) | O1—Fe1—O3vii | 95.66 (5) |
O3—Y1—O3iv | 141.64 (6) | O1vi—Fe1—O2 | 94.24 (5) |
O3—Y1—O3v | 72.38 (5) | O1vi—Fe1—O2vi | 76.64 (6) |
O3i—Y1—O3ii | 89.33 (5) | O1vi—Fe1—O3 | 95.66 (4) |
O3i—Y1—O3iii | 141.64 (6) | O1vi—Fe1—O3vii | 92.15 (5) |
O3i—Y1—O3iv | 72.38 (4) | O2—Fe1—O2vi | 87.11 (6) |
O3i—Y1—O3v | 122.82 (5) | O2—Fe1—O3 | 166.64 (6) |
O3ii—Y1—O3iii | 72.38 (5) | O2—Fe1—O3vii | 86.48 (6) |
O3ii—Y1—O3iv | 122.82 (5) | O2vi—Fe1—O3 | 86.48 (6) |
O3ii—Y1—O3v | 141.64 (3) | O2vi—Fe1—O3vii | 166.64 (5) |
O3iii—Y1—O3iv | 89.33 (5) | O3—Fe1—O3vii | 102.07 (6) |
O3iii—Y1—O3v | 89.33 (5) | Fe1—O1—Fe1ix | 104.01 (4) |
O3iv—Y1—O3v | 89.33 (5) | Fe1—O1—B1 | 128.00 (6) |
Y1—Bi1—O3 | 0 | Fe1ix—O1—B1 | 128.00 (6) |
Y1—Bi1—O3i | 0 | Fe1—O2—Fe1ix | 102.71 (5) |
Y1—Bi1—O3ii | 0 | Fe1—O2—B2 | 128.64 (9) |
Y1—Bi1—O3iii | 0 | Fe1ix—O2—B2 | 128.64 (9) |
Y1—Bi1—O3iv | 0 | Y1—O3—Bi1 | 0.0 (5) |
Y1—Bi1—O3v | 0 | Y1—O3—Fe1 | 121.01 (7) |
O3—Bi1—O3i | 89.33 (5) | Y1—O3—B2viii | 108.10 (7) |
O3—Bi1—O3ii | 89.33 (5) | Bi1—O3—Fe1 | 121.01 (7) |
O3—Bi1—O3iii | 122.82 (4) | Bi1—O3—B2viii | 108.10 (7) |
O3—Bi1—O3iv | 141.64 (6) | Fe1—O3—B2viii | 130.72 (9) |
O3—Bi1—O3v | 72.38 (5) | O1—B1—O1i | 120.00 (9) |
O3i—Bi1—O3ii | 89.33 (5) | O1—B1—O1ii | 120.00 (9) |
O3i—Bi1—O3iii | 141.64 (6) | O1i—B1—O1ii | 120.00 (9) |
O3i—Bi1—O3iv | 72.38 (4) | O2—B2—O3x | 117.59 (16) |
O3i—Bi1—O3v | 122.82 (5) | O2—B2—O3xi | 117.59 (16) |
O3ii—Bi1—O3iii | 72.38 (5) | O3x—B2—O3xi | 124.82 (11) |
O3ii—Bi1—O3iv | 122.82 (5) | | |
Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) y, x, −z; (iv) x−y, −y, −z; (v) −x, −x+y, −z; (vi) −x+y+1/3, −x+2/3, z−1/3; (vii) x−y+1/3, −y+2/3, −z+2/3; (viii) x−2/3, y−1/3, z−1/3; (ix) −y+2/3, x−y+1/3, z+1/3; (x) x+2/3, y+1/3, z+1/3; (xi) y+1/3, x+2/3, −z+2/3. |