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The structure of the transition metal oxide V6O13, a potential cathode material in lithium-polymer batteries, has been studied at 95 K using single-crystal X-ray diffraction (XRD). A phase transition has been determined by differential scanning calorimetry (DSC) measurements to occur at 153 K, with a heat of transition of -1.98 kJ mol-1. In this low-temperature phase, the V and O atoms move by up to 0.21 Å out of the mirror plane they occupy in the room-temperature structure. It is concluded that the earlier reported space group P21/a [Kawada et al. (1978). Acta Cryst. B34, 1037-1039] is incorrect and that a more appropriate choice of space group is Pc.
Supporting information
Data collection: DIF4 (Stoe, 1988) for Stoe_data. Cell refinement: LATCON (Lundgren, 1983) for Stoe_data; SAINT+ (Bruker 2001) for Bruker_data. Data reduction: STOEDATRED, LSQLIN AND ABSSTOE (Lundgren, 1983) for Stoe_data; SAINT+ (Bruker 2001) for Bruker_data. Program(s) used to solve structure: JANA2000 (Petricek,V. & Dusek,M., 2000) for Bruker_data. Program(s) used to refine structure: DUPALS (Lundgren, 1983) for Stoe_data; JANA2000 (Petricek,V. & Dusek,M., 2000) for Bruker_data. For both compounds, molecular graphics: Diamond Version 2.1c. Software used to prepare material for publication: DISTAN (Lundgren, 1983) for Stoe_data; JANA2000 (Petricek,V. & Dusek,M., 2000) for Bruker_data.
(Stoe_data) ? #Insert the chemical name here.
top
Crystal data top
V6O13 | F(000) = 484.00 |
Mr = 513.64 | Dx = 3.890 Mg m−3 |
Monoclinic, Pc | Mo Kα radiation, λ = 0.71073 Å |
a = 10.0605 (4) Å | Cell parameters from 70 reflections |
b = 3.7108 (3) Å | θ = 27.9–37.6° |
c = 11.9633 (6) Å | µ = 6.06 mm−1 |
β = 100.927 (4)° | T = 95 K |
V = 438.52 (5) Å3 | Brick, black |
Z = 2 | 0.21 × 0.10 × 0.10 mm |
Data collection top
STOE 4-circle diffractometer | 9436 reflections with Inet > −15.0σ(Inet) |
Radiation source: xray tube | Rint = 0.016 |
Graphite monochromator | θmax = 50.0°, θmin = 0.0° |
ω/2θ scan | h = −21→21 |
Absorption correction: integration ABSSTOE, (Lundgren, 1983) | k = −3→8 |
Tmin = 0.499, Tmax = 0.609 | l = −25→25 |
9436 measured reflections | 6 standard reflections every 240 min |
4604 independent reflections | intensity decay: 1.7% |
Refinement top
Refinement on F2 | Weighting scheme based on measured s.u.'s w = 1/σ2(I) |
Least-squares matrix: full | (Δ/σ)max = 0.027 |
R[F2 > 2σ(F2)] = 0.034 | Δρmax = 2.26 e Å−3 |
wR(F2) = 0.058 | Δρmin = −1.80 e Å−3 |
S = 2.60 | Extinction correction: B-C type 1 Gaussian isotropic |
9436 reflections | Extinction coefficient: 2566 (51) |
191 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
V1a | −0.006112 | 0.30547 (10) | 0.345635 | 0.00427 (4) | |
V1b | −0.00318 (4) | 0.23442 (10) | 0.64159 (4) | 0.00333 (4) | |
V2a | 0.35945 (6) | 0.25075 (15) | 0.41726 (4) | 0.00180 (3) | |
V2b | 0.63137 (6) | 0.24770 (8) | 0.59109 (4) | 0.00166 (3) | |
V3a | 0.36290 (6) | 0.24845 (8) | 0.71952 (5) | 0.00190 (4) | |
V3b | 0.62975 (6) | 0.25116 (15) | 0.28889 (4) | 0.00172 (3) | |
O1a | −0.00338 (13) | 0.2560 (6) | 0.18496 (9) | 0.00379 (18) | |
O2a | 0.38429 (12) | 0.2489 (3) | 0.88711 (9) | 0.00325 (18) | |
O3a | 0.40576 (13) | 0.2512 (7) | 0.25536 (9) | 0.00316 (18) | |
O4a | −0.00355 (15) | 0.2428 (9) | 0.50362 (10) | 0.00579 (16) | |
O5a | 0.19198 (12) | 0.2528 (6) | 0.38814 (9) | 0.0042 (2) | |
O6a | 0.19615 (13) | 0.2456 (3) | 0.68354 (10) | 0.0043 (2) | |
O7a | 0.40316 (13) | 0.2499 (6) | 0.56668 (9) | 0.00381 (19) | |
O1b | −0.00447 (13) | 0.2405 (3) | 0.83018 (9) | 0.00434 (18) | |
O2b | 0.60862 (12) | 0.2512 (6) | 0.12271 (9) | 0.00328 (18) | |
O3b | 0.58680 (13) | 0.2484 (3) | 0.75362 (9) | 0.00310 (18) | |
O5b | 0.79887 (12) | 0.2457 (3) | 0.61930 (10) | 0.0043 (2) | |
O6b | 0.79785 (13) | 0.2545 (6) | 0.32391 (9) | 0.0042 (2) | |
O7b | 0.58849 (13) | 0.2499 (7) | 0.44333 (9) | 0.0039 (2) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1a | 0.00280 (7) | 0.00449 (6) | 0.00536 (7) | 0.00000 (6) | 0.00032 (5) | −0.00182 (6) |
V1b | 0.00273 (7) | 0.00269 (6) | 0.00445 (7) | −0.00004 (7) | 0.00038 (5) | −0.00210 (7) |
V2a | 0.00193 (7) | 0.00166 (5) | 0.00183 (6) | 0.00000 (7) | 0.00041 (5) | 0.00004 (9) |
V2b | 0.00172 (7) | 0.00182 (6) | 0.00149 (5) | 0.00004 (6) | 0.00044 (5) | −0.00001 (7) |
V3a | 0.00162 (7) | 0.00150 (6) | 0.00249 (6) | −0.00003 (6) | 0.00013 (5) | 0.00000 (7) |
V3b | 0.00177 (7) | 0.00137 (5) | 0.00198 (6) | −0.00003 (7) | 0.00026 (5) | 0.00006 (9) |
O1a | 0.0042 (3) | 0.0033 (3) | 0.0038 (2) | 0.0004 (5) | 0.0008 (2) | −0.0027 (4) |
O2a | 0.0044 (3) | 0.0021 (2) | 0.0033 (2) | 0.0002 (3) | 0.0009 (2) | 0.0001 (3) |
O3a | 0.0041 (3) | 0.0018 (2) | 0.0035 (2) | −0.0001 (4) | 0.0005 (2) | 0.0001 (4) |
O4a | 0.0048 (2) | 0.0098 (3) | 0.0029 (2) | −0.0002 (4) | 0.00111 (17) | −0.0037 (5) |
O5a | 0.0030 (3) | 0.0046 (3) | 0.0052 (2) | 0.0003 (3) | 0.0012 (2) | −0.0004 (4) |
O6a | 0.0032 (4) | 0.0043 (3) | 0.0054 (3) | 0.0001 (3) | 0.0005 (2) | −0.0001 (3) |
O7a | 0.0042 (3) | 0.0038 (3) | 0.0034 (2) | −0.0003 (4) | 0.0008 (2) | 0.0000 (4) |
O1b | 0.0057 (3) | 0.0017 (2) | 0.0057 (3) | −0.0005 (3) | 0.0012 (2) | 0.0005 (3) |
O2b | 0.0049 (3) | 0.0022 (2) | 0.0028 (2) | 0.0005 (4) | 0.0009 (2) | 0.0003 (3) |
O3b | 0.0038 (3) | 0.0022 (2) | 0.0035 (2) | −0.0001 (3) | 0.0010 (2) | 0.0001 (3) |
O5b | 0.0023 (4) | 0.0048 (3) | 0.0058 (3) | −0.0002 (3) | 0.0004 (2) | −0.0003 (3) |
O6b | 0.0018 (3) | 0.0055 (3) | 0.0050 (2) | −0.0005 (3) | 0.0000 (2) | −0.0003 (4) |
O7b | 0.0050 (3) | 0.0042 (3) | 0.0028 (2) | 0.0004 (4) | 0.0012 (2) | 0.0001 (4) |
Geometric parameters (Å, º) top
V1a—O1a | 1.9363 (12) | O2a—V2av | 1.9169 (14) |
V1a—O4a | 1.8996 (13) | O2a—V3a | 1.9755 (13) |
V1a—O5a | 1.9708 (13) | O2a—O3aiv | 2.471 (2) |
V1a—O1bi | 2.0346 (12) | O2a—O3av | 2.470 (2) |
V1a—O1bii | 1.6955 (12) | O3a—V2a | 2.0763 (14) |
V1a—O6biii | 1.9491 (13) | O3a—V3ai | 1.933 (2) |
V1b—O1aiv | 1.892 (2) | O3a—V3aii | 1.936 (2) |
V1b—O1av | 1.961 (2) | O3a—V3b | 2.2127 (15) |
V1b—O4a | 1.6501 (14) | O3a—O2ai | 2.471 (2) |
V1b—O6a | 1.9731 (14) | O3a—O2aii | 2.470 (2) |
V1b—O1b | 2.2587 (14) | O4a—V1a | 1.8996 (13) |
V1b—O5biii | 1.9590 (14) | O4a—V1b | 1.6501 (14) |
V2a—O2ai | 1.9141 (14) | O5a—V1a | 1.9708 (13) |
V2a—O2aii | 1.9169 (14) | O5a—V2a | 1.6545 (14) |
V2a—O3a | 2.0763 (14) | O6a—V1b | 1.9731 (14) |
V2a—O5a | 1.6545 (14) | O6a—V3a | 1.6510 (14) |
V2a—O7a | 1.7580 (12) | O7a—V2a | 1.7580 (12) |
V2a—O7b | 2.2659 (14) | O7a—V2b | 2.2589 (14) |
V2b—O7a | 2.2589 (14) | O7a—V3a | 1.9464 (13) |
V2b—O2biv | 1.912 (2) | O1b—V1aiv | 2.0346 (12) |
V2b—O2bv | 1.920 (2) | O1b—V1av | 1.6955 (12) |
V2b—O3b | 2.0766 (14) | O1b—V1b | 2.2587 (14) |
V2b—O5b | 1.6547 (14) | O2b—V2bi | 1.912 (2) |
V2b—O7b | 1.7383 (12) | O2b—V2bii | 1.920 (2) |
V3a—O2a | 1.9755 (13) | O2b—V3b | 1.9589 (12) |
V3a—O3aiv | 1.933 (2) | O2b—O3bi | 2.463 (2) |
V3a—O3av | 1.936 (2) | O2b—O3bii | 2.466 (2) |
V3a—O6a | 1.6510 (14) | O3b—V2b | 2.0766 (14) |
V3a—O7a | 1.9464 (13) | O3b—V3a | 2.2119 (15) |
V3a—O3b | 2.2119 (15) | O3b—V3biv | 1.9317 (15) |
V3b—O3a | 2.2127 (15) | O3b—V3bv | 1.9351 (15) |
V3b—O2b | 1.9589 (12) | O3b—O2biv | 2.463 (2) |
V3b—O3bi | 1.9317 (15) | O3b—O2bv | 2.466 (2) |
V3b—O3bii | 1.9351 (15) | O5b—V1bvi | 1.9590 (14) |
V3b—O6b | 1.6635 (14) | O5b—V2b | 1.6547 (14) |
V3b—O7b | 1.9690 (13) | O6b—V1avi | 1.9491 (13) |
O1a—V1a | 1.9363 (12) | O6b—V3b | 1.6635 (14) |
O1a—V1bi | 1.892 (2) | O7b—V2a | 2.2659 (14) |
O1a—V1bii | 1.961 (2) | O7b—V2b | 1.7383 (12) |
O2a—V2aiv | 1.9141 (14) | O7b—V3b | 1.9690 (13) |
| | | |
O1a—V1a—O4a | 167.43 (12) | O2b—V3b—O6b | 99.51 (6) |
O1a—V1a—O5a | 92.45 (5) | O2b—V3b—O7b | 161.94 (6) |
O1a—V1a—O1bi | 79.25 (7) | O3bi—V3b—O3bii | 147.34 (5) |
O1a—V1a—O1bii | 89.07 (8) | O3bi—V3b—O6b | 103.70 (9) |
O1a—V1a—O6biii | 93.60 (5) | O3bi—V3b—O7b | 97.15 (8) |
O4a—V1a—O5a | 84.77 (6) | O3bii—V3b—O3bi | 147.34 (5) |
O4a—V1a—O1bi | 88.27 (10) | O3bii—V3b—O6b | 102.82 (9) |
O4a—V1a—O1bii | 103.39 (10) | O3bii—V3b—O7b | 97.40 (8) |
O4a—V1a—O6biii | 86.75 (5) | O6b—V3b—O7b | 98.55 (6) |
O5a—V1a—O1bi | 84.23 (7) | V1a—O1a—V1bi | 111.37 (10) |
O5a—V1a—O1bii | 95.53 (8) | V1a—O1a—V1bii | 99.91 (9) |
O5a—V1a—O6biii | 166.65 (8) | V1bi—O1a—V1bii | 148.72 (7) |
O1bi—V1a—O1bii | 168.28 (5) | V1bii—O1a—V1bi | 148.72 (7) |
O1bi—V1a—O6biii | 85.23 (8) | V2aiv—O2a—V2av | 151.21 (7) |
O1bii—V1a—O1bi | 168.28 (5) | V2aiv—O2a—V3a | 101.39 (5) |
O1bii—V1a—O6biii | 96.45 (8) | V2aiv—O2a—O3aiv | 54.76 (5) |
O1aiv—V1b—O1av | 148.72 (6) | V2aiv—O2a—O3av | 151.40 (7) |
O1aiv—V1b—O4a | 107.01 (12) | V2av—O2a—V2aiv | 151.21 (7) |
O1aiv—V1b—O6a | 90.25 (5) | V2av—O2a—V3a | 101.46 (5) |
O1aiv—V1b—O1b | 74.64 (5) | V2av—O2a—O3aiv | 151.39 (7) |
O1aiv—V1b—O5biii | 90.22 (5) | V2av—O2a—O3av | 54.75 (5) |
O1av—V1b—O1aiv | 148.72 (6) | V3a—O2a—O3aiv | 50.04 (5) |
O1av—V1b—O4a | 104.27 (12) | V3a—O2a—O3av | 50.12 (5) |
O1av—V1b—O6a | 87.96 (5) | O3aiv—O2a—O3av | 97.36 (7) |
O1av—V1b—O1b | 74.08 (5) | O3av—O2a—O3aiv | 97.36 (7) |
O1av—V1b—O5biii | 87.90 (5) | V2a—O3a—V3ai | 97.23 (9) |
O4a—V1b—O6a | 93.64 (7) | V2a—O3a—V3aii | 97.32 (9) |
O4a—V1b—O1b | 178.28 (11) | V2a—O3a—V3b | 103.40 (5) |
O4a—V1b—O5biii | 93.09 (6) | V2a—O3a—O2ai | 48.85 (5) |
O6a—V1b—O1b | 86.78 (5) | V2a—O3a—O2aii | 48.94 (5) |
O6a—V1b—O5biii | 172.80 (6) | V3ai—O3a—V3aii | 147.13 (6) |
O1b—V1b—O5biii | 86.42 (5) | V3ai—O3a—V3b | 102.52 (9) |
O2ai—V2a—O2aii | 151.21 (6) | V3ai—O3a—O2ai | 51.56 (6) |
O2ai—V2a—O3a | 76.39 (8) | V3ai—O3a—O2aii | 144.98 (8) |
O2ai—V2a—O5a | 97.40 (9) | V3aii—O3a—V3ai | 147.13 (6) |
O2ai—V2a—O7a | 99.98 (8) | V3aii—O3a—V3b | 102.52 (9) |
O2ai—V2a—O7b | 81.89 (8) | V3aii—O3a—O2ai | 144.99 (8) |
O2aii—V2a—O2ai | 151.21 (6) | V3aii—O3a—O2aii | 51.56 (6) |
O2aii—V2a—O3a | 76.31 (8) | V3b—O3a—O2ai | 95.36 (7) |
O2aii—V2a—O5a | 96.88 (9) | V3b—O3a—O2aii | 95.37 (7) |
O2aii—V2a—O7a | 100.18 (8) | O2ai—O3a—O2aii | 97.36 (5) |
O2aii—V2a—O7b | 82.06 (8) | O2aii—O3a—O2ai | 97.36 (5) |
O3a—V2a—O5a | 101.72 (6) | V1a—O4a—V1b | 174.0 (2) |
O3a—V2a—O7a | 153.05 (6) | V1a—O5a—V2a | 173.88 (14) |
O3a—V2a—O7b | 74.11 (5) | V1b—O6a—V3a | 179.08 (8) |
O5a—V2a—O7a | 105.22 (6) | V2a—O7a—V2b | 100.58 (6) |
O5a—V2a—O7b | 175.83 (6) | V2a—O7a—V3a | 153.99 (8) |
O7a—V2a—O7b | 78.94 (5) | V2b—O7a—V3a | 105.43 (5) |
O7a—V2b—O2biv | 82.65 (7) | V1aiv—O1b—V1av | 168.28 (7) |
O7a—V2b—O2bv | 82.29 (7) | V1aiv—O1b—V1b | 94.74 (4) |
O7a—V2b—O3b | 74.12 (5) | V1av—O1b—V1aiv | 168.28 (7) |
O7a—V2b—O5b | 175.74 (6) | V1av—O1b—V1b | 96.94 (5) |
O7a—V2b—O7b | 79.53 (5) | V2bi—O2b—V2bii | 151.12 (7) |
O2biv—V2b—O2bv | 151.12 (6) | V2bi—O2b—V3b | 101.93 (8) |
O2biv—V2b—O3b | 76.15 (5) | V2bi—O2b—O3bi | 54.94 (6) |
O2biv—V2b—O5b | 96.36 (6) | V2bi—O2b—O3bii | 152.05 (7) |
O2biv—V2b—O7b | 100.94 (9) | V2bii—O2b—V2bi | 151.12 (7) |
O2bv—V2b—O2biv | 151.12 (6) | V2bii—O2b—V3b | 101.89 (8) |
O2bv—V2b—O3b | 76.08 (5) | V2bii—O2b—O3bi | 151.94 (7) |
O2bv—V2b—O5b | 96.84 (6) | V2bii—O2b—O3bii | 54.83 (6) |
O2bv—V2b—O7b | 100.36 (9) | V3b—O2b—O3bi | 50.23 (5) |
O3b—V2b—O5b | 101.61 (6) | V3b—O2b—O3bii | 50.29 (5) |
O3b—V2b—O7b | 153.65 (6) | O3bi—O2b—O3bii | 97.68 (5) |
O5b—V2b—O7b | 104.73 (7) | O3bii—O2b—O3bi | 97.68 (5) |
O2a—V3a—O3aiv | 78.40 (5) | V2b—O3b—V3a | 102.74 (5) |
O2a—V3a—O3av | 78.33 (5) | V2b—O3b—V3biv | 97.14 (6) |
O2a—V3a—O6a | 100.05 (6) | V2b—O3b—V3bv | 97.26 (6) |
O2a—V3a—O7a | 162.07 (6) | V2b—O3b—O2biv | 48.91 (4) |
O2a—V3a—O3b | 84.36 (5) | V2b—O3b—O2bv | 49.09 (4) |
O3aiv—V3a—O3av | 147.13 (6) | V3a—O3b—V3biv | 102.60 (6) |
O3aiv—V3a—O6a | 102.98 (6) | V3a—O3b—V3bv | 102.56 (6) |
O3aiv—V3a—O7a | 97.67 (8) | V3a—O3b—O2biv | 95.35 (5) |
O3aiv—V3a—O3b | 77.43 (5) | V3a—O3b—O2bv | 95.33 (5) |
O3av—V3a—O3aiv | 147.13 (6) | V3biv—O3b—V3bv | 147.34 (6) |
O3av—V3a—O6a | 103.68 (6) | V3biv—O3b—O2biv | 51.21 (5) |
O3av—V3a—O7a | 97.36 (8) | V3biv—O3b—O2bv | 144.91 (8) |
O3av—V3a—O3b | 77.46 (5) | V3bv—O3b—V3biv | 147.34 (6) |
O6a—V3a—O7a | 97.89 (6) | V3bv—O3b—O2biv | 144.86 (8) |
O6a—V3a—O3b | 175.58 (6) | V3bv—O3b—O2bv | 51.14 (5) |
O7a—V3a—O3b | 77.71 (5) | O2biv—O3b—O2bv | 97.68 (7) |
O3a—V3b—O2b | 84.56 (5) | O2bv—O3b—O2biv | 97.68 (7) |
O3a—V3b—O3bi | 77.44 (8) | V1bvi—O5b—V2b | 176.01 (8) |
O3a—V3b—O3bii | 77.45 (8) | V1avi—O6b—V3b | 171.52 (11) |
O3a—V3b—O6b | 175.91 (6) | V2a—O7b—V2b | 100.95 (6) |
O3a—V3b—O7b | 77.38 (5) | V2a—O7b—V3b | 105.11 (5) |
O2b—V3b—O3bi | 78.56 (7) | V2b—O7b—V3b | 153.95 (8) |
O2b—V3b—O3bii | 78.57 (7) | | |
Symmetry codes: (i) x, −y, z−1/2; (ii) x, −y+1, z−1/2; (iii) x−1, y, z; (iv) x, −y, z+1/2; (v) x, −y+1, z+1/2; (vi) x+1, y, z. |
Crystal data top
V6O13 | F(000) = 484 |
Mr = 513.64 | Dx = 3.896 Mg m−3 |
Monoclinic, Pc | Mo Kα radiation, λ = 0.71073 Å |
a = 10.0543 (1) Å | Cell parameters from 4122 reflections |
b = 3.7080 (1) Å | θ = 3.5–49.4° |
c = 11.9554 (1) Å | µ = 6.23 mm−1 |
β = 100.914 (1)° | T = 95 K |
V = 437.65 (1) Å3 | Brick, black |
Z = 2 | 0.12 × 0.07 × 0.05 mm |
Data collection top
CCD area detector diffractometer | 8245 independent reflections |
Radiation source: fine-focus sealed tube | 26501 reflections with > −15σ(I) |
Graphite monochromator | Rint = 0.058 |
Detector resolution: 512*512 pixels mm-1 | θmax = 49.6°, θmin = 2.1° |
ω scans | h = −21→21 |
Absorption correction: integration | k = −7→6 |
Tmin = 0.580, Tmax = 0.775 | l = −25→24 |
26501 measured reflections | |
Refinement top
Refinement on F2 | Weighting scheme based on measured s.u.'s w = 1/σ2(I) |
R[F > 3σ(F)] = 0.078 | (Δ/σ)max = 0.023 |
wR(F) = 0.083 | Δρmax = 4.46 e Å−3 |
S = 0.58 | Δρmin = −4.75 e Å−3 |
26501 reflections | Extinction correction: B-C type 1 Gaussian isotropic |
191 parameters | Extinction coefficient: 683 (5) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
V1a | −0.006112 | 0.2974 (2) | 0.345635 | 0.00876 (12) | |
V1b | −0.00300 (8) | 0.2358 (2) | 0.64163 (8) | 0.00432 (10) | |
V2a | 0.36020 (10) | 0.2503 (3) | 0.41711 (8) | 0.00272 (10) | |
V2b | 0.63220 (10) | 0.24780 (10) | 0.59099 (8) | 0.00235 (10) | |
V3a | 0.36370 (10) | 0.24890 (10) | 0.71932 (8) | 0.00247 (10) | |
V3b | 0.63060 (10) | 0.2515 (3) | 0.28868 (8) | 0.00264 (10) | |
O1a | −0.0034 (3) | 0.2560 (10) | 0.1835 (2) | 0.0050 (4) | |
O2a | 0.3854 (3) | 0.2497 (6) | 0.8859 (2) | 0.0038 (4) | |
O3a | 0.4068 (3) | 0.2520 (10) | 0.2540 (2) | 0.0040 (4) | |
O4a | −0.0032 (3) | 0.2400 (10) | 0.5019 (2) | 0.0056 (3) | |
O5a | 0.1923 (3) | 0.2520 (10) | 0.3865 (2) | 0.0051 (5) | |
O6a | 0.1965 (3) | 0.2464 (6) | 0.6818 (2) | 0.0046 (5) | |
O7a | 0.4037 (3) | 0.2510 (10) | 0.5647 (2) | 0.0040 (4) | |
O1b | −0.0041 (3) | 0.2411 (5) | 0.8289 (2) | 0.0051 (4) | |
O2b | 0.6094 (3) | 0.2510 (10) | 0.1219 (2) | 0.0046 (4) | |
O3b | 0.5878 (3) | 0.2489 (6) | 0.7520 (2) | 0.0038 (4) | |
O5b | 0.7991 (3) | 0.2469 (6) | 0.6173 (2) | 0.0049 (5) | |
O6b | 0.7987 (3) | 0.2540 (10) | 0.3223 (2) | 0.0052 (5) | |
O7b | 0.5886 (3) | 0.2510 (10) | 0.4416 (2) | 0.0049 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1a | 0.0035 (2) | 0.0149 (2) | 0.0075 (2) | 0.00162 (19) | 0.00013 (15) | −0.0057 (2) |
V1b | 0.00295 (18) | 0.00396 (15) | 0.0059 (2) | −0.00099 (14) | 0.00033 (14) | −0.00054 (14) |
V2a | 0.00240 (18) | 0.00294 (15) | 0.00284 (17) | −0.00007 (13) | 0.00053 (13) | 0.0003 (2) |
V2b | 0.00234 (17) | 0.00300 (15) | 0.00182 (16) | −0.00013 (12) | 0.00065 (13) | 0.00035 (13) |
V3a | 0.00203 (17) | 0.00222 (15) | 0.00318 (17) | −0.00021 (11) | 0.00050 (13) | 0.00001 (13) |
V3b | 0.00253 (18) | 0.00262 (15) | 0.00257 (16) | 0.00001 (13) | 0.00000 (13) | −0.00026 (19) |
O1a | 0.0040 (8) | 0.0040 (7) | 0.0068 (7) | −0.0015 (10) | 0.0002 (5) | −0.0038 (10) |
O2a | 0.0040 (8) | 0.0035 (6) | 0.0038 (6) | −0.0005 (5) | 0.0002 (5) | −0.0004 (6) |
O3a | 0.0038 (8) | 0.0032 (7) | 0.0048 (7) | −0.0008 (7) | 0.0003 (6) | 0.0000 (8) |
O4a | 0.0046 (3) | 0.0087 (6) | 0.0035 (4) | −0.0019 (8) | 0.0005 (3) | −0.0009 (10) |
O5a | 0.0025 (8) | 0.0066 (8) | 0.0066 (7) | 0.0011 (6) | 0.0019 (6) | −0.0006 (9) |
O6a | 0.0035 (9) | 0.0049 (7) | 0.0056 (7) | −0.0001 (5) | 0.0017 (6) | 0.0005 (6) |
O7a | 0.0031 (8) | 0.0042 (7) | 0.0051 (7) | −0.0001 (7) | 0.0018 (6) | −0.0007 (7) |
O1b | 0.0055 (8) | 0.0055 (7) | 0.0042 (7) | 0.0008 (8) | 0.0007 (5) | 0.0007 (6) |
O2b | 0.0067 (9) | 0.0032 (7) | 0.0041 (6) | 0.0015 (7) | 0.0019 (5) | −0.0006 (7) |
O3b | 0.0045 (8) | 0.0036 (7) | 0.0034 (7) | 0.0003 (5) | 0.0008 (6) | 0.0002 (6) |
O5b | 0.0037 (9) | 0.0039 (7) | 0.0064 (7) | −0.0009 (5) | −0.0007 (6) | 0.0002 (6) |
O6b | 0.0022 (8) | 0.0057 (8) | 0.0072 (8) | −0.0003 (6) | −0.0002 (6) | −0.0009 (9) |
O7b | 0.0066 (9) | 0.0037 (7) | 0.0047 (7) | −0.0006 (8) | 0.0013 (6) | 0.0005 (8) |
Geometric parameters (Å, º) top
V1a—O1a | 1.950 (2) | O1a—V1a | 1.950 (2) |
V1a—O4a | 1.875 (2) | O1a—V1bi | 1.891 (3) |
V1a—O5a | 1.969 (2) | O1a—V1bii | 1.950 (3) |
V1a—O1bi | 2.007 (2) | O2a—V2aiv | 1.917 (2) |
V1a—O1bii | 1.724 (2) | O2a—V2av | 1.917 (2) |
V1a—O6biii | 1.936 (3) | O2a—V3a | 1.962 (2) |
V1b—O1aiv | 1.891 (3) | O3a—V2a | 2.090 (2) |
V1b—O1av | 1.950 (3) | O3a—V3ai | 1.934 (3) |
V1b—O4a | 1.670 (2) | O3a—V3aii | 1.928 (3) |
V1b—O6a | 1.972 (3) | O3a—V3b | 2.210 (3) |
V1b—O1b | 2.241 (2) | O4a—V1a | 1.875 (2) |
V1b—O5biii | 1.956 (3) | O4a—V1b | 1.670 (2) |
V2a—O2ai | 1.917 (2) | O5a—V1a | 1.969 (2) |
V2a—O2aii | 1.917 (2) | O5a—V2a | 1.658 (3) |
V2a—O3a | 2.090 (2) | O6a—V1b | 1.972 (3) |
V2a—O5a | 1.658 (3) | O6a—V3a | 1.656 (3) |
V2a—O7a | 1.736 (2) | O7a—V2a | 1.736 (2) |
V2a—O7b | 2.259 (3) | O7a—V2b | 2.259 (3) |
V2b—O7a | 2.259 (3) | O7a—V3a | 1.965 (2) |
V2b—O2biv | 1.908 (3) | O1b—V1aiv | 2.007 (2) |
V2b—O2bv | 1.917 (3) | O1b—V1av | 1.724 (2) |
V2b—O3b | 2.057 (2) | O1b—V1b | 2.241 (2) |
V2b—O5b | 1.648 (3) | O2b—V2bi | 1.908 (3) |
V2b—O7b | 1.757 (2) | O2b—V2bii | 1.917 (3) |
V3a—O2a | 1.962 (2) | O2b—V3b | 1.965 (2) |
V3a—O3aiv | 1.934 (3) | O3b—V2b | 2.057 (2) |
V3a—O3av | 1.928 (3) | O3b—V3a | 2.213 (3) |
V3a—O6a | 1.656 (3) | O3b—V3biv | 1.936 (2) |
V3a—O7a | 1.965 (2) | O3b—V3bv | 1.933 (2) |
V3a—O3b | 2.213 (3) | O5b—V1bvi | 1.956 (3) |
V3b—O3a | 2.210 (3) | O5b—V2b | 1.648 (3) |
V3b—O2b | 1.965 (2) | O6b—V1avi | 1.936 (3) |
V3b—O3bi | 1.936 (2) | O6b—V3b | 1.662 (3) |
V3b—O3bii | 1.933 (2) | O7b—V2a | 2.259 (3) |
V3b—O6b | 1.662 (3) | O7b—V2b | 1.757 (2) |
V3b—O7b | 1.953 (2) | O7b—V3b | 1.953 (2) |
| | | |
O1a—V1a—O4a | 168.84 (16) | O3aiv—V3a—O3av | 147.52 (12) |
O1a—V1a—O5a | 92.05 (11) | O3aiv—V3a—O6a | 103.15 (12) |
O1a—V1a—O1bi | 79.65 (13) | O3aiv—V3a—O7a | 97.36 (13) |
O1a—V1a—O1bii | 87.71 (13) | O3aiv—V3a—O3b | 77.46 (11) |
O1a—V1a—O6biii | 93.14 (11) | O3av—V3a—O3aiv | 147.52 (12) |
O4a—V1a—O5a | 85.36 (11) | O3av—V3a—O6a | 103.83 (12) |
O4a—V1a—O1bi | 89.30 (13) | O3av—V3a—O7a | 96.94 (13) |
O4a—V1a—O1bii | 103.30 (14) | O3av—V3a—O3b | 77.42 (11) |
O4a—V1a—O6biii | 87.61 (11) | O6a—V3a—O7a | 97.08 (12) |
O5a—V1a—O1bi | 84.88 (13) | O6a—V3a—O3b | 174.55 (12) |
O5a—V1a—O1bii | 94.59 (14) | O7a—V3a—O3b | 77.48 (11) |
O5a—V1a—O6biii | 168.63 (14) | O3a—V3b—O2b | 84.18 (11) |
O1bi—V1a—O1bii | 167.32 (11) | O3a—V3b—O3bi | 77.50 (13) |
O1bi—V1a—O6biii | 86.10 (14) | O3a—V3b—O3bii | 77.38 (13) |
O1bii—V1a—O1bi | 167.32 (11) | O3a—V3b—O6b | 176.86 (12) |
O1bii—V1a—O6biii | 95.72 (14) | O3a—V3b—O7b | 77.44 (11) |
O1aiv—V1b—O1av | 149.73 (12) | O2b—V3b—O3bi | 78.02 (13) |
O1aiv—V1b—O4a | 105.91 (15) | O2b—V3b—O3bii | 78.11 (13) |
O1aiv—V1b—O6a | 90.45 (11) | O2b—V3b—O6b | 98.94 (13) |
O1aiv—V1b—O1b | 75.13 (9) | O2b—V3b—O7b | 161.62 (13) |
O1aiv—V1b—O5biii | 90.38 (11) | O3bi—V3b—O3bii | 146.77 (11) |
O1av—V1b—O1aiv | 149.73 (12) | O3bi—V3b—O6b | 103.44 (16) |
O1av—V1b—O4a | 104.36 (15) | O3bi—V3b—O7b | 97.64 (14) |
O1av—V1b—O6a | 88.26 (11) | O3bii—V3b—O3bi | 146.77 (11) |
O1av—V1b—O1b | 74.60 (9) | O3bii—V3b—O6b | 102.83 (16) |
O1av—V1b—O5biii | 88.07 (11) | O3bii—V3b—O7b | 97.76 (14) |
O4a—V1b—O6a | 92.98 (13) | O6b—V3b—O7b | 99.43 (12) |
O4a—V1b—O1b | 178.91 (14) | V1a—O1a—V1bi | 109.89 (16) |
O4a—V1b—O5biii | 92.44 (12) | V1a—O1a—V1bii | 100.38 (15) |
O6a—V1b—O1b | 87.35 (10) | V1bi—O1a—V1bii | 149.73 (14) |
O6a—V1b—O5biii | 174.08 (11) | V1bii—O1a—V1bi | 149.73 (14) |
O1b—V1b—O5biii | 87.20 (11) | V2aiv—O2a—V2av | 150.44 (17) |
O2ai—V2a—O2aii | 150.44 (13) | V2aiv—O2a—V3a | 101.69 (10) |
O2ai—V2a—O3a | 76.12 (13) | V2av—O2a—V2aiv | 150.44 (17) |
O2ai—V2a—O5a | 97.31 (16) | V2av—O2a—V3a | 101.86 (10) |
O2ai—V2a—O7a | 100.49 (14) | V2a—O3a—V3ai | 96.68 (14) |
O2ai—V2a—O7b | 81.83 (13) | V2a—O3a—V3aii | 97.04 (14) |
O2aii—V2a—O2ai | 150.44 (13) | V2a—O3a—V3b | 103.01 (10) |
O2aii—V2a—O3a | 75.78 (13) | V3ai—O3a—V3aii | 147.52 (14) |
O2aii—V2a—O5a | 96.89 (16) | V3ai—O3a—V3b | 102.61 (15) |
O2aii—V2a—O7a | 100.33 (14) | V3aii—O3a—V3ai | 147.52 (14) |
O2aii—V2a—O7b | 81.70 (13) | V3aii—O3a—V3b | 102.75 (15) |
O3a—V2a—O5a | 101.11 (12) | V1a—O4a—V1b | 174.0 (2) |
O3a—V2a—O7a | 152.96 (14) | V1a—O5a—V2a | 175.0 (2) |
O3a—V2a—O7b | 73.68 (10) | V1b—O6a—V3a | 178.21 (16) |
O5a—V2a—O7a | 105.93 (14) | V2a—O7a—V2b | 101.26 (14) |
O5a—V2a—O7b | 174.79 (12) | V2a—O7a—V3a | 154.08 (18) |
O7a—V2a—O7b | 79.28 (12) | V2b—O7a—V3a | 104.66 (10) |
O7a—V2b—O2biv | 82.86 (13) | V1aiv—O1b—V1av | 167.32 (15) |
O7a—V2b—O2bv | 82.31 (13) | V1aiv—O1b—V1b | 95.33 (8) |
O7a—V2b—O3b | 74.63 (10) | V1av—O1b—V1aiv | 167.32 (15) |
O7a—V2b—O5b | 177.04 (12) | V1av—O1b—V1b | 97.30 (10) |
O7a—V2b—O7b | 78.88 (12) | V2bi—O2b—V2bii | 151.53 (17) |
O2biv—V2b—O2bv | 151.53 (13) | V2bi—O2b—V3b | 101.74 (15) |
O2biv—V2b—O3b | 76.43 (10) | V2bii—O2b—V2bi | 151.53 (17) |
O2biv—V2b—O5b | 96.68 (12) | V2bii—O2b—V3b | 101.58 (15) |
O2biv—V2b—O7b | 100.80 (14) | V2b—O3b—V3a | 103.24 (10) |
O2bv—V2b—O2biv | 151.53 (13) | V2b—O3b—V3biv | 97.57 (11) |
O2bv—V2b—O3b | 76.27 (10) | V2b—O3b—V3bv | 97.80 (11) |
O2bv—V2b—O5b | 96.88 (12) | V3a—O3b—V3biv | 102.43 (11) |
O2bv—V2b—O7b | 99.99 (14) | V3a—O3b—V3bv | 102.45 (11) |
O3b—V2b—O5b | 102.42 (12) | V3biv—O3b—V3bv | 146.77 (14) |
O3b—V2b—O7b | 153.51 (14) | V3bv—O3b—V3biv | 146.77 (14) |
O5b—V2b—O7b | 104.07 (14) | V1bvi—O5b—V2b | 177.36 (16) |
O2a—V3a—O3aiv | 78.84 (10) | V1avi—O6b—V3b | 172.9 (2) |
O2a—V3a—O3av | 78.64 (10) | V2a—O7b—V2b | 100.58 (14) |
O2a—V3a—O6a | 100.78 (13) | V2a—O7b—V3b | 105.86 (11) |
O2a—V3a—O7a | 162.13 (13) | V2b—O7b—V3b | 153.55 (18) |
O2a—V3a—O3b | 84.66 (11) | | |
Symmetry codes: (i) x, −y, z−1/2; (ii) x, −y+1, z−1/2; (iii) x−1, y, z; (iv) x, −y, z+1/2; (v) x, −y+1, z+1/2; (vi) x+1, y, z. |
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