Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768107003734/bm5044sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768107003734/bm5044BaV4O9_293Ksup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768107003734/bm5044BaV4O9_250Ksup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768107003734/bm5044BaV4O9_200Ksup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768107003734/bm5044BaV4O9_150Ksup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768107003734/bm5044BaV4O9_100Ksup6.hkl |
For all compounds, data collection: X-AREA (Stoe, 2002); cell refinement: X-AREA (Stoe, 2002); data reduction: X-RED (Stoe, 1996); program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS Version 5.1; software used to prepare material for publication: WinGX 1.64.05 (Farrugia, 1999).
O9V4·Ba | F(000) = 440 |
Mr = 485.1 | Dx = 4.895 Mg m−3 Dm = 4.895 Mg m−3 Dm measured by not measured |
Monoclinic, P2/c | Melting point: 0 K |
Hall symbol: -P 2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 7.6396 (12) Å | Cell parameters from 6832 reflections |
b = 4.9447 (7) Å | θ = 2.9–32.2° |
c = 9.3596 (14) Å | µ = 11.39 mm−1 |
β = 111.427 (11)° | T = 293 K |
V = 329.13 (9) Å3 | Parallelepiped, dark blue |
Z = 2 | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
STOE IPDS 2 diffractometer | 1031 reflections with I > 2σ(I) |
Rotation method scans | Rint = 0.045 |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | θmax = 32.2°, θmin = 2.9° |
Tmin = 0.09, Tmax = 0.19 | h = −11→11 |
5391 measured reflections | k = −7→7 |
1132 independent reflections | l = −13→13 |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.010P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.023 | (Δ/σ)max < 0.001 |
wR(F2) = 0.040 | Δρmax = 0.80 e Å−3 |
S = 1.45 | Δρmin = −0.88 e Å−3 |
1132 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
66 parameters | Extinction coefficient: 0.0104 (5) |
0 restraints |
O9V4·Ba | V = 329.13 (9) Å3 |
Mr = 485.1 | Z = 2 |
Monoclinic, P2/c | Mo Kα radiation |
a = 7.6396 (12) Å | µ = 11.39 mm−1 |
b = 4.9447 (7) Å | T = 293 K |
c = 9.3596 (14) Å | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
β = 111.427 (11)° |
STOE IPDS 2 diffractometer | 1132 independent reflections |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | 1031 reflections with I > 2σ(I) |
Tmin = 0.09, Tmax = 0.19 | Rint = 0.045 |
5391 measured reflections |
R[F2 > 2σ(F2)] = 0.023 | 66 parameters |
wR(F2) = 0.040 | 0 restraints |
S = 1.45 | Δρmax = 0.80 e Å−3 |
1132 reflections | Δρmin = −0.88 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. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0 | 0.33955 (6) | 0.25 | 0.01117 (7) | |
V1 | 0.57307 (6) | 0.25101 (9) | 0.45054 (5) | 0.00621 (9) | |
V2 | 0.68930 (6) | 0.77191 (9) | 0.34955 (5) | 0.00618 (9) | |
O1 | 0.8917 (3) | 0.8665 (5) | 0.3486 (2) | 0.0122 (4) | |
O2 | 0.7700 (3) | 0.4149 (4) | 0.4467 (2) | 0.0083 (4) | |
O3 | 0.5807 (3) | 0.4153 (4) | 0.6455 (2) | 0.0074 (3) | |
O4 | 0.6736 (3) | 0.9087 (4) | 0.5402 (2) | 0.0067 (3) | |
O5 | 0.5 | 0.0588 (6) | 0.25 | 0.0060 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.01209 (11) | 0.00953 (12) | 0.01196 (11) | 0 | 0.00449 (8) | 0 |
V1 | 0.00842 (19) | 0.0049 (2) | 0.00554 (18) | −0.00069 (14) | 0.00278 (15) | 0.00038 (13) |
V2 | 0.00677 (18) | 0.0058 (2) | 0.00593 (18) | −0.00046 (13) | 0.00228 (15) | 0.00039 (13) |
O1 | 0.0103 (8) | 0.0127 (10) | 0.0143 (9) | −0.0012 (7) | 0.0053 (7) | 0.0007 (8) |
O2 | 0.0086 (9) | 0.0072 (9) | 0.0101 (8) | −0.0007 (6) | 0.0045 (7) | −0.0002 (6) |
O3 | 0.0107 (9) | 0.0065 (8) | 0.0050 (8) | 0.0020 (6) | 0.0029 (7) | 0.0004 (6) |
O4 | 0.0080 (8) | 0.0059 (8) | 0.0062 (8) | 0.0002 (6) | 0.0025 (6) | −0.0007 (6) |
O5 | 0.0082 (11) | 0.0056 (11) | 0.0040 (10) | 0 | 0.0021 (9) | 0 |
Ba1—O1i | 2.750 (2) | V2—V1ix | 3.5107 (8) |
Ba1—O1ii | 2.750 (2) | V2—Ba1xii | 3.5621 (6) |
Ba1—O4iii | 2.8288 (19) | V2—O3 | 3.6267 (19) |
Ba1—O4iv | 2.8288 (19) | V2—O4xvi | 3.6523 (18) |
Ba1—O1v | 2.981 (2) | V2—V1xviii | 3.6613 (8) |
Ba1—O1vi | 2.981 (2) | V2—Ba1iv | 3.6723 (8) |
Ba1—O2iv | 2.996 (2) | V2—O4v | 3.750 (2) |
Ba1—O2iii | 2.996 (2) | V2—O5 | 3.796 (3) |
Ba1—O2vi | 2.9962 (18) | V2—V1v | 3.7984 (8) |
Ba1—O2v | 2.9962 (18) | V2—O1xxi | 3.849 (2) |
Ba1—O3iv | 3.225 (2) | V2—O2xi | 3.975 (2) |
Ba1—O3iii | 3.225 (2) | V2—Ba1xxii | 3.9995 (6) |
V1—O2 | 1.7209 (19) | V2—O2v | 4.001 (2) |
V1—O4vii | 1.921 (2) | V2—O2ix | 4.1414 (19) |
V1—O3 | 1.9791 (18) | V2—V2xiii | 4.9447 (7) |
V1—O5 | 1.9932 (14) | V2—V2vii | 4.9447 (7) |
V1—O3iv | 2.035 (2) | V2—V2xxi | 5.0781 (12) |
V1—O4iv | 2.0743 (19) | V2—V2xvii | 5.1950 (7) |
V1—V2vii | 2.8120 (7) | V2—V2xx | 5.1950 (7) |
V1—V1iv | 2.9870 (9) | V2—V2xvi | 5.2285 (10) |
V1—V2 | 2.9882 (7) | V2—V1xi | 5.2502 (11) |
V1—V1viii | 3.0035 (9) | V2—V2xi | 5.2849 (12) |
V1—V2iv | 3.2050 (7) | V2—V2ix | 5.3974 (8) |
V1—O3ix | 3.3161 (19) | V2—V2x | 5.3974 (8) |
V1—O4 | 3.376 (2) | V2—V2iv | 5.4296 (10) |
V1—O5viii | 3.4142 (14) | V2—V2i | 5.6877 (8) |
V1—O1vii | 3.485 (2) | V2—V2xviii | 5.6877 (8) |
V1—O3viii | 3.503 (2) | V2—V2xxiii | 5.6984 (12) |
V1—V1v | 3.5038 (11) | V2—V1xvi | 5.7966 (9) |
V1—V2x | 3.5107 (8) | V2—V1xx | 5.9711 (9) |
V1—O2iv | 3.5166 (19) | V2—V1viii | 5.9869 (9) |
V1—V2i | 3.6613 (8) | V2—V1x | 6.0076 (10) |
V1—O1x | 3.677 (2) | V2—V1xiv | 6.1560 (9) |
V1—O2v | 3.772 (2) | O1—Ba1xxii | 2.750 (2) |
V1—V2v | 3.7984 (8) | O1—Ba1xii | 2.981 (2) |
V1—O1xi | 3.869 (2) | O1—V1xiii | 3.485 (2) |
V1—Ba1iv | 3.9891 (7) | O1—V1ix | 3.677 (2) |
V1—O1i | 4.099 (2) | O1—V2xxi | 3.849 (2) |
V1—Ba1xii | 4.3388 (7) | O1—V1xi | 3.869 (2) |
V1—Ba1viii | 4.5102 (7) | O1—V1xviii | 4.099 (2) |
V1—V1xiii | 4.9447 (7) | O2—Ba1iv | 2.996 (2) |
V1—V1vii | 4.9447 (7) | O2—Ba1xii | 2.9962 (18) |
V1—V2xi | 5.2502 (11) | O2—V2vii | 3.302 (2) |
V1—V1x | 5.2881 (8) | O2—V1iv | 3.5166 (19) |
V1—V1ix | 5.2881 (8) | O2—V1v | 3.772 (2) |
V1—V1xiv | 5.2974 (8) | O2—V2xi | 3.975 (2) |
V1—V1xv | 5.2974 (8) | O2—V2v | 4.001 (2) |
V1—V2xvi | 5.7966 (9) | O2—V2x | 4.1414 (19) |
V1—V2xvii | 5.9711 (9) | O3—V2x | 2.0084 (19) |
V1—V2viii | 5.9869 (9) | O3—V1iv | 2.035 (2) |
V1—V2ix | 6.0076 (10) | O3—V2iv | 2.2765 (19) |
V1—V1i | 6.0602 (8) | O3—Ba1iv | 3.225 (2) |
V1—V1xviii | 6.0602 (8) | O3—V1x | 3.3161 (19) |
V1—V1xix | 6.1027 (12) | O3—V1viii | 3.503 (2) |
V1—V2xv | 6.1560 (9) | O4—V1xiii | 1.921 (2) |
V2—O1 | 1.619 (2) | O4—V1iv | 2.0743 (18) |
V2—O4 | 1.9521 (18) | O4—Ba1iv | 2.8288 (19) |
V2—O2 | 1.978 (2) | O4—V2xvii | 3.2620 (19) |
V2—O5xiii | 1.997 (2) | O4—V2xvi | 3.6523 (18) |
V2—O3ix | 2.0084 (19) | O4—V2v | 3.750 (2) |
V2—O3iv | 2.2765 (19) | O5—V1v | 1.9932 (14) |
V2—V2v | 2.8108 (10) | O5—V2i | 1.997 (2) |
V2—V1xiii | 2.8120 (7) | O5—V2vii | 1.997 (2) |
V2—V1iv | 3.2050 (7) | O5—V1xiv | 3.4142 (14) |
V2—O4xx | 3.2620 (19) | O5—V1viii | 3.4142 (14) |
V2—O2xiii | 3.302 (2) | O5—V2v | 3.796 (3) |
O1i—Ba1—O1ii | 63.49 (9) | O1—V2—O2xiii | 68.93 (9) |
O1i—Ba1—O4iii | 72.23 (6) | O4—V2—O2xiii | 58.84 (6) |
O1ii—Ba1—O4iii | 64.36 (6) | O2—V2—O2xiii | 137.49 (9) |
O1i—Ba1—O4iv | 64.36 (6) | O5xiii—V2—O2xiii | 58.34 (7) |
O1ii—Ba1—O4iv | 72.23 (6) | O3ix—V2—O2xiii | 132.55 (7) |
O4iii—Ba1—O4iv | 128.57 (8) | O3iv—V2—O2xiii | 117.73 (6) |
O1i—Ba1—O1v | 119.21 (7) | O4xx—V2—O2xiii | 73.79 (5) |
O1ii—Ba1—O1v | 177.30 (5) | O1—V2—O3 | 129.06 (8) |
O4iii—Ba1—O1v | 115.99 (6) | O4—V2—O3 | 50.41 (6) |
O4iv—Ba1—O1v | 108.69 (6) | O2—V2—O3 | 48.31 (6) |
O1i—Ba1—O1vi | 177.30 (5) | O5xiii—V2—O3 | 111.90 (4) |
O1ii—Ba1—O1vi | 119.21 (7) | O3ix—V2—O3 | 111.83 (5) |
O4iii—Ba1—O1vi | 108.69 (6) | O3iv—V2—O3 | 47.55 (7) |
O4iv—Ba1—O1vi | 115.99 (6) | O4xx—V2—O3 | 165.72 (5) |
O1v—Ba1—O1vi | 58.09 (8) | O2xiii—V2—O3 | 109.25 (5) |
O1i—Ba1—O2iv | 121.23 (6) | O1—V2—O4xvi | 134.58 (9) |
O1ii—Ba1—O2iv | 99.83 (6) | O4—V2—O4xvi | 44.40 (8) |
O4iii—Ba1—O2iv | 153.73 (5) | O2—V2—O4xvi | 113.42 (6) |
O4iv—Ba1—O2iv | 56.97 (5) | O5xiii—V2—O4xvi | 47.89 (3) |
O1v—Ba1—O2iv | 78.83 (6) | O3ix—V2—O4xvi | 112.05 (6) |
O1vi—Ba1—O2iv | 59.02 (6) | O3iv—V2—O4xvi | 51.91 (6) |
O1i—Ba1—O2iii | 99.83 (6) | O4xx—V2—O4xvi | 104.83 (5) |
O1ii—Ba1—O2iii | 121.23 (6) | O2xiii—V2—O4xvi | 65.83 (4) |
O4iii—Ba1—O2iii | 56.97 (5) | O3—V2—O4xvi | 65.49 (4) |
O4iv—Ba1—O2iii | 153.73 (5) | O1—V2—O4v | 108.13 (8) |
O1v—Ba1—O2iii | 59.02 (6) | O4—V2—O4v | 123.79 (6) |
O1vi—Ba1—O2iii | 78.83 (6) | O2—V2—O4v | 127.12 (7) |
O2iv—Ba1—O2iii | 132.19 (8) | O3iv—V2—O4v | 74.90 (6) |
O1i—Ba1—O2vi | 128.88 (6) | O2xiii—V2—O4v | 95.25 (5) |
O1ii—Ba1—O2vi | 65.41 (6) | O3—V2—O4v | 122.45 (4) |
O4iii—Ba1—O2vi | 85.10 (5) | O4xvi—V2—O4v | 80.16 (4) |
O4iv—Ba1—O2vi | 101.15 (5) | O1—V2—O5 | 123.11 (9) |
O1v—Ba1—O2vi | 111.89 (6) | O4—V2—O5 | 113.64 (6) |
O1vi—Ba1—O2vi | 53.82 (5) | O2—V2—O5 | 46.42 (6) |
O2iv—Ba1—O2vi | 68.90 (6) | O5xiii—V2—O5 | 113.54 (4) |
O2iii—Ba1—O2vi | 105.02 (5) | O3ix—V2—O5 | 49.49 (5) |
O1i—Ba1—O2v | 65.41 (6) | O3iv—V2—O5 | 50.24 (5) |
O1ii—Ba1—O2v | 128.88 (6) | O4xx—V2—O5 | 110.17 (4) |
O4iii—Ba1—O2v | 101.15 (5) | O2xiii—V2—O5 | 167.96 (4) |
O4iv—Ba1—O2v | 85.10 (5) | O3—V2—O5 | 64.08 (3) |
O1v—Ba1—O2v | 53.82 (5) | O4xvi—V2—O5 | 102.16 (3) |
O1vi—Ba1—O2v | 111.89 (6) | O4v—V2—O5 | 81.30 (3) |
O2iv—Ba1—O2v | 105.02 (5) | O1—V2—O1xxi | 47.91 (10) |
O2iii—Ba1—O2v | 68.90 (6) | O4—V2—O1xxi | 58.70 (6) |
O2vi—Ba1—O2v | 165.71 (8) | O2—V2—O1xxi | 92.36 (7) |
O1i—Ba1—O3iv | 91.96 (6) | O5xiii—V2—O1xxi | 106.19 (7) |
O1ii—Ba1—O3iv | 127.24 (6) | O3ix—V2—O1xxi | 148.85 (6) |
O4iii—Ba1—O3iv | 154.10 (5) | O3iv—V2—O1xxi | 133.68 (6) |
O4iv—Ba1—O3iv | 55.01 (5) | O4xx—V2—O1xxi | 100.23 (5) |
O1v—Ba1—O3iv | 53.70 (5) | O2xiii—V2—O1xxi | 47.87 (5) |
O1vi—Ba1—O3iv | 86.26 (5) | O3—V2—O1xxi | 91.50 (5) |
O2iv—Ba1—O3iv | 52.17 (5) | O4xvi—V2—O1xxi | 96.05 (5) |
O2iii—Ba1—O3iv | 107.98 (5) | O4v—V2—O1xxi | 138.70 (5) |
O2vi—Ba1—O3iv | 120.50 (5) | O5—V2—O1xxi | 138.74 (4) |
O2v—Ba1—O3iv | 53.06 (5) | O4—V2—O2xi | 92.40 (6) |
O1i—Ba1—O3iii | 127.24 (6) | O2—V2—O2xi | 58.48 (7) |
O1ii—Ba1—O3iii | 91.96 (6) | O5xiii—V2—O2xi | 146.89 (6) |
O4iii—Ba1—O3iii | 55.01 (5) | O3ix—V2—O2xi | 110.19 (6) |
O4iv—Ba1—O3iii | 154.10 (5) | O3iv—V2—O2xi | 133.33 (6) |
O1v—Ba1—O3iii | 86.26 (5) | O4xx—V2—O2xi | 103.49 (4) |
O1vi—Ba1—O3iii | 53.70 (5) | O2xiii—V2—O2xi | 92.00 (5) |
O2iv—Ba1—O3iii | 107.98 (5) | O3—V2—O2xi | 90.46 (4) |
O2iii—Ba1—O3iii | 52.17 (5) | O4xvi—V2—O2xi | 136.73 (4) |
O2vi—Ba1—O3iii | 53.06 (5) | O4v—V2—O2xi | 141.10 (4) |
O2v—Ba1—O3iii | 120.50 (5) | O5—V2—O2xi | 97.92 (4) |
O3iv—Ba1—O3iii | 135.84 (7) | O1xxi—V2—O2xi | 46.84 (4) |
O2—V1—O4vii | 102.18 (9) | O1—V2—O2v | 136.19 (8) |
O2—V1—O3 | 95.44 (9) | O4—V2—O2v | 117.07 (6) |
O4vii—V1—O3 | 94.97 (8) | O2—V2—O2v | 88.39 (8) |
O2—V1—O5 | 98.69 (7) | O5xiii—V2—O2v | 71.80 (6) |
O4vii—V1—O5 | 85.45 (9) | O3ix—V2—O2v | 35.38 (6) |
O3—V1—O5 | 165.46 (6) | O4xx—V2—O2v | 81.95 (5) |
O2—V1—O3iv | 88.67 (9) | O2xiii—V2—O2v | 130.08 (4) |
O4vii—V1—O3iv | 169.15 (8) | O3—V2—O2v | 85.83 (4) |
O3—V1—O3iv | 83.83 (8) | O4xvi—V2—O2v | 79.77 (4) |
O5—V1—O3iv | 93.02 (8) | O1xxi—V2—O2v | 175.69 (4) |
O2—V1—O4iv | 174.18 (9) | O2xi—V2—O2v | 136.44 (2) |
O4vii—V1—O4iv | 82.58 (8) | O1—V2—O2ix | 66.38 (8) |
O3—V1—O4iv | 80.71 (8) | O4—V2—O2ix | 171.37 (6) |
O5—V1—O4iv | 84.94 (6) | O2—V2—O2ix | 95.41 (5) |
O3iv—V1—O4iv | 86.59 (8) | O5xiii—V2—O2ix | 93.27 (4) |
O2—V1—O3ix | 57.12 (7) | O3ix—V2—O2ix | 34.79 (6) |
O4vii—V1—O3ix | 133.20 (6) | O3iv—V2—O2ix | 111.41 (6) |
O3—V1—O3ix | 125.86 (3) | O2xiii—V2—O2ix | 112.98 (4) |
O5—V1—O3ix | 60.90 (7) | O3—V2—O2ix | 137.63 (4) |
O3iv—V1—O3ix | 53.47 (7) | O4xvi—V2—O2ix | 137.28 (4) |
O4iv—V1—O3ix | 121.83 (7) | O4v—V2—O2ix | 57.16 (4) |
O2—V1—O4 | 55.27 (7) | O5—V2—O2ix | 74.89 (3) |
O4vii—V1—O4 | 136.22 (9) | O1xxi—V2—O2ix | 114.29 (4) |
O3—V1—O4 | 56.51 (6) | O2xi—V2—O2ix | 84.88 (5) |
O5—V1—O4 | 130.80 (8) | O2v—V2—O2ix | 69.83 (4) |
O3iv—V1—O4 | 51.01 (6) | V2—O1—V1xiii | 52.56 (7) |
O4iv—V1—O4 | 118.94 (5) | V2—O1—V1ix | 71.30 (8) |
O3ix—V1—O4 | 70.16 (5) | V1xiii—O1—V1ix | 95.36 (5) |
O2—V1—O5viii | 129.42 (7) | V2—O1—V2xxi | 132.09 (10) |
O4vii—V1—O5viii | 53.51 (6) | V1xiii—O1—V2xxi | 91.29 (5) |
O3—V1—O5viii | 52.09 (7) | V1ix—O1—V2xxi | 151.93 (6) |
O5—V1—O5viii | 119.05 (3) | V2—O1—V1xi | 142.75 (11) |
O3iv—V1—O5viii | 119.05 (6) | V1xiii—O1—V1xi | 131.97 (6) |
O4iv—V1—O5viii | 51.04 (5) | V1ix—O1—V1xi | 131.26 (6) |
O3ix—V1—O5viii | 171.68 (4) | V2—O1—V1xviii | 63.05 (7) |
O4—V1—O5viii | 108.59 (5) | V1xiii—O1—V1xviii | 54.30 (3) |
O2—V1—O1vii | 63.11 (8) | V1ix—O1—V1xviii | 45.04 (3) |
O4vii—V1—O1vii | 55.31 (6) | V2xxi—O1—V1xviii | 124.51 (6) |
O3—V1—O1vii | 133.48 (7) | V1xi—O1—V1xviii | 154.09 (6) |
O5—V1—O1vii | 57.69 (5) | V1—O2—V2 | 107.57 (10) |
O3iv—V1—O1vii | 132.04 (6) | Ba1iv—O2—Ba1xii | 111.10 (6) |
O4iv—V1—O1vii | 122.69 (6) | V1—O2—V2vii | 58.37 (6) |
O3ix—V1—O1vii | 78.59 (5) | V2—O2—V2vii | 137.49 (9) |
O4—V1—O1vii | 118.37 (5) | V1—O2—V1iv | 58.05 (6) |
O5viii—V1—O1vii | 108.66 (5) | V2—O2—V1iv | 64.42 (5) |
O2—V1—O3viii | 130.64 (7) | V2vii—O2—V1iv | 116.40 (5) |
O4vii—V1—O3viii | 47.64 (7) | V1—O2—V1v | 67.76 (6) |
O3—V1—O3viii | 121.12 (5) | V2—O2—V1v | 75.59 (6) |
O5—V1—O3viii | 50.02 (7) | V2vii—O2—V1v | 61.91 (4) |
O3iv—V1—O3viii | 124.33 (8) | V1iv—O2—V1v | 92.96 (5) |
O4iv—V1—O3viii | 55.12 (6) | V1—O2—V2xi | 130.07 (9) |
O3ix—V1—O3viii | 110.90 (3) | V2—O2—V2xi | 121.52 (7) |
O4—V1—O3viii | 173.84 (5) | V2vii—O2—V2xi | 88.00 (5) |
O5viii—V1—O3viii | 69.44 (5) | V1iv—O2—V2xi | 136.53 (6) |
O1vii—V1—O3viii | 67.60 (5) | V1v—O2—V2xi | 130.48 (5) |
O2—V1—O2iv | 121.95 (6) | V1—O2—V2v | 70.74 (7) |
O4vii—V1—O2iv | 120.91 (6) | V2vii—O2—V2v | 101.87 (5) |
O3—V1—O2iv | 47.83 (6) | V1iv—O2—V2v | 55.23 (3) |
O5—V1—O2iv | 120.09 (4) | V1v—O2—V2v | 45.10 (3) |
O3iv—V1—O2iv | 51.12 (6) | V2xi—O2—V2v | 158.39 (5) |
O4iv—V1—O2iv | 52.26 (6) | V1—O2—V2x | 56.89 (6) |
O3ix—V1—O2iv | 104.54 (5) | V2—O2—V2x | 119.50 (7) |
O4—V1—O2iv | 66.69 (4) | V2vii—O2—V2x | 87.76 (4) |
O5viii—V1—O2iv | 67.94 (5) | V1iv—O2—V2x | 58.80 (3) |
O1vii—V1—O2iv | 174.90 (5) | V1v—O2—V2x | 124.65 (5) |
O3viii—V1—O2iv | 107.37 (4) | V2xi—O2—V2x | 89.17 (4) |
O2—V1—O1x | 80.53 (8) | V2v—O2—V2x | 110.17 (4) |
O4vii—V1—O1x | 53.63 (7) | V1—O3—V2x | 123.39 (10) |
O3—V1—O1x | 49.07 (6) | V1—O3—V1iv | 96.17 (8) |
O5—V1—O1x | 137.13 (7) | V2x—O3—V1iv | 139.94 (9) |
O3iv—V1—O1x | 129.62 (7) | V1—O3—V2iv | 97.48 (8) |
O4iv—V1—O1x | 99.95 (6) | V2x—O3—V2iv | 81.73 (7) |
O3ix—V1—O1x | 137.53 (5) | V1iv—O3—V2iv | 87.57 (7) |
O4—V1—O1x | 83.92 (5) | V1—O3—V1x | 173.87 (9) |
O5viii—V1—O1x | 48.97 (3) | V2x—O3—V1x | 62.74 (5) |
O1vii—V1—O1x | 85.47 (5) | V1iv—O3—V1x | 77.77 (6) |
O3viii—V1—O1x | 98.47 (5) | V2iv—O3—V1x | 83.34 (5) |
O2iv—V1—O1x | 94.63 (5) | V1—O3—V1viii | 58.88 (5) |
O2—V1—O2v | 100.14 (8) | V2x—O3—V1viii | 78.11 (6) |
O4vii—V1—O2v | 130.01 (7) | V1iv—O3—V1viii | 124.33 (8) |
O3—V1—O2v | 126.62 (6) | V2iv—O3—V1viii | 53.23 (4) |
O5—V1—O2v | 47.13 (7) | V1x—O3—V1viii | 125.40 (5) |
O3iv—V1—O2v | 46.29 (6) | V1—O3—V2 | 55.45 (5) |
O4iv—V1—O2v | 78.95 (6) | V2x—O3—V2 | 145.08 (8) |
O4—V1—O2v | 92.93 (5) | V1iv—O3—V2 | 61.59 (5) |
O5viii—V1—O2v | 129.97 (3) | V2iv—O3—V2 | 132.45 (7) |
O1vii—V1—O2v | 98.67 (5) | V1x—O3—V2 | 119.77 (6) |
O3viii—V1—O2v | 84.37 (5) | V1viii—O3—V2 | 114.21 (5) |
O2iv—V1—O2v | 81.36 (4) | V1xiii—O4—V2 | 93.12 (8) |
O1x—V1—O2v | 175.66 (5) | V1xiii—O4—V1iv | 97.42 (8) |
O2—V1—O1xi | 45.91 (8) | V2—O4—V1iv | 105.46 (9) |
O4vii—V1—O1xi | 58.15 (7) | V1xiii—O4—V2xvii | 80.80 (6) |
O3—V1—O1xi | 86.78 (6) | V2—O4—V2xvii | 169.87 (9) |
O5—V1—O1xi | 105.58 (4) | V1iv—O4—V2xvii | 83.47 (6) |
O3iv—V1—O1xi | 132.34 (7) | V1xiii—O4—V1 | 136.22 (9) |
O4iv—V1—O1xi | 137.52 (7) | V2—O4—V1 | 61.55 (5) |
O3ix—V1—O1xi | 98.35 (5) | V1iv—O4—V1 | 61.06 (5) |
O4—V1—O1xi | 85.40 (5) | V2xvii—O4—V1 | 128.19 (6) |
O5viii—V1—O1xi | 89.68 (3) | V1xiii—O4—V2xvi | 61.21 (5) |
O1vii—V1—O1xi | 48.03 (6) | V2—O4—V2xvi | 135.60 (8) |
O3viii—V1—O1xi | 100.32 (5) | V1iv—O4—V2xvi | 50.02 (4) |
O2iv—V1—O1xi | 134.31 (5) | V2xvii—O4—V2xvi | 47.56 (3) |
O1x—V1—O1xi | 45.02 (5) | V1—O4—V2xvi | 111.07 (5) |
O2v—V1—O1xi | 137.86 (4) | V1xiii—O4—V2v | 72.45 (6) |
O2—V1—O1i | 138.58 (7) | V2—O4—V2v | 47.07 (5) |
O4vii—V1—O1i | 89.89 (7) | V1iv—O4—V2v | 67.16 (5) |
O3—V1—O1i | 123.14 (6) | V2xvii—O4—V2v | 136.48 (6) |
O3iv—V1—O1i | 81.84 (7) | V1—O4—V2v | 64.17 (3) |
O3ix—V1—O1i | 85.75 (5) | V2xvi—O4—V2v | 89.14 (4) |
O4—V1—O1i | 132.71 (5) | V1—O5—V1v | 123.03 (14) |
O5viii—V1—O1i | 89.55 (4) | V1—O5—V2i | 133.17 (5) |
O1vii—V1—O1i | 94.44 (6) | V1v—O5—V2i | 89.62 (3) |
O2iv—V1—O1i | 81.86 (5) | V1—O5—V2vii | 89.62 (3) |
O1x—V1—O1i | 134.96 (3) | V1v—O5—V2vii | 133.17 (5) |
O2v—V1—O1i | 46.34 (4) | V2i—O5—V2vii | 89.47 (11) |
O1xi—V1—O1i | 139.48 (3) | V1—O5—V1xiv | 155.99 (2) |
O1—V2—O4 | 106.40 (10) | V1v—O5—V1xiv | 60.95 (3) |
O1—V2—O2 | 97.03 (10) | V2i—O5—V1xiv | 66.80 (4) |
O4—V2—O2 | 90.11 (8) | V2vii—O5—V1xiv | 75.91 (5) |
O1—V2—O5xiii | 108.83 (10) | V1—O5—V1viii | 60.95 (3) |
O4—V2—O5xiii | 84.53 (6) | V1v—O5—V1viii | 155.99 (2) |
O2—V2—O5xiii | 154.08 (8) | V2i—O5—V1viii | 75.91 (5) |
O1—V2—O3ix | 101.07 (9) | V2vii—O5—V1viii | 66.80 (4) |
O4—V2—O3ix | 152.45 (8) | V1xiv—O5—V1viii | 126.69 (8) |
O2—V2—O3ix | 88.67 (8) | V1—O5—V2 | 51.34 (6) |
O5xiii—V2—O3ix | 84.64 (7) | V1v—O5—V2 | 74.85 (8) |
O1—V2—O3iv | 172.76 (10) | V2i—O5—V2 | 156.99 (7) |
O4—V2—O3iv | 76.34 (7) | V2vii—O5—V2 | 113.54 (4) |
O2—V2—O3iv | 76.14 (7) | V1xiv—O5—V2 | 117.15 (4) |
O5xiii—V2—O3iv | 77.95 (7) | V1viii—O5—V2 | 112.16 (4) |
O3ix—V2—O3iv | 76.65 (8) | V1—O5—V2v | 74.85 (8) |
O1—V2—O4xx | 65.21 (8) | V1v—O5—V2v | 51.34 (6) |
O4—V2—O4xx | 130.46 (3) | V2i—O5—V2v | 113.54 (4) |
O2—V2—O4xx | 138.09 (6) | V2vii—O5—V2v | 156.99 (7) |
O5xiii—V2—O4xx | 57.07 (4) | V1xiv—O5—V2v | 112.16 (4) |
O3ix—V2—O4xx | 60.71 (6) | V1viii—O5—V2v | 117.15 (4) |
O3iv—V2—O4xx | 118.37 (6) |
Symmetry codes: (i) −x+1, y−1, −z+1/2; (ii) x−1, y−1, z; (iii) x−1, −y+1, z−1/2; (iv) −x+1, −y+1, −z+1; (v) −x+1, y, −z+1/2; (vi) x−1, y, z; (vii) x, y−1, z; (viii) −x+1, −y, −z+1; (ix) x, −y+1, z−1/2; (x) x, −y+1, z+1/2; (xi) −x+2, −y+1, −z+1; (xii) x+1, y, z; (xiii) x, y+1, z; (xiv) x, −y, z−1/2; (xv) x, −y, z+1/2; (xvi) −x+1, −y+2, −z+1; (xvii) x, −y+2, z+1/2; (xviii) −x+1, y+1, −z+1/2; (xix) −x+1, y, −z+3/2; (xx) x, −y+2, z−1/2; (xxi) −x+2, −y+2, −z+1; (xxii) x+1, y+1, z; (xxiii) −x+2, y, −z+1/2. |
O9V4·Ba | F(000) = 440 |
Mr = 485.1 | Dx = 4.907 Mg m−3 Dm = 4.907 Mg m−3 Dm measured by not measured |
Monoclinic, P2/c | Melting point: 0 K |
Hall symbol: -P 2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 7.6303 (12) Å | Cell parameters from 7092 reflections |
b = 4.9405 (7) Å | θ = 2.9–32.2° |
c = 9.3547 (14) Å | µ = 11.42 mm−1 |
β = 111.395 (11)° | T = 250 K |
V = 328.35 (9) Å3 | Parallelepiped, dark blue |
Z = 2 | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
STOE IPDS 2 diffractometer | 1025 reflections with I > 2σ(I) |
Rotation method scans | Rint = 0.044 |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | θmax = 32°, θmin = 2.9° |
Tmin = 0.09, Tmax = 0.19 | h = −11→11 |
5369 measured reflections | k = −7→7 |
1125 independent reflections | l = −13→13 |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.010P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.022 | (Δ/σ)max < 0.001 |
wR(F2) = 0.038 | Δρmax = 0.72 e Å−3 |
S = 1.41 | Δρmin = −0.76 e Å−3 |
1125 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
66 parameters | Extinction coefficient: 0.0087 (7) |
0 restraints |
O9V4·Ba | V = 328.35 (9) Å3 |
Mr = 485.1 | Z = 2 |
Monoclinic, P2/c | Mo Kα radiation |
a = 7.6303 (12) Å | µ = 11.42 mm−1 |
b = 4.9405 (7) Å | T = 250 K |
c = 9.3547 (14) Å | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
β = 111.395 (11)° |
STOE IPDS 2 diffractometer | 1125 independent reflections |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | 1025 reflections with I > 2σ(I) |
Tmin = 0.09, Tmax = 0.19 | Rint = 0.044 |
5369 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 66 parameters |
wR(F2) = 0.038 | 0 restraints |
S = 1.41 | Δρmax = 0.72 e Å−3 |
1125 reflections | Δρmin = −0.76 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. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0 | 0.34046 (5) | 0.25 | 0.00928 (7) | |
V1 | 0.57371 (6) | 0.25063 (9) | 0.45061 (5) | 0.00519 (9) | |
V2 | 0.68899 (6) | 0.77267 (9) | 0.34971 (5) | 0.00521 (9) | |
O1 | 0.8919 (3) | 0.8673 (4) | 0.3484 (2) | 0.0099 (3) | |
O2 | 0.7700 (2) | 0.4151 (4) | 0.4463 (2) | 0.0074 (3) | |
O3 | 0.5809 (2) | 0.4151 (4) | 0.64559 (19) | 0.0062 (3) | |
O4 | 0.6741 (2) | 0.9087 (4) | 0.5410 (2) | 0.0058 (3) | |
O5 | 0.5 | 0.0599 (5) | 0.25 | 0.0055 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.00998 (10) | 0.00815 (11) | 0.00977 (10) | 0 | 0.00367 (7) | 0 |
V1 | 0.00716 (18) | 0.00415 (18) | 0.00448 (17) | −0.00072 (13) | 0.00242 (14) | −0.00003 (13) |
V2 | 0.00591 (17) | 0.0050 (2) | 0.00470 (17) | −0.00042 (12) | 0.00198 (13) | 0.00028 (13) |
O1 | 0.0092 (7) | 0.0103 (9) | 0.0106 (8) | −0.0010 (7) | 0.0040 (6) | 0.0006 (7) |
O2 | 0.0083 (7) | 0.0063 (8) | 0.0078 (7) | −0.0001 (6) | 0.0032 (6) | 0.0019 (6) |
O3 | 0.0092 (7) | 0.0058 (8) | 0.0033 (7) | 0.0009 (6) | 0.0020 (6) | 0.0003 (6) |
O4 | 0.0072 (7) | 0.0045 (8) | 0.0057 (7) | 0.0007 (6) | 0.0025 (6) | 0.0003 (6) |
O5 | 0.0092 (10) | 0.0051 (11) | 0.0019 (10) | 0 | 0.0015 (8) | 0 |
Ba1—O1i | 2.747 (2) | V2—V1ix | 3.5114 (8) |
Ba1—O1ii | 2.747 (2) | V2—Ba1xii | 3.5604 (6) |
Ba1—O4iii | 2.8242 (18) | V2—O3 | 3.6233 (18) |
Ba1—O4iv | 2.8242 (18) | V2—O4xvi | 3.6422 (18) |
Ba1—O1v | 2.976 (2) | V2—V1xviii | 3.6576 (7) |
Ba1—O1vi | 2.976 (2) | V2—Ba1iv | 3.6719 (8) |
Ba1—O2vi | 2.9898 (17) | V2—O4vi | 3.7543 (19) |
Ba1—O2v | 2.9898 (17) | V2—O5 | 3.791 (3) |
Ba1—O2iv | 2.9957 (19) | V2—V1vi | 3.8018 (7) |
Ba1—O2iii | 2.9957 (19) | V2—O1xxi | 3.844 (2) |
Ba1—O3iv | 3.2189 (18) | V2—O2xi | 3.9745 (19) |
Ba1—O3iii | 3.2189 (18) | V2—O2vi | 3.997 (2) |
V1—O2 | 1.7172 (18) | V2—Ba1xxii | 3.9982 (6) |
V1—O4vii | 1.9190 (19) | V2—O2ix | 4.1457 (18) |
V1—O3 | 1.9792 (17) | V2—V2vii | 4.9405 (7) |
V1—O5 | 1.9890 (14) | V2—V2xiii | 4.9405 (7) |
V1—O3iv | 2.0381 (19) | V2—V2xxi | 5.0736 (11) |
V1—O4iv | 2.0758 (18) | V2—V2xvii | 5.1887 (7) |
V1—V2vii | 2.8012 (7) | V2—V2xx | 5.1887 (8) |
V1—V2 | 2.9870 (7) | V2—V2xvi | 5.2141 (10) |
V1—V1iv | 2.9915 (9) | V2—V1xi | 5.2426 (11) |
V1—V1viii | 3.0018 (9) | V2—V2xi | 5.2873 (11) |
V1—V2iv | 3.2019 (7) | V2—V2ix | 5.3979 (8) |
V1—O3ix | 3.3145 (18) | V2—V2x | 5.3979 (8) |
V1—O4 | 3.376 (2) | V2—V2iv | 5.4222 (10) |
V1—O5viii | 3.4151 (13) | V2—V2i | 5.6817 (8) |
V1—O1vii | 3.477 (2) | V2—V2xviii | 5.6817 (8) |
V1—O3viii | 3.499 (2) | V2—V2xxiii | 5.6979 (11) |
V1—V1vi | 3.5031 (10) | V2—V1xvi | 5.7899 (9) |
V1—V2x | 3.5114 (8) | V2—V1xx | 5.9666 (9) |
V1—O2iv | 3.5187 (18) | V2—V1viii | 5.9832 (9) |
V1—V2i | 3.6576 (7) | V2—V1x | 5.9994 (10) |
V1—O1x | 3.673 (2) | V2—V1xiv | 6.1544 (9) |
V1—O2vi | 3.771 (2) | O1—Ba1xxii | 2.747 (2) |
V1—V2vi | 3.8018 (7) | O1—Ba1xii | 2.976 (2) |
V1—O1xi | 3.861 (2) | O1—V1xiii | 3.477 (2) |
V1—Ba1iv | 3.9823 (7) | O1—V1ix | 3.673 (2) |
V1—O1i | 4.097 (2) | O1—V2xxi | 3.844 (2) |
V1—Ba1xii | 4.3304 (7) | O1—V1xi | 3.861 (2) |
V1—Ba1viii | 4.5062 (7) | O1—V1xviii | 4.097 (2) |
V1—V1vii | 4.9405 (7) | O2—Ba1xii | 2.9898 (17) |
V1—V1xiii | 4.9405 (7) | O2—Ba1iv | 2.9957 (19) |
V1—V2xi | 5.2426 (11) | O2—V2vii | 3.296 (2) |
V1—V1x | 5.2867 (8) | O2—V1iv | 3.5187 (18) |
V1—V1ix | 5.2867 (8) | O2—V1vi | 3.771 (2) |
V1—V1xiv | 5.2925 (8) | O2—V2xi | 3.9745 (19) |
V1—V1xv | 5.2925 (8) | O2—V2vi | 3.997 (2) |
V1—V2xvi | 5.7899 (8) | O2—V2x | 4.1458 (18) |
V1—V2xvii | 5.9666 (9) | O3—V2x | 2.0095 (18) |
V1—V2viii | 5.9832 (9) | O3—V1iv | 2.0381 (19) |
V1—V2ix | 5.9994 (10) | O3—V2iv | 2.2735 (18) |
V1—V1i | 6.0564 (8) | O3—Ba1iv | 3.2189 (18) |
V1—V1xviii | 6.0564 (8) | O3—V1x | 3.3145 (18) |
V1—V1xix | 6.1023 (12) | O3—V1viii | 3.499 (2) |
V1—V2xv | 6.1544 (9) | O4—V1xiii | 1.9190 (19) |
V2—O1 | 1.6217 (19) | O4—V1iv | 2.0758 (18) |
V2—O4 | 1.9529 (18) | O4—Ba1iv | 2.8242 (18) |
V2—O2 | 1.978 (2) | O4—V2xvii | 3.2548 (18) |
V2—O5xiii | 1.995 (2) | O4—V2xvi | 3.6422 (17) |
V2—O3ix | 2.0095 (18) | O4—V2vi | 3.7543 (19) |
V2—O3iv | 2.2735 (18) | O5—V1vi | 1.9890 (14) |
V2—V1xiii | 2.8012 (7) | O5—V2i | 1.995 (2) |
V2—V2vi | 2.8059 (10) | O5—V2vii | 1.995 (2) |
V2—V1iv | 3.2019 (7) | O5—V1xiv | 3.4151 (13) |
V2—O4xx | 3.2548 (18) | O5—V1viii | 3.4151 (13) |
V2—O2xiii | 3.296 (2) | O5—V2vi | 3.791 (3) |
O1i—Ba1—O1ii | 63.36 (8) | O4xx—V2—O4xvi | 104.84 (5) |
O1i—Ba1—O4iii | 72.13 (5) | O2xiii—V2—O4xvi | 65.96 (4) |
O1ii—Ba1—O4iii | 64.22 (6) | O3—V2—O4xvi | 65.65 (4) |
O1i—Ba1—O4iv | 64.22 (5) | O1—V2—O4vi | 107.99 (7) |
O1ii—Ba1—O4iv | 72.13 (5) | O4—V2—O4vi | 124.14 (6) |
O4iii—Ba1—O4iv | 128.32 (8) | O2—V2—O4vi | 126.95 (6) |
O1i—Ba1—O1v | 177.32 (4) | O3iv—V2—O4vi | 74.93 (5) |
O1ii—Ba1—O1v | 119.31 (6) | O2xiii—V2—O4vi | 95.30 (4) |
O4iii—Ba1—O1v | 108.79 (5) | O3—V2—O4vi | 122.55 (4) |
O4iv—Ba1—O1v | 116.12 (5) | O4xvi—V2—O4vi | 80.17 (4) |
O1i—Ba1—O1vi | 119.31 (6) | O1—V2—O5 | 122.99 (8) |
O1ii—Ba1—O1vi | 177.32 (4) | O4—V2—O5 | 113.64 (6) |
O4iii—Ba1—O1vi | 116.12 (5) | O2—V2—O5 | 46.37 (6) |
O4iv—Ba1—O1vi | 108.79 (5) | O5xiii—V2—O5 | 113.60 (4) |
O1v—Ba1—O1vi | 58.01 (7) | O3ix—V2—O5 | 49.45 (5) |
O1i—Ba1—O2vi | 65.41 (5) | O3iv—V2—O5 | 50.19 (5) |
O1ii—Ba1—O2vi | 128.75 (6) | O4xx—V2—O5 | 110.12 (4) |
O4iii—Ba1—O2vi | 101.21 (5) | O2xiii—V2—O5 | 168.08 (3) |
O4iv—Ba1—O2vi | 85.01 (5) | O3—V2—O5 | 64.08 (3) |
O1v—Ba1—O2vi | 111.91 (5) | O4xvi—V2—O5 | 102.16 (3) |
O1vi—Ba1—O2vi | 53.92 (5) | O4vi—V2—O5 | 81.22 (3) |
O1i—Ba1—O2v | 128.75 (6) | O1—V2—O1xxi | 48.03 (9) |
O1ii—Ba1—O2v | 65.41 (5) | O4—V2—O1xxi | 58.58 (6) |
O4iii—Ba1—O2v | 85.01 (5) | O2—V2—O1xxi | 92.31 (7) |
O4iv—Ba1—O2v | 101.21 (5) | O5xiii—V2—O1xxi | 106.26 (6) |
O1v—Ba1—O2v | 53.92 (5) | O3ix—V2—O1xxi | 148.74 (6) |
O1vi—Ba1—O2v | 111.91 (5) | O3iv—V2—O1xxi | 133.73 (5) |
O2vi—Ba1—O2v | 165.83 (8) | O4xx—V2—O1xxi | 100.28 (5) |
O1i—Ba1—O2iv | 121.16 (6) | O2xiii—V2—O1xxi | 47.97 (5) |
O1ii—Ba1—O2iv | 99.72 (5) | O3—V2—O1xxi | 91.42 (4) |
O4iii—Ba1—O2iv | 153.60 (5) | O4xvi—V2—O1xxi | 96.19 (4) |
O4iv—Ba1—O2iv | 57.02 (5) | O4vi—V2—O1xxi | 138.84 (4) |
O1v—Ba1—O2iv | 59.10 (5) | O5—V2—O1xxi | 138.64 (4) |
O1vi—Ba1—O2iv | 78.95 (5) | O4—V2—O2xi | 92.17 (6) |
O2vi—Ba1—O2iv | 105.11 (5) | O2—V2—O2xi | 58.37 (7) |
O2v—Ba1—O2iv | 68.89 (6) | O5xiii—V2—O2xi | 146.86 (6) |
O1i—Ba1—O2iii | 99.72 (5) | O3ix—V2—O2xi | 110.06 (6) |
O1ii—Ba1—O2iii | 121.16 (6) | O3iv—V2—O2xi | 133.23 (6) |
O4iii—Ba1—O2iii | 57.02 (5) | O4xx—V2—O2xi | 103.47 (4) |
O4iv—Ba1—O2iii | 153.60 (5) | O2xiii—V2—O2xi | 92.01 (4) |
O1v—Ba1—O2iii | 78.95 (5) | O3—V2—O2xi | 90.31 (4) |
O1vi—Ba1—O2iii | 59.10 (5) | O4xvi—V2—O2xi | 136.82 (4) |
O2vi—Ba1—O2iii | 68.89 (6) | O4vi—V2—O2xi | 141.03 (4) |
O2v—Ba1—O2iii | 105.11 (5) | O5—V2—O2xi | 97.85 (3) |
O2iv—Ba1—O2iii | 132.45 (7) | O1xxi—V2—O2xi | 46.79 (4) |
O1i—Ba1—O3iv | 91.98 (5) | O1—V2—O2vi | 136.05 (7) |
O1ii—Ba1—O3iv | 127.16 (5) | O4—V2—O2vi | 117.23 (6) |
O4iii—Ba1—O3iv | 154.17 (4) | O2—V2—O2vi | 88.30 (8) |
O4iv—Ba1—O3iv | 55.04 (5) | O5xiii—V2—O2vi | 71.90 (6) |
O1v—Ba1—O3iv | 86.26 (5) | O4xx—V2—O2vi | 82.00 (4) |
O1vi—Ba1—O3iv | 53.77 (5) | O2xiii—V2—O2vi | 130.15 (4) |
O2vi—Ba1—O3iv | 53.08 (5) | O3—V2—O2vi | 85.84 (4) |
O2v—Ba1—O3iv | 120.55 (5) | O4xvi—V2—O2vi | 79.73 (4) |
O2iv—Ba1—O3iv | 52.22 (4) | O1xxi—V2—O2vi | 175.75 (4) |
O2iii—Ba1—O3iv | 108.06 (5) | O2xi—V2—O2vi | 136.35 (2) |
O1i—Ba1—O3iii | 127.16 (5) | O1—V2—O2ix | 66.30 (7) |
O1ii—Ba1—O3iii | 91.98 (5) | O4—V2—O2ix | 171.42 (6) |
O4iii—Ba1—O3iii | 55.04 (5) | O2—V2—O2ix | 95.19 (5) |
O4iv—Ba1—O3iii | 154.17 (4) | O5xiii—V2—O2ix | 93.20 (3) |
O1v—Ba1—O3iii | 53.77 (5) | O3iv—V2—O2ix | 111.29 (5) |
O1vi—Ba1—O3iii | 86.26 (5) | O2xiii—V2—O2ix | 112.93 (4) |
O2vi—Ba1—O3iii | 120.55 (5) | O3—V2—O2ix | 137.51 (4) |
O2v—Ba1—O3iii | 53.08 (5) | O4xvi—V2—O2ix | 137.19 (4) |
O2iv—Ba1—O3iii | 108.06 (5) | O4vi—V2—O2ix | 57.04 (4) |
O2iii—Ba1—O3iii | 52.22 (4) | O5—V2—O2ix | 74.80 (3) |
O3iv—Ba1—O3iii | 135.93 (7) | O1xxi—V2—O2ix | 114.33 (4) |
O2—V1—O4vii | 102.45 (8) | O2xi—V2—O2ix | 84.91 (4) |
O2—V1—O3 | 95.53 (8) | O2vi—V2—O2ix | 69.78 (4) |
O4vii—V1—O3 | 94.77 (8) | V2—O1—Ba1xxii | 130.68 (11) |
O2—V1—O5 | 98.67 (7) | V2—O1—Ba1xii | 97.09 (9) |
O4vii—V1—O5 | 85.90 (9) | Ba1xxii—O1—Ba1xii | 119.31 (6) |
O3—V1—O5 | 165.30 (6) | V2—O1—V1xiii | 52.45 (6) |
O2—V1—O3iv | 88.59 (8) | Ba1xxii—O1—V1xiii | 87.34 (6) |
O4vii—V1—O3iv | 168.95 (7) | Ba1xii—O1—V1xiii | 149.49 (7) |
O3—V1—O3iv | 83.75 (7) | V2—O1—V1ix | 71.43 (7) |
O5—V1—O3iv | 92.78 (8) | Ba1xxii—O1—V1ix | 87.91 (5) |
O2—V1—O4iv | 174.01 (8) | Ba1xii—O1—V1ix | 72.73 (4) |
O4vii—V1—O4iv | 82.65 (8) | V1xiii—O1—V1ix | 95.45 (5) |
O3—V1—O4iv | 80.79 (7) | V2—O1—V2xxi | 131.97 (9) |
O5—V1—O4iv | 84.73 (6) | Ba1xxii—O1—V2xxi | 65.26 (4) |
O3iv—V1—O4iv | 86.31 (7) | Ba1xii—O1—V2xxi | 112.46 (6) |
O2—V1—O3ix | 57.01 (7) | V1xiii—O1—V2xxi | 91.33 (5) |
O4vii—V1—O3ix | 133.51 (6) | V1ix—O1—V2xxi | 152.00 (6) |
O3—V1—O3ix | 125.82 (3) | V2—O1—V1xi | 142.62 (10) |
O5—V1—O3ix | 60.77 (7) | Ba1xxii—O1—V1xi | 84.19 (5) |
O3iv—V1—O3ix | 53.47 (7) | Ba1xii—O1—V1xi | 69.89 (4) |
O4iv—V1—O3ix | 121.53 (6) | V1xiii—O1—V1xi | 131.89 (6) |
O2—V1—O4 | 55.26 (7) | V1ix—O1—V1xi | 131.28 (5) |
O4vii—V1—O4 | 136.04 (8) | V2—O1—V1xviii | 62.97 (6) |
O3—V1—O4 | 56.39 (6) | Ba1xxii—O1—V1xviii | 70.69 (4) |
O5—V1—O4 | 130.75 (7) | Ba1xii—O1—V1xviii | 117.53 (6) |
O3iv—V1—O4 | 51.11 (6) | V1xiii—O1—V1xviii | 54.35 (3) |
O4iv—V1—O4 | 118.83 (5) | V1ix—O1—V1xviii | 45.04 (3) |
O3ix—V1—O4 | 70.26 (4) | V2xxi—O1—V1xviii | 124.71 (6) |
O2—V1—O5viii | 129.63 (6) | V1xi—O1—V1xviii | 154.29 (6) |
O4vii—V1—O5viii | 53.27 (6) | V1—O2—V2 | 107.67 (9) |
O3—V1—O5viii | 52.13 (7) | V1—O2—Ba1xii | 131.96 (9) |
O5—V1—O5viii | 119.11 (3) | V2—O2—Ba1xii | 89.16 (6) |
O3iv—V1—O5viii | 118.96 (6) | V1—O2—Ba1iv | 112.49 (8) |
O4iv—V1—O5viii | 51.23 (5) | V2—O2—Ba1iv | 92.89 (7) |
O3ix—V1—O5viii | 171.57 (4) | Ba1xii—O2—Ba1iv | 111.11 (6) |
O4—V1—O5viii | 108.51 (5) | V1—O2—V2vii | 58.20 (6) |
O2—V1—O1vii | 63.17 (7) | V2—O2—V2vii | 137.64 (8) |
O4vii—V1—O1vii | 55.60 (6) | Ba1xii—O2—V2vii | 78.83 (4) |
O3—V1—O1vii | 133.60 (6) | Ba1iv—O2—V2vii | 129.39 (6) |
O5—V1—O1vii | 57.86 (4) | V1—O2—V1iv | 58.13 (5) |
O3iv—V1—O1vii | 132.05 (6) | V2—O2—V1iv | 64.28 (5) |
O4iv—V1—O1vii | 122.75 (6) | Ba1xii—O2—V1iv | 152.80 (7) |
O3ix—V1—O1vii | 78.60 (5) | Ba1iv—O2—V1iv | 77.77 (4) |
O4—V1—O1vii | 118.42 (5) | V2vii—O2—V1iv | 116.31 (5) |
O5viii—V1—O1vii | 108.73 (5) | V1—O2—V1vi | 67.79 (6) |
O2—V1—O3viii | 130.82 (7) | V2—O2—V1vi | 75.73 (6) |
O4vii—V1—O3viii | 47.83 (6) | Ba1xii—O2—V1vi | 73.86 (4) |
O3—V1—O3viii | 121.08 (5) | Ba1iv—O2—V1vi | 167.73 (7) |
O5—V1—O3viii | 50.15 (7) | V2vii—O2—V1vi | 61.91 (3) |
O3iv—V1—O3viii | 124.17 (7) | V1iv—O2—V1vi | 92.92 (4) |
O4iv—V1—O3viii | 55.05 (6) | V1—O2—V2xi | 129.81 (8) |
O3ix—V1—O3viii | 110.90 (3) | V2—O2—V2xi | 121.63 (7) |
O4—V1—O3viii | 173.67 (4) | Ba1xii—O2—V2xi | 61.74 (3) |
O5viii—V1—O3viii | 69.38 (5) | Ba1iv—O2—V2xi | 59.48 (3) |
O1vii—V1—O3viii | 67.73 (4) | V2vii—O2—V2xi | 87.99 (4) |
O2—V1—O2iv | 121.87 (5) | V1iv—O2—V2xi | 136.50 (5) |
O4vii—V1—O2iv | 120.67 (6) | V1vi—O2—V2xi | 130.54 (5) |
O3—V1—O2iv | 47.74 (6) | V1—O2—V2vi | 70.99 (6) |
O5—V1—O2iv | 119.91 (4) | Ba1xii—O2—V2vi | 101.03 (5) |
O3iv—V1—O2iv | 51.07 (5) | Ba1iv—O2—V2vi | 122.75 (6) |
O4iv—V1—O2iv | 52.22 (6) | V2vii—O2—V2vi | 101.92 (5) |
O3ix—V1—O2iv | 104.49 (5) | V1iv—O2—V2vi | 55.26 (3) |
O4—V1—O2iv | 66.61 (4) | V1vi—O2—V2vi | 45.11 (2) |
O5viii—V1—O2iv | 67.90 (4) | V2xi—O2—V2vi | 158.41 (5) |
O1vii—V1—O2iv | 174.92 (5) | V1—O2—V2x | 56.75 (5) |
O3viii—V1—O2iv | 107.26 (4) | V2—O2—V2x | 119.35 (7) |
O2—V1—O1x | 80.74 (7) | Ba1xii—O2—V2x | 147.92 (6) |
O4vii—V1—O1x | 53.42 (7) | Ba1iv—O2—V2x | 57.12 (3) |
O3—V1—O1x | 49.13 (6) | V2vii—O2—V2x | 87.64 (4) |
O5—V1—O1x | 137.36 (7) | V1iv—O2—V2x | 58.80 (3) |
O3iv—V1—O1x | 129.64 (6) | V1vi—O2—V2x | 124.55 (5) |
O4iv—V1—O1x | 100.14 (6) | V2xi—O2—V2x | 89.10 (4) |
O3ix—V1—O1x | 137.63 (5) | V2vi—O2—V2x | 110.22 (4) |
O4—V1—O1x | 83.88 (5) | V1—O3—V2x | 123.36 (9) |
O5viii—V1—O1x | 48.98 (3) | V1—O3—V1iv | 96.25 (7) |
O1vii—V1—O1x | 85.54 (4) | V2x—O3—V1iv | 139.86 (9) |
O3viii—V1—O1x | 98.50 (5) | V1—O3—V2iv | 97.45 (8) |
O2iv—V1—O1x | 94.59 (4) | V2x—O3—V2iv | 81.60 (6) |
O2—V1—O2vi | 100.02 (7) | V1iv—O3—V2iv | 87.53 (7) |
O4vii—V1—O2vi | 130.22 (6) | V1—O3—Ba1iv | 97.13 (6) |
O3—V1—O2vi | 126.47 (6) | V2x—O3—Ba1iv | 82.35 (6) |
O5—V1—O2vi | 46.95 (7) | V1iv—O3—Ba1iv | 100.42 (7) |
O3iv—V1—O2vi | 46.22 (6) | V2iv—O3—Ba1iv | 162.52 (7) |
O4iv—V1—O2vi | 78.65 (6) | V1—O3—V1x | 173.89 (8) |
O4—V1—O2vi | 92.97 (4) | V2x—O3—V1x | 62.74 (5) |
O5viii—V1—O2vi | 129.85 (3) | V1iv—O3—V1x | 77.75 (6) |
O1vii—V1—O2vi | 98.70 (4) | V2iv—O3—V1x | 83.52 (5) |
O3viii—V1—O2vi | 84.33 (4) | Ba1iv—O3—V1x | 83.02 (4) |
O2iv—V1—O2vi | 81.29 (4) | V1—O3—V1viii | 58.92 (5) |
O1x—V1—O2vi | 175.58 (4) | V2x—O3—V1viii | 78.08 (6) |
O2—V1—O1xi | 46.18 (7) | V1iv—O3—V1viii | 124.17 (7) |
O4vii—V1—O1xi | 58.12 (6) | V2iv—O3—V1viii | 53.04 (4) |
O3—V1—O1xi | 86.79 (6) | Ba1iv—O3—V1viii | 129.42 (5) |
O5—V1—O1xi | 105.83 (4) | V1x—O3—V1viii | 125.44 (5) |
O3iv—V1—O1xi | 132.49 (6) | V1—O3—V2 | 55.50 (4) |
O4iv—V1—O1xi | 137.65 (6) | V2x—O3—V2 | 145.29 (7) |
O3ix—V1—O1xi | 98.52 (4) | V1iv—O3—V2 | 61.58 (4) |
O4—V1—O1xi | 85.44 (4) | V2iv—O3—V2 | 132.37 (6) |
O5viii—V1—O1xi | 89.63 (3) | Ba1iv—O3—V2 | 64.60 (3) |
O1vii—V1—O1xi | 48.11 (6) | V1x—O3—V2 | 119.64 (6) |
O3viii—V1—O1xi | 100.40 (4) | V1viii—O3—V2 | 114.28 (5) |
O2iv—V1—O1xi | 134.24 (4) | V1xiii—O4—V2 | 92.68 (8) |
O1x—V1—O1xi | 44.96 (5) | V1xiii—O4—V1iv | 97.35 (8) |
O2vi—V1—O1xi | 138.03 (4) | V2—O4—V1iv | 105.23 (8) |
O2—V1—O1i | 138.51 (7) | V1xiii—O4—Ba1iv | 142.92 (9) |
O4vii—V1—O1i | 90.06 (6) | V2—O4—Ba1iv | 98.83 (7) |
O3—V1—O1i | 123.00 (6) | V1iv—O4—Ba1iv | 113.12 (7) |
O3iv—V1—O1i | 81.67 (6) | V1xiii—O4—V2xvii | 81.04 (6) |
O3ix—V1—O1i | 85.70 (4) | V2—O4—V2xvii | 169.90 (9) |
O4—V1—O1i | 132.62 (4) | V1iv—O4—V2xvii | 83.52 (5) |
O5viii—V1—O1i | 89.49 (4) | Ba1iv—O4—V2xvii | 81.92 (5) |
O1vii—V1—O1i | 94.54 (5) | V1xiii—O4—V1 | 136.04 (8) |
O2iv—V1—O1i | 81.77 (4) | V2—O4—V1 | 61.51 (5) |
O1x—V1—O1i | 134.96 (3) | V1iv—O4—V1 | 61.17 (5) |
O2vi—V1—O1i | 46.28 (4) | Ba1iv—O4—V1 | 79.38 (5) |
O1xi—V1—O1i | 139.60 (3) | V2xvii—O4—V1 | 128.26 (6) |
O1—V2—O4 | 106.41 (9) | V1xiii—O4—V2xvi | 61.38 (5) |
O1—V2—O2 | 96.93 (9) | V2—O4—V2xvi | 135.27 (7) |
O4—V2—O2 | 90.11 (8) | V1iv—O4—V2xvi | 49.96 (4) |
O1—V2—O5xiii | 108.72 (9) | Ba1iv—O4—V2xvi | 124.18 (6) |
O4—V2—O5xiii | 84.83 (6) | V2xvii—O4—V2xvi | 47.60 (3) |
O2—V2—O5xiii | 154.26 (7) | V1—O4—V2xvi | 111.11 (5) |
O1—V2—O3ix | 100.85 (8) | V1xiii—O4—V2vi | 72.22 (5) |
O4—V2—O3ix | 152.68 (7) | V2—O4—V2vi | 46.81 (4) |
O2—V2—O3ix | 88.46 (8) | V1iv—O4—V2vi | 67.06 (5) |
O5xiii—V2—O3ix | 84.72 (7) | Ba1iv—O4—V2vi | 138.31 (6) |
O1—V2—O3iv | 172.63 (9) | V2xvii—O4—V2vi | 136.46 (5) |
O4—V2—O3iv | 76.51 (7) | V1—O4—V2vi | 64.18 (3) |
O2—V2—O3iv | 76.17 (7) | V2xvi—O4—V2vi | 89.08 (4) |
O5xiii—V2—O3iv | 78.11 (6) | V1—O5—V1vi | 123.43 (14) |
O3ix—V2—O3iv | 76.66 (8) | V1—O5—V2i | 133.27 (5) |
O1—V2—O4xx | 65.07 (8) | V1vi—O5—V2i | 89.34 (3) |
O4—V2—O4xx | 130.67 (3) | V1—O5—V2vii | 89.34 (3) |
O2—V2—O4xx | 137.84 (6) | V1vi—O5—V2vii | 133.27 (5) |
O5xiii—V2—O4xx | 57.03 (3) | V2i—O5—V2vii | 89.35 (11) |
O3ix—V2—O4xx | 60.71 (6) | V1—O5—V1xiv | 155.800 (19) |
O3iv—V2—O4xx | 118.41 (6) | V1vi—O5—V1xiv | 60.89 (3) |
O1—V2—O2xiii | 68.93 (8) | V2i—O5—V1xiv | 66.69 (4) |
O4—V2—O2xiii | 59.03 (6) | V2vii—O5—V1xiv | 75.92 (5) |
O2—V2—O2xiii | 137.64 (8) | V1—O5—V1viii | 60.89 (3) |
O5xiii—V2—O2xiii | 58.31 (6) | V1vi—O5—V1viii | 155.800 (19) |
O3ix—V2—O2xiii | 132.52 (6) | V2i—O5—V1viii | 75.92 (5) |
O3iv—V2—O2xiii | 117.92 (6) | V2vii—O5—V1viii | 66.69 (4) |
O4xx—V2—O2xiii | 73.73 (5) | V1xiv—O5—V1viii | 126.62 (8) |
O1—V2—O3 | 129.06 (8) | V1—O5—V2 | 51.42 (6) |
O4—V2—O3 | 50.38 (6) | V1vi—O5—V2 | 75.12 (8) |
O2—V2—O3 | 48.38 (6) | V2i—O5—V2 | 157.04 (7) |
O5xiii—V2—O3 | 112.13 (4) | V2vii—O5—V2 | 113.60 (4) |
O3ix—V2—O3 | 111.83 (4) | V1xiv—O5—V2 | 117.22 (4) |
O3iv—V2—O3 | 47.63 (6) | V1viii—O5—V2 | 112.16 (3) |
O4xx—V2—O3 | 165.86 (4) | V1—O5—V2vi | 75.12 (8) |
O2xiii—V2—O3 | 109.41 (4) | V1vi—O5—V2vi | 51.42 (6) |
O1—V2—O4xvi | 134.72 (8) | V2i—O5—V2vi | 113.60 (4) |
O2—V2—O4xvi | 113.63 (6) | V2vii—O5—V2vi | 157.04 (7) |
O5xiii—V2—O4xvi | 47.93 (3) | V1xiv—O5—V2vi | 112.16 (3) |
O3ix—V2—O4xvi | 112.07 (6) | V1viii—O5—V2vi | 117.22 (4) |
O3iv—V2—O4xvi | 51.97 (5) |
Symmetry codes: (i) −x+1, y−1, −z+1/2; (ii) x−1, y−1, z; (iii) x−1, −y+1, z−1/2; (iv) −x+1, −y+1, −z+1; (v) x−1, y, z; (vi) −x+1, y, −z+1/2; (vii) x, y−1, z; (viii) −x+1, −y, −z+1; (ix) x, −y+1, z−1/2; (x) x, −y+1, z+1/2; (xi) −x+2, −y+1, −z+1; (xii) x+1, y, z; (xiii) x, y+1, z; (xiv) x, −y, z−1/2; (xv) x, −y, z+1/2; (xvi) −x+1, −y+2, −z+1; (xvii) x, −y+2, z+1/2; (xviii) −x+1, y+1, −z+1/2; (xix) −x+1, y, −z+3/2; (xx) x, −y+2, z−1/2; (xxi) −x+2, −y+2, −z+1; (xxii) x+1, y+1, z; (xxiii) −x+2, y, −z+1/2. |
O9V4·Ba | F(000) = 440 |
Mr = 485.1 | Dx = 4.915 Mg m−3 Dm = 4.915 Mg m−3 Dm measured by not measured |
Monoclinic, P2/c | Melting point: 0 K |
Hall symbol: -P 2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 7.6231 (12) Å | Cell parameters from 7300 reflections |
b = 4.9370 (7) Å | θ = 2.9–32.2° |
c = 9.3528 (14) Å | µ = 11.44 mm−1 |
β = 111.386 (11)° | T = 200 K |
V = 327.76 (9) Å3 | Parallelepiped, dark blue |
Z = 2 | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
STOE IPDS 2 diffractometer | 1025 reflections with I > 2σ(I) |
Rotation method scans | Rint = 0.043 |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | θmax = 32.0°, θmin = 2.9° |
Tmin = 0.09, Tmax = 0.19 | h = −11→11 |
5359 measured reflections | k = −7→7 |
1122 independent reflections | l = −13→13 |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.010P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.022 | (Δ/σ)max < 0.001 |
wR(F2) = 0.038 | Δρmax = 0.83 e Å−3 |
S = 1.46 | Δρmin = −0.77 e Å−3 |
1122 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
66 parameters | Extinction coefficient: 0.0077 (6) |
0 restraints |
O9V4·Ba | V = 327.76 (9) Å3 |
Mr = 485.1 | Z = 2 |
Monoclinic, P2/c | Mo Kα radiation |
a = 7.6231 (12) Å | µ = 11.44 mm−1 |
b = 4.9370 (7) Å | T = 200 K |
c = 9.3528 (14) Å | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
β = 111.386 (11)° |
STOE IPDS 2 diffractometer | 1122 independent reflections |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | 1025 reflections with I > 2σ(I) |
Tmin = 0.09, Tmax = 0.19 | Rint = 0.043 |
5359 measured reflections |
R[F2 > 2σ(F2)] = 0.022 | 66 parameters |
wR(F2) = 0.038 | 0 restraints |
S = 1.46 | Δρmax = 0.83 e Å−3 |
1122 reflections | Δρmin = −0.77 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. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0 | 0.34139 (5) | 0.25 | 0.00841 (7) | |
V1 | 0.57423 (6) | 0.25025 (9) | 0.45056 (5) | 0.00521 (9) | |
V2 | 0.68889 (6) | 0.77337 (9) | 0.34993 (5) | 0.00520 (9) | |
O1 | 0.8921 (3) | 0.8677 (4) | 0.3484 (2) | 0.0093 (3) | |
O2 | 0.7707 (3) | 0.4156 (4) | 0.4469 (2) | 0.0072 (3) | |
O3 | 0.5805 (3) | 0.4148 (4) | 0.64552 (19) | 0.0064 (3) | |
O4 | 0.6743 (2) | 0.9081 (4) | 0.5417 (2) | 0.0061 (3) | |
O5 | 0.5 | 0.0602 (5) | 0.25 | 0.0053 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.00936 (10) | 0.00726 (11) | 0.00881 (10) | 0 | 0.00354 (7) | 0 |
V1 | 0.00687 (18) | 0.00420 (19) | 0.00476 (18) | −0.00059 (13) | 0.00234 (14) | −0.00009 (14) |
V2 | 0.00577 (17) | 0.0051 (2) | 0.00484 (17) | −0.00029 (13) | 0.00206 (14) | 0.00032 (13) |
O1 | 0.0100 (8) | 0.0084 (9) | 0.0103 (8) | 0.0001 (6) | 0.0048 (6) | 0.0010 (7) |
O2 | 0.0086 (8) | 0.0058 (8) | 0.0076 (7) | −0.0002 (6) | 0.0034 (6) | 0.0004 (6) |
O3 | 0.0100 (8) | 0.0054 (8) | 0.0037 (7) | 0.0009 (6) | 0.0025 (6) | 0.0010 (6) |
O4 | 0.0071 (7) | 0.0048 (8) | 0.0064 (7) | 0.0010 (6) | 0.0025 (6) | 0.0005 (6) |
O5 | 0.0077 (10) | 0.0053 (11) | 0.0027 (10) | 0 | 0.0016 (8) | 0 |
Ba1—O1i | 2.747 (2) | V2—Ba1xii | 3.5585 (6) |
Ba1—O1ii | 2.747 (2) | V2—O3 | 3.6228 (18) |
Ba1—O4iii | 2.8195 (19) | V2—O4xvi | 3.6352 (17) |
Ba1—O4iv | 2.8195 (19) | V2—V1xviii | 3.6543 (7) |
Ba1—O1v | 2.971 (2) | V2—Ba1iv | 3.6708 (8) |
Ba1—O1vi | 2.971 (2) | V2—O4vi | 3.759 (2) |
Ba1—O2iv | 2.9863 (19) | V2—O5 | 3.790 (3) |
Ba1—O2iii | 2.9863 (19) | V2—V1vi | 3.8053 (8) |
Ba1—O2vi | 2.9875 (17) | V2—O1xxi | 3.838 (2) |
Ba1—O2v | 2.9875 (17) | V2—O2xi | 3.968 (2) |
Ba1—O3iv | 3.2173 (19) | V2—Ba1xxii | 3.9973 (6) |
Ba1—O3iii | 3.2173 (19) | V2—O2vi | 4.001 (2) |
V1—O2 | 1.7174 (19) | V2—O2ix | 4.1457 (18) |
V1—O4vii | 1.9203 (19) | V2—O1vi | 4.157 (2) |
V1—O3 | 1.9809 (17) | V2—V2xiii | 4.9370 (7) |
V1—O5 | 1.9861 (14) | V2—V2vii | 4.9370 (7) |
V1—O3iv | 2.0395 (19) | V2—V2xxi | 5.0671 (11) |
V1—O4iv | 2.0754 (18) | V2—V2xvii | 5.1842 (7) |
V1—V2vii | 2.7916 (7) | V2—V2xx | 5.1842 (7) |
V1—V2 | 2.9866 (7) | V2—V2xvi | 5.2036 (10) |
V1—V1iv | 2.9968 (9) | V2—V1xi | 5.2350 (11) |
V1—V1viii | 3.0009 (9) | V2—V2xi | 5.2871 (11) |
V1—V2iv | 3.2013 (7) | V2—V2ix | 5.3995 (8) |
V1—O3ix | 3.3128 (18) | V2—V2x | 5.3995 (8) |
V1—O4 | 3.374 (2) | V2—V2iv | 5.4181 (10) |
V1—O5viii | 3.4160 (13) | V2—V2ii | 5.6777 (8) |
V1—O1vii | 3.470 (2) | V2—V2xviii | 5.6777 (8) |
V1—O3viii | 3.494 (2) | V2—V2xxiii | 5.6972 (11) |
V1—V1vi | 3.5013 (10) | V2—V1xvi | 5.7854 (8) |
V1—V2x | 3.5140 (8) | V2—V1xx | 5.9642 (9) |
V1—O2iv | 3.5210 (18) | V2—V1viii | 5.9811 (9) |
V1—V2ii | 3.6543 (8) | V2—V1x | 5.9930 (10) |
V1—O1x | 3.672 (2) | V2—V1xiv | 6.1542 (9) |
V1—O2vi | 3.778 (2) | O1—Ba1xxii | 2.747 (2) |
V1—V2vi | 3.8053 (8) | O1—Ba1xii | 2.971 (2) |
V1—O1xi | 3.853 (2) | O1—V1xiii | 3.470 (2) |
V1—Ba1iv | 3.9766 (7) | O1—V1ix | 3.672 (2) |
V1—O1ii | 4.096 (2) | O1—V2xxi | 3.838 (2) |
V1—Ba1xii | 4.3238 (7) | O1—V1xi | 3.853 (2) |
V1—Ba1viii | 4.5034 (7) | O1—V1xviii | 4.096 (2) |
V1—V1vii | 4.9370 (7) | O1—V2vi | 4.157 (2) |
V1—V1xiii | 4.9370 (7) | O2—Ba1iv | 2.9863 (19) |
V1—V2xi | 5.2350 (11) | O2—Ba1xii | 2.9875 (17) |
V1—V1x | 5.2868 (7) | O2—V2vii | 3.294 (2) |
V1—V1ix | 5.2868 (8) | O2—V1iv | 3.5210 (18) |
V1—V1xiv | 5.2891 (8) | O2—V1vi | 3.778 (2) |
V1—V1xv | 5.2891 (7) | O2—V2xi | 3.968 (2) |
V1—V2xvi | 5.7854 (8) | O2—V2vi | 4.001 (2) |
V1—V2xvii | 5.9642 (9) | O2—V2x | 4.1457 (18) |
V1—V2viii | 5.9811 (9) | O3—V2x | 2.0122 (18) |
V1—V2ix | 5.9930 (10) | O3—V1iv | 2.0395 (19) |
V1—V1ii | 6.0525 (8) | O3—V2iv | 2.2685 (18) |
V1—V1xviii | 6.0525 (8) | O3—Ba1iv | 3.2173 (19) |
V1—V1xix | 6.1055 (12) | O3—V1x | 3.3128 (18) |
V1—V2xv | 6.1542 (9) | O3—V1viii | 3.494 (2) |
V2—O1 | 1.6227 (19) | O4—V1xiii | 1.9203 (19) |
V2—O4 | 1.9534 (18) | O4—V1iv | 2.0754 (18) |
V2—O2 | 1.979 (2) | O4—Ba1iv | 2.8195 (19) |
V2—O5xiii | 1.993 (2) | O4—V2xvii | 3.2503 (18) |
V2—O3ix | 2.0122 (18) | O4—V2xvi | 3.6352 (17) |
V2—O3iv | 2.2685 (18) | O4—V2vi | 3.759 (2) |
V2—V1xiii | 2.7916 (7) | O5—V1vi | 1.9861 (14) |
V2—V2vi | 2.8039 (10) | O5—V2ii | 1.993 (2) |
V2—V1iv | 3.2013 (7) | O5—V2vii | 1.993 (2) |
V2—O4xx | 3.2503 (18) | O5—V1xiv | 3.4160 (13) |
V2—O2xiii | 3.294 (2) | O5—V1viii | 3.4160 (13) |
V2—V1ix | 3.5140 (8) | O5—V2vi | 3.790 (3) |
O1i—Ba1—O1ii | 63.27 (8) | O3—V2—O4vi | 122.55 (4) |
O1i—Ba1—O4iii | 64.15 (6) | O4xvi—V2—O4vi | 80.20 (4) |
O1ii—Ba1—O4iii | 72.07 (5) | O1—V2—O5 | 122.86 (8) |
O1i—Ba1—O4iv | 72.07 (5) | O4—V2—O5 | 113.52 (6) |
O1ii—Ba1—O4iv | 64.15 (6) | O2—V2—O5 | 46.52 (6) |
O4iii—Ba1—O4iv | 128.19 (8) | O5xiii—V2—O5 | 113.58 (4) |
O1i—Ba1—O1v | 119.36 (6) | O3ix—V2—O5 | 49.40 (5) |
O1ii—Ba1—O1v | 177.37 (4) | O3iv—V2—O5 | 50.13 (5) |
O4iii—Ba1—O1v | 108.83 (5) | O4xx—V2—O5 | 110.10 (4) |
O4iv—Ba1—O1v | 116.19 (6) | O2xiii—V2—O5 | 168.21 (3) |
O1i—Ba1—O1vi | 177.37 (4) | O3—V2—O5 | 64.05 (3) |
O1ii—Ba1—O1vi | 119.36 (6) | O4xvi—V2—O5 | 102.19 (3) |
O4iii—Ba1—O1vi | 116.19 (5) | O4vi—V2—O5 | 81.11 (3) |
O4iv—Ba1—O1vi | 108.83 (5) | O1—V2—O1xxi | 48.13 (9) |
O1v—Ba1—O1vi | 58.02 (7) | O4—V2—O1xxi | 58.57 (6) |
O1i—Ba1—O2iv | 99.61 (5) | O2—V2—O1xxi | 92.09 (7) |
O1ii—Ba1—O2iv | 121.14 (6) | O5xiii—V2—O1xxi | 106.37 (7) |
O4iii—Ba1—O2iv | 153.46 (5) | O3ix—V2—O1xxi | 148.76 (6) |
O4iv—Ba1—O2iv | 57.07 (5) | O3iv—V2—O1xxi | 133.77 (5) |
O1v—Ba1—O2iv | 59.12 (5) | O4xx—V2—O1xxi | 100.30 (5) |
O1vi—Ba1—O2iv | 79.08 (5) | O2xiii—V2—O1xxi | 47.93 (5) |
O1i—Ba1—O2iii | 121.14 (6) | O3—V2—O1xxi | 91.43 (4) |
O1ii—Ba1—O2iii | 99.61 (5) | O4xvi—V2—O1xxi | 96.29 (4) |
O4iii—Ba1—O2iii | 57.07 (5) | O4vi—V2—O1xxi | 138.98 (4) |
O4iv—Ba1—O2iii | 153.46 (5) | O5—V2—O1xxi | 138.58 (4) |
O1v—Ba1—O2iii | 79.08 (5) | O4—V2—O2xi | 92.12 (6) |
O1vi—Ba1—O2iii | 59.12 (5) | O2—V2—O2xi | 58.13 (7) |
O2iv—Ba1—O2iii | 132.63 (8) | O5xiii—V2—O2xi | 146.95 (6) |
O1i—Ba1—O2vi | 128.67 (5) | O3ix—V2—O2xi | 109.96 (6) |
O1ii—Ba1—O2vi | 65.42 (5) | O3iv—V2—O2xi | 133.12 (6) |
O4iii—Ba1—O2vi | 101.14 (5) | O4xx—V2—O2xi | 103.44 (4) |
O4iv—Ba1—O2vi | 85.06 (5) | O2xiii—V2—O2xi | 92.01 (4) |
O1v—Ba1—O2vi | 111.95 (5) | O3—V2—O2xi | 90.31 (4) |
O1vi—Ba1—O2vi | 53.95 (5) | O4xvi—V2—O2xi | 137.01 (4) |
O2iv—Ba1—O2vi | 105.34 (5) | O4vi—V2—O2xi | 140.86 (4) |
O2iii—Ba1—O2vi | 68.71 (6) | O5—V2—O2xi | 97.73 (3) |
O1i—Ba1—O2v | 65.42 (5) | O1xxi—V2—O2xi | 46.85 (4) |
O1ii—Ba1—O2v | 128.67 (6) | O1—V2—O2vi | 135.89 (7) |
O4iii—Ba1—O2v | 85.06 (5) | O4—V2—O2vi | 117.30 (6) |
O4iv—Ba1—O2v | 101.14 (5) | O2—V2—O2vi | 88.51 (8) |
O1v—Ba1—O2v | 53.95 (5) | O5xiii—V2—O2vi | 71.83 (6) |
O1vi—Ba1—O2v | 111.95 (5) | O4xx—V2—O2vi | 81.96 (4) |
O2iv—Ba1—O2v | 68.71 (6) | O2xiii—V2—O2vi | 130.23 (4) |
O2iii—Ba1—O2v | 105.34 (5) | O3—V2—O2vi | 85.87 (4) |
O2vi—Ba1—O2v | 165.91 (8) | O4xvi—V2—O2vi | 79.69 (4) |
O1i—Ba1—O3iv | 127.05 (5) | O1xxi—V2—O2vi | 175.82 (4) |
O1ii—Ba1—O3iv | 91.97 (5) | O2xi—V2—O2vi | 136.23 (2) |
O4iii—Ba1—O3iv | 154.23 (4) | O1—V2—O2ix | 66.17 (7) |
O4iv—Ba1—O3iv | 54.99 (5) | O4—V2—O2ix | 171.57 (6) |
O1v—Ba1—O3iv | 86.30 (5) | O2—V2—O2ix | 95.10 (5) |
O1vi—Ba1—O3iv | 53.86 (5) | O5xiii—V2—O2ix | 93.22 (3) |
O2iv—Ba1—O3iv | 52.31 (4) | O3iv—V2—O2ix | 111.24 (5) |
O2iii—Ba1—O3iv | 108.11 (5) | O2xiii—V2—O2ix | 113.00 (4) |
O2vi—Ba1—O3iv | 53.22 (5) | O3—V2—O2ix | 137.37 (4) |
O2v—Ba1—O3iv | 120.46 (5) | O4xvi—V2—O2ix | 137.18 (4) |
O1i—Ba1—O3iii | 91.97 (5) | O4vi—V2—O2ix | 57.00 (4) |
O1ii—Ba1—O3iii | 127.05 (5) | O5—V2—O2ix | 74.71 (3) |
O4iii—Ba1—O3iii | 54.99 (5) | O1xxi—V2—O2ix | 114.30 (4) |
O4iv—Ba1—O3iii | 154.23 (4) | O2xi—V2—O2ix | 84.75 (4) |
O1v—Ba1—O3iii | 53.86 (5) | O2vi—V2—O2ix | 69.75 (4) |
O1vi—Ba1—O3iii | 86.30 (5) | O1—V2—O1vi | 146.02 (8) |
O2iv—Ba1—O3iii | 108.11 (5) | O4—V2—O1vi | 87.91 (6) |
O2iii—Ba1—O3iii | 52.31 (4) | O2—V2—O1vi | 114.26 (6) |
O2vi—Ba1—O3iii | 120.46 (5) | O3ix—V2—O1vi | 68.05 (6) |
O2v—Ba1—O3iii | 53.22 (5) | O4xx—V2—O1vi | 82.17 (4) |
O3iv—Ba1—O3iii | 136.07 (7) | O2xiii—V2—O1vi | 94.53 (5) |
O2—V1—O4vii | 102.64 (8) | O3—V2—O1vi | 83.85 (4) |
O2—V1—O3 | 95.46 (8) | O5—V2—O1vi | 75.33 (3) |
O4vii—V1—O3 | 94.60 (8) | O1xxi—V2—O1vi | 137.90 (3) |
O2—V1—O5 | 98.96 (7) | O2xi—V2—O1vi | 172.39 (4) |
O4vii—V1—O5 | 86.21 (9) | O2ix—V2—O1vi | 96.23 (4) |
O3—V1—O5 | 165.03 (6) | V2—O1—Ba1xxii | 130.59 (11) |
O2—V1—O3iv | 88.53 (8) | V2—O1—Ba1xii | 97.17 (9) |
O4vii—V1—O3iv | 168.82 (7) | Ba1xxii—O1—Ba1xii | 119.36 (6) |
O3—V1—O3iv | 83.63 (8) | V2—O1—V1xiii | 52.33 (6) |
O5—V1—O3iv | 92.69 (8) | Ba1xxii—O1—V1xiii | 87.32 (5) |
O2—V1—O4iv | 173.70 (8) | Ba1xii—O1—V1xiii | 149.46 (7) |
O4vii—V1—O4iv | 82.72 (8) | V2—O1—V1ix | 71.57 (7) |
O3—V1—O4iv | 80.68 (7) | Ba1xxii—O1—V1ix | 87.88 (5) |
O5—V1—O4iv | 84.60 (6) | Ba1xii—O1—V1ix | 72.68 (4) |
O3iv—V1—O4iv | 86.11 (7) | V1xiii—O1—V1ix | 95.52 (5) |
O2—V1—O3ix | 57.23 (7) | V2—O1—V2xxi | 131.87 (9) |
O4vii—V1—O3ix | 133.87 (6) | Ba1xxii—O1—V2xxi | 65.33 (4) |
O3—V1—O3ix | 125.80 (3) | Ba1xii—O1—V2xxi | 112.42 (6) |
O5—V1—O3ix | 60.72 (7) | V1xiii—O1—V2xxi | 91.37 (5) |
O3iv—V1—O3ix | 53.38 (7) | V1ix—O1—V2xxi | 152.00 (6) |
O4iv—V1—O3ix | 121.21 (6) | V2—O1—V1xi | 142.56 (10) |
O2—V1—O4 | 55.17 (7) | Ba1xxii—O1—V1xi | 84.28 (5) |
O4vii—V1—O4 | 135.90 (8) | Ba1xii—O1—V1xi | 69.93 (4) |
O3—V1—O4 | 56.31 (6) | V1xiii—O1—V1xi | 131.84 (6) |
O5—V1—O4 | 130.81 (8) | V1ix—O1—V1xi | 131.28 (5) |
O3iv—V1—O4 | 51.10 (6) | V2—O1—V1xviii | 62.90 (7) |
O4iv—V1—O4 | 118.62 (5) | Ba1xxii—O1—V1xviii | 70.73 (4) |
O3ix—V1—O4 | 70.37 (4) | Ba1xii—O1—V1xviii | 117.46 (6) |
O2—V1—O5viii | 129.52 (7) | V1xiii—O1—V1xviii | 54.37 (3) |
O4vii—V1—O5viii | 53.08 (6) | V1ix—O1—V1xviii | 45.04 (3) |
O3—V1—O5viii | 52.05 (7) | V2xxi—O1—V1xviii | 124.85 (6) |
O5—V1—O5viii | 119.15 (3) | V1xi—O1—V1xviii | 154.42 (5) |
O3iv—V1—O5viii | 118.88 (6) | Ba1xxii—O1—V2vi | 110.26 (6) |
O4iv—V1—O5viii | 51.39 (5) | Ba1xii—O1—V2vi | 97.70 (5) |
O3ix—V1—O5viii | 171.39 (4) | V1xiii—O1—V2vi | 56.39 (3) |
O4—V1—O5viii | 108.35 (5) | V1ix—O1—V2vi | 47.77 (3) |
O2—V1—O1vii | 63.35 (7) | V2xxi—O1—V2vi | 147.71 (5) |
O4vii—V1—O1vii | 55.87 (6) | V1xi—O1—V2vi | 164.65 (6) |
O3—V1—O1vii | 133.78 (7) | V1—O2—V2 | 107.57 (9) |
O5—V1—O1vii | 57.99 (4) | V1—O2—Ba1iv | 112.62 (8) |
O3iv—V1—O1vii | 132.05 (6) | V2—O2—Ba1iv | 93.10 (7) |
O4iv—V1—O1vii | 122.87 (6) | V1—O2—Ba1xii | 131.66 (9) |
O3ix—V1—O1vii | 78.68 (5) | V2—O2—Ba1xii | 89.13 (6) |
O4—V1—O1vii | 118.50 (5) | Ba1iv—O2—Ba1xii | 111.29 (6) |
O5viii—V1—O1vii | 108.82 (5) | V1—O2—V2vii | 57.92 (6) |
O2—V1—O3viii | 131.05 (7) | V2—O2—V2vii | 137.42 (8) |
O4vii—V1—O3viii | 47.91 (6) | Ba1iv—O2—V2vii | 129.38 (6) |
O3—V1—O3viii | 120.99 (5) | Ba1xii—O2—V2vii | 78.87 (4) |
O5—V1—O3viii | 50.21 (7) | V1—O2—V1iv | 58.24 (5) |
O3iv—V1—O3viii | 124.18 (8) | V2—O2—V1iv | 64.20 (5) |
O4iv—V1—O3viii | 55.12 (6) | Ba1iv—O2—V1iv | 77.86 (4) |
O3ix—V1—O3viii | 110.92 (3) | Ba1xii—O2—V1iv | 152.66 (7) |
O4—V1—O3viii | 173.57 (4) | V2vii—O2—V1iv | 116.14 (5) |
O5viii—V1—O3viii | 69.38 (5) | V1—O2—V1vi | 67.52 (6) |
O1vii—V1—O3viii | 67.78 (4) | V2—O2—V1vi | 75.65 (6) |
O2—V1—O2iv | 121.76 (5) | Ba1iv—O2—V1vi | 167.80 (7) |
O4vii—V1—O2iv | 120.44 (6) | Ba1xii—O2—V1vi | 73.79 (4) |
O3—V1—O2iv | 47.68 (6) | V2vii—O2—V1vi | 61.78 (3) |
O5—V1—O2iv | 119.65 (4) | V1iv—O2—V1vi | 92.77 (4) |
O3iv—V1—O2iv | 51.01 (5) | V1—O2—V2xi | 129.75 (9) |
O4iv—V1—O2iv | 52.03 (6) | V2—O2—V2xi | 121.87 (7) |
O3ix—V1—O2iv | 104.33 (5) | Ba1iv—O2—V2xi | 59.59 (3) |
O4—V1—O2iv | 66.60 (4) | Ba1xii—O2—V2xi | 61.83 (3) |
O5viii—V1—O2iv | 67.88 (4) | V2vii—O2—V2xi | 87.99 (4) |
O1vii—V1—O2iv | 174.87 (5) | V1iv—O2—V2xi | 136.70 (5) |
O3viii—V1—O2iv | 107.14 (4) | V1vi—O2—V2xi | 130.48 (5) |
O2—V1—O1x | 80.65 (7) | V1—O2—V2vi | 70.99 (6) |
O4vii—V1—O1x | 53.29 (7) | Ba1iv—O2—V2vi | 122.86 (6) |
O3—V1—O1x | 49.21 (6) | Ba1xii—O2—V2vi | 100.82 (5) |
O5—V1—O1x | 137.54 (7) | V2vii—O2—V2vi | 101.76 (5) |
O3iv—V1—O1x | 129.57 (6) | V1iv—O2—V2vi | 55.26 (3) |
O4iv—V1—O1x | 100.27 (6) | V1vi—O2—V2vi | 45.04 (2) |
O3ix—V1—O1x | 137.77 (5) | V2xi—O2—V2vi | 158.39 (5) |
O4—V1—O1x | 83.79 (5) | V1—O2—V2x | 56.84 (5) |
O5viii—V1—O1x | 48.96 (3) | V2—O2—V2x | 119.37 (7) |
O1vii—V1—O1x | 85.62 (4) | Ba1iv—O2—V2x | 57.12 (3) |
O3viii—V1—O1x | 98.50 (5) | Ba1xii—O2—V2x | 148.06 (6) |
O2iv—V1—O1x | 94.63 (4) | V2vii—O2—V2x | 87.56 (4) |
O2—V1—O2vi | 100.18 (8) | V1iv—O2—V2x | 58.85 (3) |
O4vii—V1—O2vi | 130.40 (7) | V1vi—O2—V2x | 124.37 (5) |
O3—V1—O2vi | 126.27 (6) | V2xi—O2—V2x | 89.18 (4) |
O5—V1—O2vi | 46.87 (7) | V2vi—O2—V2x | 110.25 (4) |
O3iv—V1—O2vi | 46.21 (6) | V1—O3—V2x | 123.29 (10) |
O4iv—V1—O2vi | 78.41 (6) | V1—O3—V1iv | 96.37 (8) |
O4—V1—O2vi | 93.02 (4) | V2x—O3—V1iv | 139.83 (9) |
O5viii—V1—O2vi | 129.77 (3) | V1—O3—V2iv | 97.53 (8) |
O1vii—V1—O2vi | 98.76 (4) | V2x—O3—V2iv | 81.60 (6) |
O3viii—V1—O2vi | 84.34 (4) | V1iv—O3—V2iv | 87.61 (7) |
O2iv—V1—O2vi | 81.13 (4) | V1—O3—Ba1iv | 96.93 (6) |
O1x—V1—O2vi | 175.46 (4) | V2x—O3—Ba1iv | 82.29 (6) |
O2—V1—O1xi | 46.22 (7) | V1iv—O3—Ba1iv | 100.47 (7) |
O4vii—V1—O1xi | 58.17 (6) | V2iv—O3—Ba1iv | 162.53 (7) |
O3—V1—O1xi | 86.91 (6) | V1—O3—V1x | 173.92 (9) |
O5—V1—O1xi | 106.02 (4) | V2x—O3—V1x | 62.75 (5) |
O3iv—V1—O1xi | 132.50 (6) | V1iv—O3—V1x | 77.71 (6) |
O4iv—V1—O1xi | 137.82 (6) | V2iv—O3—V1x | 83.73 (5) |
O3ix—V1—O1xi | 98.71 (4) | Ba1iv—O3—V1x | 82.91 (5) |
O4—V1—O1xi | 85.46 (5) | V1—O3—V1viii | 59.01 (5) |
O5viii—V1—O1xi | 89.61 (3) | V2x—O3—V1viii | 78.09 (6) |
O1vii—V1—O1xi | 48.16 (6) | V1iv—O3—V1viii | 124.18 (7) |
O3viii—V1—O1xi | 100.42 (5) | V2iv—O3—V1viii | 52.91 (4) |
O2iv—V1—O1xi | 134.30 (4) | Ba1iv—O3—V1viii | 129.39 (6) |
O1x—V1—O1xi | 44.95 (5) | V1x—O3—V1viii | 125.52 (5) |
O2vi—V1—O1xi | 138.17 (4) | V1—O3—V2 | 55.50 (4) |
O2—V1—O1ii | 138.74 (7) | V2x—O3—V2 | 145.26 (8) |
O4vii—V1—O1ii | 90.16 (7) | V1iv—O3—V2 | 61.57 (4) |
O3—V1—O1ii | 122.77 (6) | V2iv—O3—V2 | 132.41 (7) |
O3iv—V1—O1ii | 81.63 (6) | Ba1iv—O3—V2 | 64.59 (3) |
O3ix—V1—O1ii | 85.62 (4) | V1x—O3—V2 | 119.49 (6) |
O4—V1—O1ii | 132.56 (4) | V1viii—O3—V2 | 114.36 (5) |
O5viii—V1—O1ii | 89.47 (4) | V1xiii—O4—V2 | 92.21 (8) |
O1vii—V1—O1ii | 94.62 (6) | V1xiii—O4—V1iv | 97.28 (8) |
O2iv—V1—O1ii | 81.58 (4) | V2—O4—V1iv | 105.20 (9) |
O1x—V1—O1ii | 134.96 (3) | V1xiii—O4—Ba1iv | 142.96 (9) |
O2vi—V1—O1ii | 46.24 (4) | V2—O4—Ba1iv | 98.93 (7) |
O1xi—V1—O1ii | 139.70 (3) | V1iv—O4—Ba1iv | 113.35 (7) |
O1—V2—O4 | 106.52 (9) | V1xiii—O4—V2xvii | 81.23 (6) |
O1—V2—O2 | 96.75 (9) | V2—O4—V2xvii | 169.76 (9) |
O4—V2—O2 | 89.85 (8) | V1iv—O4—V2xvii | 83.54 (5) |
O1—V2—O5xiii | 108.72 (9) | Ba1iv—O4—V2xvii | 82.05 (5) |
O4—V2—O5xiii | 85.14 (6) | V1xiii—O4—V1 | 135.90 (8) |
O2—V2—O5xiii | 154.44 (7) | V2—O4—V1 | 61.55 (5) |
O1—V2—O3ix | 100.77 (9) | V1iv—O4—V1 | 61.38 (5) |
O4—V2—O3ix | 152.66 (8) | Ba1iv—O4—V1 | 79.34 (5) |
O2—V2—O3ix | 88.55 (8) | V2xvii—O4—V1 | 128.40 (5) |
O5xiii—V2—O3ix | 84.63 (7) | V1xiii—O4—V2xvi | 61.54 (5) |
O1—V2—O3iv | 172.47 (9) | V2—O4—V2xvi | 135.03 (8) |
O4—V2—O3iv | 76.55 (7) | V1iv—O4—V2xvi | 49.85 (4) |
O2—V2—O3iv | 76.25 (7) | Ba1iv—O4—V2xvi | 124.37 (6) |
O5xiii—V2—O3iv | 78.21 (6) | V2xvii—O4—V2xvi | 47.66 (3) |
O3ix—V2—O3iv | 76.57 (8) | V1—O4—V2xvi | 111.21 (5) |
O1—V2—O4xx | 65.00 (8) | V1xiii—O4—V2vi | 72.00 (5) |
O4—V2—O4xx | 130.89 (3) | V2—O4—V2vi | 46.64 (4) |
O2—V2—O4xx | 137.82 (6) | V1iv—O4—V2vi | 67.04 (5) |
O5xiii—V2—O4xx | 56.98 (3) | Ba1iv—O4—V2vi | 138.27 (6) |
O3ix—V2—O4xx | 60.74 (6) | V2xvii—O4—V2vi | 136.45 (5) |
O3iv—V2—O4xx | 118.45 (6) | V1—O4—V2vi | 64.22 (3) |
O1—V2—O2xiii | 68.94 (8) | V2xvi—O4—V2vi | 89.02 (4) |
O4—V2—O2xiii | 59.21 (6) | V1—O5—V1vi | 123.63 (14) |
O2—V2—O2xiii | 137.42 (8) | V1—O5—V2ii | 133.39 (5) |
O5xiii—V2—O2xiii | 58.46 (6) | V1vi—O5—V2ii | 89.11 (3) |
O3ix—V2—O2xiii | 132.60 (6) | V1—O5—V2vii | 89.11 (3) |
O3iv—V2—O2xiii | 118.10 (6) | V1vi—O5—V2vii | 133.39 (5) |
O4xx—V2—O2xiii | 73.75 (5) | V2ii—O5—V2vii | 89.42 (11) |
O1—V2—O3 | 129.12 (8) | V1—O5—V1xiv | 155.63 (2) |
O4—V2—O3 | 50.26 (6) | V1vi—O5—V1xiv | 60.85 (3) |
O2—V2—O3 | 48.40 (6) | V2ii—O5—V1xiv | 66.67 (4) |
O5xiii—V2—O3 | 112.23 (4) | V2vii—O5—V1xiv | 76.01 (5) |
O3ix—V2—O3 | 111.75 (4) | V1—O5—V1viii | 60.85 (3) |
O3iv—V2—O3 | 47.59 (7) | V1vi—O5—V1viii | 155.63 (2) |
O4xx—V2—O3 | 165.88 (5) | V2ii—O5—V1viii | 76.01 (5) |
O2xiii—V2—O3 | 109.47 (4) | V2vii—O5—V1viii | 66.67 (4) |
O1—V2—O4xvi | 134.83 (8) | V1xiv—O5—V1viii | 126.67 (8) |
O4—V2—O4xvi | 44.97 (8) | V1—O5—V2 | 51.43 (6) |
O2—V2—O4xvi | 113.78 (6) | V1vi—O5—V2 | 75.28 (8) |
O5xiii—V2—O4xvi | 47.92 (3) | V2ii—O5—V2 | 157.00 (7) |
O3ix—V2—O4xvi | 111.97 (6) | V2vii—O5—V2 | 113.58 (4) |
O3iv—V2—O4xvi | 52.06 (6) | V1xiv—O5—V2 | 117.22 (4) |
O4xx—V2—O4xvi | 104.77 (5) | V1viii—O5—V2 | 112.11 (3) |
O2xiii—V2—O4xvi | 66.04 (4) | V1—O5—V2vi | 75.28 (8) |
O3—V2—O4xvi | 65.77 (4) | V1vi—O5—V2vi | 51.43 (6) |
O1—V2—O4vi | 107.89 (7) | V2ii—O5—V2vi | 113.58 (4) |
O4—V2—O4vi | 124.47 (6) | V2vii—O5—V2vi | 157.00 (7) |
O2—V2—O4vi | 126.97 (7) | V1xiv—O5—V2vi | 112.11 (3) |
O3iv—V2—O4vi | 74.96 (5) | V1viii—O5—V2vi | 117.22 (4) |
O2xiii—V2—O4vi | 95.52 (4) |
Symmetry codes: (i) x−1, y−1, z; (ii) −x+1, y−1, −z+1/2; (iii) x−1, −y+1, z−1/2; (iv) −x+1, −y+1, −z+1; (v) x−1, y, z; (vi) −x+1, y, −z+1/2; (vii) x, y−1, z; (viii) −x+1, −y, −z+1; (ix) x, −y+1, z−1/2; (x) x, −y+1, z+1/2; (xi) −x+2, −y+1, −z+1; (xii) x+1, y, z; (xiii) x, y+1, z; (xiv) x, −y, z−1/2; (xv) x, −y, z+1/2; (xvi) −x+1, −y+2, −z+1; (xvii) x, −y+2, z+1/2; (xviii) −x+1, y+1, −z+1/2; (xix) −x+1, y, −z+3/2; (xx) x, −y+2, z−1/2; (xxi) −x+2, −y+2, −z+1; (xxii) x+1, y+1, z; (xxiii) −x+2, y, −z+1/2. |
O9V4·Ba | F(000) = 440 |
Mr = 485.1 | Dx = 4.929 Mg m−3 Dm = 4.929 Mg m−3 Dm measured by not measured |
Monoclinic, P2/c | Melting point: 0 K |
Hall symbol: -P 2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 7.6140 (12) Å | Cell parameters from 7386 reflections |
b = 4.9319 (7) Å | θ = 2.9–32.2° |
c = 9.3470 (14) Å | µ = 11.47 mm−1 |
β = 111.371 (11)° | T = 150 K |
V = 326.86 (8) Å3 | Parallelepiped, dark blue |
Z = 2 | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
STOE IPDS 2 diffractometer | 1021 reflections with I > 2σ(I) |
Rotation method scans | Rint = 0.042 |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | θmax = 32.0°, θmin = 2.9° |
Tmin = 0.09, Tmax = 0.19 | h = −11→11 |
5337 measured reflections | k = −7→7 |
1119 independent reflections | l = −13→13 |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.010P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.020 | (Δ/σ)max < 0.001 |
wR(F2) = 0.036 | Δρmax = 0.69 e Å−3 |
S = 1.38 | Δρmin = −0.78 e Å−3 |
1119 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
66 parameters | Extinction coefficient: 0.0078 (7) |
0 restraints |
O9V4·Ba | V = 326.86 (8) Å3 |
Mr = 485.1 | Z = 2 |
Monoclinic, P2/c | Mo Kα radiation |
a = 7.6140 (12) Å | µ = 11.47 mm−1 |
b = 4.9319 (7) Å | T = 150 K |
c = 9.3470 (14) Å | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
β = 111.371 (11)° |
STOE IPDS 2 diffractometer | 1119 independent reflections |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | 1021 reflections with I > 2σ(I) |
Tmin = 0.09, Tmax = 0.19 | Rint = 0.042 |
5337 measured reflections |
R[F2 > 2σ(F2)] = 0.020 | 66 parameters |
wR(F2) = 0.036 | 0 restraints |
S = 1.38 | Δρmax = 0.69 e Å−3 |
1119 reflections | Δρmin = −0.78 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. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0 | 0.34228 (5) | 0.25 | 0.00639 (6) | |
V1 | 0.57483 (6) | 0.25007 (8) | 0.45067 (5) | 0.00399 (8) | |
V2 | 0.68888 (6) | 0.77404 (8) | 0.35006 (5) | 0.00411 (8) | |
O1 | 0.8925 (2) | 0.8680 (4) | 0.34864 (19) | 0.0076 (3) | |
O2 | 0.7715 (2) | 0.4158 (4) | 0.44699 (19) | 0.0057 (3) | |
O3 | 0.5802 (2) | 0.4145 (3) | 0.64535 (18) | 0.0048 (3) | |
O4 | 0.6747 (2) | 0.9082 (4) | 0.54216 (18) | 0.0047 (3) | |
O5 | 0.5 | 0.0607 (5) | 0.25 | 0.0046 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.00720 (9) | 0.00548 (10) | 0.00662 (9) | 0 | 0.00268 (6) | 0 |
V1 | 0.00528 (17) | 0.00313 (18) | 0.00374 (18) | −0.00040 (12) | 0.00186 (13) | −0.00004 (12) |
V2 | 0.00497 (16) | 0.00390 (18) | 0.00362 (16) | −0.00035 (12) | 0.00177 (13) | 0.00001 (12) |
O1 | 0.0078 (7) | 0.0073 (8) | 0.0083 (7) | −0.0002 (6) | 0.0035 (6) | 0.0008 (6) |
O2 | 0.0067 (7) | 0.0047 (8) | 0.0056 (7) | 0.0007 (6) | 0.0021 (6) | 0.0010 (6) |
O3 | 0.0080 (7) | 0.0048 (7) | 0.0017 (6) | 0.0009 (6) | 0.0021 (6) | 0.0000 (5) |
O4 | 0.0063 (7) | 0.0042 (7) | 0.0043 (7) | 0.0003 (5) | 0.0026 (6) | 0.0001 (5) |
O5 | 0.0077 (10) | 0.0036 (10) | 0.0027 (9) | 0 | 0.0024 (8) | 0 |
Ba1—O1i | 2.7462 (19) | V2—O3 | 3.6210 (16) |
Ba1—O1ii | 2.7462 (19) | V2—O4xvi | 3.6284 (16) |
Ba1—O4iii | 2.8158 (17) | V2—V1xviii | 3.6512 (7) |
Ba1—O4iv | 2.8158 (17) | V2—Ba1iv | 3.6689 (7) |
Ba1—O1v | 2.9650 (19) | V2—O4vi | 3.7608 (18) |
Ba1—O1vi | 2.965 (2) | V2—O5 | 3.787 (2) |
Ba1—O2iv | 2.9800 (18) | V2—V1vi | 3.8076 (7) |
Ba1—O2iii | 2.9800 (18) | V2—O1xxi | 3.830 (2) |
Ba1—O2vi | 2.9802 (16) | V2—O2xi | 3.9589 (18) |
Ba1—O2v | 2.9802 (16) | V2—Ba1xxii | 3.9944 (6) |
Ba1—O3iv | 3.2148 (17) | V2—O2vi | 4.0034 (19) |
Ba1—O3iii | 3.2148 (17) | V2—O2ix | 4.1467 (17) |
V1—O2 | 1.7176 (17) | V2—O1vi | 4.155 (2) |
V1—O4vii | 1.9180 (18) | V2—V2xiii | 4.9319 (7) |
V1—O3 | 1.9792 (16) | V2—V2vii | 4.9319 (7) |
V1—O5 | 1.9839 (13) | V2—V2xxi | 5.0589 (11) |
V1—O3iv | 2.0402 (18) | V2—V2xvii | 5.1778 (7) |
V1—O4iv | 2.0772 (16) | V2—V2xx | 5.1778 (7) |
V1—V2vii | 2.7830 (6) | V2—V2xvi | 5.1935 (9) |
V1—V2 | 2.9852 (6) | V2—V1xi | 5.2251 (11) |
V1—V1iv | 2.9988 (8) | V2—V2xi | 5.2850 (11) |
V1—V1viii | 2.9998 (8) | V2—V2ix | 5.3989 (8) |
V1—V2iv | 3.2001 (7) | V2—V2x | 5.3989 (8) |
V1—O3ix | 3.3116 (16) | V2—V2iv | 5.4140 (9) |
V1—O4 | 3.3719 (18) | V2—Ba1xvi | 5.6680 (8) |
V1—O5viii | 3.4153 (13) | V2—V2i | 5.6722 (8) |
V1—O1vii | 3.4631 (18) | V2—V2xviii | 5.6722 (8) |
V1—O3viii | 3.4885 (18) | V2—V2xxiii | 5.6925 (11) |
V1—V1vi | 3.5007 (10) | V2—V1xvi | 5.7785 (8) |
V1—V2x | 3.5131 (8) | V2—V1xx | 5.9576 (9) |
V1—O2iv | 3.5250 (17) | V2—V1viii | 5.9780 (9) |
V1—V2i | 3.6512 (7) | V2—V1x | 5.9863 (10) |
V1—O1x | 3.6701 (19) | V2—V1xiv | 6.1513 (9) |
V1—O2vi | 3.7808 (19) | O1—Ba1xxii | 2.7462 (19) |
V1—V2vi | 3.8076 (7) | O1—Ba1xii | 2.9650 (19) |
V1—O1xi | 3.8420 (19) | O1—V1xiii | 3.4631 (18) |
V1—Ba1iv | 3.9685 (7) | O1—V1ix | 3.6701 (19) |
V1—O1i | 4.0969 (19) | O1—V2xxi | 3.829 (2) |
V1—Ba1xii | 4.3162 (7) | O1—V1xi | 3.8420 (19) |
V1—Ba1viii | 4.4990 (7) | O1—V1xviii | 4.0969 (19) |
V1—V1xiii | 4.9319 (7) | O1—V2vi | 4.155 (2) |
V1—V1vii | 4.9319 (7) | O2—Ba1iv | 2.9800 (18) |
V1—V2xi | 5.2251 (11) | O2—Ba1xii | 2.9802 (16) |
V1—V1x | 5.2839 (7) | O2—V2vii | 3.2891 (19) |
V1—V1ix | 5.2839 (7) | O2—V1iv | 3.5250 (17) |
V1—V1xiv | 5.2845 (7) | O2—V1vi | 3.7808 (19) |
V1—V1xv | 5.2845 (7) | O2—V2xi | 3.9589 (18) |
V1—V2xvi | 5.7785 (8) | O2—V2vi | 4.0034 (19) |
V1—V2xvii | 5.9576 (9) | O2—V2x | 4.1467 (17) |
V1—V2viii | 5.9780 (8) | O3—V2x | 2.0143 (17) |
V1—V2ix | 5.9863 (10) | O3—V1iv | 2.0402 (18) |
V1—V1i | 6.0480 (8) | O3—V2iv | 2.2643 (17) |
V1—V1xviii | 6.0480 (8) | O3—Ba1iv | 3.2148 (17) |
V1—V1xix | 6.1039 (11) | O3—V1x | 3.3116 (16) |
V1—V2xv | 6.1513 (9) | O3—V1viii | 3.4885 (18) |
V2—O1 | 1.6229 (18) | O4—V1xiii | 1.9180 (18) |
V2—O4 | 1.9532 (16) | O4—V1iv | 2.0772 (16) |
V2—O2 | 1.9808 (18) | O4—Ba1iv | 2.8158 (17) |
V2—O5xiii | 1.9904 (18) | O4—V2xvii | 3.2440 (17) |
V2—O3ix | 2.0143 (17) | O4—V2xvi | 3.6284 (16) |
V2—O3iv | 2.2643 (17) | O4—V2vi | 3.7608 (18) |
V2—V1xiii | 2.7830 (6) | O5—V1vi | 1.9839 (13) |
V2—V2vi | 2.8019 (10) | O5—V2i | 1.9904 (18) |
V2—V1iv | 3.2001 (7) | O5—V2vii | 1.9904 (18) |
V2—O4xx | 3.2440 (17) | O5—V1xiv | 3.4153 (12) |
V2—O2xiii | 3.2891 (19) | O5—V1viii | 3.4153 (12) |
V2—V1ix | 3.5131 (8) | O5—V2vi | 3.787 (2) |
V2—Ba1xii | 3.5546 (5) | ||
O1i—Ba1—O1ii | 63.18 (7) | O2xiii—V2—O4vi | 95.64 (4) |
O1i—Ba1—O4iii | 71.92 (5) | O3—V2—O4vi | 122.53 (4) |
O1ii—Ba1—O4iii | 64.09 (5) | O4xvi—V2—O4vi | 80.20 (3) |
O1i—Ba1—O4iv | 64.09 (5) | O1—V2—O5 | 122.76 (7) |
O1ii—Ba1—O4iv | 71.92 (5) | O4—V2—O5 | 113.48 (5) |
O4iii—Ba1—O4iv | 127.96 (7) | O2—V2—O5 | 46.61 (5) |
O1i—Ba1—O1v | 177.43 (4) | O5xiii—V2—O5 | 113.55 (4) |
O1ii—Ba1—O1v | 119.38 (6) | O3ix—V2—O5 | 49.37 (5) |
O4iii—Ba1—O1v | 108.97 (5) | O3iv—V2—O5 | 50.08 (4) |
O4iv—Ba1—O1v | 116.24 (5) | O4xx—V2—O5 | 110.05 (3) |
O1i—Ba1—O1vi | 119.38 (6) | O2xiii—V2—O5 | 168.33 (3) |
O1ii—Ba1—O1vi | 177.43 (4) | O3—V2—O5 | 64.00 (3) |
O4iii—Ba1—O1vi | 116.24 (5) | O4xvi—V2—O5 | 102.15 (3) |
O4iv—Ba1—O1vi | 108.97 (5) | O4vi—V2—O5 | 81.04 (3) |
O1v—Ba1—O1vi | 58.05 (7) | O1—V2—O1xxi | 48.15 (8) |
O1i—Ba1—O2iv | 121.20 (5) | O4—V2—O1xxi | 58.53 (5) |
O1ii—Ba1—O2iv | 99.45 (5) | O2—V2—O1xxi | 91.97 (6) |
O4iii—Ba1—O2iv | 153.31 (4) | O5xiii—V2—O1xxi | 106.46 (6) |
O4iv—Ba1—O2iv | 57.17 (5) | O3ix—V2—O1xxi | 148.79 (5) |
O1v—Ba1—O2iv | 59.07 (5) | O3iv—V2—O1xxi | 133.76 (5) |
O1vi—Ba1—O2iv | 79.27 (5) | O4xx—V2—O1xxi | 100.34 (4) |
O1i—Ba1—O2iii | 99.45 (5) | O2xiii—V2—O1xxi | 47.88 (4) |
O1ii—Ba1—O2iii | 121.20 (5) | O3—V2—O1xxi | 91.45 (4) |
O4iii—Ba1—O2iii | 57.17 (5) | O4xvi—V2—O1xxi | 96.39 (4) |
O4iv—Ba1—O2iii | 153.31 (4) | O4vi—V2—O1xxi | 139.07 (4) |
O1v—Ba1—O2iii | 79.27 (5) | O5—V2—O1xxi | 138.54 (3) |
O1vi—Ba1—O2iii | 59.07 (5) | O4—V2—O2xi | 92.01 (6) |
O2iv—Ba1—O2iii | 132.79 (7) | O2—V2—O2xi | 57.90 (7) |
O1i—Ba1—O2vi | 65.40 (5) | O5xiii—V2—O2xi | 147.04 (6) |
O1ii—Ba1—O2vi | 128.57 (5) | O3ix—V2—O2xi | 109.97 (6) |
O4iii—Ba1—O2vi | 101.06 (5) | O3iv—V2—O2xi | 132.98 (5) |
O4iv—Ba1—O2vi | 85.11 (5) | O4xx—V2—O2xi | 103.45 (4) |
O1v—Ba1—O2vi | 112.03 (5) | O2xiii—V2—O2xi | 91.98 (4) |
O1vi—Ba1—O2vi | 54.00 (5) | O3—V2—O2xi | 90.26 (4) |
O2iv—Ba1—O2vi | 105.58 (5) | O4xvi—V2—O2xi | 137.10 (4) |
O2iii—Ba1—O2vi | 68.54 (5) | O4vi—V2—O2xi | 140.83 (4) |
O1i—Ba1—O2v | 128.57 (5) | O5—V2—O2xi | 97.65 (3) |
O1ii—Ba1—O2v | 65.40 (5) | O1xxi—V2—O2xi | 46.87 (4) |
O4iii—Ba1—O2v | 85.11 (5) | O1—V2—O2vi | 135.89 (7) |
O4iv—Ba1—O2v | 101.06 (5) | O4—V2—O2vi | 117.33 (6) |
O1v—Ba1—O2v | 54.00 (5) | O2—V2—O2vi | 88.60 (8) |
O1vi—Ba1—O2v | 112.03 (5) | O5xiii—V2—O2vi | 71.79 (6) |
O2iv—Ba1—O2v | 68.54 (5) | O3ix—V2—O2vi | 35.36 (5) |
O2iii—Ba1—O2v | 105.58 (5) | O4xx—V2—O2vi | 81.97 (4) |
O2vi—Ba1—O2v | 166.03 (7) | O2xiii—V2—O2vi | 130.32 (4) |
O1i—Ba1—O3iv | 92.01 (5) | O3—V2—O2vi | 85.81 (4) |
O1ii—Ba1—O3iv | 126.91 (5) | O4xvi—V2—O2vi | 79.60 (4) |
O4iii—Ba1—O3iv | 154.26 (4) | O1xxi—V2—O2vi | 175.81 (4) |
O4iv—Ba1—O3iv | 55.00 (5) | O2xi—V2—O2vi | 136.18 (2) |
O1v—Ba1—O3iv | 86.31 (5) | O1—V2—O2ix | 66.12 (7) |
O1vi—Ba1—O3iv | 53.98 (5) | O4—V2—O2ix | 171.61 (6) |
O2iv—Ba1—O3iv | 52.42 (4) | O2—V2—O2ix | 94.94 (4) |
O2iii—Ba1—O3iv | 108.13 (4) | O5xiii—V2—O2ix | 93.23 (3) |
O2vi—Ba1—O3iv | 53.35 (4) | O3iv—V2—O2ix | 111.25 (5) |
O2v—Ba1—O3iv | 120.41 (4) | O2xiii—V2—O2ix | 112.97 (4) |
O1i—Ba1—O3iii | 126.91 (5) | O3—V2—O2ix | 137.27 (4) |
O1ii—Ba1—O3iii | 92.01 (5) | O4xvi—V2—O2ix | 137.18 (4) |
O4iii—Ba1—O3iii | 55.00 (5) | O4vi—V2—O2ix | 57.01 (3) |
O4iv—Ba1—O3iii | 154.26 (4) | O5—V2—O2ix | 74.67 (3) |
O1v—Ba1—O3iii | 53.98 (5) | O1xxi—V2—O2ix | 114.27 (4) |
O1vi—Ba1—O3iii | 86.31 (5) | O2xi—V2—O2ix | 84.68 (4) |
O2iv—Ba1—O3iii | 108.13 (4) | O2vi—V2—O2ix | 69.80 (4) |
O2iii—Ba1—O3iii | 52.42 (4) | O1—V2—O1vi | 146.08 (8) |
O2vi—Ba1—O3iii | 120.41 (4) | O4—V2—O1vi | 88.06 (6) |
O2v—Ba1—O3iii | 53.35 (4) | O2—V2—O1vi | 114.40 (6) |
O3iv—Ba1—O3iii | 136.19 (6) | O3ix—V2—O1vi | 67.96 (5) |
O2—V1—O4vii | 102.74 (8) | O4xx—V2—O1vi | 82.18 (4) |
O2—V1—O3 | 95.60 (8) | O2xiii—V2—O1vi | 94.68 (4) |
O4vii—V1—O3 | 94.49 (7) | O3—V2—O1vi | 83.86 (4) |
O2—V1—O5 | 99.04 (7) | O5—V2—O1vi | 75.31 (3) |
O4vii—V1—O5 | 86.47 (8) | O1xxi—V2—O1vi | 137.98 (3) |
O3—V1—O5 | 164.75 (5) | O2xi—V2—O1vi | 172.29 (4) |
O2—V1—O3iv | 88.53 (8) | O2ix—V2—O1vi | 96.24 (4) |
O4vii—V1—O3iv | 168.71 (7) | V2—O1—Ba1xxii | 130.42 (10) |
O3—V1—O3iv | 83.51 (7) | V2—O1—Ba1xii | 97.22 (9) |
O5—V1—O3iv | 92.58 (7) | Ba1xxii—O1—Ba1xii | 119.38 (6) |
O2—V1—O4iv | 173.63 (8) | V2—O1—V1xiii | 52.25 (5) |
O4vii—V1—O4iv | 82.75 (7) | Ba1xxii—O1—V1xiii | 87.27 (5) |
O3—V1—O4iv | 80.61 (7) | Ba1xii—O1—V1xiii | 149.44 (6) |
O5—V1—O4iv | 84.42 (5) | V2—O1—V1ix | 71.59 (6) |
O3iv—V1—O4iv | 85.96 (7) | Ba1xxii—O1—V1ix | 87.81 (5) |
O2—V1—O3ix | 57.35 (7) | Ba1xii—O1—V1ix | 72.59 (4) |
O4vii—V1—O3ix | 134.11 (5) | V1xiii—O1—V1ix | 95.56 (5) |
O3—V1—O3ix | 125.80 (3) | V2—O1—V2xxi | 131.85 (8) |
O5—V1—O3ix | 60.65 (7) | Ba1xxii—O1—V2xxi | 65.43 (4) |
O3iv—V1—O3ix | 53.32 (6) | Ba1xii—O1—V2xxi | 112.44 (5) |
O4iv—V1—O3ix | 120.93 (6) | V1xiii—O1—V2xxi | 91.39 (4) |
O2—V1—O4 | 55.21 (6) | V1ix—O1—V2xxi | 152.01 (5) |
O4vii—V1—O4 | 135.81 (8) | V2—O1—V1xi | 142.60 (9) |
O3—V1—O4 | 56.30 (6) | Ba1xxii—O1—V1xi | 84.39 (4) |
O5—V1—O4 | 130.80 (7) | Ba1xii—O1—V1xi | 69.97 (4) |
O3iv—V1—O4 | 51.09 (6) | V1xiii—O1—V1xi | 131.83 (5) |
O4iv—V1—O4 | 118.54 (5) | V1ix—O1—V1xi | 131.26 (5) |
O3ix—V1—O4 | 70.45 (4) | V2—O1—V1xviii | 62.76 (6) |
O2—V1—O5viii | 129.57 (6) | Ba1xxii—O1—V1xviii | 70.72 (4) |
O4vii—V1—O5viii | 52.95 (6) | Ba1xii—O1—V1xviii | 117.34 (5) |
O3—V1—O5viii | 52.00 (6) | V1xiii—O1—V1xviii | 54.39 (3) |
O5—V1—O5viii | 119.15 (3) | V1ix—O1—V1xviii | 45.02 (2) |
O3iv—V1—O5viii | 118.80 (5) | V2xxi—O1—V1xviii | 124.97 (5) |
O4iv—V1—O5viii | 51.49 (5) | V1xi—O1—V1xviii | 154.52 (5) |
O3ix—V1—O5viii | 171.21 (4) | Ba1xxii—O1—V2vi | 110.13 (5) |
O4—V1—O5viii | 108.28 (5) | Ba1xii—O1—V2vi | 97.66 (5) |
O2—V1—O1vii | 63.36 (7) | V1xiii—O1—V2vi | 56.39 (3) |
O4vii—V1—O1vii | 56.03 (5) | V1ix—O1—V2vi | 47.78 (3) |
O3—V1—O1vii | 133.94 (6) | V2xxi—O1—V2vi | 147.74 (5) |
O5—V1—O1vii | 58.15 (4) | V1xi—O1—V2vi | 164.66 (6) |
O3iv—V1—O1vii | 132.08 (5) | V1—O2—V2 | 107.43 (9) |
O4iv—V1—O1vii | 122.90 (6) | V1—O2—Ba1iv | 112.51 (7) |
O3ix—V1—O1vii | 78.78 (4) | V2—O2—Ba1iv | 93.19 (7) |
O4—V1—O1vii | 118.56 (4) | V1—O2—Ba1xii | 131.61 (9) |
O5viii—V1—O1vii | 108.85 (4) | V2—O2—Ba1xii | 89.18 (6) |
O2—V1—O3viii | 131.12 (6) | Ba1iv—O2—Ba1xii | 111.46 (5) |
O4vii—V1—O3viii | 47.98 (6) | V1—O2—V2vii | 57.79 (5) |
O3—V1—O3viii | 120.88 (5) | V2—O2—V2vii | 137.34 (8) |
O5—V1—O3viii | 50.27 (7) | Ba1iv—O2—V2vii | 129.34 (6) |
O3iv—V1—O3viii | 124.15 (7) | Ba1xii—O2—V2vii | 78.99 (4) |
O4iv—V1—O3viii | 55.09 (5) | V1—O2—V1iv | 58.19 (5) |
O3ix—V1—O3viii | 110.91 (3) | V2—O2—V1iv | 64.06 (4) |
O4—V1—O3viii | 173.47 (4) | Ba1iv—O2—V1iv | 77.89 (4) |
O5viii—V1—O3viii | 69.35 (4) | Ba1xii—O2—V1iv | 152.55 (6) |
O1vii—V1—O3viii | 67.83 (4) | V2vii—O2—V1iv | 115.95 (5) |
O2—V1—O2iv | 121.81 (5) | V1—O2—V1vi | 67.41 (6) |
O4vii—V1—O2iv | 120.28 (5) | V2—O2—V1vi | 75.62 (5) |
O3—V1—O2iv | 47.59 (6) | Ba1iv—O2—V1vi | 167.79 (6) |
O5—V1—O2iv | 119.42 (4) | Ba1xii—O2—V1vi | 73.82 (4) |
O3iv—V1—O2iv | 50.97 (5) | V2vii—O2—V1vi | 61.72 (3) |
O4iv—V1—O2iv | 51.94 (5) | V1iv—O2—V1vi | 92.58 (4) |
O3ix—V1—O2iv | 104.22 (4) | V1—O2—V2xi | 129.66 (8) |
O4—V1—O2iv | 66.60 (4) | V2—O2—V2xi | 122.10 (7) |
O5viii—V1—O2iv | 67.84 (4) | Ba1iv—O2—V2xi | 59.66 (3) |
O1vii—V1—O2iv | 174.81 (4) | Ba1xii—O2—V2xi | 61.96 (3) |
O3viii—V1—O2iv | 107.02 (4) | V2vii—O2—V2xi | 88.02 (4) |
O2—V1—O1x | 80.69 (7) | V1iv—O2—V2xi | 136.80 (5) |
O4vii—V1—O1x | 53.19 (6) | V1vi—O2—V2xi | 130.56 (5) |
O3—V1—O1x | 49.31 (6) | V1—O2—V2vi | 70.99 (6) |
O5—V1—O1x | 137.71 (7) | Ba1iv—O2—V2vi | 122.87 (5) |
O3iv—V1—O1x | 129.52 (6) | Ba1xii—O2—V2vi | 100.71 (5) |
O4iv—V1—O1x | 100.39 (6) | V2vii—O2—V2vi | 101.67 (4) |
O3ix—V1—O1x | 137.92 (4) | V1iv—O2—V2vi | 55.19 (3) |
O4—V1—O1x | 83.76 (4) | V2xi—O2—V2vi | 158.47 (5) |
O5viii—V1—O1x | 48.97 (3) | V1—O2—V2x | 56.78 (5) |
O1vii—V1—O1x | 85.66 (4) | V2—O2—V2x | 119.26 (6) |
O3viii—V1—O1x | 98.51 (4) | Ba1iv—O2—V2x | 57.06 (3) |
O2iv—V1—O1x | 94.65 (4) | Ba1xii—O2—V2x | 148.20 (6) |
O2—V1—O2vi | 100.28 (7) | V2vii—O2—V2x | 87.47 (4) |
O4vii—V1—O2vi | 130.50 (6) | V1iv—O2—V2x | 58.85 (3) |
O3—V1—O2vi | 126.05 (6) | V1vi—O2—V2x | 124.19 (4) |
O5—V1—O2vi | 46.78 (6) | V2xi—O2—V2x | 89.19 (4) |
O3iv—V1—O2vi | 46.20 (5) | V2vi—O2—V2x | 110.20 (4) |
O4iv—V1—O2vi | 78.14 (5) | V1—O3—V2x | 123.22 (9) |
O3ix—V1—O2vi | 42.95 (4) | V1—O3—V1iv | 96.49 (7) |
O4—V1—O2vi | 93.05 (4) | V2x—O3—V1iv | 139.80 (8) |
O5viii—V1—O2vi | 129.61 (3) | V1—O3—V2iv | 97.67 (7) |
O1vii—V1—O2vi | 98.85 (4) | V2x—O3—V2iv | 81.59 (6) |
O3viii—V1—O2vi | 84.31 (4) | V1iv—O3—V2iv | 87.66 (6) |
O2iv—V1—O2vi | 80.96 (3) | V1—O3—Ba1iv | 96.75 (6) |
O1x—V1—O2vi | 175.35 (4) | V2x—O3—Ba1iv | 82.20 (5) |
O2—V1—O1xi | 46.27 (7) | V1iv—O3—Ba1iv | 100.54 (6) |
O4vii—V1—O1xi | 58.18 (6) | V2iv—O3—Ba1iv | 162.48 (7) |
O3—V1—O1xi | 87.07 (6) | V1—O3—V1x | 173.97 (8) |
O5—V1—O1xi | 106.18 (4) | V2x—O3—V1x | 62.73 (4) |
O3iv—V1—O1xi | 132.54 (6) | V1iv—O3—V1x | 77.72 (5) |
O4iv—V1—O1xi | 137.93 (6) | V2iv—O3—V1x | 83.89 (5) |
O3ix—V1—O1xi | 98.87 (4) | Ba1iv—O3—V1x | 82.79 (4) |
O4—V1—O1xi | 85.51 (4) | V1—O3—V1viii | 59.12 (5) |
O5viii—V1—O1xi | 89.63 (3) | V2x—O3—V1viii | 78.11 (5) |
O1vii—V1—O1xi | 48.17 (5) | V1iv—O3—V1viii | 124.15 (7) |
O3viii—V1—O1xi | 100.44 (4) | V2iv—O3—V1viii | 52.80 (4) |
O2iv—V1—O1xi | 134.38 (4) | Ba1iv—O3—V1viii | 129.38 (5) |
O1x—V1—O1xi | 44.97 (5) | V1x—O3—V1viii | 125.58 (5) |
O2vi—V1—O1xi | 138.32 (4) | V1—O3—V2 | 55.51 (4) |
O2—V1—O1i | 138.76 (6) | V2x—O3—V2 | 145.21 (7) |
O4vii—V1—O1i | 90.26 (6) | V1iv—O3—V2 | 61.57 (4) |
O3—V1—O1i | 122.55 (6) | V2iv—O3—V2 | 132.47 (6) |
O5—V1—O1i | 42.20 (3) | Ba1iv—O3—V2 | 64.60 (3) |
O3iv—V1—O1i | 81.57 (6) | V1x—O3—V2 | 119.36 (5) |
O3ix—V1—O1i | 85.51 (4) | V1viii—O3—V2 | 114.45 (4) |
O4—V1—O1i | 132.48 (4) | V1xiii—O4—V2 | 91.92 (7) |
O5viii—V1—O1i | 89.44 (3) | V1xiii—O4—V1iv | 97.25 (7) |
O1vii—V1—O1i | 94.69 (5) | V2—O4—V1iv | 105.08 (8) |
O2iv—V1—O1i | 81.42 (4) | V1xiii—O4—Ba1iv | 143.07 (8) |
O1x—V1—O1i | 134.98 (2) | V2—O4—Ba1iv | 98.98 (6) |
O2vi—V1—O1i | 46.13 (4) | V1iv—O4—Ba1iv | 113.45 (7) |
O1xi—V1—O1i | 139.76 (2) | V1xiii—O4—V2xvii | 81.40 (6) |
O1—V2—O4 | 106.50 (8) | V2—O4—V2xvii | 169.76 (8) |
O1—V2—O2 | 96.49 (9) | V1iv—O4—V2xvii | 83.58 (5) |
O4—V2—O2 | 89.80 (7) | Ba1iv—O4—V2xvii | 82.14 (4) |
O1—V2—O5xiii | 108.80 (8) | V1xiii—O4—V1 | 135.81 (8) |
O4—V2—O5xiii | 85.34 (6) | V2—O4—V1 | 61.56 (5) |
O2—V2—O5xiii | 154.60 (7) | V1iv—O4—V1 | 61.46 (5) |
O1—V2—O3ix | 100.79 (8) | Ba1iv—O4—V1 | 79.23 (4) |
O4—V2—O3ix | 152.67 (7) | V2xvii—O4—V1 | 128.43 (5) |
O2—V2—O3ix | 88.55 (7) | V1xiii—O4—V2xvi | 61.68 (4) |
O5xiii—V2—O3ix | 84.56 (6) | V2—O4—V2xvi | 134.83 (7) |
O1—V2—O3iv | 172.31 (8) | V1iv—O4—V2xvi | 49.77 (4) |
O4—V2—O3iv | 76.59 (6) | Ba1iv—O4—V2xvi | 124.49 (5) |
O2—V2—O3iv | 76.34 (7) | V2xvii—O4—V2xvi | 47.72 (3) |
O5xiii—V2—O3iv | 78.29 (6) | V1—O4—V2xvi | 111.22 (4) |
O3ix—V2—O3iv | 76.52 (7) | V1xiii—O4—V2vi | 71.86 (5) |
O1—V2—O4xx | 65.04 (7) | V2—O4—V2vi | 46.53 (4) |
O4—V2—O4xx | 131.06 (3) | V1iv—O4—V2vi | 66.95 (5) |
O2—V2—O4xx | 137.65 (6) | Ba1iv—O4—V2vi | 138.19 (6) |
O5xiii—V2—O4xx | 56.98 (3) | V2xvii—O4—V2vi | 136.43 (5) |
O3ix—V2—O4xx | 60.73 (6) | V1—O4—V2vi | 64.26 (3) |
O3iv—V2—O4xx | 118.51 (5) | V2xvi—O4—V2vi | 88.95 (4) |
O1—V2—O2xiii | 68.90 (7) | V1—O5—V1vi | 123.84 (13) |
O4—V2—O2xiii | 59.34 (6) | V1—O5—V2i | 133.47 (4) |
O2—V2—O2xiii | 137.34 (8) | V1vi—O5—V2i | 88.89 (3) |
O5xiii—V2—O2xiii | 58.59 (6) | V1—O5—V2vii | 88.89 (3) |
O3ix—V2—O2xiii | 132.62 (6) | V1vi—O5—V2vii | 133.47 (4) |
O3iv—V2—O2xiii | 118.27 (5) | V2i—O5—V2vii | 89.47 (11) |
O4xx—V2—O2xiii | 73.78 (4) | V1—O5—V1xiv | 155.452 (19) |
O1—V2—O3 | 129.09 (7) | V1vi—O5—V1xiv | 60.85 (3) |
O4—V2—O3 | 50.24 (6) | V2i—O5—V1xiv | 66.67 (4) |
O2—V2—O3 | 48.50 (5) | V2vii—O5—V1xiv | 76.02 (5) |
O5xiii—V2—O3 | 112.29 (4) | V1—O5—V1viii | 60.85 (3) |
O3ix—V2—O3 | 111.66 (4) | V1vi—O5—V1viii | 155.452 (19) |
O3iv—V2—O3 | 47.53 (6) | V2i—O5—V1viii | 76.02 (5) |
O4xx—V2—O3 | 165.88 (4) | V2vii—O5—V1viii | 66.67 (4) |
O2xiii—V2—O3 | 109.58 (4) | V1xiv—O5—V1viii | 126.66 (8) |
O1—V2—O4xvi | 134.97 (8) | V1—O5—V2 | 51.45 (6) |
O4—V2—O4xvi | 45.17 (7) | V1vi—O5—V2 | 75.44 (7) |
O2—V2—O4xvi | 113.94 (5) | V2i—O5—V2 | 156.98 (7) |
O5xiii—V2—O4xvi | 47.93 (3) | V2vii—O5—V2 | 113.55 (4) |
O3ix—V2—O4xvi | 111.85 (6) | V1xiv—O5—V2 | 117.23 (3) |
O3iv—V2—O4xvi | 52.07 (5) | V1viii—O5—V2 | 112.11 (3) |
O4xx—V2—O4xvi | 104.80 (5) | V1—O5—V2vi | 75.44 (7) |
O2xiii—V2—O4xvi | 66.21 (4) | V1vi—O5—V2vi | 51.45 (6) |
O3—V2—O4xvi | 65.82 (4) | V2i—O5—V2vi | 113.55 (4) |
O1—V2—O4vi | 107.92 (7) | V2vii—O5—V2vi | 156.98 (7) |
O4—V2—O4vi | 124.67 (6) | V1xiv—O5—V2vi | 112.11 (3) |
O2—V2—O4vi | 126.95 (6) | V1viii—O5—V2vi | 117.23 (3) |
O3iv—V2—O4vi | 75.00 (5) |
Symmetry codes: (i) −x+1, y−1, −z+1/2; (ii) x−1, y−1, z; (iii) x−1, −y+1, z−1/2; (iv) −x+1, −y+1, −z+1; (v) x−1, y, z; (vi) −x+1, y, −z+1/2; (vii) x, y−1, z; (viii) −x+1, −y, −z+1; (ix) x, −y+1, z−1/2; (x) x, −y+1, z+1/2; (xi) −x+2, −y+1, −z+1; (xii) x+1, y, z; (xiii) x, y+1, z; (xiv) x, −y, z−1/2; (xv) x, −y, z+1/2; (xvi) −x+1, −y+2, −z+1; (xvii) x, −y+2, z+1/2; (xviii) −x+1, y+1, −z+1/2; (xix) −x+1, y, −z+3/2; (xx) x, −y+2, z−1/2; (xxi) −x+2, −y+2, −z+1; (xxii) x+1, y+1, z; (xxiii) −x+2, y, −z+1/2. |
O9V4·Ba | F(000) = 440 |
Mr = 485.1 | Dx = 4.936 Mg m−3 Dm = 4.936 Mg m−3 Dm measured by not measured |
Monoclinic, P2/c | Melting point: 0 K |
Hall symbol: -P 2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 7.6084 (13) Å | Cell parameters from 7538 reflections |
b = 4.9291 (7) Å | θ = 2.9–32.2° |
c = 9.3464 (15) Å | µ = 11.48 mm−1 |
β = 111.371 (12)° | T = 100 K |
V = 326.41 (9) Å3 | Parallelepiped, dark blue |
Z = 2 | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
STOE IPDS 2 diffractometer | 1027 reflections with I > 2σ(I) |
Rotation method scans | Rint = 0.038 |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | θmax = 32.0°, θmin = 2.9° |
Tmin = 0.09, Tmax = 0.19 | h = −11→11 |
5334 measured reflections | k = −7→7 |
1119 independent reflections | l = −13→13 |
Refinement on F2 | 0 constraints |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.010P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.021 | (Δ/σ)max < 0.001 |
wR(F2) = 0.035 | Δρmax = 0.77 e Å−3 |
S = 1.46 | Δρmin = −0.81 e Å−3 |
1119 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
66 parameters | Extinction coefficient: 0.0084 (7) |
0 restraints |
O9V4·Ba | V = 326.41 (9) Å3 |
Mr = 485.1 | Z = 2 |
Monoclinic, P2/c | Mo Kα radiation |
a = 7.6084 (13) Å | µ = 11.48 mm−1 |
b = 4.9291 (7) Å | T = 100 K |
c = 9.3464 (15) Å | 0.24 × 0.21 × 0.15 × 0 (radius) mm |
β = 111.371 (12)° |
STOE IPDS 2 diffractometer | 1119 independent reflections |
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996) | 1027 reflections with I > 2σ(I) |
Tmin = 0.09, Tmax = 0.19 | Rint = 0.038 |
5334 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 66 parameters |
wR(F2) = 0.035 | 0 restraints |
S = 1.46 | Δρmax = 0.77 e Å−3 |
1119 reflections | Δρmin = −0.81 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. |
x | y | z | Uiso*/Ueq | ||
Ba1 | 0 | 0.34284 (4) | 0.25 | 0.00500 (6) | |
V1 | 0.57508 (6) | 0.24983 (8) | 0.45065 (4) | 0.00343 (8) | |
V2 | 0.68887 (6) | 0.77436 (8) | 0.35012 (5) | 0.00357 (8) | |
O1 | 0.8926 (3) | 0.8688 (4) | 0.3485 (2) | 0.0067 (3) | |
O2 | 0.7720 (2) | 0.4163 (4) | 0.44693 (19) | 0.0047 (3) | |
O3 | 0.5800 (2) | 0.4146 (3) | 0.64517 (18) | 0.0046 (3) | |
O4 | 0.6744 (2) | 0.9082 (3) | 0.54209 (19) | 0.0044 (3) | |
O5 | 0.5 | 0.0605 (5) | 0.25 | 0.0042 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba1 | 0.00593 (9) | 0.00435 (10) | 0.00482 (9) | 0 | 0.00208 (6) | 0 |
V1 | 0.00451 (16) | 0.00299 (18) | 0.00288 (17) | −0.00032 (12) | 0.00144 (13) | −0.00009 (12) |
V2 | 0.00403 (16) | 0.00357 (18) | 0.00320 (16) | −0.00021 (12) | 0.00142 (13) | 0.00003 (12) |
O1 | 0.0085 (7) | 0.0046 (8) | 0.0077 (7) | 0.0000 (6) | 0.0039 (6) | 0.0008 (6) |
O2 | 0.0053 (7) | 0.0038 (7) | 0.0053 (7) | 0.0003 (6) | 0.0022 (5) | 0.0012 (6) |
O3 | 0.0073 (7) | 0.0047 (7) | 0.0017 (7) | 0.0005 (6) | 0.0015 (6) | −0.0003 (5) |
O4 | 0.0053 (7) | 0.0047 (7) | 0.0031 (7) | 0.0002 (5) | 0.0016 (5) | −0.0004 (5) |
O5 | 0.0071 (10) | 0.0036 (10) | 0.0014 (9) | 0 | 0.0009 (8) | 0 |
Ba1—O1i | 2.7428 (19) | V2—O3 | 3.6196 (16) |
Ba1—O1ii | 2.7428 (19) | V2—O4xvi | 3.6236 (17) |
Ba1—O4iii | 2.8172 (17) | V2—V1xviii | 3.6488 (7) |
Ba1—O4iv | 2.8172 (17) | V2—Ba1iv | 3.6685 (8) |
Ba1—O1v | 2.9641 (19) | V2—O4v | 3.7587 (19) |
Ba1—O1vi | 2.9641 (19) | V2—O5 | 3.787 (2) |
Ba1—O2vi | 2.9760 (16) | V2—V1v | 3.8086 (7) |
Ba1—O2v | 2.9760 (16) | V2—O1xxi | 3.825 (2) |
Ba1—O2iv | 2.9768 (18) | V2—O2xi | 3.9546 (19) |
Ba1—O2iii | 2.9768 (18) | V2—Ba1xxii | 3.9931 (6) |
Ba1—O3iv | 3.2125 (17) | V2—O2v | 4.0027 (19) |
Ba1—O3iii | 3.2125 (17) | V2—O2ix | 4.1496 (17) |
V1—O2 | 1.7194 (17) | V2—O1v | 4.153 (2) |
V1—O4vii | 1.9147 (18) | V2—V2vii | 4.9291 (7) |
V1—O3 | 1.9790 (16) | V2—V2xiii | 4.9291 (7) |
V1—O5 | 1.9833 (13) | V2—V2xxi | 5.0542 (11) |
V1—O3iv | 2.0397 (17) | V2—V2xvii | 5.1756 (8) |
V1—O4iv | 2.0754 (17) | V2—V2xx | 5.1756 (8) |
V1—V2vii | 2.7781 (6) | V2—V2xvi | 5.1890 (10) |
V1—V2 | 2.9849 (7) | V2—V1xi | 5.2195 (11) |
V1—V1viii | 2.9984 (9) | V2—V2xi | 5.2832 (11) |
V1—V1iv | 3.0010 (9) | V2—V2ix | 5.3995 (8) |
V1—V2iv | 3.2000 (7) | V2—V2x | 5.3995 (8) |
V1—O3ix | 3.3117 (17) | V2—V2iv | 5.4124 (10) |
V1—O4 | 3.3707 (18) | V2—Ba1xvi | 5.6621 (8) |
V1—O5viii | 3.4145 (13) | V2—V2i | 5.6691 (8) |
V1—O1vii | 3.4576 (18) | V2—V2xviii | 5.6691 (8) |
V1—O3viii | 3.4855 (18) | V2—V2xxiii | 5.6898 (11) |
V1—V1v | 3.5001 (10) | V2—V1xvi | 5.7758 (8) |
V1—V2x | 3.5139 (8) | V2—V1xx | 5.9555 (9) |
V1—O2iv | 3.5268 (17) | V2—V1viii | 5.9759 (9) |
V1—V2i | 3.6488 (7) | V2—V1x | 5.9841 (10) |
V1—O1x | 3.669 (2) | V2—V1xiv | 6.1497 (9) |
V1—O2v | 3.7819 (19) | O1—Ba1xxii | 2.7428 (19) |
V1—V2v | 3.8086 (7) | O1—Ba1xii | 2.9641 (19) |
V1—O1xi | 3.838 (2) | O1—V1xiii | 3.4576 (18) |
V1—Ba1iv | 3.9647 (7) | O1—V1ix | 3.669 (2) |
V1—O1i | 4.093 (2) | O1—V2xxi | 3.825 (2) |
V1—Ba1xii | 4.3125 (7) | O1—V1xi | 3.838 (2) |
V1—Ba1viii | 4.4968 (7) | O1—V1xviii | 4.093 (2) |
V1—V1vii | 4.9291 (7) | O1—V2v | 4.153 (2) |
V1—V1xiii | 4.9291 (7) | O2—Ba1xii | 2.9760 (16) |
V1—V2xi | 5.2195 (11) | O2—Ba1iv | 2.9768 (18) |
V1—V1xiv | 5.2825 (8) | O2—V2vii | 3.2885 (18) |
V1—V1xv | 5.2825 (8) | O2—V1iv | 3.5268 (17) |
V1—V1x | 5.2840 (8) | O2—V1v | 3.7819 (19) |
V1—V1ix | 5.2840 (8) | O2—V2xi | 3.9546 (19) |
V1—V2xvi | 5.7758 (8) | O2—V2v | 4.0027 (19) |
V1—V2xvii | 5.9555 (9) | O2—V2x | 4.1496 (17) |
V1—V2viii | 5.9759 (8) | O3—V2x | 2.0165 (17) |
V1—V2ix | 5.9841 (10) | O3—V1iv | 2.0397 (17) |
V1—V1i | 6.0454 (8) | O3—V2iv | 2.2625 (17) |
V1—V1xviii | 6.0454 (8) | O3—Ba1iv | 3.2125 (17) |
V1—V1xix | 6.1054 (12) | O3—V1x | 3.3117 (17) |
V1—V2xv | 6.1497 (9) | O3—V1viii | 3.4855 (18) |
V2—O1 | 1.6237 (18) | O4—V1xiii | 1.9147 (18) |
V2—O4 | 1.9522 (16) | O4—V1iv | 2.0754 (17) |
V2—O2 | 1.9789 (18) | O4—Ba1iv | 2.8172 (17) |
V2—O5xiii | 1.9875 (19) | O4—V2xvii | 3.2430 (17) |
V2—O3ix | 2.0165 (17) | O4—V2xvi | 3.6236 (17) |
V2—O3iv | 2.2625 (17) | O4—V2v | 3.7587 (19) |
V2—V1xiii | 2.7781 (6) | O5—V1v | 1.9833 (13) |
V2—V2v | 2.8004 (10) | O5—V2i | 1.9875 (19) |
V2—V1iv | 3.2000 (7) | O5—V2vii | 1.9875 (19) |
V2—O4xx | 3.2430 (17) | O5—V1xiv | 3.4145 (13) |
V2—O2xiii | 3.2885 (18) | O5—V1viii | 3.4145 (13) |
V2—V1ix | 3.5139 (8) | O5—V2v | 3.787 (2) |
V2—Ba1xii | 3.5522 (6) | ||
O1i—Ba1—O1ii | 63.17 (7) | O3—V2—O4v | 122.54 (4) |
O1i—Ba1—O4iii | 71.88 (5) | O4xvi—V2—O4v | 80.28 (3) |
O1ii—Ba1—O4iii | 64.07 (5) | O1—V2—O5 | 122.80 (7) |
O1i—Ba1—O4iv | 64.07 (5) | O4—V2—O5 | 113.43 (5) |
O1ii—Ba1—O4iv | 71.88 (5) | O2—V2—O5 | 46.65 (5) |
O4iii—Ba1—O4iv | 127.89 (7) | O5xiii—V2—O5 | 113.51 (4) |
O1i—Ba1—O1v | 119.42 (6) | O3ix—V2—O5 | 49.36 (5) |
O1ii—Ba1—O1v | 177.41 (4) | O3iv—V2—O5 | 50.06 (4) |
O4iii—Ba1—O1v | 116.27 (5) | O4xx—V2—O5 | 109.99 (3) |
O4iv—Ba1—O1v | 109.01 (5) | O2xiii—V2—O5 | 168.41 (3) |
O1i—Ba1—O1vi | 177.41 (4) | O3—V2—O5 | 63.99 (3) |
O1ii—Ba1—O1vi | 119.42 (6) | O4xvi—V2—O5 | 102.16 (3) |
O4iii—Ba1—O1vi | 109.01 (5) | O4v—V2—O5 | 81.03 (3) |
O4iv—Ba1—O1vi | 116.27 (5) | O1—V2—O1xxi | 48.21 (8) |
O1v—Ba1—O1vi | 57.99 (7) | O4—V2—O1xxi | 58.57 (5) |
O1i—Ba1—O2vi | 128.57 (5) | O2—V2—O1xxi | 91.83 (6) |
O1ii—Ba1—O2vi | 65.41 (5) | O5xiii—V2—O1xxi | 106.59 (6) |
O4iii—Ba1—O2vi | 85.16 (5) | O3ix—V2—O1xxi | 148.81 (5) |
O4iv—Ba1—O2vi | 101.02 (5) | O3iv—V2—O1xxi | 133.70 (5) |
O1v—Ba1—O2vi | 112.00 (5) | O4xx—V2—O1xxi | 100.47 (4) |
O1vi—Ba1—O2vi | 54.02 (5) | O2xiii—V2—O1xxi | 47.93 (4) |
O1i—Ba1—O2v | 65.41 (5) | O3—V2—O1xxi | 91.41 (4) |
O1ii—Ba1—O2v | 128.57 (5) | O4xvi—V2—O1xxi | 96.39 (4) |
O4iii—Ba1—O2v | 101.02 (5) | O4v—V2—O1xxi | 139.15 (4) |
O4iv—Ba1—O2v | 85.16 (5) | O5—V2—O1xxi | 138.45 (3) |
O1v—Ba1—O2v | 54.02 (5) | O4—V2—O2xi | 92.04 (6) |
O1vi—Ba1—O2v | 112.00 (5) | O2—V2—O2xi | 57.73 (7) |
O2vi—Ba1—O2v | 166.02 (7) | O5xiii—V2—O2xi | 147.16 (6) |
O1i—Ba1—O2iv | 121.17 (5) | O3ix—V2—O2xi | 109.95 (6) |
O1ii—Ba1—O2iv | 99.32 (5) | O3iv—V2—O2xi | 132.85 (5) |
O4iii—Ba1—O2iv | 153.21 (4) | O4xx—V2—O2xi | 103.55 (4) |
O4iv—Ba1—O2iv | 57.16 (5) | O2xiii—V2—O2xi | 92.00 (4) |
O1v—Ba1—O2iv | 79.38 (5) | O3—V2—O2xi | 90.20 (4) |
O1vi—Ba1—O2iv | 59.11 (5) | O4xvi—V2—O2xi | 137.07 (4) |
O2vi—Ba1—O2iv | 68.41 (5) | O4v—V2—O2xi | 140.81 (4) |
O2v—Ba1—O2iv | 105.72 (5) | O5—V2—O2xi | 97.56 (3) |
O1i—Ba1—O2iii | 99.32 (5) | V1v—V2—O2xi | 111.62 (3) |
O1ii—Ba1—O2iii | 121.17 (5) | O1xxi—V2—O2xi | 46.87 (4) |
O4iii—Ba1—O2iii | 57.16 (5) | O1—V2—O2v | 135.88 (7) |
O4iv—Ba1—O2iii | 153.21 (4) | O4—V2—O2v | 117.25 (6) |
O1v—Ba1—O2iii | 59.11 (5) | O2—V2—O2v | 88.69 (7) |
O1vi—Ba1—O2iii | 79.38 (5) | O5xiii—V2—O2v | 71.70 (6) |
O2vi—Ba1—O2iii | 105.72 (5) | O4xx—V2—O2v | 81.90 (4) |
O2v—Ba1—O2iii | 68.41 (5) | O2xiii—V2—O2v | 130.32 (4) |
O2iv—Ba1—O2iii | 132.99 (7) | O3—V2—O2v | 85.79 (4) |
O1i—Ba1—O3iv | 91.98 (5) | O4xvi—V2—O2v | 79.58 (4) |
O1ii—Ba1—O3iv | 126.84 (5) | O1xxi—V2—O2v | 175.78 (4) |
O4iii—Ba1—O3iv | 154.28 (4) | O2xi—V2—O2v | 136.16 (2) |
O4iv—Ba1—O3iv | 54.98 (5) | O1—V2—O2ix | 66.09 (7) |
O1v—Ba1—O3iv | 54.05 (5) | O4—V2—O2ix | 171.70 (6) |
O1vi—Ba1—O3iv | 86.32 (5) | O2—V2—O2ix | 94.83 (4) |
O2vi—Ba1—O3iv | 120.36 (4) | O5xiii—V2—O2ix | 93.24 (3) |
O2v—Ba1—O3iv | 53.41 (4) | O3iv—V2—O2ix | 111.25 (5) |
O2iv—Ba1—O3iv | 52.50 (4) | O2xiii—V2—O2ix | 112.97 (4) |
O2iii—Ba1—O3iv | 108.17 (4) | O3—V2—O2ix | 137.21 (4) |
O1i—Ba1—O3iii | 126.84 (5) | O4xvi—V2—O2ix | 137.25 (4) |
O1ii—Ba1—O3iii | 91.98 (5) | O4v—V2—O2ix | 56.99 (4) |
O4iii—Ba1—O3iii | 54.98 (5) | O5—V2—O2ix | 74.62 (3) |
O4iv—Ba1—O3iii | 154.28 (4) | O1xxi—V2—O2ix | 114.29 (4) |
O1v—Ba1—O3iii | 86.32 (5) | O2xi—V2—O2ix | 84.67 (4) |
O1vi—Ba1—O3iii | 54.05 (5) | O2v—V2—O2ix | 69.82 (4) |
O2vi—Ba1—O3iii | 53.41 (4) | O1—V2—O1v | 145.96 (8) |
O2v—Ba1—O3iii | 120.36 (4) | O4—V2—O1v | 88.01 (6) |
O2iv—Ba1—O3iii | 108.17 (4) | O2—V2—O1v | 114.53 (6) |
O2iii—Ba1—O3iii | 52.50 (4) | O3ix—V2—O1v | 67.98 (5) |
O3iv—Ba1—O3iii | 136.29 (6) | O4xx—V2—O1v | 82.12 (4) |
O2—V1—O4vii | 102.93 (8) | O2xiii—V2—O1v | 94.69 (4) |
O2—V1—O3 | 95.62 (8) | O3—V2—O1v | 83.87 (4) |
O4vii—V1—O3 | 94.50 (7) | O5—V2—O1v | 75.36 (3) |
O2—V1—O5 | 99.11 (7) | O1xxi—V2—O1v | 137.99 (3) |
O4vii—V1—O5 | 86.51 (8) | O2xi—V2—O1v | 172.25 (4) |
O3—V1—O5 | 164.63 (6) | O2v—V2—O1v | 38.58 (4) |
O2—V1—O3iv | 88.44 (8) | O2ix—V2—O1v | 96.28 (4) |
O4vii—V1—O3iv | 168.59 (7) | V2—O1—Ba1xxii | 130.50 (10) |
O3—V1—O3iv | 83.39 (7) | V2—O1—Ba1xii | 97.13 (8) |
O5—V1—O3iv | 92.59 (8) | Ba1xxii—O1—Ba1xii | 119.42 (6) |
O2—V1—O4iv | 173.51 (8) | V2—O1—V1xiii | 52.25 (5) |
O4vii—V1—O4iv | 82.65 (7) | Ba1xxii—O1—V1xiii | 87.34 (5) |
O3—V1—O4iv | 80.52 (7) | Ba1xii—O1—V1xiii | 149.35 (6) |
O5—V1—O4iv | 84.41 (5) | V2—O1—V1ix | 71.66 (6) |
O3iv—V1—O4iv | 85.94 (7) | Ba1xxii—O1—V1ix | 87.83 (5) |
O2—V1—O3ix | 57.36 (7) | Ba1xii—O1—V1ix | 72.54 (4) |
O4vii—V1—O3ix | 134.23 (6) | V1xiii—O1—V1ix | 95.63 (5) |
O3—V1—O3ix | 125.78 (3) | V2—O1—V2xxi | 131.79 (8) |
O5—V1—O3ix | 60.64 (7) | Ba1xxii—O1—V2xxi | 65.52 (4) |
O3iv—V1—O3ix | 53.33 (6) | Ba1xii—O1—V2xxi | 112.41 (5) |
O4iv—V1—O3ix | 120.89 (6) | V1xiii—O1—V2xxi | 91.43 (4) |
O2—V1—O4 | 55.20 (6) | V1ix—O1—V2xxi | 152.09 (5) |
O4vii—V1—O4 | 135.89 (8) | V2—O1—V1xi | 142.44 (9) |
O3—V1—O4 | 56.26 (6) | Ba1xxii—O1—V1xi | 84.47 (5) |
O5—V1—O4 | 130.80 (7) | Ba1xii—O1—V1xi | 69.96 (4) |
O3iv—V1—O4 | 51.01 (6) | V1xiii—O1—V1xi | 131.82 (5) |
O4iv—V1—O4 | 118.44 (5) | V1ix—O1—V1xi | 131.24 (5) |
O3ix—V1—O4 | 70.48 (4) | V2—O1—V1xviii | 62.79 (6) |
O2—V1—O5viii | 129.61 (6) | Ba1xxii—O1—V1xviii | 70.79 (4) |
O4vii—V1—O5viii | 52.91 (6) | Ba1xii—O1—V1xviii | 117.29 (5) |
O3—V1—O5viii | 51.96 (6) | V1xiii—O1—V1xviii | 54.44 (3) |
O5—V1—O5viii | 119.17 (3) | V1ix—O1—V1xviii | 45.03 (3) |
O3iv—V1—O5viii | 118.71 (5) | V2xxi—O1—V1xviii | 125.12 (5) |
O4iv—V1—O5viii | 51.47 (5) | V1xi—O1—V1xviii | 154.66 (5) |
O3ix—V1—O5viii | 171.12 (4) | Ba1xxii—O1—V2v | 110.15 (5) |
O4—V1—O5viii | 108.21 (5) | Ba1xii—O1—V2v | 97.61 (5) |
O2—V1—O1vii | 63.39 (7) | V1xiii—O1—V2v | 56.41 (3) |
O4vii—V1—O1vii | 56.21 (5) | V1ix—O1—V2v | 47.80 (3) |
O3—V1—O1vii | 134.05 (6) | V2xxi—O1—V2v | 147.79 (5) |
O5—V1—O1vii | 58.19 (4) | V1xi—O1—V2v | 164.57 (6) |
O3iv—V1—O1vii | 132.05 (5) | V1—O2—V2 | 107.42 (9) |
O4iv—V1—O1vii | 122.98 (6) | V1—O2—Ba1xii | 131.53 (8) |
O3ix—V1—O1vii | 78.74 (4) | V2—O2—Ba1xii | 89.25 (6) |
O4—V1—O1vii | 118.58 (4) | V1—O2—Ba1iv | 112.40 (7) |
O5viii—V1—O1vii | 108.98 (5) | V2—O2—Ba1iv | 93.31 (6) |
O2—V1—O3viii | 131.23 (6) | Ba1xii—O2—Ba1iv | 111.59 (5) |
O4vii—V1—O3viii | 47.93 (6) | V1—O2—V2vii | 57.64 (5) |
O3—V1—O3viii | 120.85 (5) | V2—O2—V2vii | 137.30 (8) |
O5—V1—O3viii | 50.29 (7) | Ba1xii—O2—V2vii | 79.03 (4) |
O3iv—V1—O3viii | 124.18 (7) | Ba1iv—O2—V2vii | 129.24 (6) |
O4iv—V1—O3viii | 55.10 (5) | V1—O2—V1iv | 58.22 (5) |
O3ix—V1—O3viii | 110.91 (3) | V2—O2—V1iv | 64.02 (4) |
O4—V1—O3viii | 173.38 (4) | Ba1xii—O2—V1iv | 152.56 (6) |
O5viii—V1—O3viii | 69.36 (4) | Ba1iv—O2—V1iv | 77.88 (4) |
O1vii—V1—O3viii | 67.90 (4) | V2vii—O2—V1iv | 115.84 (5) |
O2—V1—O2iv | 121.78 (5) | V1—O2—V1v | 67.35 (6) |
O4vii—V1—O2iv | 120.12 (5) | V2—O2—V1v | 75.64 (5) |
O3—V1—O2iv | 47.51 (6) | Ba1xii—O2—V1v | 73.83 (4) |
O5—V1—O2iv | 119.34 (4) | Ba1iv—O2—V1v | 167.86 (6) |
O3iv—V1—O2iv | 50.97 (5) | V2vii—O2—V1v | 61.67 (3) |
O4iv—V1—O2iv | 51.85 (5) | V1iv—O2—V1v | 92.54 (4) |
O3ix—V1—O2iv | 104.22 (4) | V1—O2—V2xi | 129.49 (8) |
O4—V1—O2iv | 66.59 (4) | V2—O2—V2xi | 122.27 (7) |
O5viii—V1—O2iv | 67.75 (4) | Ba1xii—O2—V2xi | 62.04 (3) |
O1vii—V1—O2iv | 174.81 (4) | Ba1iv—O2—V2xi | 59.69 (3) |
O3viii—V1—O2iv | 106.94 (4) | V2vii—O2—V2xi | 88.00 (4) |
O2—V1—O1x | 80.78 (7) | V1iv—O2—V2xi | 136.81 (5) |
O4vii—V1—O1x | 53.16 (6) | V1v—O2—V2xi | 130.58 (4) |
O3—V1—O1x | 49.40 (6) | V1—O2—V2v | 71.04 (6) |
O5—V1—O1x | 137.72 (7) | Ba1xii—O2—V2v | 100.69 (5) |
O3iv—V1—O1x | 129.51 (6) | Ba1iv—O2—V2v | 122.93 (5) |
O4iv—V1—O1x | 100.33 (6) | V2vii—O2—V2v | 101.62 (4) |
O3ix—V1—O1x | 138.02 (4) | V1iv—O2—V2v | 55.20 (3) |
O4—V1—O1x | 83.83 (4) | V2xi—O2—V2v | 158.57 (5) |
O5viii—V1—O1x | 48.93 (3) | V1—O2—V2x | 56.73 (5) |
O1vii—V1—O1x | 85.70 (4) | V2—O2—V2x | 119.22 (6) |
O3viii—V1—O1x | 98.45 (4) | Ba1xii—O2—V2x | 148.23 (6) |
O2iv—V1—O1x | 94.64 (4) | Ba1iv—O2—V2x | 56.98 (3) |
O2—V1—O2v | 100.25 (7) | V2vii—O2—V2x | 87.38 (4) |
O4vii—V1—O2v | 130.54 (6) | V1iv—O2—V2x | 58.82 (3) |
O3—V1—O2v | 125.89 (6) | V1v—O2—V2x | 124.08 (4) |
O5—V1—O2v | 46.81 (6) | V2xi—O2—V2x | 89.16 (4) |
O3iv—V1—O2v | 46.18 (5) | V2v—O2—V2x | 110.18 (4) |
O4iv—V1—O2v | 78.12 (5) | V1—O3—V2x | 123.15 (9) |
O4—V1—O2v | 92.98 (4) | V1—O3—V1iv | 96.61 (7) |
O5viii—V1—O2v | 129.56 (3) | V2x—O3—V1iv | 139.76 (8) |
O1vii—V1—O2v | 98.89 (4) | V1—O3—V2iv | 97.73 (7) |
O3viii—V1—O2v | 84.36 (4) | V2x—O3—V2iv | 81.54 (6) |
O2iv—V1—O2v | 80.89 (3) | V1iv—O3—V2iv | 87.71 (6) |
O1x—V1—O2v | 175.29 (4) | V1—O3—Ba1iv | 96.69 (6) |
O2—V1—O1xi | 46.43 (7) | V2x—O3—Ba1iv | 82.15 (5) |
O4vii—V1—O1xi | 58.21 (6) | V1iv—O3—Ba1iv | 100.60 (6) |
O3—V1—O1xi | 87.13 (6) | V2iv—O3—Ba1iv | 162.40 (7) |
O5—V1—O1xi | 106.25 (4) | V1—O3—V1x | 174.04 (8) |
O3iv—V1—O1xi | 132.59 (6) | V2x—O3—V1x | 62.71 (4) |
O4iv—V1—O1xi | 137.86 (6) | V1iv—O3—V1x | 77.70 (5) |
O3ix—V1—O1xi | 99.00 (4) | V2iv—O3—V1x | 83.94 (5) |
O4—V1—O1xi | 85.62 (4) | Ba1iv—O3—V1x | 82.74 (4) |
O5viii—V1—O1xi | 89.59 (3) | V1—O3—V1viii | 59.15 (5) |
O1vii—V1—O1xi | 48.18 (5) | V2x—O3—V1viii | 78.09 (5) |
O3viii—V1—O1xi | 100.40 (4) | V1iv—O3—V1viii | 124.18 (7) |
O2iv—V1—O1xi | 134.38 (4) | V2iv—O3—V1viii | 52.74 (4) |
O2v—V1—O1xi | 138.43 (4) | Ba1iv—O3—V1viii | 129.35 (5) |
O2—V1—O1i | 138.76 (6) | V1x—O3—V1viii | 125.57 (5) |
O4vii—V1—O1i | 90.27 (6) | V1—O3—V2 | 55.53 (4) |
O3—V1—O1i | 122.44 (6) | V2x—O3—V2 | 145.20 (7) |
O3iv—V1—O1i | 81.51 (6) | V1iv—O3—V2 | 61.60 (4) |
O3ix—V1—O1i | 85.43 (4) | V2iv—O3—V2 | 132.54 (6) |
O4—V1—O1i | 132.35 (4) | Ba1iv—O3—V2 | 64.63 (3) |
O5viii—V1—O1i | 89.48 (3) | V1x—O3—V2 | 119.32 (5) |
O1vii—V1—O1i | 94.77 (5) | V1viii—O3—V2 | 114.49 (4) |
O2iv—V1—O1i | 81.32 (4) | V1xiii—O4—V2 | 91.85 (7) |
O1x—V1—O1i | 134.97 (3) | V1xiii—O4—V1iv | 97.35 (7) |
O2v—V1—O1i | 46.09 (4) | V2—O4—V1iv | 105.18 (8) |
O1xi—V1—O1i | 139.81 (2) | V1xiii—O4—Ba1iv | 143.03 (8) |
O1—V2—O4 | 106.58 (8) | V2—O4—Ba1iv | 98.94 (6) |
O1—V2—O2 | 96.49 (8) | V1iv—O4—Ba1iv | 113.42 (7) |
O4—V2—O2 | 89.81 (7) | V1xiii—O4—V2xvii | 81.50 (6) |
O1—V2—O5xiii | 108.73 (8) | V2—O4—V2xvii | 169.72 (8) |
O4—V2—O5xiii | 85.39 (6) | V1iv—O4—V2xvii | 83.56 (5) |
O2—V2—O5xiii | 154.67 (7) | Ba1iv—O4—V2xvii | 82.11 (4) |
O1—V2—O3ix | 100.77 (8) | V1xiii—O4—V1 | 135.89 (8) |
O4—V2—O3ix | 152.61 (7) | V2—O4—V1 | 61.58 (5) |
O2—V2—O3ix | 88.55 (7) | V1iv—O4—V1 | 61.56 (5) |
O5xiii—V2—O3ix | 84.50 (6) | Ba1iv—O4—V1 | 79.14 (4) |
O1—V2—O3iv | 172.34 (8) | V2xvii—O4—V1 | 128.43 (5) |
O4—V2—O3iv | 76.52 (7) | V1xiii—O4—V2xvi | 61.80 (4) |
O2—V2—O3iv | 76.38 (7) | V2—O4—V2xvi | 134.89 (7) |
O5xiii—V2—O3iv | 78.32 (6) | V1iv—O4—V2xvi | 49.74 (4) |
O3ix—V2—O3iv | 76.53 (7) | Ba1iv—O4—V2xvi | 124.47 (5) |
O1—V2—O4xx | 64.99 (7) | V2xvii—O4—V2xvi | 47.74 (3) |
O4—V2—O4xx | 131.13 (3) | V1—O4—V2xvi | 111.29 (4) |
O2—V2—O4xx | 137.57 (6) | V1xiii—O4—V2v | 71.87 (5) |
O5xiii—V2—O4xx | 56.96 (3) | V2—O4—V2v | 46.53 (4) |
O3ix—V2—O4xx | 60.67 (6) | V1iv—O4—V2v | 67.03 (5) |
O3iv—V2—O4xx | 118.51 (5) | Ba1iv—O4—V2v | 138.15 (6) |
O1—V2—O2xiii | 68.79 (7) | V2xvii—O4—V2v | 136.51 (5) |
O4—V2—O2xiii | 59.44 (6) | V1—O4—V2v | 64.31 (3) |
O2—V2—O2xiii | 137.30 (8) | V2xvi—O4—V2v | 89.01 (4) |
O5xiii—V2—O2xiii | 58.68 (6) | V1—O5—V1v | 123.86 (13) |
O3ix—V2—O2xiii | 132.61 (6) | V1—O5—V2i | 133.54 (4) |
O3iv—V2—O2xiii | 118.37 (5) | V1v—O5—V2i | 88.80 (3) |
O4xx—V2—O2xiii | 73.80 (4) | V1—O5—V2vii | 88.80 (3) |
O1—V2—O3 | 129.18 (7) | V1v—O5—V2vii | 133.54 (4) |
O4—V2—O3 | 50.21 (6) | V2i—O5—V2vii | 89.58 (11) |
O2—V2—O3 | 48.57 (5) | V1—O5—V1xiv | 155.376 (19) |
O5xiii—V2—O3 | 112.30 (4) | V1v—O5—V1xiv | 60.83 (3) |
O3ix—V2—O3 | 111.63 (4) | V2i—O5—V1xiv | 66.70 (4) |
O3iv—V2—O3 | 47.46 (6) | V2vii—O5—V1xiv | 76.10 (5) |
O4xx—V2—O3 | 165.82 (4) | V1—O5—V1viii | 60.83 (3) |
O2xiii—V2—O3 | 109.65 (4) | V1v—O5—V1viii | 155.376 (19) |
O1—V2—O4xvi | 134.92 (8) | V2i—O5—V1viii | 76.10 (5) |
O4—V2—O4xvi | 45.11 (7) | V2vii—O5—V1viii | 66.70 (4) |
O2—V2—O4xvi | 114.01 (5) | V1xiv—O5—V1viii | 126.77 (8) |
O5xiii—V2—O4xvi | 47.98 (3) | V1—O5—V2 | 51.43 (6) |
O3ix—V2—O4xvi | 111.87 (6) | V1v—O5—V2 | 75.47 (7) |
O3iv—V2—O4xvi | 52.10 (5) | V2i—O5—V2 | 156.91 (7) |
O4xx—V2—O4xvi | 104.82 (5) | V2vii—O5—V2 | 113.51 (4) |
O2xiii—V2—O4xvi | 66.27 (4) | V1xiv—O5—V2 | 117.19 (4) |
O3—V2—O4xvi | 65.81 (4) | V1viii—O5—V2 | 112.06 (3) |
O1—V2—O4v | 107.81 (7) | V1—O5—V2v | 75.47 (7) |
O4—V2—O4v | 124.70 (6) | V1v—O5—V2v | 51.43 (6) |
O2—V2—O4v | 126.96 (6) | V2i—O5—V2v | 113.51 (4) |
O3iv—V2—O4v | 75.08 (5) | V2vii—O5—V2v | 156.91 (7) |
O4xx—V2—O4v | 43.49 (5) | V1xiv—O5—V2v | 112.06 (3) |
O2xiii—V2—O4v | 95.67 (4) | V1viii—O5—V2v | 117.19 (4) |
Symmetry codes: (i) −x+1, y−1, −z+1/2; (ii) x−1, y−1, z; (iii) x−1, −y+1, z−1/2; (iv) −x+1, −y+1, −z+1; (v) −x+1, y, −z+1/2; (vi) x−1, y, z; (vii) x, y−1, z; (viii) −x+1, −y, −z+1; (ix) x, −y+1, z−1/2; (x) x, −y+1, z+1/2; (xi) −x+2, −y+1, −z+1; (xii) x+1, y, z; (xiii) x, y+1, z; (xiv) x, −y, z−1/2; (xv) x, −y, z+1/2; (xvi) −x+1, −y+2, −z+1; (xvii) x, −y+2, z+1/2; (xviii) −x+1, y+1, −z+1/2; (xix) −x+1, y, −z+3/2; (xx) x, −y+2, z−1/2; (xxi) −x+2, −y+2, −z+1; (xxii) x+1, y+1, z; (xxiii) −x+2, y, −z+1/2. |
Experimental details
(BaV4O9_293K) | (BaV4O9_250K) | (BaV4O9_200K) | (BaV4O9_150K) | |
Crystal data | ||||
Chemical formula | O9V4·Ba | O9V4·Ba | O9V4·Ba | O9V4·Ba |
Mr | 485.1 | 485.1 | 485.1 | 485.1 |
Crystal system, space group | Monoclinic, P2/c | Monoclinic, P2/c | Monoclinic, P2/c | Monoclinic, P2/c |
Temperature (K) | 293 | 250 | 200 | 150 |
a, b, c (Å) | 7.6396 (12), 4.9447 (7), 9.3596 (14) | 7.6303 (12), 4.9405 (7), 9.3547 (14) | 7.6231 (12), 4.9370 (7), 9.3528 (14) | 7.6140 (12), 4.9319 (7), 9.3470 (14) |
α, β, γ (°) | 90, 111.427 (11), 90 | 90, 111.395 (11), 90 | 90, 111.386 (11), 90 | 90, 111.371 (11), 90 |
V (Å3) | 329.13 (9) | 328.35 (9) | 327.76 (9) | 326.86 (8) |
Z | 2 | 2 | 2 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 11.39 | 11.42 | 11.44 | 11.47 |
Crystal size (mm) | 0.24 × 0.21 × 0.15 × 0 (radius) | 0.24 × 0.21 × 0.15 × 0 (radius) | 0.24 × 0.21 × 0.15 × 0 (radius) | 0.24 × 0.21 × 0.15 × 0 (radius) |
Data collection | ||||
Diffractometer | STOE IPDS 2 diffractometer | STOE IPDS 2 diffractometer | STOE IPDS 2 diffractometer | STOE IPDS 2 diffractometer |
Absorption correction | Numerical X-SHAPE (Stoe & Cie, 1996) | Numerical X-SHAPE (Stoe & Cie, 1996) | Numerical X-SHAPE (Stoe & Cie, 1996) | Numerical X-SHAPE (Stoe & Cie, 1996) |
Tmin, Tmax | 0.09, 0.19 | 0.09, 0.19 | 0.09, 0.19 | 0.09, 0.19 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5391, 1132, 1031 | 5369, 1125, 1025 | 5359, 1122, 1025 | 5337, 1119, 1021 |
Rint | 0.045 | 0.044 | 0.043 | 0.042 |
(sin θ/λ)max (Å−1) | 0.749 | 0.746 | 0.745 | 0.746 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.023, 0.040, 1.45 | 0.022, 0.038, 1.41 | 0.022, 0.038, 1.46 | 0.020, 0.036, 1.38 |
No. of reflections | 1132 | 1125 | 1122 | 1119 |
No. of parameters | 66 | 66 | 66 | 66 |
Δρmax, Δρmin (e Å−3) | 0.80, −0.88 | 0.72, −0.76 | 0.83, −0.77 | 0.69, −0.78 |
(BaV4O9_100K) | |
Crystal data | |
Chemical formula | O9V4·Ba |
Mr | 485.1 |
Crystal system, space group | Monoclinic, P2/c |
Temperature (K) | 100 |
a, b, c (Å) | 7.6084 (13), 4.9291 (7), 9.3464 (15) |
α, β, γ (°) | 90, 111.371 (12), 90 |
V (Å3) | 326.41 (9) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 11.48 |
Crystal size (mm) | 0.24 × 0.21 × 0.15 × 0 (radius) |
Data collection | |
Diffractometer | STOE IPDS 2 diffractometer |
Absorption correction | Numerical X-SHAPE (Stoe & Cie, 1996) |
Tmin, Tmax | 0.09, 0.19 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5334, 1119, 1027 |
Rint | 0.038 |
(sin θ/λ)max (Å−1) | 0.746 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.035, 1.46 |
No. of reflections | 1119 |
No. of parameters | 66 |
Δρmax, Δρmin (e Å−3) | 0.77, −0.81 |
Computer programs: X-AREA (Stoe, 2002), X-RED (Stoe, 1996), SIR2002 (Burla et al., 2003), SHELXL97 (Sheldrick, 1997), ATOMS Version 5.1, WinGX 1.64.05 (Farrugia, 1999).