Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0021889813015756/nb5067sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0021889813015756/nb5067sup2.hkl | |
Chemical Markup Language (CML) file https://doi.org/10.1107/S0021889813015756/nb5067sup3.cml |
Data collection: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40); cell refinement: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40); data reduction: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) in WinGX v1.80.05 (Farrugia, 1999).
B3Ba5FO9 | Dx = 5.049 Mg m−3 |
Mr = 882.13 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pnma | Cell parameters from 12561 reflections |
a = 7.60788 (12) Å | θ = 2.0–31.8° |
b = 14.8299 (2) Å | µ = 16.76 mm−1 |
c = 10.28650 (16) Å | T = 293 K |
V = 1160.57 (3) Å3 | Tabular, colourless |
Z = 4 | 0.26 × 0.13 × 0.05 mm |
F(000) = 1504 |
Xcalibur, Ruby, Gemini ultra diffractometer | 2020 independent reflections |
Radiation source: Enhance (Mo) X-ray Source | 1875 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: 10.3457 pixels mm-1 | θmax = 31.9°, θmin = 2.4° |
ω scans | h = −11→11 |
Absorption correction: multi-scan CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. | k = −21→21 |
Tmin = 0.254, Tmax = 1.000 | l = −15→14 |
22057 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.021 | w = 1/[σ2(Fo2) + (0.0305P)2 + 1.4282P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.056 | (Δ/σ)max = 0.002 |
S = 1.11 | Δρmax = 1.82 e Å−3 |
2020 reflections | Δρmin = −1.76 e Å−3 |
92 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.0347 (5) |
B3Ba5FO9 | V = 1160.57 (3) Å3 |
Mr = 882.13 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 7.60788 (12) Å | µ = 16.76 mm−1 |
b = 14.8299 (2) Å | T = 293 K |
c = 10.28650 (16) Å | 0.26 × 0.13 × 0.05 mm |
Xcalibur, Ruby, Gemini ultra diffractometer | 2020 independent reflections |
Absorption correction: multi-scan CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. | 1875 reflections with I > 2σ(I) |
Tmin = 0.254, Tmax = 1.000 | Rint = 0.051 |
22057 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 92 parameters |
wR(F2) = 0.056 | 0 restraints |
S = 1.11 | Δρmax = 1.82 e Å−3 |
2020 reflections | Δρmin = −1.76 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0.21232 (4) | 0.7500 | 0.02070 (3) | 0.00983 (9) | |
Ba2 | −0.02618 (3) | 0.610112 (13) | −0.251686 (16) | 0.00897 (8) | |
Ba3 | −0.25591 (3) | 0.619490 (14) | 0.12631 (2) | 0.01346 (8) | |
B1 | 0.1996 (5) | 0.5407 (2) | 0.0597 (3) | 0.0110 (6) | |
O1 | 0.0919 (3) | 0.58837 (17) | 0.1428 (2) | 0.0166 (5) | |
O2 | 0.2193 (3) | 0.53729 (18) | −0.3948 (3) | 0.0158 (5) | |
O3 | 0.2265 (3) | 0.56854 (17) | −0.0664 (2) | 0.0138 (5) | |
B2 | 0.2194 (7) | 0.7500 | −0.3853 (5) | 0.0089 (9) | |
O4 | 0.2187 (4) | 0.7500 | −0.2506 (3) | 0.0093 (6) | |
O5 | 0.5654 (5) | 0.7500 | −0.0461 (3) | 0.0155 (7) | |
O6 | −0.1206 (4) | 0.7500 | −0.0507 (3) | 0.0136 (6) | |
F | 0.3984 (5) | 0.7500 | 0.2351 (3) | 0.0249 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.00910 (14) | 0.01085 (14) | 0.00955 (14) | 0.000 | −0.00146 (8) | 0.000 |
Ba2 | 0.00593 (12) | 0.01069 (12) | 0.01028 (12) | −0.00003 (6) | 0.00025 (6) | −0.00038 (5) |
Ba3 | 0.01634 (13) | 0.01413 (12) | 0.00993 (12) | −0.00146 (7) | 0.00123 (6) | 0.00058 (6) |
B1 | 0.0106 (15) | 0.0120 (16) | 0.0105 (15) | −0.0013 (12) | −0.0031 (12) | −0.0018 (12) |
O1 | 0.0150 (12) | 0.0203 (12) | 0.0145 (11) | 0.0019 (10) | 0.0011 (9) | −0.0029 (9) |
O2 | 0.0152 (12) | 0.0154 (12) | 0.0169 (12) | 0.0034 (9) | 0.0008 (9) | −0.0058 (10) |
O3 | 0.0170 (12) | 0.0144 (12) | 0.0100 (11) | −0.0004 (9) | 0.0006 (8) | 0.0030 (9) |
B2 | 0.008 (2) | 0.009 (2) | 0.009 (2) | 0.000 | 0.0005 (15) | 0.000 |
O4 | 0.0101 (16) | 0.0096 (15) | 0.0083 (15) | 0.000 | 0.0012 (10) | 0.000 |
O5 | 0.0095 (15) | 0.0222 (17) | 0.0148 (15) | 0.000 | 0.0040 (12) | 0.000 |
O6 | 0.0067 (15) | 0.0199 (17) | 0.0143 (15) | 0.000 | −0.0031 (12) | 0.000 |
F | 0.0316 (19) | 0.0260 (17) | 0.0169 (14) | 0.000 | −0.0036 (13) | 0.000 |
Ba1—F | 2.621 (3) | Ba3—Ba2vi | 3.9897 (3) |
Ba1—O6 | 2.637 (3) | B1—O3 | 1.376 (4) |
Ba1—O5 | 2.772 (3) | B1—O1 | 1.380 (4) |
Ba1—O4 | 2.791 (3) | B1—O2vii | 1.392 (4) |
Ba1—O3 | 2.838 (2) | B1—Ba3iii | 3.080 (4) |
Ba1—O3i | 2.838 (2) | B1—Ba2iii | 3.263 (4) |
Ba1—O1 | 2.857 (3) | B1—Ba3viii | 3.452 (4) |
Ba1—O1i | 2.857 (3) | O1—Ba3viii | 2.682 (2) |
Ba1—B1i | 3.131 (4) | O1—Ba2iii | 3.189 (3) |
Ba1—B1 | 3.131 (4) | O2—B1ix | 1.392 (4) |
Ba1—Ba2 | 3.9302 (3) | O2—Ba2x | 2.681 (3) |
Ba1—Ba2i | 3.9302 (3) | O2—Ba3x | 2.682 (3) |
Ba2—O2 | 2.612 (2) | O3—Ba2x | 2.725 (2) |
Ba2—O2ii | 2.681 (3) | O3—Ba3iii | 2.865 (3) |
Ba2—O3ii | 2.725 (2) | B2—O5ii | 1.368 (6) |
Ba2—O3 | 2.777 (2) | B2—O6x | 1.384 (6) |
Ba2—O4 | 2.788 (2) | B2—O4 | 1.386 (6) |
Ba2—O4ii | 2.841 (2) | B2—Ba2i | 3.112 (4) |
Ba2—O6 | 3.015 (2) | B2—Ba3x | 3.151 (4) |
Ba2—O5ii | 3.019 (3) | B2—Ba3xi | 3.151 (4) |
Ba2—B2 | 3.112 (4) | B2—Ba2xi | 3.168 (4) |
Ba2—B2ii | 3.168 (4) | B2—Ba2x | 3.168 (4) |
Ba2—O1iii | 3.189 (3) | O4—Ba2i | 2.788 (2) |
Ba2—B1iii | 3.263 (4) | O4—Ba2xi | 2.841 (2) |
Ba3—Fiv | 2.675 (2) | O4—Ba2x | 2.841 (2) |
Ba3—O2ii | 2.682 (3) | O5—B2x | 1.368 (6) |
Ba3—O1iv | 2.682 (2) | O5—Ba3xii | 2.956 (3) |
Ba3—O1 | 2.691 (3) | O5—Ba3xiii | 2.956 (3) |
Ba3—O6 | 2.850 (2) | O5—Ba2x | 3.019 (3) |
Ba3—O3iii | 2.865 (3) | O5—Ba2xi | 3.019 (3) |
Ba3—O5v | 2.956 (3) | O6—B2ii | 1.384 (6) |
Ba3—B1iii | 3.080 (4) | O6—Ba3i | 2.850 (2) |
Ba3—B2ii | 3.151 (4) | O6—Ba2i | 3.015 (2) |
Ba3—B1iv | 3.452 (4) | F—Ba3xiv | 2.675 (2) |
Ba3—Ba3i | 3.8709 (4) | F—Ba3viii | 2.675 (2) |
F—Ba1—O6 | 138.87 (11) | O3iii—Ba3—B2ii | 115.67 (8) |
F—Ba1—O5 | 71.65 (11) | O5v—Ba3—B2ii | 25.64 (11) |
O6—Ba1—O5 | 149.48 (11) | B1iii—Ba3—B2ii | 89.62 (9) |
F—Ba1—O4 | 146.32 (10) | Fiv—Ba3—B1iv | 77.83 (8) |
O6—Ba1—O4 | 74.81 (10) | O2ii—Ba3—B1iv | 132.09 (8) |
O5—Ba1—O4 | 74.66 (10) | O1iv—Ba3—B1iv | 21.69 (8) |
F—Ba1—O3 | 104.18 (5) | O1—Ba3—B1iv | 88.81 (8) |
O6—Ba1—O3 | 87.05 (5) | O6—Ba3—B1iv | 149.68 (8) |
O5—Ba1—O3 | 83.40 (5) | O3iii—Ba3—B1iv | 83.09 (8) |
O4—Ba1—O3 | 71.57 (5) | O5v—Ba3—B1iv | 137.55 (9) |
F—Ba1—O3i | 104.18 (5) | B1iii—Ba3—B1iv | 109.50 (4) |
O6—Ba1—O3i | 87.05 (5) | B2ii—Ba3—B1iv | 159.79 (9) |
O5—Ba1—O3i | 83.40 (5) | Fiv—Ba3—Ba3i | 43.65 (5) |
O4—Ba1—O3i | 71.57 (5) | O2ii—Ba3—Ba3i | 117.04 (6) |
O3—Ba1—O3i | 142.94 (10) | O1iv—Ba3—Ba3i | 99.91 (6) |
F—Ba1—O1 | 78.65 (6) | O1—Ba3—Ba3i | 99.87 (6) |
O6—Ba1—O1 | 79.31 (6) | O6—Ba3—Ba3i | 47.23 (5) |
O5—Ba1—O1 | 114.81 (6) | O3iii—Ba3—Ba3i | 166.76 (5) |
O4—Ba1—O1 | 116.44 (5) | O5v—Ba3—Ba3i | 49.10 (5) |
O3—Ba1—O1 | 49.88 (7) | B1iii—Ba3—Ba3i | 140.48 (7) |
O3i—Ba1—O1 | 161.15 (7) | B2ii—Ba3—Ba3i | 52.10 (6) |
F—Ba1—O1i | 78.65 (6) | B1iv—Ba3—Ba3i | 109.78 (6) |
O6—Ba1—O1i | 79.31 (6) | Fiv—Ba3—Ba2vi | 129.21 (5) |
O5—Ba1—O1i | 114.81 (6) | O2ii—Ba3—Ba2vi | 82.08 (6) |
O4—Ba1—O1i | 116.44 (5) | O1iv—Ba3—Ba2vi | 52.79 (6) |
O3—Ba1—O1i | 161.15 (7) | O1—Ba3—Ba2vi | 104.02 (5) |
O3i—Ba1—O1i | 49.88 (7) | O6—Ba3—Ba2vi | 158.54 (5) |
O1—Ba1—O1i | 114.05 (10) | O3iii—Ba3—Ba2vi | 43.06 (5) |
F—Ba1—B1i | 84.78 (6) | O5v—Ba3—Ba2vi | 123.80 (6) |
O6—Ba1—B1i | 90.34 (7) | B1iii—Ba3—Ba2vi | 66.10 (7) |
O5—Ba1—B1i | 93.53 (7) | B2ii—Ba3—Ba2vi | 138.33 (7) |
O4—Ba1—B1i | 97.38 (7) | B1iv—Ba3—Ba2vi | 51.40 (6) |
O3—Ba1—B1i | 168.95 (8) | Ba3i—Ba3—Ba2vi | 148.589 (4) |
O3i—Ba1—B1i | 26.06 (8) | O3—B1—O1 | 121.3 (3) |
O1—Ba1—B1i | 139.94 (9) | O3—B1—O2vii | 120.0 (3) |
O1i—Ba1—B1i | 26.13 (8) | O1—B1—O2vii | 118.7 (3) |
F—Ba1—B1 | 84.78 (6) | O3—B1—Ba3iii | 68.00 (18) |
O6—Ba1—B1 | 90.34 (7) | O1—B1—Ba3iii | 149.6 (2) |
O5—Ba1—B1 | 93.53 (7) | O2vii—B1—Ba3iii | 60.41 (17) |
O4—Ba1—B1 | 97.38 (7) | O3—B1—Ba1 | 65.01 (18) |
O3—Ba1—B1 | 26.06 (8) | O1—B1—Ba1 | 65.80 (17) |
O3i—Ba1—B1 | 168.95 (8) | O2vii—B1—Ba1 | 148.6 (2) |
O1—Ba1—B1 | 26.13 (8) | Ba3iii—B1—Ba1 | 132.91 (12) |
O1i—Ba1—B1 | 139.94 (9) | O3—B1—Ba2iii | 146.7 (2) |
B1i—Ba1—B1 | 164.87 (13) | O1—B1—Ba2iii | 74.66 (18) |
F—Ba1—Ba2 | 148.139 (3) | O2vii—B1—Ba2iii | 53.54 (16) |
O6—Ba1—Ba2 | 50.06 (5) | Ba3iii—B1—Ba2iii | 84.45 (9) |
O5—Ba1—Ba2 | 105.70 (6) | Ba1—B1—Ba2iii | 140.32 (12) |
O4—Ba1—Ba2 | 45.19 (4) | O3—B1—Ba3viii | 140.0 (2) |
O3—Ba1—Ba2 | 44.94 (5) | O1—B1—Ba3viii | 45.93 (15) |
O3i—Ba1—Ba2 | 107.04 (5) | O2vii—B1—Ba3viii | 85.59 (19) |
O1—Ba1—Ba2 | 73.90 (5) | Ba3iii—B1—Ba3viii | 145.95 (12) |
O1i—Ba1—Ba2 | 127.46 (5) | Ba1—B1—Ba3viii | 77.37 (8) |
B1i—Ba1—Ba2 | 126.89 (6) | Ba2iii—B1—Ba3viii | 72.85 (7) |
B1—Ba1—Ba2 | 63.50 (6) | B1—O1—Ba3viii | 112.4 (2) |
F—Ba1—Ba2i | 148.140 (3) | B1—O1—Ba3 | 129.3 (2) |
O6—Ba1—Ba2i | 50.06 (5) | Ba3viii—O1—Ba3 | 116.81 (9) |
O5—Ba1—Ba2i | 105.70 (6) | B1—O1—Ba1 | 88.07 (19) |
O4—Ba1—Ba2i | 45.19 (4) | Ba3viii—O1—Ba1 | 96.11 (8) |
O3—Ba1—Ba2i | 107.04 (5) | Ba3—O1—Ba1 | 98.26 (8) |
O3i—Ba1—Ba2i | 44.94 (5) | B1—O1—Ba2iii | 80.69 (19) |
O1—Ba1—Ba2i | 127.46 (5) | Ba3viii—O1—Ba2iii | 85.16 (6) |
O1i—Ba1—Ba2i | 73.90 (5) | Ba3—O1—Ba2iii | 91.51 (7) |
B1i—Ba1—Ba2i | 63.50 (6) | Ba1—O1—Ba2iii | 168.26 (10) |
B1—Ba1—Ba2i | 126.89 (6) | B1ix—O2—Ba2 | 148.2 (2) |
Ba2—Ba1—Ba2i | 63.719 (7) | B1ix—O2—Ba2x | 101.77 (19) |
O2—Ba2—O2ii | 131.82 (11) | Ba2—O2—Ba2x | 91.89 (8) |
O2—Ba2—O3ii | 90.75 (8) | B1ix—O2—Ba3x | 92.76 (19) |
O2ii—Ba2—O3ii | 78.24 (8) | Ba2—O2—Ba3x | 111.27 (9) |
O2—Ba2—O3 | 78.47 (8) | Ba2x—O2—Ba3x | 105.39 (9) |
O2ii—Ba2—O3 | 91.41 (7) | B1—O3—Ba2x | 144.9 (2) |
O3ii—Ba2—O3 | 154.09 (10) | B1—O3—Ba2 | 127.6 (2) |
O2—Ba2—O4 | 80.34 (8) | Ba2x—O3—Ba2 | 87.49 (7) |
O2ii—Ba2—O4 | 141.25 (9) | B1—O3—Ba1 | 88.92 (19) |
O3ii—Ba2—O4 | 129.24 (8) | Ba2x—O3—Ba1 | 91.63 (7) |
O3—Ba2—O4 | 72.53 (8) | Ba2—O3—Ba1 | 88.84 (7) |
O2—Ba2—O4ii | 142.66 (9) | B1—O3—Ba3iii | 85.56 (19) |
O2ii—Ba2—O4ii | 78.24 (8) | Ba2x—O3—Ba3iii | 91.06 (7) |
O3ii—Ba2—O4ii | 72.48 (8) | Ba2—O3—Ba3iii | 97.03 (7) |
O3—Ba2—O4ii | 129.02 (8) | Ba1—O3—Ba3iii | 173.64 (10) |
O4—Ba2—O4ii | 85.018 (6) | O5ii—B2—O6x | 120.5 (4) |
O2—Ba2—O6 | 147.26 (8) | O5ii—B2—O4 | 120.8 (4) |
O2ii—Ba2—O6 | 73.72 (8) | O6x—B2—O4 | 118.6 (4) |
O3ii—Ba2—O6 | 117.52 (8) | O5ii—B2—Ba2 | 73.36 (19) |
O3—Ba2—O6 | 81.20 (8) | O6x—B2—Ba2 | 137.58 (8) |
O4—Ba2—O6 | 69.17 (8) | O4—B2—Ba2 | 63.64 (16) |
O4ii—Ba2—O6 | 47.88 (8) | O5ii—B2—Ba2i | 73.36 (19) |
O2—Ba2—O5ii | 74.38 (8) | O6x—B2—Ba2i | 137.58 (8) |
O2ii—Ba2—O5ii | 146.18 (8) | O4—B2—Ba2i | 63.64 (16) |
O3ii—Ba2—O5ii | 80.88 (8) | Ba2—B2—Ba2i | 83.62 (12) |
O3—Ba2—O5ii | 117.77 (8) | O5ii—B2—Ba3x | 69.20 (19) |
O4—Ba2—O5ii | 48.51 (9) | O6x—B2—Ba3x | 64.75 (18) |
O4ii—Ba2—O5ii | 70.22 (8) | O4—B2—Ba3x | 141.92 (6) |
O6—Ba2—O5ii | 93.13 (7) | Ba2—B2—Ba3x | 88.50 (6) |
O2—Ba2—B2 | 66.26 (9) | Ba2i—B2—Ba3x | 142.45 (17) |
O2ii—Ba2—B2 | 161.90 (9) | O5ii—B2—Ba3xi | 69.20 (19) |
O3ii—Ba2—B2 | 105.20 (11) | O6x—B2—Ba3xi | 64.75 (18) |
O3—Ba2—B2 | 92.04 (10) | O4—B2—Ba3xi | 141.92 (6) |
O4—Ba2—B2 | 26.45 (11) | Ba2—B2—Ba3xi | 142.45 (17) |
O4ii—Ba2—B2 | 85.82 (8) | Ba2i—B2—Ba3xi | 88.50 (6) |
O6—Ba2—B2 | 89.26 (8) | Ba3x—B2—Ba3xi | 75.79 (11) |
O5ii—Ba2—B2 | 25.73 (11) | O5ii—B2—Ba2xi | 138.84 (7) |
O2—Ba2—B2ii | 163.41 (9) | O6x—B2—Ba2xi | 70.98 (19) |
O2ii—Ba2—B2ii | 64.69 (8) | O4—B2—Ba2xi | 63.75 (17) |
O3ii—Ba2—B2ii | 91.82 (10) | Ba2—B2—Ba2xi | 127.38 (17) |
O3—Ba2—B2ii | 105.25 (10) | Ba2i—B2—Ba2xi | 74.57 (6) |
O4—Ba2—B2ii | 85.36 (8) | Ba3x—B2—Ba2xi | 135.71 (17) |
O4ii—Ba2—B2ii | 25.94 (10) | Ba3xi—B2—Ba2xi | 84.91 (6) |
O6—Ba2—B2ii | 25.71 (10) | O5ii—B2—Ba2x | 138.84 (7) |
O5ii—Ba2—B2ii | 89.85 (8) | O6x—B2—Ba2x | 70.98 (19) |
B2—Ba2—B2ii | 97.28 (7) | O4—B2—Ba2x | 63.75 (17) |
O2—Ba2—O1iii | 85.89 (7) | Ba2—B2—Ba2x | 74.57 (6) |
O2ii—Ba2—O1iii | 46.96 (7) | Ba2i—B2—Ba2x | 127.38 (17) |
O3ii—Ba2—O1iii | 85.65 (7) | Ba3x—B2—Ba2x | 84.91 (6) |
O3—Ba2—O1iii | 70.27 (7) | Ba3xi—B2—Ba2x | 135.71 (17) |
O4—Ba2—O1iii | 142.19 (7) | Ba2xi—B2—Ba2x | 81.82 (12) |
O4ii—Ba2—O1iii | 124.34 (7) | B2—O4—Ba2 | 89.92 (18) |
O6—Ba2—O1iii | 110.92 (6) | B2—O4—Ba2i | 89.92 (18) |
O5ii—Ba2—O1iii | 155.83 (6) | Ba2—O4—Ba2i | 96.16 (10) |
B2—Ba2—O1iii | 149.84 (8) | B2—O4—Ba1 | 179.2 (3) |
B2ii—Ba2—O1iii | 110.65 (8) | Ba2—O4—Ba1 | 89.58 (8) |
O2—Ba2—B1iii | 110.30 (9) | Ba2i—O4—Ba1 | 89.58 (8) |
O2ii—Ba2—B1iii | 24.69 (8) | B2—O4—Ba2xi | 90.31 (18) |
O3ii—Ba2—B1iii | 88.94 (8) | Ba2—O4—Ba2xi | 178.80 (10) |
O3—Ba2—B1iii | 73.27 (8) | Ba2i—O4—Ba2xi | 85.022 (6) |
O4—Ba2—B1iii | 141.05 (9) | Ba1—O4—Ba2xi | 90.21 (8) |
O4ii—Ba2—B1iii | 102.67 (9) | B2—O4—Ba2x | 90.31 (18) |
O6—Ba2—B1iii | 87.73 (8) | Ba2—O4—Ba2x | 85.022 (6) |
O5ii—Ba2—B1iii | 168.94 (9) | Ba2i—O4—Ba2x | 178.80 (10) |
B2—Ba2—B1iii | 165.28 (11) | Ba1—O4—Ba2x | 90.21 (8) |
B2ii—Ba2—B1iii | 86.14 (9) | Ba2xi—O4—Ba2x | 93.80 (9) |
O1iii—Ba2—B1iii | 24.66 (8) | B2x—O5—Ba1 | 163.3 (3) |
Fiv—Ba3—O2ii | 146.40 (9) | B2x—O5—Ba3xii | 85.2 (2) |
Fiv—Ba3—O1iv | 80.92 (8) | Ba1—O5—Ba3xii | 107.28 (9) |
O2ii—Ba3—O1iv | 132.66 (8) | B2x—O5—Ba3xiii | 85.2 (2) |
Fiv—Ba3—O1 | 70.06 (9) | Ba1—O5—Ba3xiii | 107.28 (9) |
O2ii—Ba3—O1 | 92.71 (7) | Ba3xii—O5—Ba3xiii | 81.80 (9) |
O1iv—Ba3—O1 | 109.82 (6) | B2x—O5—Ba2x | 80.91 (19) |
Fiv—Ba3—O6 | 71.98 (8) | Ba1—O5—Ba2x | 86.97 (8) |
O2ii—Ba3—O6 | 76.51 (7) | Ba3xii—O5—Ba2x | 165.75 (13) |
O1iv—Ba3—O6 | 146.99 (7) | Ba3xiii—O5—Ba2x | 93.988 (18) |
O1—Ba3—O6 | 78.56 (8) | B2x—O5—Ba2xi | 80.91 (19) |
Fiv—Ba3—O3iii | 141.70 (8) | Ba1—O5—Ba2xi | 86.97 (8) |
O2ii—Ba3—O3iii | 51.09 (8) | Ba3xii—O5—Ba2xi | 93.988 (18) |
O1iv—Ba3—O3iii | 93.26 (7) | Ba3xiii—O5—Ba2xi | 165.75 (13) |
O1—Ba3—O3iii | 76.70 (7) | Ba2x—O5—Ba2xi | 86.80 (9) |
O6—Ba3—O3iii | 119.69 (7) | B2ii—O6—Ba1 | 167.8 (3) |
Fiv—Ba3—O5v | 92.74 (7) | B2ii—O6—Ba3i | 89.2 (2) |
O2ii—Ba3—O5v | 74.50 (7) | Ba1—O6—Ba3i | 99.72 (9) |
O1iv—Ba3—O5v | 116.43 (9) | B2ii—O6—Ba3 | 89.2 (2) |
O1—Ba3—O5v | 127.04 (8) | Ba1—O6—Ba3 | 99.72 (9) |
O6—Ba3—O5v | 48.57 (9) | Ba3i—O6—Ba3 | 85.54 (9) |
O3iii—Ba3—O5v | 122.97 (7) | B2ii—O6—Ba2 | 83.31 (19) |
Fiv—Ba3—B1iii | 145.90 (10) | Ba1—O6—Ba2 | 87.84 (8) |
O2ii—Ba3—B1iii | 26.84 (8) | Ba3i—O6—Ba2 | 172.44 (12) |
O1iv—Ba3—B1iii | 118.50 (9) | Ba3—O6—Ba2 | 93.261 (10) |
O1—Ba3—B1iii | 76.72 (8) | B2ii—O6—Ba2i | 83.31 (19) |
O6—Ba3—B1iii | 94.40 (8) | Ba1—O6—Ba2i | 87.84 (8) |
O3iii—Ba3—B1iii | 26.44 (8) | Ba3i—O6—Ba2i | 93.261 (10) |
O5v—Ba3—B1iii | 101.33 (8) | Ba3—O6—Ba2i | 172.44 (12) |
Fiv—Ba3—B2ii | 90.06 (8) | Ba2—O6—Ba2i | 86.94 (9) |
O2ii—Ba3—B2ii | 64.93 (8) | Ba1—F—Ba3xiv | 102.21 (10) |
O1iv—Ba3—B2ii | 140.95 (10) | Ba1—F—Ba3viii | 102.21 (10) |
O1—Ba3—B2ii | 102.33 (10) | Ba3xiv—F—Ba3viii | 92.70 (10) |
O6—Ba3—B2ii | 26.05 (11) |
Symmetry codes: (i) x, −y+3/2, z; (ii) x−1/2, y, −z−1/2; (iii) −x, −y+1, −z; (iv) x−1/2, y, −z+1/2; (v) x−1, y, z; (vi) −x−1/2, −y+1, z+1/2; (vii) −x+1/2, −y+1, z+1/2; (viii) x+1/2, y, −z+1/2; (ix) −x+1/2, −y+1, z−1/2; (x) x+1/2, y, −z−1/2; (xi) x+1/2, −y+3/2, −z−1/2; (xii) x+1, −y+3/2, z; (xiii) x+1, y, z; (xiv) x+1/2, −y+3/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | B3Ba5FO9 |
Mr | 882.13 |
Crystal system, space group | Orthorhombic, Pnma |
Temperature (K) | 293 |
a, b, c (Å) | 7.60788 (12), 14.8299 (2), 10.28650 (16) |
V (Å3) | 1160.57 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 16.76 |
Crystal size (mm) | 0.26 × 0.13 × 0.05 |
Data collection | |
Diffractometer | Xcalibur, Ruby, Gemini ultra diffractometer |
Absorption correction | Multi-scan CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. |
Tmin, Tmax | 0.254, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 22057, 2020, 1875 |
Rint | 0.051 |
(sin θ/λ)max (Å−1) | 0.743 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.056, 1.11 |
No. of reflections | 2020 |
No. of parameters | 92 |
Δρmax, Δρmin (e Å−3) | 1.82, −1.76 |
Computer programs: CrysAlis PRO, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008) in WinGX v1.80.05 (Farrugia, 1999).
Subscribe to Journal of Applied Crystallography
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- Purchase subscription
- Reduced-price subscriptions
- If you have already subscribed, you may need to register