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The V4+ (spin ½) oxovanadates AV3O7 (A = Ca, Sr) were synthesized and studied by means of single-crystal X-ray diffraction. The room-temperature structures of both compounds are orthorhombic and their respective space groups are Pnma and Pmmn. The previously assumed structure of SrV3O7 has been revised and the temperature dependence of both crystal structures in the temperature ranges 297-100 K and 315-100 K, respectively, is discussed for the first time.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768107050550/bm5051sup1.cif
Contains datablocks SrV3O7_315K, SrV3O7_298K, SrV3O7_275K, SrV3O7_262K, SrV3O7_250K, SrV3O7_225K, SrV3O7_200K, SrV3O7_187K, SrV3O7_175K, SrV3O7_150K, SrV3O7_125K, SrV3O7_100K, CaV3O7_297K, CaV3O7_287K, CaV3O7_275k, CaV3O7_262K, CaV3O7_250K, CaV3O7_237K, CaV3O7_225K, CaV3O7_219K, CaV3O7_212K, CaV3O7_206K, CaV3O7_200K, CaV3O7_187K, CaV3O7_175K, CaV3O7_162K, CaV3O7_150K, CaV3O7_137K, CaV3O7_125K, CaV3O7_112K, CaV3O7_100K

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_315Ksup2.fcf
Contains datablock SrV3O7_315K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_225Ksup3.fcf
Contains datablock SrV3O7_225K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_200Ksup4.fcf
Contains datablock SrV3O7_200K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_187Ksup5.fcf
Contains datablock SrV3O7_187K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_175Ksup6.fcf
Contains datablock SrV3O7_175K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_150Ksup7.fcf
Contains datablock SrV3O7_150K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_125Ksup8.fcf
Contains datablock SrV3O7_125K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_100Ksup9.fcf
Contains datablock SrV3O7_100K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_297Ksup10.fcf
Contains datablock CaV3O7_297K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_287Ksup11.fcf
Contains datablock CaV3O7_287K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_275Ksup12.fcf
Contains datablock CaV3O7_275K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_262Ksup13.fcf
Contains datablock CaV3O7_262K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_250Ksup14.fcf
Contains datablock CaV3O7_250K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_237Ksup15.fcf
Contains datablock CaV3O7_237K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_225Ksup16.fcf
Contains datablock CaV3O7_225K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_219Ksup17.fcf
Contains datablock CaV3O7_219K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_212Ksup18.fcf
Contains datablock CaV3O7_212K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_206Ksup19.fcf
Contains datablock CaV3O7_206K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_200Ksup20.fcf
Contains datablock CaV3O7_200K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_187Ksup21.fcf
Contains datablock CaV3O7_187K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_175Ksup22.fcf
Contains datablock CaV3O7_175K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_162Ksup23.fcf
Contains datablock CaV3O7_162K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_150Ksup24.fcf
Contains datablock CaV3O7_150K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_137Ksup25.fcf
Contains datablock CaV3O7_137K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_125Ksup26.fcf
Contains datablock CaV3O7_125K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_112Ksup27.fcf
Contains datablock CaV3O7_112K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051CaV3O7_100Ksup28.fcf
Contains datablock CaV3O7_100K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_298Ksup29.fcf
Contains datablock SrV3O7_298K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_275Ksup30.fcf
Contains datablock SrV3O7_275K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_262Ksup31.fcf
Contains datablock SrV3O7_262K

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768107050550/bm5051SrV3O7_250Ksup32.fcf
Contains datablock SrV3O7_250K

Computing details top

Data collection: X-Pose (Stoe, 2002) for SrV3O7_315K, SrV3O7_298K, SrV3O7_275K, SrV3O7_262K, SrV3O7_250K, SrV3O7_225K, SrV3O7_200K, SrV3O7_187K, SrV3O7_175K, SrV3O7_150K, SrV3O7_125K; X-AREA (Stoe, 2002) for SrV3O7_100K, CaV3O7_297K, CaV3O7_287K, CaV3O7_275k, CaV3O7_262K, CaV3O7_250K, CaV3O7_237K, CaV3O7_225K, CaV3O7_219K, CaV3O7_212K, CaV3O7_206K, CaV3O7_200K, CaV3O7_187K, CaV3O7_175K, CaV3O7_162K, CaV3O7_150K, CaV3O7_137K, CaV3O7_125K, CaV3O7_112K, CaV3O7_100K. For all compounds, cell refinement: X-AREA (Stoe, 2002); data reduction: X-RED (Stoe, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: SHELXS97 (Sheldrick, 1997) for SrV3O7_315K, SrV3O7_298K, SrV3O7_275K, SrV3O7_262K, SrV3O7_250K, SrV3O7_225K, SrV3O7_200K, SrV3O7_187K, SrV3O7_175K, SrV3O7_150K, SrV3O7_125K; ATOMS Version 5.1 for SrV3O7_100K, CaV3O7_297K, CaV3O7_287K, CaV3O7_275k, CaV3O7_262K, CaV3O7_250K, CaV3O7_237K, CaV3O7_225K, CaV3O7_219K, CaV3O7_212K, CaV3O7_206K, CaV3O7_200K, CaV3O7_187K, CaV3O7_175K, CaV3O7_162K, CaV3O7_150K, CaV3O7_137K, CaV3O7_125K, CaV3O7_112K, CaV3O7_100K. For all compounds, software used to prepare material for publication: WinGX 1.64.05 (Farrugia, 1999).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
(SrV3O7_315K) top
Crystal data top
O7V3·SrDx = 3.945 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 10067 reflections
a = 5.2988 (9) Åθ = 3.9–32.2°
b = 10.527 (2) ŵ = 13.49 mm1
c = 5.3183 (9) ÅT = 315 K
V = 296.66 (10) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
336 independent reflections
Radiation source: fine-focus sealed tube317 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.066
Detector resolution: 0 pixels mm-1θmax = 25.8°, θmin = 3.8°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.220, Tmax = 0.569l = 66
5461 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.031 w = 1/[σ2(Fo2) + (0.0493P)2 + 0.2079P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.080(Δ/σ)max < 0.001
S = 1.21Δρmax = 0.82 e Å3
336 reflectionsΔρmin = 0.88 e Å3
24 parameters
Crystal data top
O7V3·SrV = 296.66 (10) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2988 (9) ŵ = 13.49 mm1
b = 10.527 (2) ÅT = 315 K
c = 5.3183 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
336 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
317 reflections with I > 2σ(I)
Tmin = 0.220, Tmax = 0.569Rint = 0.066
5461 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03124 parameters
wR(F2) = 0.0800 restraints
S = 1.21Δρmax = 0.82 e Å3
336 reflectionsΔρmin = 0.88 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14871 (16)0.0188 (3)
V10.25000.51544 (10)0.62025 (19)0.0150 (3)
V20.25000.75000.5909 (3)0.0149 (4)
O10.25000.75000.1058 (12)0.0237 (15)*
O20.25000.5455 (4)0.0812 (9)0.0245 (11)*
O30.0120 (5)0.6209 (3)0.4635 (5)0.0169 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0181 (5)0.0162 (5)0.0222 (5)0.0000.0000.000
V10.0099 (5)0.0128 (6)0.0225 (6)0.0000.0000.0005 (4)
V20.0105 (7)0.0126 (7)0.0216 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.476 (5)V2—V1i3.6250 (9)
Sr1—O2i2.476 (5)V2—V1xxi3.6250 (9)
Sr1—O3i2.565 (3)V2—V1xxiv3.6250 (9)
Sr1—O3ii2.565 (3)V2—O13.706 (6)
Sr1—O3iii2.565 (3)V2—O2xix3.833 (3)
Sr1—O32.565 (3)V2—O2xxv3.833 (3)
Sr1—O12.975 (3)V2—O2v3.833 (3)
Sr1—O1iv2.975 (3)V2—O2xxviii3.833 (3)
Sr1—V1i3.5194 (13)V2—Sr1v3.9773 (14)
Sr1—V13.5194 (13)V2—Sr1xxv3.9773 (14)
Sr1—V2iv3.5427 (12)V2—O2xxvii4.059 (5)
Sr1—V23.5427 (12)V2—O2vi4.059 (5)
V1—O2v1.619 (5)V2—O2x4.126 (5)
V1—O3vi1.962 (3)V2—O2xxix4.126 (5)
V1—O3vii1.962 (3)V2—O3xiii4.154 (3)
V1—O3iii1.963 (3)V2—O3xxx4.154 (3)
V1—O31.963 (3)V2—O3vi4.154 (3)
V1—V1vi2.9599 (10)V2—O3xxvii4.154 (3)
V1—V1viii2.9599 (10)V2—O3xxi4.314 (3)
V1—V2vi3.0117 (13)V2—O3i4.314 (3)
V1—V2iv3.6250 (9)V2—O3xxxi4.314 (3)
V1—V23.6250 (9)V2—O3iii4.314 (3)
V1—O2viii3.666 (3)V2—O2xxi4.943 (4)
V1—O2vi3.666 (3)V2—O2xxiv4.943 (4)
V1—Sr1v3.7411 (13)V2—O24.943 (4)
V1—O23.744 (5)V2—O2i4.943 (4)
V1—O1vi3.805 (4)V2—O3xxxii4.997 (3)
V1—O1ix3.904 (3)V2—O3xxviii4.997 (3)
V1—O1v3.904 (3)V2—O3v4.997 (3)
V1—O1x3.911 (5)V2—O3xxxiii4.997 (3)
V1—O2x3.956 (4)V2—V1xxxiv5.0406 (18)
V1—O2xi3.956 (4)V2—V1xviii5.0406 (18)
V1—Sr1vi4.0420 (10)V2—V2iv5.2988 (9)
V1—Sr1viii4.0420 (10)V2—V2xxi5.2988 (9)
V1—O3iv4.150 (3)V2—V2xxii5.3183 (9)
V1—O3xii4.150 (3)V2—V2v5.3183 (9)
V1—O3i4.157 (3)V2—Sr1xxxv5.4427 (12)
V1—O3ii4.157 (3)V2—Sr1vi5.4427 (12)
V1—O3xiii4.308 (3)V2—O3xxxvi5.534 (3)
V1—O3viii4.308 (3)V2—O3xxxvii5.534 (3)
V1—O3xiv4.363 (3)O1—V2xxii1.613 (6)
V1—O3xv4.363 (3)O1—Sr1xxi2.975 (3)
V1—O3xvi4.824 (3)O1—V1xxvii3.805 (4)
V1—O3v4.824 (3)O1—V1vi3.805 (4)
V1—V1xvii4.8415 (18)O1—V1xxxviii3.904 (2)
V1—V1xviii4.8415 (18)O1—V1xxxix3.904 (2)
V1—O2xix4.887 (5)O1—V1xl3.904 (2)
V1—V1i4.938 (2)O1—V1xxii3.904 (2)
V1—V2xviii5.0406 (17)O1—V1x3.911 (5)
V1—O3xx5.234 (3)O1—V1xxix3.911 (5)
V1—O3xviii5.234 (3)O2—V1xxii1.619 (5)
V1—O15.294 (5)O2—V1viii3.666 (3)
V1—O1iv5.294 (5)O2—V1vi3.666 (3)
V1—V1xxi5.2988 (9)O2—V2xli3.833 (3)
V1—V1iv5.2988 (9)O2—V2xxii3.833 (3)
V1—V1xxii5.3183 (9)O2—V1x3.956 (4)
V1—O3xxiii5.536 (3)O2—V1xi3.956 (4)
V1—O3xxiv5.536 (3)O2—V2vi4.059 (5)
V1—O2ix5.5406 (17)O2—V2x4.126 (5)
V1—O2xxv5.5406 (17)O2—V1xxxix4.887 (5)
V1—V1xxvi5.589 (2)O3—V1vi1.962 (3)
V2—O1v1.613 (6)O3—V1xxi4.150 (3)
V2—O3xii1.974 (3)O3—V2vi4.154 (3)
V2—O3ii1.974 (3)O3—V1i4.157 (3)
V2—O3xxiv1.974 (3)O3—V1viii4.308 (3)
V2—O31.974 (3)O3—V2iv4.314 (3)
V2—V1vi3.0117 (13)O3—V1xxvii4.363 (3)
V2—V1xxvii3.0117 (13)O3—V1xxii4.824 (3)
V2—Sr1xxi3.5427 (12)O3—V2xxii4.997 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x1, y, z; (xxii) x, y, z1; (xxiii) x+1, y+3/2, z; (xxiv) x1/2, y+3/2, z; (xxv) x1, y, z+1; (xxvi) x+1/2, y+1/2, z; (xxvii) x1/2, y+1/2, z+1; (xxviii) x1/2, y+3/2, z+1; (xxix) x1/2, y+1/2, z; (xxx) x, y+1/2, z+1; (xxxi) x1, y+3/2, z; (xxxii) x, y+3/2, z+1; (xxxiii) x1/2, y, z+1; (xxxiv) x1/2, y+1/2, z+2; (xxxv) x, y+2, z+1; (xxxvi) x1, y+1, z+1; (xxxvii) x+1/2, y+1/2, z+1; (xxxviii) x1, y, z1; (xxxix) x+1/2, y+3/2, z1; (xl) x1/2, y+3/2, z1; (xli) x+1, y, z1.
(SrV3O7_298K) top
Crystal data top
O7V3·SrDx = 3.949 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11182 reflections
a = 5.2979 (8) Åθ = 3.8–32.1°
b = 10.529 (2) ŵ = 13.51 mm1
c = 5.3139 (9) ÅT = 298 K
V = 296.41 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
331 independent reflections
Radiation source: fine-focus sealed tube317 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.065
Detector resolution: 0 pixels mm-1θmax = 25.5°, θmin = 3.8°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.220, Tmax = 0.569l = 66
5486 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.031Secondary atom site location: difference Fourier map
wR(F2) = 0.078 w = 1/[σ2(Fo2) + (0.0431P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.38(Δ/σ)max < 0.001
331 reflectionsΔρmax = 0.82 e Å3
24 parametersΔρmin = 0.92 e Å3
Crystal data top
O7V3·SrV = 296.41 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2979 (8) ŵ = 13.51 mm1
b = 10.529 (2) ÅT = 298 K
c = 5.3139 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
331 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
317 reflections with I > 2σ(I)
Tmin = 0.220, Tmax = 0.569Rint = 0.065
5486 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03124 parameters
wR(F2) = 0.0780 restraints
S = 1.38Δρmax = 0.82 e Å3
331 reflectionsΔρmin = 0.92 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14873 (15)0.0184 (3)
V10.25000.51539 (10)0.62054 (19)0.0148 (3)
V20.75000.75000.5911 (3)0.0143 (4)
O10.75000.75000.1056 (12)0.0233 (15)*
O20.25000.5455 (4)0.0809 (9)0.0235 (10)*
O30.0121 (5)0.6206 (3)0.4640 (5)0.0166 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0172 (5)0.0159 (5)0.0219 (5)0.0000.0000.000
V10.0095 (5)0.0124 (6)0.0226 (6)0.0000.0000.0004 (4)
V20.0108 (7)0.0118 (7)0.0204 (7)0.0000.0000.000
Geometric parameters (Å, º) top
Sr1—O22.475 (5)V1—V1viii2.9603 (10)
Sr1—O2i2.475 (5)V1—V2viii3.0120 (13)
Sr1—O3i2.567 (3)V1—V2i3.6253 (8)
Sr1—O3ii2.567 (3)V1—Sr1v3.7389 (12)
Sr1—O32.567 (3)V2—O1v1.612 (6)
Sr1—O3iii2.567 (3)V2—O3ii1.975 (3)
Sr1—O1iv2.974 (3)V2—O3ix1.975 (3)
Sr1—O12.974 (3)V2—O3x1.975 (3)
Sr1—V1i3.5195 (13)V2—O3i1.975 (3)
Sr1—V13.5195 (13)V2—V1viii3.0120 (13)
Sr1—V23.5415 (12)V2—V1xi3.0120 (13)
Sr1—V2i3.5415 (12)V2—Sr1x3.5415 (12)
V1—O2v1.618 (5)O1—V2xii1.612 (6)
V1—O3vi1.960 (3)O1—Sr1x2.974 (3)
V1—O3vii1.960 (3)O2—V1xii1.618 (5)
V1—O3ii1.962 (3)O3—V1vi1.960 (3)
V1—O31.962 (3)O3—V2i1.975 (3)
V1—V1vi2.9603 (10)
O2—Sr1—O2i120.9 (2)O3ii—V1—V1viii40.97 (9)
O2—Sr1—O3i141.57 (8)O3—V1—V1viii120.79 (10)
O2i—Sr1—O3i81.97 (11)V1vi—V1—V1viii126.98 (7)
O2—Sr1—O3ii81.97 (11)O2v—V1—V2viii123.22 (16)
O2i—Sr1—O3ii141.57 (8)O3vi—V1—V2viii40.23 (8)
O3i—Sr1—O3ii64.09 (13)O3vii—V1—V2viii40.23 (8)
O2—Sr1—O381.97 (11)O3ii—V1—V2viii111.45 (9)
O2i—Sr1—O3141.57 (8)O3—V1—V2viii111.45 (9)
O3i—Sr1—O398.52 (13)V1vi—V1—V2viii74.74 (4)
O3ii—Sr1—O365.49 (13)V1viii—V1—V2viii74.74 (4)
O2—Sr1—O3iii141.57 (8)O2v—V1—Sr1124.12 (16)
O2i—Sr1—O3iii81.97 (11)O3vi—V1—Sr1110.46 (9)
O3i—Sr1—O3iii65.49 (13)O3vii—V1—Sr1110.46 (9)
O3ii—Sr1—O3iii98.52 (13)O3ii—V1—Sr145.70 (9)
O3—Sr1—O3iii64.09 (13)O3—V1—Sr145.70 (9)
O2—Sr1—O1iv77.05 (6)V1vi—V1—Sr176.62 (4)
O2i—Sr1—O1iv77.05 (6)V1viii—V1—Sr176.62 (4)
O3i—Sr1—O1iv141.12 (9)V2viii—V1—Sr1112.65 (4)
O3ii—Sr1—O1iv141.12 (9)O2v—V1—V2i84.77 (11)
O3—Sr1—O1iv79.33 (11)O3vi—V1—V2i91.04 (8)
O3iii—Sr1—O1iv79.33 (11)O3vii—V1—V2i163.30 (9)
O2—Sr1—O177.05 (6)O3ii—V1—V2i96.55 (9)
O2i—Sr1—O177.05 (6)O3—V1—V2i23.01 (8)
O3i—Sr1—O179.33 (11)V1vi—V1—V2i53.28 (3)
O3ii—Sr1—O179.33 (11)V1viii—V1—V2i135.21 (6)
O3—Sr1—O1141.12 (9)V2viii—V1—V2i128.022 (18)
O3iii—Sr1—O1141.12 (9)Sr1—V1—V2i59.41 (3)
O1iv—Sr1—O1125.9 (2)O2v—V1—Sr1v30.05 (16)
O2—Sr1—V1i164.12 (11)O3vi—V1—Sr1v130.91 (8)
O2i—Sr1—V1i74.97 (10)O3vii—V1—Sr1v130.91 (8)
O3i—Sr1—V1i33.15 (6)O3ii—V1—Sr1v86.85 (9)
O3ii—Sr1—V1i84.69 (7)O3—V1—Sr1v86.85 (9)
O3—Sr1—V1i84.69 (7)V1vi—V1—Sr1v113.40 (4)
O3iii—Sr1—V1i33.15 (6)V1viii—V1—Sr1v113.40 (4)
O1iv—Sr1—V1i108.89 (7)V2viii—V1—Sr1v153.27 (4)
O1—Sr1—V1i108.89 (7)Sr1—V1—Sr1v94.08 (3)
O2—Sr1—V174.97 (10)V2i—V1—Sr1v65.31 (3)
O2i—Sr1—V1164.12 (11)O1v—V2—O3ii109.99 (9)
O3i—Sr1—V184.69 (7)O1v—V2—O3ix109.99 (9)
O3ii—Sr1—V133.15 (6)O3ii—V2—O3ix140.02 (17)
O3—Sr1—V133.15 (6)O1v—V2—O3x109.99 (9)
O3iii—Sr1—V184.69 (7)O3ii—V2—O3x79.32 (16)
O1iv—Sr1—V1108.89 (7)O3ix—V2—O3x87.22 (17)
O1—Sr1—V1108.89 (7)O1v—V2—O3i109.99 (9)
V1i—Sr1—V189.15 (4)O3ii—V2—O3i87.22 (17)
O2—Sr1—V2109.11 (6)O3ix—V2—O3i79.32 (16)
O2i—Sr1—V2109.11 (6)O3x—V2—O3i140.02 (17)
O3i—Sr1—V233.10 (6)O1v—V2—V1viii111.92 (3)
O3ii—Sr1—V233.10 (6)O3ii—V2—V1viii39.87 (8)
O3—Sr1—V288.36 (7)O3ix—V2—V1viii120.81 (9)
O3iii—Sr1—V288.36 (7)O3x—V2—V1viii39.87 (8)
O1iv—Sr1—V2165.45 (11)O3i—V2—V1viii120.81 (9)
O1—Sr1—V268.62 (11)O1v—V2—V1xi111.92 (3)
V1i—Sr1—V261.784 (19)O3ii—V2—V1xi120.81 (9)
V1—Sr1—V261.784 (19)O3ix—V2—V1xi39.87 (8)
O2—Sr1—V2i109.11 (6)O3x—V2—V1xi120.81 (9)
O2i—Sr1—V2i109.11 (6)O3i—V2—V1xi39.87 (8)
O3i—Sr1—V2i88.36 (7)V1viii—V2—V1xi136.16 (6)
O3ii—Sr1—V2i88.36 (7)O1v—V2—Sr1131.58 (2)
O3—Sr1—V2i33.10 (6)O3ii—V2—Sr145.23 (9)
O3iii—Sr1—V2i33.10 (6)O3ix—V2—Sr1104.50 (9)
O1iv—Sr1—V2i68.62 (11)O3x—V2—Sr1104.50 (9)
O1—Sr1—V2i165.45 (11)O3i—V2—Sr145.23 (9)
V1i—Sr1—V2i61.784 (19)V1viii—V2—Sr175.65 (2)
V1—Sr1—V2i61.784 (19)V1xi—V2—Sr175.65 (2)
V2—Sr1—V2i96.83 (4)O1v—V2—Sr1x131.58 (2)
O2v—V1—O3vi111.59 (15)O3ii—V2—Sr1x104.50 (9)
O2v—V1—O3vii111.59 (15)O3ix—V2—Sr1x45.23 (9)
O3vi—V1—O3vii80.04 (17)O3x—V2—Sr1x45.23 (9)
O2v—V1—O3ii107.76 (14)O3i—V2—Sr1x104.50 (9)
O3vi—V1—O3ii140.42 (7)V1viii—V2—Sr1x75.65 (2)
O3vii—V1—O3ii81.97 (13)V1xi—V2—Sr1x75.65 (2)
O2v—V1—O3107.76 (14)Sr1—V2—Sr1x96.83 (4)
O3vi—V1—O381.97 (13)V2xii—O1—Sr1x117.03 (11)
O3vii—V1—O3140.42 (7)V2xii—O1—Sr1117.03 (11)
O3ii—V1—O390.13 (17)Sr1x—O1—Sr1125.9 (2)
O2v—V1—V1vi116.48 (4)V1xii—O2—Sr1130.8 (2)
O3vi—V1—V1vi41.01 (9)V1vi—O3—V198.03 (13)
O3vii—V1—V1vi113.34 (10)V1vi—O3—V2i99.90 (12)
O3ii—V1—V1vi120.79 (10)V1—O3—V2i134.15 (15)
O3—V1—V1vi40.97 (9)V1vi—O3—Sr1125.86 (13)
O2v—V1—V1viii116.48 (4)V1—O3—Sr1101.16 (11)
O3vi—V1—V1viii113.34 (10)V2i—O3—Sr1101.68 (12)
O3vii—V1—V1viii41.01 (9)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x+1/2, y, z; (iii) x, y+3/2, z; (iv) x1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y+3/2, z; (x) x+1, y, z; (xi) x+1/2, y+1/2, z+1; (xii) x, y, z1.
(SrV3O7_275K) top
Crystal data top
O7V3·SrDx = 3.953 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11380 reflections
a = 5.2968 (8) Åθ = 3.8–32.0°
b = 10.530 (2) ŵ = 13.53 mm1
c = 5.3089 (9) ÅT = 275 K
V = 296.11 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Radiation source: fine-focus sealed tube322 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.067
Detector resolution: 0 pixels mm-1θmax = 25.6°, θmin = 3.8°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.219, Tmax = 0.569l = 66
5445 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.033Secondary atom site location: difference Fourier map
wR(F2) = 0.082 w = 1/[σ2(Fo2) + (0.0472P)2 + 0.5886P]
where P = (Fo2 + 2Fc2)/3
S = 1.22(Δ/σ)max < 0.001
334 reflectionsΔρmax = 0.74 e Å3
24 parametersΔρmin = 0.92 e Å3
Crystal data top
O7V3·SrV = 296.11 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2968 (8) ŵ = 13.53 mm1
b = 10.530 (2) ÅT = 275 K
c = 5.3089 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
322 reflections with I > 2σ(I)
Tmin = 0.219, Tmax = 0.569Rint = 0.067
5445 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03324 parameters
wR(F2) = 0.0820 restraints
S = 1.22Δρmax = 0.74 e Å3
334 reflectionsΔρmin = 0.92 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14876 (16)0.0178 (3)
V10.25000.51541 (10)0.6206 (2)0.0146 (3)
V20.25000.75000.5914 (3)0.0140 (4)
O10.25000.75000.1044 (12)0.0222 (16)*
O20.25000.5455 (5)0.0801 (9)0.0229 (11)*
O30.0119 (6)0.6206 (3)0.4640 (6)0.0162 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0160 (5)0.0158 (5)0.0215 (5)0.0000.0000.000
V10.0093 (6)0.0123 (6)0.0222 (6)0.0000.0000.0007 (4)
V20.0103 (7)0.0117 (7)0.0200 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.473 (5)V2—V1xxi3.6249 (9)
Sr1—O2i2.473 (5)V2—V1i3.6249 (9)
Sr1—O3i2.565 (3)V2—V1xxiv3.6249 (9)
Sr1—O3ii2.565 (3)V2—O13.694 (7)
Sr1—O3iii2.565 (3)V2—O2xix3.833 (4)
Sr1—O32.565 (3)V2—O2xxv3.833 (4)
Sr1—O12.970 (3)V2—O2v3.833 (4)
Sr1—O1iv2.970 (3)V2—O2xxvii3.833 (4)
Sr1—V1i3.5181 (14)V2—Sr1v3.9712 (14)
Sr1—V13.5181 (14)V2—Sr1xxv3.9712 (14)
Sr1—V2iv3.5405 (13)V2—O2xxvi4.051 (5)
Sr1—V23.5405 (13)V2—O2vi4.051 (5)
V1—O2v1.620 (5)V2—O2x4.129 (5)
V1—O3vi1.961 (3)V2—O2xxviii4.129 (5)
V1—O3vii1.961 (3)V2—O3xiii4.152 (3)
V1—O3iii1.960 (3)V2—O3xxix4.152 (3)
V1—O31.960 (3)V2—O3vi4.152 (3)
V1—V1vi2.9596 (10)V2—O3xxvi4.152 (3)
V1—V1viii2.9596 (10)V2—O3xxi4.313 (3)
V1—V2vi3.0129 (14)V2—O3i4.313 (3)
V1—V2iv3.6249 (9)V2—O3xxx4.313 (3)
V1—V23.6249 (9)V2—O3iii4.313 (3)
V1—O2viii3.657 (4)V2—O2xxi4.935 (5)
V1—O2vi3.657 (4)V2—O24.935 (4)
V1—O23.733 (5)V2—O2xxiv4.935 (4)
V1—Sr1v3.7369 (13)V2—O2i4.935 (5)
V1—O1vi3.796 (5)V2—O3xxxi4.991 (3)
V1—O1ix3.905 (3)V2—O3v4.991 (3)
V1—O1v3.905 (3)V2—O3xxvii4.991 (3)
V1—O1x3.914 (5)V2—O3xxxii4.991 (3)
V1—O2x3.957 (4)V2—V1xxxiii5.0313 (18)
V1—O2xi3.957 (4)V2—V1xviii5.0313 (18)
V1—Sr1vi4.0404 (10)V2—V2iv5.2968 (8)
V1—Sr1viii4.0404 (10)V2—V2xxi5.2968 (8)
V1—O3iv4.148 (3)V2—V2xxii5.3089 (9)
V1—O3xii4.148 (3)V2—V2v5.3089 (9)
V1—O3i4.160 (3)V2—Sr1xxxiv5.4429 (12)
V1—O3ii4.160 (3)V2—Sr1vi5.4429 (12)
V1—O3xiii4.306 (3)V2—O1ix5.538 (2)
V1—O3viii4.306 (3)V2—O1xxv5.538 (2)
V1—O3xiv4.368 (3)O1—V2xxii1.615 (7)
V1—O3xv4.368 (3)O1—Sr1xxi2.970 (3)
V1—O3xvi4.817 (3)O1—V1xxvi3.796 (5)
V1—O3v4.817 (3)O1—V1vi3.796 (5)
V1—V1xvii4.8319 (19)O1—V1xxxv3.905 (3)
V1—V1xviii4.8319 (19)O1—V1xxxvi3.905 (3)
V1—O2xix4.889 (5)O1—V1xxii3.905 (3)
V1—V1i4.940 (2)O1—V1xxxvii3.905 (3)
V1—V2xviii5.0313 (18)O1—V1x3.914 (5)
V1—O3xx5.221 (3)O1—V1xxviii3.914 (5)
V1—O3xviii5.221 (3)O2—V1xxii1.620 (5)
V1—O15.285 (5)O2—V1viii3.657 (4)
V1—O1iv5.285 (5)O2—V1vi3.657 (4)
V1—V1xxi5.2968 (8)O2—V2xxxviii3.833 (4)
V1—V1iv5.2968 (8)O2—V2xxii3.833 (4)
V1—V1xxii5.3089 (9)O2—V1x3.957 (4)
V1—V1v5.3089 (9)O2—V1xi3.957 (4)
V1—O3xxiii5.538 (3)O2—V2vi4.051 (5)
V1—O3xxiv5.538 (3)O2—V2x4.129 (5)
V1—O2ix5.5391 (17)O2—V1xxxvi4.889 (5)
V1—O2xxv5.5391 (17)O3—V1vi1.961 (3)
V2—O1v1.615 (7)O3—V1xxi4.148 (3)
V2—O3xii1.976 (3)O3—V2vi4.152 (3)
V2—O3ii1.976 (3)O3—V1i4.160 (3)
V2—O31.976 (3)O3—V1viii4.306 (3)
V2—O3xxiv1.976 (3)O3—V2iv4.313 (3)
V2—V1vi3.0129 (14)O3—V1xxvi4.368 (3)
V2—V1xxvi3.0129 (14)O3—V1xxii4.817 (3)
V2—Sr1xxi3.5405 (13)O3—V2xxii4.991 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x1, y, z; (xxii) x, y, z1; (xxiii) x+1, y+3/2, z; (xxiv) x1/2, y+3/2, z; (xxv) x1, y, z+1; (xxvi) x1/2, y+1/2, z+1; (xxvii) x1/2, y+3/2, z+1; (xxviii) x1/2, y+1/2, z; (xxix) x, y+1/2, z+1; (xxx) x1, y+3/2, z; (xxxi) x, y+3/2, z+1; (xxxii) x1/2, y, z+1; (xxxiii) x1/2, y+1/2, z+2; (xxxiv) x, y+2, z+1; (xxxv) x1, y, z1; (xxxvi) x+1/2, y+3/2, z1; (xxxvii) x1/2, y+3/2, z1; (xxxviii) x+1, y, z1.
(SrV3O7_262K) top
Crystal data top
O7V3·SrDx = 3.956 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11083 reflections
a = 5.2956 (8) Åθ = 3.8–32.1°
b = 10.532 (2) ŵ = 13.54 mm1
c = 5.3055 (9) ÅT = 262 K
V = 295.90 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Radiation source: fine-focus sealed tube321 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.067
Detector resolution: 0 pixels mm-1θmax = 25.6°, θmin = 3.8°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.218, Tmax = 0.568l = 66
5436 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.032Secondary atom site location: difference Fourier map
wR(F2) = 0.078 w = 1/[σ2(Fo2) + (0.0397P)2 + 0.8062P]
where P = (Fo2 + 2Fc2)/3
S = 1.24(Δ/σ)max < 0.001
334 reflectionsΔρmax = 0.69 e Å3
24 parametersΔρmin = 0.96 e Å3
Crystal data top
O7V3·SrV = 295.90 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2956 (8) ŵ = 13.54 mm1
b = 10.532 (2) ÅT = 262 K
c = 5.3055 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
321 reflections with I > 2σ(I)
Tmin = 0.218, Tmax = 0.568Rint = 0.067
5436 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03224 parameters
wR(F2) = 0.0780 restraints
S = 1.24Δρmax = 0.69 e Å3
334 reflectionsΔρmin = 0.96 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14895 (17)0.0174 (3)
V10.25000.51532 (10)0.6207 (2)0.0141 (3)
V20.25000.75000.5915 (3)0.0139 (4)
O10.25000.75000.1043 (12)0.0215 (15)*
O20.25000.5452 (5)0.0804 (9)0.0216 (11)*
O30.0119 (6)0.6205 (3)0.4635 (6)0.0158 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0160 (5)0.0149 (5)0.0212 (5)0.0000.0000.000
V10.0089 (5)0.0119 (6)0.0214 (6)0.0000.0000.0003 (4)
V20.0103 (7)0.0117 (7)0.0198 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.477 (5)V2—V1i3.6254 (9)
Sr1—O2i2.477 (5)V2—V1xxi3.6254 (9)
Sr1—O3i2.563 (3)V2—V1xxv3.6254 (9)
Sr1—O3ii2.563 (3)V2—O13.692 (7)
Sr1—O32.563 (3)V2—O2xix3.833 (4)
Sr1—O3iii2.563 (3)V2—O2xxvii3.833 (4)
Sr1—O12.969 (3)V2—O2xxiii3.833 (4)
Sr1—O1iv2.969 (3)V2—O2v3.833 (4)
Sr1—V1i3.5175 (13)V2—Sr1v3.9697 (14)
Sr1—V13.5175 (14)V2—Sr1xxiii3.9697 (14)
Sr1—V2iv3.5388 (13)V2—O2xxvi4.049 (5)
Sr1—V23.5388 (13)V2—O2vi4.049 (5)
V1—O2v1.617 (5)V2—O2x4.125 (5)
V1—O3vi1.958 (3)V2—O2xxviii4.125 (5)
V1—O3vii1.958 (3)V2—O3xxix4.151 (3)
V1—O3iii1.961 (3)V2—O3xxvi4.151 (3)
V1—O31.961 (3)V2—O3xiii4.151 (3)
V1—V1vi2.9589 (10)V2—O3vi4.151 (3)
V1—V1viii2.9589 (10)V2—O3xxi4.313 (3)
V1—V2vi3.0125 (14)V2—O3i4.313 (3)
V1—V2iv3.6254 (9)V2—O3xxx4.313 (3)
V1—V23.6254 (9)V2—O3iii4.313 (3)
V1—O2viii3.656 (3)V2—O2xxi4.937 (4)
V1—O2vi3.656 (3)V2—O2xxv4.937 (4)
V1—O23.733 (5)V2—O24.937 (4)
V1—Sr1v3.7369 (13)V2—O2i4.937 (4)
V1—O1vi3.794 (5)V2—O3xxxi4.986 (3)
V1—O1ix3.905 (3)V2—O3xxvii4.986 (3)
V1—O1v3.905 (3)V2—O3v4.986 (3)
V1—O1x3.913 (5)V2—O3xxxii4.986 (3)
V1—O2x3.954 (4)V2—V1xxxiii5.0279 (18)
V1—O2xi3.954 (4)V2—V1xviii5.0279 (18)
V1—Sr1vi4.0389 (10)V2—V2iv5.2956 (8)
V1—Sr1viii4.0389 (10)V2—V2xxi5.2956 (8)
V1—O3iv4.147 (3)V2—V2v5.3055 (9)
V1—O3xii4.147 (3)V2—V2xxii5.3055 (9)
V1—O3i4.163 (3)V2—Sr1xxxiv5.4431 (12)
V1—O3ii4.163 (3)V2—Sr1vi5.4430 (12)
V1—O3xiii4.304 (3)V2—O3xxxv5.530 (3)
V1—O3viii4.304 (3)V2—O3xxxvi5.530 (3)
V1—O3xiv4.368 (3)O1—V2xxii1.614 (7)
V1—O3xv4.368 (3)O1—Sr1xxi2.969 (3)
V1—O3xvi4.811 (3)O1—V1xxvi3.794 (5)
V1—O3v4.811 (3)O1—V1vi3.794 (5)
V1—V1xvii4.8285 (19)O1—V1xxxvii3.905 (3)
V1—V1xviii4.8285 (19)O1—V1xxxviii3.905 (3)
V1—O2xix4.893 (5)O1—V1xxxix3.905 (3)
V1—V1i4.943 (2)O1—V1xxii3.905 (3)
V1—V2xviii5.0279 (18)O1—V1x3.913 (5)
V1—O3xx5.219 (3)O1—V1xxviii3.913 (5)
V1—O3xviii5.219 (3)O2—V1xxii1.617 (5)
V1—O15.284 (5)O2—V1viii3.656 (3)
V1—O1iv5.284 (5)O2—V1vi3.656 (3)
V1—V1xxi5.2956 (8)O2—V2xl3.833 (4)
V1—V1iv5.2956 (8)O2—V2xxii3.833 (4)
V1—V1xxii5.3055 (9)O2—V1x3.954 (4)
V1—V1v5.3055 (9)O2—V1xi3.954 (4)
V1—O2ix5.5369 (16)O2—V2vi4.049 (5)
V1—O2xxiii5.5369 (16)O2—V2x4.125 (5)
V1—O3xxiv5.539 (3)O2—V1xxxviii4.893 (5)
V1—O3xxv5.539 (3)O3—V1vi1.958 (3)
V2—O1v1.614 (7)O3—V1xxi4.147 (3)
V2—O3ii1.978 (3)O3—V2vi4.151 (3)
V2—O3xxv1.978 (3)O3—V1i4.163 (3)
V2—O3xii1.978 (3)O3—V1viii4.304 (3)
V2—O31.978 (3)O3—V2iv4.313 (3)
V2—V1vi3.0125 (14)O3—V1xxvi4.368 (3)
V2—V1xxvi3.0125 (14)O3—V1xxii4.811 (3)
V2—Sr1xxi3.5388 (13)O3—V2xxii4.986 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x1, y, z; (xxii) x, y, z1; (xxiii) x1, y, z+1; (xxiv) x+1, y+3/2, z; (xxv) x1/2, y+3/2, z; (xxvi) x1/2, y+1/2, z+1; (xxvii) x1/2, y+3/2, z+1; (xxviii) x1/2, y+1/2, z; (xxix) x, y+1/2, z+1; (xxx) x1, y+3/2, z; (xxxi) x, y+3/2, z+1; (xxxii) x1/2, y, z+1; (xxxiii) x1/2, y+1/2, z+2; (xxxiv) x, y+2, z+1; (xxxv) x+1/2, y+1/2, z+1; (xxxvi) x1, y+1, z+1; (xxxvii) x1, y, z1; (xxxviii) x+1/2, y+3/2, z1; (xxxix) x1/2, y+3/2, z1; (xl) x+1, y, z1.
(SrV3O7_250K) top
Crystal data top
O7V3·SrDx = 3.958 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11262 reflections
a = 5.2959 (8) Åθ = 3.8–32.1°
b = 10.534 (2) ŵ = 13.54 mm1
c = 5.3014 (9) ÅT = 250 K
V = 295.74 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
332 independent reflections
Radiation source: fine-focus sealed tube316 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.067
Detector resolution: 0 pixels mm-1θmax = 25.8°, θmin = 3.8°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.217, Tmax = 0.568l = 66
5416 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.031Secondary atom site location: difference Fourier map
wR(F2) = 0.078 w = 1/[σ2(Fo2) + (0.0371P)2 + 1.0548P]
where P = (Fo2 + 2Fc2)/3
S = 1.24(Δ/σ)max < 0.001
332 reflectionsΔρmax = 0.69 e Å3
24 parametersΔρmin = 0.99 e Å3
Crystal data top
O7V3·SrV = 295.74 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2959 (8) ŵ = 13.54 mm1
b = 10.534 (2) ÅT = 250 K
c = 5.3014 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
332 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
316 reflections with I > 2σ(I)
Tmin = 0.217, Tmax = 0.568Rint = 0.067
5416 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03124 parameters
wR(F2) = 0.0780 restraints
S = 1.24Δρmax = 0.69 e Å3
332 reflectionsΔρmin = 0.99 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14883 (17)0.0168 (3)
V10.25000.51530 (10)0.6207 (2)0.0139 (3)
V20.25000.75000.5916 (3)0.0136 (4)
O10.25000.75000.1042 (13)0.0205 (16)*
O20.25000.5453 (5)0.0797 (9)0.0216 (11)*
O30.0120 (6)0.6208 (3)0.4640 (6)0.0153 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0154 (5)0.0144 (5)0.0207 (5)0.0000.0000.000
V10.0087 (6)0.0119 (6)0.0211 (6)0.0000.0000.0003 (4)
V20.0098 (8)0.0109 (8)0.0200 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.473 (5)V2—V1i3.6259 (9)
Sr1—O2i2.473 (5)V2—V1xxi3.6259 (9)
Sr1—O3i2.563 (3)V2—V1xxiv3.6259 (9)
Sr1—O32.563 (3)V2—O13.689 (7)
Sr1—O3ii2.563 (3)V2—O2xix3.834 (4)
Sr1—O3iii2.563 (3)V2—O2xxv3.834 (4)
Sr1—O12.968 (3)V2—O2v3.834 (4)
Sr1—O1iv2.968 (3)V2—O2xxvii3.834 (4)
Sr1—V1i3.5169 (14)V2—Sr1v3.9672 (15)
Sr1—V13.5169 (14)V2—Sr1xxv3.9672 (15)
Sr1—V2iv3.5385 (13)V2—O2xxvi4.046 (5)
Sr1—V23.5385 (13)V2—O2vi4.046 (5)
V1—O2v1.620 (5)V2—O2x4.128 (5)
V1—O3iii1.962 (3)V2—O2xxviii4.128 (5)
V1—O31.962 (3)V2—O3xiii4.156 (3)
V1—O3vi1.961 (3)V2—O3xxix4.156 (3)
V1—O3vii1.961 (3)V2—O3vi4.156 (3)
V1—V1vi2.9584 (11)V2—O3xxvi4.156 (3)
V1—V1viii2.9584 (11)V2—O3xxi4.312 (3)
V1—V2vi3.0126 (14)V2—O3i4.312 (3)
V1—V2iv3.6259 (9)V2—O3xxx4.312 (3)
V1—V23.6259 (9)V2—O3iii4.312 (3)
V1—O2viii3.652 (4)V2—O2xxi4.932 (5)
V1—O2vi3.652 (4)V2—O2xxiv4.932 (5)
V1—O23.726 (5)V2—O2i4.932 (5)
V1—Sr1v3.7353 (14)V2—O24.932 (5)
V1—O1vi3.792 (5)V2—O3xxxi4.983 (3)
V1—O1ix3.905 (3)V2—O3xxvii4.983 (3)
V1—O1v3.905 (3)V2—O3v4.983 (3)
V1—O1x3.912 (5)V2—O3xxxii4.983 (3)
V1—O2x3.955 (4)V2—V1xxxiii5.0250 (18)
V1—O2xi3.955 (4)V2—V1xviii5.0250 (19)
V1—Sr1vi4.0391 (10)V2—V2iv5.2959 (8)
V1—Sr1viii4.0391 (10)V2—V2xxi5.2959 (8)
V1—O3iv4.147 (3)V2—V2xxii5.3014 (9)
V1—O3xii4.147 (3)V2—V2v5.3014 (9)
V1—O3i4.160 (3)V2—Sr1xxxiv5.4436 (12)
V1—O3ii4.160 (3)V2—Sr1vi5.4436 (12)
V1—O3xiii4.306 (3)V2—O3xxxv5.534 (3)
V1—O3viii4.306 (3)V2—O3xxxvi5.534 (3)
V1—O3xiv4.365 (3)O1—V2xxii1.613 (7)
V1—O3xv4.365 (3)O1—Sr1xxi2.968 (3)
V1—O3xvi4.812 (3)O1—V1xxvi3.792 (5)
V1—O3v4.812 (3)O1—V1vi3.792 (5)
V1—V1xvii4.8263 (19)O1—V1xxxvii3.905 (3)
V1—V1xviii4.826 (2)O1—V1xxxviii3.905 (3)
V1—O2xix4.893 (5)O1—V1xxxix3.905 (3)
V1—V1i4.944 (2)O1—V1xxii3.905 (3)
V1—V2xviii5.0250 (18)O1—V1x3.912 (5)
V1—O3xx5.214 (3)O1—V1xxviii3.912 (5)
V1—O3xviii5.214 (3)O2—V1xxii1.620 (5)
V1—O15.281 (5)O2—V1viii3.652 (4)
V1—O1iv5.281 (5)O2—V1vi3.652 (4)
V1—V1xxi5.2959 (8)O2—V2xl3.834 (4)
V1—V1iv5.2959 (8)O2—V2xxii3.834 (4)
V1—V1xxii5.3014 (9)O2—V1x3.955 (4)
V1—V1v5.3014 (9)O2—V1xi3.955 (4)
V1—O3xxiii5.537 (3)O2—V2vi4.046 (5)
V1—O3xxiv5.537 (3)O2—V2x4.128 (5)
V1—O2ix5.5381 (17)O2—V1xxxviii4.893 (5)
V1—O2xxv5.5381 (17)O3—V1vi1.961 (3)
V2—O1v1.613 (7)O3—V1xxi4.147 (3)
V2—O3xii1.974 (3)O3—V2vi4.156 (3)
V2—O3ii1.974 (3)O3—V1i4.160 (3)
V2—O3xxiv1.974 (3)O3—V1viii4.306 (3)
V2—O31.974 (3)O3—V2iv4.312 (3)
V2—V1vi3.0126 (14)O3—V1xxvi4.365 (3)
V2—V1xxvi3.0126 (14)O3—V1xxii4.812 (3)
V2—Sr1xxi3.5385 (13)O3—V2xxii4.983 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x1, y, z; (xxii) x, y, z1; (xxiii) x+1, y+3/2, z; (xxiv) x1/2, y+3/2, z; (xxv) x1, y, z+1; (xxvi) x1/2, y+1/2, z+1; (xxvii) x1/2, y+3/2, z+1; (xxviii) x1/2, y+1/2, z; (xxix) x, y+1/2, z+1; (xxx) x1, y+3/2, z; (xxxi) x, y+3/2, z+1; (xxxii) x1/2, y, z+1; (xxxiii) x1/2, y+1/2, z+2; (xxxiv) x, y+2, z+1; (xxxv) x1, y+1, z+1; (xxxvi) x+1/2, y+1/2, z+1; (xxxvii) x1, y, z1; (xxxviii) x+1/2, y+3/2, z1; (xxxix) x1/2, y+3/2, z1; (xl) x+1, y, z1.
(SrV3O7_225K) top
Crystal data top
O7V3·SrDx = 3.963 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11381 reflections
a = 5.2954 (8) Åθ = 3.9–32.1°
b = 10.534 (2) ŵ = 13.56 mm1
c = 5.2952 (9) ÅT = 225 K
V = 295.38 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Radiation source: fine-focus sealed tube320 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.067
Detector resolution: 0 pixels mm-1θmax = 25.8°, θmin = 3.9°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.218, Tmax = 0.568l = 66
5414 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.033Secondary atom site location: difference Fourier map
wR(F2) = 0.077 w = 1/[σ2(Fo2) + (0.0346P)2 + 0.5753P]
where P = (Fo2 + 2Fc2)/3
S = 1.39(Δ/σ)max < 0.001
334 reflectionsΔρmax = 0.71 e Å3
24 parametersΔρmin = 1.01 e Å3
Crystal data top
O7V3·SrV = 295.38 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2954 (8) ŵ = 13.56 mm1
b = 10.534 (2) ÅT = 225 K
c = 5.2952 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
320 reflections with I > 2σ(I)
Tmin = 0.218, Tmax = 0.568Rint = 0.067
5414 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03324 parameters
wR(F2) = 0.0770 restraints
S = 1.39Δρmax = 0.71 e Å3
334 reflectionsΔρmin = 1.01 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14899 (17)0.0162 (3)
V10.25000.51522 (10)0.6210 (2)0.0135 (3)
V20.25000.75000.5921 (3)0.0134 (4)
O10.25000.75000.1024 (12)0.0200 (15)*
O20.25000.5452 (5)0.0795 (9)0.0210 (11)*
O30.0121 (6)0.6207 (3)0.4641 (6)0.0146 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0145 (5)0.0140 (5)0.0201 (5)0.0000.0000.000
V10.0087 (5)0.0112 (6)0.0205 (6)0.0000.0000.0003 (4)
V20.0098 (7)0.0114 (7)0.0190 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.474 (5)V2—V1i3.6263 (9)
Sr1—O2i2.474 (5)V2—V1xxii3.6263 (9)
Sr1—O3i2.562 (3)V2—V1xxiv3.6263 (9)
Sr1—O32.562 (3)V2—O13.677 (7)
Sr1—O3ii2.562 (3)V2—O2xix3.833 (4)
Sr1—O3iii2.562 (3)V2—O2xxv3.833 (4)
Sr1—O12.963 (3)V2—O2v3.833 (4)
Sr1—O1iv2.963 (3)V2—O2xxvii3.833 (4)
Sr1—V1i3.5161 (14)V2—Sr1v3.9633 (14)
Sr1—V13.5161 (14)V2—Sr1xxv3.9633 (14)
Sr1—V2iv3.5376 (13)V2—O2xxvi4.041 (5)
Sr1—V23.5376 (13)V2—O2vi4.041 (5)
V1—O2v1.617 (5)V2—O2x4.127 (5)
V1—O3vi1.960 (3)V2—O2xxviii4.127 (5)
V1—O3vii1.960 (3)V2—O3xxix4.155 (3)
V1—O3iii1.962 (3)V2—O3xiii4.155 (3)
V1—O31.962 (3)V2—O3xxvi4.155 (3)
V1—V1vi2.9588 (10)V2—O3vi4.155 (3)
V1—V1viii2.9588 (10)V2—O3xxii4.313 (3)
V1—V2vi3.0131 (14)V2—O3i4.313 (3)
V1—V2iv3.6263 (9)V2—O3xxx4.313 (3)
V1—V23.6263 (9)V2—O3iii4.313 (3)
V1—O2viii3.648 (3)V2—O2xxii4.931 (4)
V1—O2vi3.648 (3)V2—O2xxiv4.931 (4)
V1—O23.723 (5)V2—O24.931 (4)
V1—Sr1v3.7328 (13)V2—O2i4.931 (4)
V1—O1vi3.782 (4)V2—O3xxxi4.976 (3)
V1—O1ix3.908 (3)V2—O3xxvii4.976 (3)
V1—O1v3.908 (3)V2—O3v4.976 (3)
V1—O1x3.917 (5)V2—O3xxxii4.976 (3)
V1—O2x3.954 (4)V2—V1xxxiii5.0171 (18)
V1—O2xi3.954 (4)V2—V1xviii5.0171 (18)
V1—Sr1vi4.0373 (10)V2—V2v5.2952 (9)
V1—Sr1viii4.0373 (10)V2—V2xxi5.2952 (9)
V1—O3iv4.147 (3)V2—V2iv5.2954 (8)
V1—O3xii4.147 (3)V2—V2xxii5.2954 (8)
V1—O3i4.162 (3)V2—Sr1xxxiv5.4427 (12)
V1—O3ii4.162 (3)V2—Sr1vi5.4427 (12)
V1—O3xiii4.306 (3)V2—O1ix5.537 (2)
V1—O3viii4.306 (3)V2—O1xxv5.537 (2)
V1—O3xiv4.366 (3)O1—V2xxi1.618 (7)
V1—O3xv4.366 (3)O1—Sr1xxii2.963 (3)
V1—O3xvi4.805 (3)O1—V1xxvi3.782 (4)
V1—O3v4.805 (3)O1—V1vi3.782 (4)
V1—V1xvii4.8193 (19)O1—V1xxxv3.908 (3)
V1—V1xviii4.8193 (19)O1—V1xxxvi3.908 (3)
V1—O2xix4.895 (5)O1—V1xxxvii3.908 (3)
V1—V1i4.946 (2)O1—V1xxi3.908 (3)
V1—V2xviii5.0171 (18)O1—V1x3.917 (5)
V1—O3xx5.207 (3)O1—V1xxviii3.917 (5)
V1—O3xviii5.207 (3)O2—V1xxi1.617 (5)
V1—O15.272 (5)O2—V1viii3.648 (3)
V1—O1iv5.272 (5)O2—V1vi3.648 (3)
V1—V1v5.2952 (9)O2—V2xxxviii3.833 (4)
V1—V1xxi5.2952 (9)O2—V2xxi3.833 (4)
V1—V1xxii5.2954 (8)O2—V1x3.954 (4)
V1—V1iv5.2954 (8)O2—V1xi3.954 (4)
V1—O3xxiii5.538 (3)O2—V2vi4.041 (5)
V1—O3xxiv5.538 (3)O2—V2x4.127 (5)
V1—O2ix5.5368 (16)O2—V1xxxvi4.895 (5)
V1—O2xxv5.5368 (16)O3—V1vi1.960 (3)
V2—O1v1.618 (7)O3—V1xxii4.147 (3)
V2—O3xii1.975 (3)O3—V2vi4.155 (3)
V2—O3xxiv1.975 (3)O3—V1i4.162 (3)
V2—O3ii1.975 (3)O3—V1viii4.306 (3)
V2—O31.975 (3)O3—V2iv4.313 (3)
V2—V1vi3.0131 (14)O3—V1xxvi4.366 (3)
V2—V1xxvi3.0131 (14)O3—V1xxi4.805 (3)
V2—Sr1xxii3.5376 (13)O3—V2xxi4.976 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x, y, z1; (xxii) x1, y, z; (xxiii) x+1, y+3/2, z; (xxiv) x1/2, y+3/2, z; (xxv) x1, y, z+1; (xxvi) x1/2, y+1/2, z+1; (xxvii) x1/2, y+3/2, z+1; (xxviii) x1/2, y+1/2, z; (xxix) x, y+1/2, z+1; (xxx) x1, y+3/2, z; (xxxi) x, y+3/2, z+1; (xxxii) x1/2, y, z+1; (xxxiii) x1/2, y+1/2, z+2; (xxxiv) x, y+2, z+1; (xxxv) x1, y, z1; (xxxvi) x+1/2, y+3/2, z1; (xxxvii) x1/2, y+3/2, z1; (xxxviii) x+1, y, z1.
(SrV3O7_200K) top
Crystal data top
O7V3·SrDx = 3.968 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11571 reflections
a = 5.2934 (8) Åθ = 3.9–32.1°
b = 10.537 (2) ŵ = 13.58 mm1
c = 5.2889 (9) ÅT = 200 K
V = 294.99 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
335 independent reflections
Radiation source: fine-focus sealed tube319 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.068
Detector resolution: 0 pixels mm-1θmax = 25.9°, θmin = 3.9°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.218, Tmax = 0.568l = 66
5382 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.033Secondary atom site location: difference Fourier map
wR(F2) = 0.080 w = 1/[σ2(Fo2) + (0.0415P)2 + 0.9218P]
where P = (Fo2 + 2Fc2)/3
S = 1.23(Δ/σ)max < 0.001
335 reflectionsΔρmax = 0.61 e Å3
24 parametersΔρmin = 0.86 e Å3
Crystal data top
O7V3·SrV = 294.99 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2934 (8) ŵ = 13.58 mm1
b = 10.537 (2) ÅT = 200 K
c = 5.2889 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
335 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
319 reflections with I > 2σ(I)
Tmin = 0.218, Tmax = 0.568Rint = 0.068
5382 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03324 parameters
wR(F2) = 0.0800 restraints
S = 1.23Δρmax = 0.61 e Å3
335 reflectionsΔρmin = 0.86 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14897 (17)0.0155 (3)
V10.25000.51518 (11)0.6211 (2)0.0131 (3)
V20.25000.75000.5922 (3)0.0132 (4)
O10.25000.75000.1024 (12)0.0185 (15)*
O20.25000.5449 (5)0.0786 (9)0.0195 (11)*
O30.0116 (6)0.6205 (3)0.4639 (6)0.0144 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0134 (5)0.0134 (5)0.0196 (5)0.0000.0000.000
V10.0084 (6)0.0117 (6)0.0193 (6)0.0000.0000.0002 (4)
V20.0094 (8)0.0112 (8)0.0189 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.474 (5)V2—V1i3.6263 (9)
Sr1—O2i2.474 (5)V2—V1xxii3.6263 (9)
Sr1—O3i2.560 (3)V2—V1xxv3.6263 (9)
Sr1—O32.560 (3)V2—O13.674 (7)
Sr1—O3ii2.560 (3)V2—O2xix3.835 (4)
Sr1—O3iii2.560 (3)V2—O2xxiii3.835 (4)
Sr1—O12.962 (3)V2—O2v3.835 (4)
Sr1—O1iv2.962 (3)V2—O2xxviii3.835 (4)
Sr1—V1i3.5153 (14)V2—Sr1v3.9592 (14)
Sr1—V13.5153 (14)V2—Sr1xxiii3.9592 (14)
Sr1—V2iv3.5357 (13)V2—O2xxvii4.033 (5)
Sr1—V23.5357 (13)V2—O2vi4.033 (5)
V1—O2v1.619 (5)V2—O2x4.127 (5)
V1—O3iii1.960 (3)V2—O2xxix4.127 (5)
V1—O31.960 (3)V2—O3xiii4.153 (3)
V1—O3vi1.959 (3)V2—O3xxx4.153 (3)
V1—O3vii1.959 (3)V2—O3vi4.153 (3)
V1—V1vi2.9578 (10)V2—O3xxvii4.153 (3)
V1—V1viii2.9578 (10)V2—O3xxii4.310 (3)
V1—V2vi3.0134 (14)V2—O3i4.310 (3)
V1—V2iv3.6263 (9)V2—O3xxxi4.310 (3)
V1—V23.6263 (9)V2—O3iii4.310 (3)
V1—O2viii3.641 (3)V2—O2xxii4.926 (4)
V1—O2vi3.641 (3)V2—O24.926 (4)
V1—O23.714 (5)V2—O2xxv4.926 (4)
V1—Sr1v3.7304 (14)V2—O2i4.926 (4)
V1—O1vi3.780 (4)V2—O3xxxii4.971 (3)
V1—O1ix3.907 (3)V2—O3xxviii4.971 (3)
V1—O1v3.907 (3)V2—O3v4.971 (3)
V1—O1x3.916 (5)V2—O3xxxiii4.971 (3)
V1—O2x3.955 (4)V2—V1xxxiv5.0116 (18)
V1—O2xi3.955 (4)V2—V1xviii5.0116 (18)
V1—Sr1vi4.0362 (10)V2—V2xxi5.2889 (9)
V1—Sr1viii4.0362 (10)V2—V2v5.2889 (9)
V1—O3iv4.148 (3)V2—V2iv5.2934 (8)
V1—O3xii4.148 (3)V2—V2xxii5.2934 (8)
V1—O3i4.165 (3)V2—Sr1xxxv5.4432 (12)
V1—O3ii4.165 (3)V2—Sr1vi5.4432 (12)
V1—O3xiii4.301 (3)V2—O3xxxvi5.532 (3)
V1—O3viii4.301 (3)V2—O3xxxvii5.532 (3)
V1—O3xiv4.369 (3)O1—V2xxi1.615 (7)
V1—O3xv4.369 (3)O1—Sr1xxii2.962 (3)
V1—O3xvi4.798 (3)O1—V1xxvii3.780 (4)
V1—O3v4.798 (3)O1—V1vi3.780 (4)
V1—V1xvii4.8135 (19)O1—V1xxxviii3.907 (3)
V1—V1xviii4.8135 (19)O1—V1xxxix3.907 (3)
V1—O2xix4.900 (5)O1—V1xl3.907 (3)
V1—V1i4.948 (2)O1—V1xxi3.907 (3)
V1—V2xviii5.0116 (18)O1—V1x3.916 (5)
V1—O3xx5.202 (3)O1—V1xxix3.916 (5)
V1—O3xviii5.202 (3)O2—V1xxi1.619 (5)
V1—O15.270 (5)O2—V1viii3.641 (3)
V1—O1iv5.270 (5)O2—V1vi3.641 (3)
V1—V1xxi5.2889 (9)O2—V2xli3.835 (4)
V1—V1xxii5.2934 (8)O2—V2xxi3.835 (4)
V1—V1iv5.2934 (8)O2—V1x3.955 (4)
V1—O2ix5.5354 (17)O2—V1xi3.955 (4)
V1—O2xxiii5.5354 (16)O2—V2vi4.033 (5)
V1—O3xxiv5.541 (3)O2—V2x4.127 (5)
V1—O3xxv5.541 (3)O2—V1xxxix4.900 (5)
V1—V1xxvi5.588 (3)O3—V1vi1.959 (3)
V2—O1v1.615 (7)O3—V1xxii4.148 (3)
V2—O3xii1.979 (3)O3—V2vi4.153 (3)
V2—O3ii1.979 (3)O3—V1i4.165 (3)
V2—O31.979 (3)O3—V1viii4.301 (3)
V2—O3xxv1.979 (3)O3—V2iv4.310 (3)
V2—V1vi3.0134 (14)O3—V1xxvii4.369 (3)
V2—V1xxvii3.0134 (14)O3—V1xxi4.798 (3)
V2—Sr1xxii3.5357 (13)O3—V2xxi4.971 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x, y, z1; (xxii) x1, y, z; (xxiii) x1, y, z+1; (xxiv) x+1, y+3/2, z; (xxv) x1/2, y+3/2, z; (xxvi) x+1/2, y+1/2, z; (xxvii) x1/2, y+1/2, z+1; (xxviii) x1/2, y+3/2, z+1; (xxix) x1/2, y+1/2, z; (xxx) x, y+1/2, z+1; (xxxi) x1, y+3/2, z; (xxxii) x, y+3/2, z+1; (xxxiii) x1/2, y, z+1; (xxxiv) x1/2, y+1/2, z+2; (xxxv) x, y+2, z+1; (xxxvi) x1, y+1, z+1; (xxxvii) x+1/2, y+1/2, z+1; (xxxviii) x1, y, z1; (xxxix) x+1/2, y+3/2, z1; (xl) x1/2, y+3/2, z1; (xli) x+1, y, z1.
(SrV3O7_187K) top
Crystal data top
O7V3·SrDx = 3.970 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11507 reflections
a = 5.2923 (8) Åθ = 3.9–32.1°
b = 10.539 (2) ŵ = 13.59 mm1
c = 5.2864 (9) ÅT = 187 K
V = 294.84 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Radiation source: fine-focus sealed tube317 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.070
Detector resolution: 0 pixels mm-1θmax = 25.8°, θmin = 3.9°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.217, Tmax = 0.567l = 66
5376 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.033Secondary atom site location: difference Fourier map
wR(F2) = 0.079 w = 1/[σ2(Fo2) + (0.038P)2 + 0.5256P]
where P = (Fo2 + 2Fc2)/3
S = 1.34(Δ/σ)max < 0.001
334 reflectionsΔρmax = 0.68 e Å3
24 parametersΔρmin = 1.08 e Å3
Crystal data top
O7V3·SrV = 294.84 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2923 (8) ŵ = 13.59 mm1
b = 10.539 (2) ÅT = 187 K
c = 5.2864 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
317 reflections with I > 2σ(I)
Tmin = 0.217, Tmax = 0.567Rint = 0.070
5376 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03324 parameters
wR(F2) = 0.0790 restraints
S = 1.34Δρmax = 0.68 e Å3
334 reflectionsΔρmin = 1.08 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14884 (16)0.0153 (3)
V10.25000.51513 (10)0.6211 (2)0.0129 (3)
V20.25000.75000.5921 (3)0.0128 (4)
O10.25000.75000.1020 (12)0.0185 (15)*
O20.25000.5449 (4)0.0784 (9)0.0187 (10)*
O30.0119 (6)0.6207 (3)0.4642 (6)0.0142 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0133 (5)0.0133 (5)0.0192 (5)0.0000.0000.000
V10.0080 (6)0.0111 (6)0.0195 (6)0.0000.0000.0000 (4)
V20.0090 (7)0.0106 (7)0.0187 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.473 (5)V2—V1i3.6266 (9)
Sr1—O2i2.473 (5)V2—V1xxii3.6266 (9)
Sr1—O3i2.561 (3)V2—V1xxv3.6266 (9)
Sr1—O3ii2.561 (3)V2—O13.669 (7)
Sr1—O3iii2.561 (3)V2—O2xix3.835 (3)
Sr1—O32.561 (3)V2—O2xxiii3.835 (3)
Sr1—O12.960 (3)V2—O2v3.835 (3)
Sr1—O1iv2.960 (3)V2—O2xxvii3.835 (3)
Sr1—V1i3.5156 (14)V2—Sr1v3.9577 (14)
Sr1—V13.5156 (14)V2—Sr1xxiii3.9577 (14)
Sr1—V2iv3.5346 (13)V2—O2xxvi4.033 (5)
Sr1—V23.5346 (13)V2—O2vi4.033 (5)
V1—O2v1.620 (5)V2—O2x4.128 (5)
V1—O3vi1.960 (3)V2—O2xxviii4.128 (5)
V1—O3vii1.960 (3)V2—O3xiii4.156 (3)
V1—O3iii1.962 (3)V2—O3xxix4.156 (3)
V1—O31.962 (3)V2—O3xxvi4.156 (3)
V1—V1vi2.9568 (10)V2—O3vi4.156 (3)
V1—V1viii2.9568 (10)V2—O3xxii4.310 (3)
V1—V2vi3.0129 (14)V2—O3i4.310 (3)
V1—V2iv3.6266 (9)V2—O3xxx4.310 (3)
V1—V23.6266 (9)V2—O3iii4.310 (3)
V1—O2viii3.640 (3)V2—O2xxii4.923 (4)
V1—O2vi3.640 (3)V2—O2xxv4.923 (4)
V1—O23.711 (5)V2—O24.923 (4)
V1—Sr1v3.7296 (13)V2—O2i4.923 (4)
V1—O1vi3.777 (4)V2—O3xxxi4.969 (3)
V1—O1ix3.908 (3)V2—O3xxvii4.969 (3)
V1—O1v3.908 (3)V2—O3v4.969 (3)
V1—O1x3.916 (5)V2—O3xxxii4.969 (3)
V1—O2x3.954 (4)V2—V1xxxiii5.0107 (18)
V1—O2xi3.954 (4)V2—V1xviii5.0107 (18)
V1—Sr1vi4.0359 (10)V2—V2v5.2864 (9)
V1—Sr1viii4.0359 (10)V2—V2xxi5.2864 (9)
V1—O3iv4.145 (3)V2—V2iv5.2923 (8)
V1—O3xii4.145 (3)V2—V2xxii5.2923 (8)
V1—O3i4.164 (3)V2—Sr1xxxiv5.4444 (12)
V1—O3ii4.164 (3)V2—Sr1vi5.4444 (12)
V1—O3xiii4.303 (3)V2—O1ix5.534 (2)
V1—O3viii4.303 (3)V2—O1xxiii5.534 (2)
V1—O3xiv4.367 (3)O1—V2xxi1.617 (6)
V1—O3xv4.367 (3)O1—Sr1xxii2.960 (3)
V1—O3xvi4.798 (3)O1—V1xxvi3.777 (4)
V1—O3v4.798 (3)O1—V1vi3.777 (4)
V1—V1xvii4.8117 (19)O1—V1xxxv3.908 (3)
V1—V1xviii4.8117 (19)O1—V1xxxvi3.908 (3)
V1—O2xix4.901 (5)O1—V1xxxvii3.908 (3)
V1—V1i4.950 (2)O1—V1xxi3.908 (3)
V1—V2xviii5.0107 (18)O1—V1x3.916 (5)
V1—O3xx5.198 (3)O1—V1xxviii3.916 (5)
V1—O3xviii5.198 (3)O2—V1xxi1.620 (5)
V1—O15.267 (5)O2—V1viii3.640 (3)
V1—O1iv5.267 (5)O2—V1vi3.640 (3)
V1—V1xxi5.2864 (9)O2—V2xxxviii3.835 (3)
V1—V1v5.2864 (9)O2—V2xxi3.835 (3)
V1—V1xxii5.2923 (8)O2—V1x3.954 (4)
V1—V1iv5.2923 (8)O2—V1xi3.954 (4)
V1—O2ix5.5346 (16)O2—V2vi4.033 (5)
V1—O2xxiii5.5346 (16)O2—V2x4.128 (5)
V1—O3xxiv5.538 (3)O2—V1xxxvi4.901 (5)
V1—O3xxv5.538 (3)O3—V1vi1.960 (3)
V2—O1v1.617 (6)O3—V1xxii4.145 (3)
V2—O3xii1.975 (3)O3—V2vi4.156 (3)
V2—O3ii1.975 (3)O3—V1i4.164 (3)
V2—O31.975 (3)O3—V1viii4.303 (3)
V2—O3xxv1.975 (3)O3—V2iv4.310 (3)
V2—V1vi3.0129 (14)O3—V1xxvi4.367 (3)
V2—V1xxvi3.0129 (14)O3—V1xxi4.798 (3)
V2—Sr1xxii3.5346 (13)O3—V2xxi4.969 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x, y, z1; (xxii) x1, y, z; (xxiii) x1, y, z+1; (xxiv) x+1, y+3/2, z; (xxv) x1/2, y+3/2, z; (xxvi) x1/2, y+1/2, z+1; (xxvii) x1/2, y+3/2, z+1; (xxviii) x1/2, y+1/2, z; (xxix) x, y+1/2, z+1; (xxx) x1, y+3/2, z; (xxxi) x, y+3/2, z+1; (xxxii) x1/2, y, z+1; (xxxiii) x1/2, y+1/2, z+2; (xxxiv) x, y+2, z+1; (xxxv) x1, y, z1; (xxxvi) x+1/2, y+3/2, z1; (xxxvii) x1/2, y+3/2, z1; (xxxviii) x+1, y, z1.
(SrV3O7_175K) top
Crystal data top
O7V3·SrDx = 3.973 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11566 reflections
a = 5.2914 (8) Åθ = 3.9–32.1°
b = 10.539 (2) ŵ = 13.60 mm1
c = 5.2828 (9) ÅT = 175 K
V = 294.60 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
333 independent reflections
Radiation source: fine-focus sealed tube317 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.070
Detector resolution: 0 pixels mm-1θmax = 25.6°, θmin = 3.9°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.213, Tmax = 0.567l = 66
5350 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.034Secondary atom site location: difference Fourier map
wR(F2) = 0.082 w = 1/[σ2(Fo2) + (0.0452P)2 + 0.7112P]
where P = (Fo2 + 2Fc2)/3
S = 1.22(Δ/σ)max < 0.001
333 reflectionsΔρmax = 0.60 e Å3
24 parametersΔρmin = 1.14 e Å3
Crystal data top
O7V3·SrV = 294.60 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2914 (8) ŵ = 13.60 mm1
b = 10.539 (2) ÅT = 175 K
c = 5.2828 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
333 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
317 reflections with I > 2σ(I)
Tmin = 0.213, Tmax = 0.567Rint = 0.070
5350 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03424 parameters
wR(F2) = 0.0820 restraints
S = 1.22Δρmax = 0.60 e Å3
333 reflectionsΔρmin = 1.14 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14892 (16)0.0151 (3)
V10.25000.51511 (11)0.6211 (2)0.0129 (3)
V20.25000.75000.5923 (3)0.0129 (4)
O10.25000.75000.1027 (12)0.0177 (15)*
O20.25000.5448 (4)0.0779 (9)0.0182 (10)*
O30.0118 (6)0.6208 (3)0.4644 (6)0.0143 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0123 (5)0.0132 (5)0.0197 (5)0.0000.0000.000
V10.0083 (6)0.0112 (6)0.0191 (6)0.0000.0000.0002 (4)
V20.0092 (8)0.0112 (8)0.0182 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.473 (5)V2—V1i3.6265 (9)
Sr1—O2i2.473 (5)V2—V1xxii3.6265 (9)
Sr1—O3i2.560 (3)V2—V1xxv3.6265 (9)
Sr1—O3ii2.560 (3)V2—O13.671 (7)
Sr1—O3iii2.560 (3)V2—O2xix3.836 (3)
Sr1—O32.560 (3)V2—O2xxvii3.836 (3)
Sr1—O12.961 (3)V2—O2xxiii3.836 (3)
Sr1—O1iv2.961 (3)V2—O2v3.836 (3)
Sr1—V1i3.5144 (14)V2—Sr1v3.9556 (14)
Sr1—V13.5144 (14)V2—Sr1xxiii3.9556 (14)
Sr1—V2iv3.5335 (13)V2—O2xxvi4.029 (5)
Sr1—V23.5335 (13)V2—O2vi4.029 (5)
V1—O2v1.620 (5)V2—O2x4.127 (5)
V1—O3vi1.961 (3)V2—O2xxviii4.127 (5)
V1—O3vii1.961 (3)V2—O3xiii4.157 (3)
V1—O3iii1.961 (3)V2—O3xxix4.157 (3)
V1—O31.961 (3)V2—O3xxvi4.157 (3)
V1—V1vi2.9562 (10)V2—O3vi4.157 (3)
V1—V1viii2.9562 (10)V2—O3xxii4.308 (3)
V1—V2vi3.0129 (14)V2—O3xxx4.308 (3)
V1—V2iv3.6265 (9)V2—O3i4.308 (3)
V1—V23.6265 (9)V2—O3iii4.308 (3)
V1—O2viii3.636 (3)V2—O2xxii4.921 (4)
V1—O2vi3.636 (3)V2—O2xxv4.921 (4)
V1—O23.706 (5)V2—O24.921 (4)
V1—Sr1v3.7286 (13)V2—O2i4.921 (4)
V1—O1vi3.779 (4)V2—O3xxxi4.967 (3)
V1—O1ix3.906 (3)V2—O3xxvii4.967 (3)
V1—O1v3.906 (3)V2—O3v4.967 (3)
V1—O1x3.912 (5)V2—O3xxxii4.967 (3)
V1—O2x3.954 (4)V2—V1xxxiii5.0074 (18)
V1—O2xi3.954 (4)V2—V1xviii5.0074 (18)
V1—Sr1vi4.0351 (10)V2—V2xxi5.2828 (9)
V1—Sr1viii4.0351 (10)V2—V2v5.2828 (9)
V1—O3iv4.145 (3)V2—V2iv5.2914 (8)
V1—O3xii4.145 (3)V2—V2xxii5.2914 (8)
V1—O3i4.163 (3)V2—Sr1xxxiv5.4440 (12)
V1—O3ii4.163 (3)V2—Sr1vi5.4440 (12)
V1—O3xiii4.302 (3)V2—O1ix5.531 (2)
V1—O3viii4.302 (3)V2—O1xxiii5.531 (2)
V1—O3xiv4.366 (3)O1—V2xxi1.611 (7)
V1—O3xv4.366 (3)O1—Sr1xxii2.961 (3)
V1—O3xvi4.797 (3)O1—V1xxvi3.779 (4)
V1—O3v4.797 (3)O1—V1vi3.779 (4)
V1—V1xvii4.8088 (19)O1—V1xxxv3.906 (3)
V1—V1xviii4.8088 (19)O1—V1xxxvi3.906 (3)
V1—O2xix4.903 (5)O1—V1xxxvii3.906 (3)
V1—V1i4.951 (2)O1—V1xxi3.906 (3)
V1—V2xviii5.0074 (18)O1—V1x3.912 (5)
V1—O3xx5.194 (3)O1—V1xxviii3.912 (5)
V1—O3xviii5.194 (3)O2—V1xxi1.620 (5)
V1—O15.268 (5)O2—V1viii3.636 (3)
V1—O1iv5.268 (5)O2—V1vi3.636 (3)
V1—V1v5.2828 (9)O2—V2xxxviii3.836 (3)
V1—V1xxi5.2828 (9)O2—V2xxi3.836 (3)
V1—V1xxii5.2914 (8)O2—V1x3.954 (4)
V1—V1iv5.2914 (8)O2—V1xi3.954 (4)
V1—O2ix5.5339 (16)O2—V2vi4.029 (5)
V1—O2xxiii5.5339 (16)O2—V2x4.127 (5)
V1—O3xxiv5.538 (3)O2—V1xxxvi4.903 (5)
V1—O3xxv5.538 (3)O3—V1vi1.961 (3)
V2—O1v1.611 (7)O3—V1xxii4.145 (3)
V2—O3xii1.975 (3)O3—V2vi4.157 (3)
V2—O3xxv1.975 (3)O3—V1i4.163 (3)
V2—O3ii1.975 (3)O3—V1viii4.302 (3)
V2—O31.975 (3)O3—V2iv4.308 (3)
V2—V1vi3.0129 (14)O3—V1xxvi4.366 (3)
V2—V1xxvi3.0129 (14)O3—V1xxi4.797 (3)
V2—Sr1xxii3.5335 (13)O3—V2xxi4.967 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x, y, z1; (xxii) x1, y, z; (xxiii) x1, y, z+1; (xxiv) x+1, y+3/2, z; (xxv) x1/2, y+3/2, z; (xxvi) x1/2, y+1/2, z+1; (xxvii) x1/2, y+3/2, z+1; (xxviii) x1/2, y+1/2, z; (xxix) x, y+1/2, z+1; (xxx) x1, y+3/2, z; (xxxi) x, y+3/2, z+1; (xxxii) x1/2, y, z+1; (xxxiii) x1/2, y+1/2, z+2; (xxxiv) x, y+2, z+1; (xxxv) x1, y, z1; (xxxvi) x+1/2, y+3/2, z1; (xxxvii) x1/2, y+3/2, z1; (xxxviii) x+1, y, z1.
(SrV3O7_150K) top
Crystal data top
O7V3·SrDx = 3.977 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11695 reflections
a = 5.2909 (8) Åθ = 3.9–32.1°
b = 10.544 (2) ŵ = 13.61 mm1
c = 5.2763 (9) ÅT = 150 K
V = 294.34 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Radiation source: fine-focus sealed tube320 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.070
Detector resolution: 0 pixels mm-1θmax = 25.9°, θmin = 3.9°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.217, Tmax = 0.567l = 66
5332 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.034Secondary atom site location: difference Fourier map
wR(F2) = 0.080 w = 1/[σ2(Fo2) + (0.041P)2 + 0.4275P]
where P = (Fo2 + 2Fc2)/3
S = 1.33(Δ/σ)max < 0.001
334 reflectionsΔρmax = 0.60 e Å3
24 parametersΔρmin = 1.24 e Å3
Crystal data top
O7V3·SrV = 294.34 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2909 (8) ŵ = 13.61 mm1
b = 10.544 (2) ÅT = 150 K
c = 5.2763 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
334 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
320 reflections with I > 2σ(I)
Tmin = 0.217, Tmax = 0.567Rint = 0.070
5332 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03424 parameters
wR(F2) = 0.0800 restraints
S = 1.33Δρmax = 0.60 e Å3
334 reflectionsΔρmin = 1.24 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14892 (16)0.0144 (3)
V10.25000.51507 (10)0.6213 (2)0.0125 (3)
V20.25000.75000.5928 (3)0.0124 (4)
O10.25000.75000.1015 (12)0.0168 (14)*
O20.25000.5447 (4)0.0776 (9)0.0185 (10)*
O30.0117 (5)0.6207 (3)0.4644 (6)0.0137 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0117 (5)0.0128 (5)0.0188 (5)0.0000.0000.000
V10.0079 (6)0.0106 (6)0.0190 (6)0.0000.0000.0003 (4)
V20.0088 (7)0.0110 (8)0.0174 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.473 (5)V2—V1i3.6273 (9)
Sr1—O2i2.473 (5)V2—V1xxii3.6273 (9)
Sr1—O3i2.559 (3)V2—V1xxv3.6273 (9)
Sr1—O3ii2.559 (3)V2—O13.663 (6)
Sr1—O3iii2.559 (3)V2—O2xix3.835 (3)
Sr1—O32.559 (3)V2—O2xxiii3.835 (3)
Sr1—O12.957 (3)V2—O2v3.835 (3)
Sr1—O1iv2.957 (3)V2—O2xxvii3.835 (3)
Sr1—V1i3.5140 (14)V2—Sr1v3.9509 (14)
Sr1—V13.5140 (13)V2—Sr1xxiii3.9509 (14)
Sr1—V2iv3.5331 (12)V2—O2xxvi4.024 (5)
Sr1—V23.5331 (12)V2—O2vi4.024 (5)
V1—O2v1.619 (5)V2—O2x4.128 (5)
V1—O3iii1.960 (3)V2—O2xxviii4.128 (5)
V1—O31.960 (3)V2—O3xiii4.157 (3)
V1—O3vi1.960 (3)V2—O3xxix4.157 (3)
V1—O3vii1.960 (3)V2—O3vi4.157 (3)
V1—V1vi2.9560 (10)V2—O3xxvi4.157 (3)
V1—V1viii2.9560 (10)V2—O3xxii4.308 (3)
V1—V2vi3.0144 (14)V2—O3i4.308 (3)
V1—V2iv3.6273 (9)V2—O3xxx4.308 (3)
V1—V23.6273 (9)V2—O3iii4.308 (3)
V1—O2viii3.632 (3)V2—O2xxii4.919 (4)
V1—O2vi3.632 (3)V2—O2xxv4.919 (4)
V1—O23.701 (5)V2—O24.919 (4)
V1—Sr1v3.7264 (13)V2—O2i4.919 (4)
V1—O1vi3.772 (4)V2—O3xxxi4.960 (3)
V1—O1ix3.908 (2)V2—O3xxvii4.960 (3)
V1—O1v3.908 (2)V2—O3v4.960 (3)
V1—O1x3.916 (5)V2—O3xxxii4.960 (3)
V1—O2x3.953 (4)V2—V1xxxiii5.0007 (18)
V1—O2xi3.953 (4)V2—V1xviii5.0007 (18)
V1—Sr1vi4.0347 (10)V2—V2v5.2763 (9)
V1—Sr1viii4.0347 (10)V2—V2xxi5.2763 (9)
V1—O3iv4.145 (3)V2—V2iv5.2909 (8)
V1—O3xii4.145 (3)V2—V2xxii5.2909 (8)
V1—O3i4.166 (3)V2—Sr1xxxiv5.4452 (12)
V1—O3ii4.166 (3)V2—Sr1vi5.4452 (12)
V1—O3xiii4.300 (3)V2—O1ix5.531 (2)
V1—O3viii4.300 (3)V2—O1xxiii5.531 (2)
V1—O3xiv4.369 (3)O1—V2xxi1.613 (6)
V1—O3xv4.369 (3)O1—Sr1xxii2.957 (3)
V1—O3xvi4.790 (3)O1—V1xxvi3.772 (4)
V1—O3v4.790 (3)O1—V1vi3.772 (4)
V1—V1xvii4.8030 (19)O1—V1xxxv3.908 (2)
V1—V1xviii4.8030 (19)O1—V1xxxvi3.908 (2)
V1—O2xix4.906 (5)O1—V1xxxvii3.908 (2)
V1—V1i4.954 (2)O1—V1xxi3.908 (2)
V1—V2xviii5.0007 (18)O1—V1x3.916 (5)
V1—O3xx5.187 (3)O1—V1xxviii3.916 (5)
V1—O3xviii5.187 (3)O2—V1xxi1.619 (5)
V1—O15.261 (5)O2—V1viii3.632 (3)
V1—O1iv5.261 (5)O2—V1vi3.632 (3)
V1—V1xxi5.2763 (9)O2—V2xxxviii3.835 (3)
V1—V1v5.2763 (9)O2—V2xxi3.835 (3)
V1—V1xxii5.2909 (8)O2—V1x3.953 (4)
V1—V1iv5.2909 (8)O2—V1xi3.953 (4)
V1—O2ix5.5331 (16)O2—V2vi4.024 (5)
V1—O2xxiii5.5331 (16)O2—V2x4.128 (5)
V1—O3xxiv5.540 (3)O2—V1xxxvi4.906 (5)
V1—O3xxv5.540 (3)O3—V1vi1.960 (3)
V2—O1v1.613 (6)O3—V1xxii4.145 (3)
V2—O3xii1.977 (3)O3—V2vi4.157 (3)
V2—O3ii1.977 (3)O3—V1i4.166 (3)
V2—O31.977 (3)O3—V1viii4.300 (3)
V2—O3xxv1.977 (3)O3—V2iv4.308 (3)
V2—V1vi3.0144 (14)O3—V1xxvi4.369 (3)
V2—V1xxvi3.0144 (14)O3—V1xxi4.790 (3)
V2—Sr1xxii3.5331 (12)O3—V2xxi4.960 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x, y, z1; (xxii) x1, y, z; (xxiii) x1, y, z+1; (xxiv) x+1, y+3/2, z; (xxv) x1/2, y+3/2, z; (xxvi) x1/2, y+1/2, z+1; (xxvii) x1/2, y+3/2, z+1; (xxviii) x1/2, y+1/2, z; (xxix) x, y+1/2, z+1; (xxx) x1, y+3/2, z; (xxxi) x, y+3/2, z+1; (xxxii) x1/2, y, z+1; (xxxiii) x1/2, y+1/2, z+2; (xxxiv) x, y+2, z+1; (xxxv) x1, y, z1; (xxxvi) x+1/2, y+3/2, z1; (xxxvii) x1/2, y+3/2, z1; (xxxviii) x+1, y, z1.
(SrV3O7_125K) top
Crystal data top
O7V3·SrDx = 3.981 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 11774 reflections
a = 5.2894 (8) Åθ = 3.9–32.1°
b = 10.547 (2) ŵ = 13.63 mm1
c = 5.2697 (9) ÅT = 125 K
V = 293.99 (9) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
331 independent reflections
Radiation source: fine-focus sealed tube321 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.072
Detector resolution: 0 pixels mm-1θmax = 25.6°, θmin = 3.9°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.213, Tmax = 0.567l = 66
5316 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.035Secondary atom site location: difference Fourier map
wR(F2) = 0.082 w = 1/[σ2(Fo2) + (0.0404P)2 + 0.623P]
where P = (Fo2 + 2Fc2)/3
S = 1.34(Δ/σ)max < 0.001
331 reflectionsΔρmax = 0.63 e Å3
24 parametersΔρmin = 0.91 e Å3
Crystal data top
O7V3·SrV = 293.99 (9) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2894 (8) ŵ = 13.63 mm1
b = 10.547 (2) ÅT = 125 K
c = 5.2697 (9) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
331 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
321 reflections with I > 2σ(I)
Tmin = 0.213, Tmax = 0.567Rint = 0.072
5316 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03524 parameters
wR(F2) = 0.0820 restraints
S = 1.34Δρmax = 0.63 e Å3
331 reflectionsΔρmin = 0.91 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14880 (17)0.0138 (3)
V10.25000.51499 (11)0.6214 (2)0.0120 (4)
V20.25000.75000.5930 (3)0.0123 (4)
O10.25000.75000.1008 (13)0.0173 (15)*
O20.25000.5443 (5)0.0765 (9)0.0170 (11)*
O30.0119 (6)0.6209 (3)0.4646 (6)0.0134 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0110 (5)0.0124 (5)0.0181 (5)0.0000.0000.000
V10.0077 (6)0.0107 (6)0.0177 (7)0.0000.0000.0001 (4)
V20.0093 (8)0.0105 (8)0.0170 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.473 (5)V2—V1i3.6278 (9)
Sr1—O2i2.473 (5)V2—V1xxii3.6278 (9)
Sr1—O3i2.558 (3)V2—V1xxv3.6278 (9)
Sr1—O32.558 (3)V2—O13.656 (7)
Sr1—O3ii2.558 (3)V2—O2xix3.839 (4)
Sr1—O3iii2.558 (3)V2—O2xxvii3.839 (4)
Sr1—O12.954 (3)V2—O2xxiii3.839 (4)
Sr1—O1iv2.954 (3)V2—O2v3.839 (4)
Sr1—V1i3.5139 (14)V2—Sr1v3.9462 (14)
Sr1—V13.5139 (14)V2—Sr1xxiii3.9462 (14)
Sr1—V2iv3.5319 (13)V2—O2xxvi4.015 (5)
Sr1—V23.5319 (13)V2—O2vi4.015 (5)
V1—O2v1.622 (5)V2—O2x4.128 (5)
V1—O3vi1.961 (3)V2—O2xxviii4.128 (5)
V1—O3vii1.961 (3)V2—O3xxix4.161 (3)
V1—O3iii1.962 (3)V2—O3xiii4.161 (3)
V1—O31.962 (3)V2—O3xxvi4.161 (3)
V1—V1vi2.9551 (11)V2—O3vi4.161 (3)
V1—V1viii2.9551 (11)V2—O3xxii4.307 (3)
V1—V2vi3.0147 (14)V2—O3i4.307 (3)
V1—O2viii3.624 (3)V2—O3xxx4.307 (3)
V1—O2vi3.624 (3)V2—O3iii4.307 (3)
V1—V2iv3.6278 (9)V2—O2xxii4.914 (4)
V1—V23.6278 (9)V2—O2xxv4.914 (4)
V1—O23.691 (5)V2—O24.914 (4)
V1—Sr1v3.7238 (14)V2—O2i4.914 (4)
V1—O1vi3.767 (5)V2—O3xxxi4.953 (3)
V1—O1ix3.909 (3)V2—O3xxvii4.953 (3)
V1—O1v3.909 (3)V2—O3v4.953 (3)
V1—O1x3.917 (5)V2—O3xxxii4.953 (3)
V1—O2x3.954 (4)V2—V1xxxiii4.9948 (18)
V1—O2xi3.954 (4)V2—V1xviii4.9948 (18)
V1—Sr1vi4.0339 (10)V2—V2v5.2697 (9)
V1—Sr1viii4.0339 (10)V2—V2xxi5.2697 (9)
V1—O3iv4.144 (3)V2—V2iv5.2894 (8)
V1—O3xii4.144 (3)V2—V2xxii5.2894 (8)
V1—O3i4.166 (3)V2—Sr1xxxiv5.4463 (12)
V1—O3ii4.166 (3)V2—Sr1vi5.4463 (12)
V1—O3xiii4.301 (3)V2—O1ix5.530 (2)
V1—O3viii4.301 (3)V2—O1xxiii5.530 (2)
V1—O3xiv4.367 (3)O1—V2xxi1.614 (7)
V1—O3xv4.367 (3)O1—Sr1xxii2.954 (3)
V1—O3xvi4.786 (3)O1—V1xxvi3.767 (4)
V1—O3v4.786 (3)O1—V1vi3.767 (4)
V1—V1xvii4.797 (2)O1—V1xxxv3.909 (3)
V1—V1xviii4.7972 (19)O1—V1xxxvi3.909 (3)
V1—O2xix4.914 (5)O1—V1xxxvii3.909 (3)
V1—V1i4.957 (3)O1—V1xxi3.909 (3)
V1—V2xviii4.9948 (18)O1—V1x3.917 (5)
V1—O3xx5.181 (3)O1—V1xxviii3.917 (5)
V1—O3xviii5.181 (3)O2—V1xxi1.622 (5)
V1—O15.256 (5)O2—V1viii3.624 (3)
V1—O1iv5.256 (5)O2—V1vi3.624 (3)
V1—V1v5.2697 (9)O2—V2xxxviii3.839 (4)
V1—V1xxi5.2697 (9)O2—V2xxi3.839 (4)
V1—V1xxii5.2894 (8)O2—V1x3.954 (4)
V1—V1iv5.2894 (8)O2—V1xi3.954 (4)
V1—O2ix5.5324 (16)O2—V2vi4.015 (5)
V1—O2xxiii5.5324 (16)O2—V2x4.128 (5)
V1—O3xxiv5.539 (3)O2—V2iv4.914 (4)
V1—O3xxv5.539 (3)O3—V1vi1.961 (3)
V2—O1v1.614 (7)O3—V1xxii4.144 (3)
V2—O3xii1.975 (3)O3—V2vi4.161 (3)
V2—O3xxv1.975 (3)O3—V1i4.166 (3)
V2—O3ii1.975 (3)O3—V1viii4.301 (3)
V2—O31.975 (3)O3—V2iv4.307 (3)
V2—V1vi3.0147 (14)O3—V1xxvi4.367 (3)
V2—V1xxvi3.0147 (14)O3—V1xxi4.786 (3)
V2—Sr1xxii3.5319 (13)O3—V2xxi4.953 (3)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x, y, z1; (xxii) x1, y, z; (xxiii) x1, y, z+1; (xxiv) x+1, y+3/2, z; (xxv) x1/2, y+3/2, z; (xxvi) x1/2, y+1/2, z+1; (xxvii) x1/2, y+3/2, z+1; (xxviii) x1/2, y+1/2, z; (xxix) x, y+1/2, z+1; (xxx) x1, y+3/2, z; (xxxi) x, y+3/2, z+1; (xxxii) x1/2, y, z+1; (xxxiii) x1/2, y+1/2, z+2; (xxxiv) x, y+2, z+1; (xxxv) x1, y, z1; (xxxvi) x+1/2, y+3/2, z1; (xxxvii) x1/2, y+3/2, z1; (xxxviii) x+1, y, z1.
(SrV3O7_100K) top
Crystal data top
O7V3·SrDx = 3.977 Mg m3
Mr = 352.44Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PmmnCell parameters from 10067 reflections
a = 5.2918 (12) Åθ = 3.8–32.3°
b = 10.550 (3) ŵ = 13.61 mm1
c = 5.2717 (14) ÅT = 100 K
V = 294.32 (14) Å3Needle, brown
Z = 20.15 × 0.1 × 0.02 mm
F(000) = 326
Data collection top
STOE IPDS 2
diffractometer
321 independent reflections
Radiation source: fine-focus sealed tube307 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.073
Detector resolution: 0 pixels mm-1θmax = 25.5°, θmin = 3.9°
Rotation method scansh = 56
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1212
Tmin = 0.207, Tmax = 0.567l = 66
5327 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.032Secondary atom site location: difference Fourier map
wR(F2) = 0.079 w = 1/[σ2(Fo2) + (0.0396P)2 + 1.0644P]
where P = (Fo2 + 2Fc2)/3
S = 1.24(Δ/σ)max < 0.001
321 reflectionsΔρmax = 0.68 e Å3
24 parametersΔρmin = 1.16 e Å3
Crystal data top
O7V3·SrV = 294.32 (14) Å3
Mr = 352.44Z = 2
Orthorhombic, PmmnMo Kα radiation
a = 5.2918 (12) ŵ = 13.61 mm1
b = 10.550 (3) ÅT = 100 K
c = 5.2717 (14) Å0.15 × 0.1 × 0.02 mm
Data collection top
STOE IPDS 2
diffractometer
321 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
307 reflections with I > 2σ(I)
Tmin = 0.207, Tmax = 0.567Rint = 0.073
5327 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03224 parameters
wR(F2) = 0.0790 restraints
S = 1.24Δρmax = 0.68 e Å3
321 reflectionsΔρmin = 1.16 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sr10.25000.75000.14894 (17)0.0127 (3)
V10.25000.51497 (11)0.6214 (2)0.0114 (4)
V20.25000.75000.5931 (3)0.0114 (4)
O10.25000.75000.1003 (12)0.0143 (15)*
O20.25000.5444 (5)0.0759 (9)0.0156 (11)*
O30.0117 (6)0.6210 (3)0.4651 (6)0.0128 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sr10.0095 (5)0.0113 (5)0.0175 (5)0.0000.0000.000
V10.0073 (6)0.0100 (6)0.0168 (7)0.0000.0000.0000 (4)
V20.0076 (8)0.0096 (8)0.0171 (8)0.0000.0000.000
Bond lengths (Å) top
Sr1—O22.472 (5)V2—Sr1xxii3.5333 (14)
Sr1—O2i2.472 (5)V2—V1xxii3.6293 (11)
Sr1—O3i2.559 (3)V2—V1i3.6293 (11)
Sr1—O3ii2.559 (3)V2—V1xxv3.6293 (11)
Sr1—O3iii2.559 (3)V2—O13.656 (7)
Sr1—O32.559 (3)V2—O2xix3.841 (4)
Sr1—O12.954 (3)V2—O2xxiii3.841 (4)
Sr1—O1iv2.954 (3)V2—O2v3.841 (4)
Sr1—V1i3.5144 (15)V2—O2xxviii3.841 (4)
Sr1—V13.5144 (15)V2—Sr1v3.9479 (16)
Sr1—V2iv3.5333 (14)V2—Sr1xxiii3.9479 (16)
Sr1—V23.5333 (14)V2—O2xxvii4.015 (5)
V1—O2v1.626 (5)V2—O2vi4.015 (5)
V1—O3iii1.962 (3)V2—O2x4.133 (5)
V1—O31.962 (3)V2—O2xxix4.133 (5)
V1—O3vi1.963 (3)V2—O3xiii4.163 (3)
V1—O3vii1.963 (3)V2—O3xxx4.163 (3)
V1—V1vi2.9560 (11)V2—O3vi4.163 (3)
V1—V1viii2.9560 (11)V2—O3xxvii4.163 (3)
V1—V2vi3.0156 (16)V2—O3xxii4.308 (3)
V1—O2viii3.624 (3)V2—O3i4.308 (3)
V1—O2vi3.624 (3)V2—O3xxxi4.308 (3)
V1—V2iv3.6293 (11)V2—O3iii4.308 (3)
V1—V23.6293 (11)V2—O2xxii4.914 (5)
V1—O23.689 (5)V2—O2xxv4.914 (4)
V1—Sr1v3.7261 (15)V2—O24.914 (4)
V1—O1vi3.767 (4)V2—O2i4.914 (5)
V1—O1ix3.912 (3)V2—O3xxxii4.957 (4)
V1—O1v3.912 (3)V2—O3xxviii4.957 (4)
V1—O1x3.919 (5)V2—O3v4.957 (4)
V1—O2x3.958 (4)V2—O3xxxiii4.957 (4)
V1—O2xi3.958 (4)V2—V1xxxiv4.996 (2)
V1—Sr1vi4.0352 (12)V2—V1xviii4.996 (2)
V1—Sr1viii4.0352 (12)V2—V2v5.2717 (14)
V1—O3iv4.146 (3)V2—V2xxi5.2717 (14)
V1—O3xii4.146 (3)V2—V2iv5.2918 (12)
V1—O3i4.165 (4)V2—V2xxii5.2918 (12)
V1—O3ii4.165 (4)V2—Sr1xxxv5.4477 (17)
V1—O3xiii4.303 (3)V2—Sr1vi5.4477 (17)
V1—O3viii4.303 (3)V2—O1ix5.533 (2)
V1—O3xiv4.368 (4)V2—O1xxiii5.533 (2)
V1—O3xv4.368 (4)O1—V2xxi1.616 (7)
V1—O3xvi4.791 (3)O1—O3xxxvi2.948 (6)
V1—O3v4.791 (3)O1—O3xxxvii2.948 (6)
V1—V1xvii4.800 (2)O1—O3xxi2.948 (6)
V1—V1xviii4.800 (2)O1—O3xxxviii2.948 (6)
V1—O2xix4.916 (5)O1—Sr1xxii2.954 (3)
V1—V1i4.959 (3)O1—O3ii3.511 (6)
V1—V2xviii4.996 (2)O1—O3xxv3.511 (6)
V1—O3xx5.181 (4)O1—O33.511 (6)
V1—O3xviii5.181 (4)O1—O3xii3.511 (6)
V1—O15.256 (5)O2—V1xxi1.626 (5)
V1—O1iv5.256 (5)O2—O3xxi2.903 (5)
V1—V1xxi5.2717 (14)O2—O3xxxix2.903 (5)
V1—V1xxii5.2918 (12)O2—O3x2.974 (5)
V1—V1iv5.2918 (12)O2—O3xl2.974 (5)
V1—O2ix5.5360 (19)O2—O3iii3.272 (5)
V1—O2xxiii5.5360 (19)O2—O33.272 (5)
V1—O3xxiv5.540 (3)O2—V1viii3.624 (3)
V1—O3xxv5.540 (3)O2—V1vi3.624 (3)
V1—V1xxvi5.591 (3)O2—V2xli3.841 (4)
V2—O1v1.616 (7)O3—V1vi1.963 (3)
V2—O3xii1.974 (3)O3—O3xii2.522 (6)
V2—O3ii1.974 (3)O3—O3vi2.582 (6)
V2—O3xxv1.974 (3)O3—O3ii2.722 (6)
V2—O31.974 (3)O3—O3iii2.770 (6)
V2—V1vi3.0156 (15)O3—O2v2.903 (5)
V2—V1xxvii3.0156 (16)O3—O1v2.948 (6)
Symmetry codes: (i) x+1/2, y+3/2, z; (ii) x, y+3/2, z; (iii) x+1/2, y, z; (iv) x+1, y, z; (v) x, y, z+1; (vi) x, y+1, z+1; (vii) x+1/2, y+1, z+1; (viii) x+1, y+1, z+1; (ix) x+1, y, z+1; (x) x, y+1, z; (xi) x+1, y+1, z; (xii) x1/2, y, z; (xiii) x1/2, y+1, z+1; (xiv) x, y1/2, z+1; (xv) x+1/2, y1/2, z+1; (xvi) x+1/2, y, z+1; (xvii) x+1, y+1, z+2; (xviii) x, y+1, z+2; (xix) x+1/2, y+3/2, z+1; (xx) x+1/2, y+1, z+2; (xxi) x, y, z1; (xxii) x1, y, z; (xxiii) x1, y, z+1; (xxiv) x+1, y+3/2, z; (xxv) x1/2, y+3/2, z; (xxvi) x+1/2, y+1/2, z; (xxvii) x1/2, y+1/2, z+1; (xxviii) x1/2, y+3/2, z+1; (xxix) x1/2, y+1/2, z; (xxx) x, y+1/2, z+1; (xxxi) x1, y+3/2, z; (xxxii) x, y+3/2, z+1; (xxxiii) x1/2, y, z+1; (xxxiv) x1/2, y+1/2, z+2; (xxxv) x, y+2, z+1; (xxxvi) x1/2, y, z1; (xxxvii) x1/2, y+3/2, z1; (xxxviii) x, y+3/2, z1; (xxxix) x+1/2, y, z1; (xl) x+1/2, y+1, z; (xli) x+1, y, z1.
(CaV3O7_297K) top
Crystal data top
O7V3·CaF(000) = 580
Mr = 304.90Dx = 3.537 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2764 reflections
a = 10.446 (3) Åθ = 1.3–23.4°
b = 10.365 (2) ŵ = 5.67 mm1
c = 5.2889 (15) ÅT = 297 K
V = 572.6 (3) Å3, brown
Z = 40.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
389 independent reflections
Radiation source: fine-focus sealed tube365 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
Detector resolution: 0 pixels mm-1θmax = 22.9°, θmin = 3.9°
Rotation method scansh = 1111
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1010
Tmin = 0.319, Tmax = 0.471l = 55
2489 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020 w = 1/[σ2(Fo2) + (0.0331P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.054(Δ/σ)max < 0.001
S = 1.28Δρmax = 0.36 e Å3
389 reflectionsΔρmin = 0.31 e Å3
38 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.020 (2)
Crystal data top
O7V3·CaV = 572.6 (3) Å3
Mr = 304.90Z = 4
Orthorhombic, PnmaMo Kα radiation
a = 10.446 (3) ŵ = 5.67 mm1
b = 10.365 (2) ÅT = 297 K
c = 5.2889 (15) Å0.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
389 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
365 reflections with I > 2σ(I)
Tmin = 0.319, Tmax = 0.471Rint = 0.030
2489 measured reflectionsθmax = 22.9°
Refinement top
R[F2 > 2σ(F2)] = 0.02038 parameters
wR(F2) = 0.0540 restraints
S = 1.28Δρmax = 0.36 e Å3
389 reflectionsΔρmin = 0.31 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.08454 (9)0.25000.29937 (14)0.0090 (3)
V10.28850 (7)0.25000.79190 (12)0.0069 (3)
V20.18751 (5)0.52039 (6)0.78356 (9)0.0071 (3)
O10.4431 (3)0.25000.8079 (5)0.0138 (8)*
O20.0405 (2)0.5653 (3)0.7673 (4)0.0162 (6)*
O30.22034 (19)0.3799 (2)0.0257 (4)0.0085 (5)*
O40.22625 (18)0.3796 (2)0.5483 (4)0.0085 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0071 (5)0.0093 (6)0.0106 (5)0.0000.0004 (3)0.000
V10.0074 (5)0.0066 (6)0.0069 (5)0.0000.0005 (3)0.000
V20.0077 (4)0.0066 (4)0.0071 (4)0.0010 (2)0.0002 (2)0.00028 (19)
Geometric parameters (Å, º) top
Ca1—O2i2.344 (3)Ca1—O14.611 (3)
Ca1—O2ii2.344 (3)V1—O11.617 (3)
Ca1—O42.393 (2)V1—O3xi1.962 (2)
Ca1—O4iii2.393 (2)V1—O3xii1.962 (2)
Ca1—O3iii2.433 (2)V1—O4iii1.972 (2)
Ca1—O32.433 (2)V1—O41.972 (2)
Ca1—O1iv2.549 (3)V1—V2iii2.9948 (9)
Ca1—V13.3653 (12)V1—V22.9948 (9)
Ca1—V2v3.3676 (11)V1—Ca1xi3.4268 (13)
Ca1—V2vi3.3676 (11)V1—Ca1xv3.7732 (14)
Ca1—V1vii3.4268 (13)V1—Ca1xvi4.3981 (14)
Ca1—O1viii3.536 (3)V1—Ca1xiii5.3494 (12)
Ca1—V2i3.7326 (11)V2—O21.607 (2)
Ca1—V2ii3.7326 (11)V2—O41.960 (2)
Ca1—V1iv3.7732 (14)V2—O4xiii1.961 (2)
Ca1—V23.9457 (10)V2—O3xiii1.963 (2)
Ca1—V2iii3.9457 (10)V2—O3xi1.969 (2)
Ca1—V2ix4.0562 (10)V2—V2xiii2.9793 (9)
Ca1—V2vii4.0562 (10)V2—V2v2.9793 (9)
Ca1—O24.125 (3)V2—Ca1xiii3.3676 (11)
Ca1—O2iii4.125 (3)V2—Ca1ii3.7326 (11)
Ca1—O3x4.141 (2)V2—Ca1xi4.0562 (10)
Ca1—O3viii4.141 (2)O1—Ca1xv2.549 (3)
Ca1—O3xi4.311 (2)O1—Ca1xvi3.536 (3)
Ca1—O3xii4.311 (2)O1—Ca1xi4.559 (3)
Ca1—O2ix4.337 (3)O2—Ca1ii2.344 (3)
Ca1—O2vii4.337 (3)O2—Ca1xi4.337 (3)
Ca1—O2v4.362 (3)O2—Ca1xiii4.362 (3)
Ca1—O2vi4.362 (3)O3—V1vii1.962 (2)
Ca1—O4x4.381 (2)O3—V2v1.963 (2)
Ca1—O4viii4.381 (2)O3—V2vii1.969 (2)
Ca1—V1viii4.3981 (14)O3—Ca1xvi4.141 (2)
Ca1—O4ix4.447 (2)O3—Ca1vii4.311 (2)
Ca1—O4vii4.447 (2)O3—Ca1v4.505 (2)
Ca1—O3xiii4.505 (2)O4—V2v1.961 (2)
Ca1—O3xiv4.505 (2)O4—Ca1xvi4.381 (2)
Ca1—O4vi4.518 (2)O4—Ca1xi4.447 (2)
Ca1—O4v4.518 (2)O4—Ca1xiii4.518 (2)
Ca1—O1vii4.559 (3)O4—Ca1ii5.092 (2)
O2i—Ca1—O2ii109.47 (12)O2vii—Ca1—V1viii57.60 (3)
O2i—Ca1—O4152.33 (8)O2v—Ca1—V1viii127.13 (3)
O2ii—Ca1—O488.24 (7)O2vi—Ca1—V1viii127.13 (3)
O2i—Ca1—O4iii88.24 (7)O4x—Ca1—V1viii25.95 (3)
O2ii—Ca1—O4iii152.33 (8)O4viii—Ca1—V1viii25.95 (3)
O4—Ca1—O4iii68.27 (10)O2i—Ca1—O4ix78.74 (6)
O2i—Ca1—O3iii77.50 (7)O2ii—Ca1—O4ix107.33 (6)
O2ii—Ca1—O3iii133.43 (8)O4—Ca1—O4ix117.06 (7)
O4—Ca1—O3iii106.09 (8)O4iii—Ca1—O4ix96.66 (6)
O4iii—Ca1—O3iii69.88 (7)O3iii—Ca1—O4ix26.81 (5)
O2i—Ca1—O3133.43 (8)O3—Ca1—O4ix56.07 (6)
O2ii—Ca1—O377.50 (7)O1iv—Ca1—O4ix157.05 (5)
O4—Ca1—O369.88 (7)V1—Ca1—O4ix118.73 (4)
O4iii—Ca1—O3106.09 (8)V2v—Ca1—O4ix87.47 (3)
O3iii—Ca1—O367.22 (10)V2vi—Ca1—O4ix61.90 (3)
O2i—Ca1—O1iv78.42 (7)V1vii—Ca1—O4ix24.96 (3)
O2ii—Ca1—O1iv78.42 (7)O1viii—Ca1—O4ix47.75 (6)
O4—Ca1—O1iv84.86 (8)V2i—Ca1—O4ix87.47 (3)
O4iii—Ca1—O1iv84.86 (8)V2ii—Ca1—O4ix109.94 (3)
O3iii—Ca1—O1iv145.35 (5)V1iv—Ca1—O4ix141.69 (3)
O3—Ca1—O1iv145.35 (5)V2—Ca1—O4ix134.71 (3)
O2i—Ca1—V1117.99 (6)V2iii—Ca1—O4ix105.93 (3)
O2ii—Ca1—V1117.99 (6)V2ix—Ca1—O4ix26.14 (3)
O4—Ca1—V135.18 (5)V2vii—Ca1—O4ix61.29 (3)
O4iii—Ca1—V135.18 (5)O2—Ca1—O4ix144.32 (4)
O3iii—Ca1—V195.24 (6)O2iii—Ca1—O4ix109.49 (4)
O3—Ca1—V195.24 (6)O3x—Ca1—O4ix114.03 (4)
O1iv—Ca1—V174.71 (7)O3viii—Ca1—O4ix127.13 (4)
O2i—Ca1—V2v165.34 (6)O3xi—Ca1—O4ix141.34 (5)
O2ii—Ca1—V2v79.25 (6)O3xii—Ca1—O4ix126.31 (5)
O4—Ca1—V2v34.89 (5)O2ix—Ca1—O4ix39.48 (4)
O4iii—Ca1—V2v88.45 (6)O2vii—Ca1—O4ix71.53 (4)
O3iii—Ca1—V2v87.95 (6)O2v—Ca1—O4ix78.40 (4)
O3—Ca1—V2v35.10 (5)O2vi—Ca1—O4ix62.22 (4)
O1iv—Ca1—V2v115.48 (5)O4x—Ca1—O4ix79.45 (3)
V1—Ca1—V2v64.63 (2)O4viii—Ca1—O4ix90.12 (3)
O2i—Ca1—V2vi79.25 (6)V1viii—Ca1—O4ix66.35 (3)
O2ii—Ca1—V2vi165.34 (6)O2i—Ca1—O4vii107.33 (6)
O4—Ca1—V2vi88.45 (6)O2ii—Ca1—O4vii78.74 (6)
O4iii—Ca1—V2vi34.89 (5)O4—Ca1—O4vii96.66 (6)
O3iii—Ca1—V2vi35.10 (5)O4iii—Ca1—O4vii117.06 (7)
O3—Ca1—V2vi87.95 (6)O3iii—Ca1—O4vii56.07 (6)
O1iv—Ca1—V2vi115.48 (5)O3—Ca1—O4vii26.81 (5)
V1—Ca1—V2vi64.63 (2)O1iv—Ca1—O4vii157.05 (5)
V2v—Ca1—V2vi89.93 (4)V1—Ca1—O4vii118.73 (4)
O2i—Ca1—V1vii103.23 (5)V2v—Ca1—O4vii61.90 (3)
O2ii—Ca1—V1vii103.23 (5)V2vi—Ca1—O4vii87.47 (3)
O4—Ca1—V1vii92.65 (6)V1vii—Ca1—O4vii24.96 (3)
O4iii—Ca1—V1vii92.65 (6)O1viii—Ca1—O4vii47.75 (6)
O3iii—Ca1—V1vii34.07 (5)V2i—Ca1—O4vii109.94 (3)
O3—Ca1—V1vii34.07 (5)V2ii—Ca1—O4vii87.47 (3)
O1iv—Ca1—V1vii176.99 (8)V1iv—Ca1—O4vii141.69 (3)
V1—Ca1—V1vii102.28 (4)V2—Ca1—O4vii105.93 (3)
V2v—Ca1—V1vii62.67 (2)V2iii—Ca1—O4vii134.71 (3)
V2vi—Ca1—V1vii62.67 (2)V2ix—Ca1—O4vii61.29 (3)
O2i—Ca1—O1viii68.31 (6)V2vii—Ca1—O4vii26.14 (3)
O2ii—Ca1—O1viii68.31 (6)O2—Ca1—O4vii109.49 (5)
O4—Ca1—O1viii139.31 (6)O2iii—Ca1—O4vii144.32 (4)
O4iii—Ca1—O1viii139.31 (6)O3x—Ca1—O4vii127.13 (4)
O3iii—Ca1—O1viii72.74 (6)O3viii—Ca1—O4vii114.03 (4)
O3—Ca1—O1viii72.74 (6)O3xi—Ca1—O4vii126.31 (5)
O1iv—Ca1—O1viii119.86 (11)O3xii—Ca1—O4vii141.34 (5)
V1—Ca1—O1viii165.43 (6)O2ix—Ca1—O4vii71.53 (4)
V2v—Ca1—O1viii105.84 (4)O2vii—Ca1—O4vii39.48 (4)
V2vi—Ca1—O1viii105.84 (4)O2v—Ca1—O4vii62.22 (4)
V1vii—Ca1—O1viii63.15 (6)O2vi—Ca1—O4vii78.40 (4)
O2i—Ca1—V2i15.71 (6)O4x—Ca1—O4vii90.12 (3)
O2ii—Ca1—V2i94.50 (7)O4viii—Ca1—O4vii79.45 (3)
O4—Ca1—V2i153.29 (5)V1viii—Ca1—O4vii66.35 (3)
O4iii—Ca1—V2i100.24 (5)O4ix—Ca1—O4vii35.16 (5)
O3iii—Ca1—V2i91.21 (5)O2i—Ca1—O3xiii170.83 (6)
O3—Ca1—V2i136.62 (6)O2ii—Ca1—O3xiii66.24 (7)
O1iv—Ca1—V2i69.78 (5)O4—Ca1—O3xiii25.35 (5)
V1—Ca1—V2i124.96 (2)O4iii—Ca1—O3xiii92.96 (6)
V2v—Ca1—V2i170.40 (2)O3iii—Ca1—O3xiii111.44 (4)
V2vi—Ca1—V2i94.87 (2)O3—Ca1—O3xiii54.77 (4)
V1vii—Ca1—V2i112.42 (2)O1iv—Ca1—O3xiii92.62 (5)
O1viii—Ca1—V2i64.85 (4)V1—Ca1—O3xiii60.52 (3)
O2i—Ca1—V2ii94.50 (7)V2v—Ca1—O3xiii23.81 (3)
O2ii—Ca1—V2ii15.71 (6)V2vi—Ca1—O3xiii106.76 (4)
O4—Ca1—V2ii100.24 (5)V1vii—Ca1—O3xiii85.80 (3)
O4iii—Ca1—V2ii153.29 (5)O1viii—Ca1—O3xiii115.50 (3)
O3iii—Ca1—V2ii136.62 (6)V2i—Ca1—O3xiii156.70 (3)
O3—Ca1—V2ii91.21 (5)V2ii—Ca1—O3xiii80.38 (3)
O1iv—Ca1—V2ii69.78 (5)V1iv—Ca1—O3xiii102.63 (3)
V1—Ca1—V2ii124.96 (2)V2—Ca1—O3xiii25.79 (3)
V2v—Ca1—V2ii94.87 (2)V2iii—Ca1—O3xiii107.99 (3)
V2vi—Ca1—V2ii170.40 (2)V2ix—Ca1—O3xiii130.31 (3)
V1vii—Ca1—V2ii112.42 (2)V2vii—Ca1—O3xiii58.03 (3)
O1viii—Ca1—V2ii64.85 (4)O2—Ca1—O3xiii38.42 (4)
V2i—Ca1—V2ii79.22 (3)O2iii—Ca1—O3xiii124.44 (5)
O2i—Ca1—V1iv68.24 (6)O3x—Ca1—O3xiii129.29 (4)
O2ii—Ca1—V1iv68.24 (6)O3viii—Ca1—O3xiii94.56 (4)
O4—Ca1—V1iv101.06 (5)O3xi—Ca1—O3xiii49.34 (4)
O4iii—Ca1—V1iv101.06 (5)O3xii—Ca1—O3xiii83.13 (3)
O3iii—Ca1—V1iv144.94 (5)O2ix—Ca1—O3xiii149.52 (4)
O3—Ca1—V1iv144.94 (5)O2vii—Ca1—O3xiii65.09 (4)
O1iv—Ca1—V1iv19.61 (7)O2v—Ca1—O3xiii39.71 (4)
V1—Ca1—V1iv94.33 (3)O2vi—Ca1—O3xiii88.72 (5)
V2v—Ca1—V1iv126.43 (2)O4x—Ca1—O3xiii139.38 (4)
V2vi—Ca1—V1iv126.43 (2)O4viii—Ca1—O3xiii103.71 (4)
V1vii—Ca1—V1iv163.40 (3)V1viii—Ca1—O3xiii120.47 (3)
O1viii—Ca1—V1iv100.25 (6)O4ix—Ca1—O3xiii110.11 (4)
V2i—Ca1—V1iv56.17 (2)O4vii—Ca1—O3xiii80.19 (4)
V2ii—Ca1—V1iv56.17 (2)O2i—Ca1—O3xiv66.24 (7)
O2i—Ca1—V2146.04 (6)O2ii—Ca1—O3xiv170.83 (6)
O2ii—Ca1—V270.71 (6)O4—Ca1—O3xiv92.96 (6)
O4—Ca1—V222.46 (5)O4iii—Ca1—O3xiv25.35 (5)
O4iii—Ca1—V282.70 (5)O3iii—Ca1—O3xiv54.77 (4)
O3iii—Ca1—V2128.33 (6)O3—Ca1—O3xiv111.44 (4)
O3—Ca1—V280.44 (5)O1iv—Ca1—O3xiv92.62 (5)
O1iv—Ca1—V268.24 (5)V1—Ca1—O3xiv60.52 (3)
V1—Ca1—V247.548 (15)V2v—Ca1—O3xiv106.76 (4)
V2v—Ca1—V247.268 (14)V2vi—Ca1—O3xiv23.81 (3)
V2vi—Ca1—V2108.98 (3)V1vii—Ca1—O3xiv85.80 (3)
V1vii—Ca1—V2109.81 (3)O1viii—Ca1—O3xiv115.50 (3)
O1viii—Ca1—V2134.712 (15)V2i—Ca1—O3xiv80.38 (3)
V2i—Ca1—V2137.45 (2)V2ii—Ca1—O3xiv156.70 (3)
V2ii—Ca1—V280.27 (2)V1iv—Ca1—O3xiv102.63 (3)
V1iv—Ca1—V281.47 (2)V2—Ca1—O3xiv107.99 (3)
O2i—Ca1—V2iii70.71 (6)V2iii—Ca1—O3xiv25.79 (3)
O2ii—Ca1—V2iii146.04 (6)V2ix—Ca1—O3xiv58.03 (3)
O4—Ca1—V2iii82.70 (5)V2vii—Ca1—O3xiv130.31 (3)
O4iii—Ca1—V2iii22.46 (5)O2—Ca1—O3xiv124.44 (5)
O3iii—Ca1—V2iii80.44 (5)O2iii—Ca1—O3xiv38.42 (4)
O3—Ca1—V2iii128.33 (6)O3x—Ca1—O3xiv94.56 (4)
O1iv—Ca1—V2iii68.24 (5)O3viii—Ca1—O3xiv129.29 (4)
V1—Ca1—V2iii47.548 (15)O3xi—Ca1—O3xiv83.13 (3)
V2v—Ca1—V2iii108.98 (3)O3xii—Ca1—O3xiv49.34 (4)
V2vi—Ca1—V2iii47.268 (14)O2ix—Ca1—O3xiv65.09 (4)
V1vii—Ca1—V2iii109.81 (3)O2vii—Ca1—O3xiv149.52 (4)
O1viii—Ca1—V2iii134.712 (15)O2v—Ca1—O3xiv88.72 (5)
V2i—Ca1—V2iii80.27 (2)O2vi—Ca1—O3xiv39.71 (4)
V2ii—Ca1—V2iii137.45 (2)O4x—Ca1—O3xiv103.71 (4)
V1iv—Ca1—V2iii81.47 (2)O4viii—Ca1—O3xiv139.38 (4)
V2—Ca1—V2iii90.51 (3)V1viii—Ca1—O3xiv120.47 (3)
O2i—Ca1—V2ix58.84 (5)O4ix—Ca1—O3xiv80.19 (4)
O2ii—Ca1—V2ix127.65 (6)O4vii—Ca1—O3xiv110.11 (4)
O4—Ca1—V2ix126.41 (6)O3xiii—Ca1—O3xiv116.71 (5)
O4iii—Ca1—V2ix79.53 (5)O2i—Ca1—O4vi60.39 (6)
O3iii—Ca1—V2ix20.44 (5)O2ii—Ca1—O4vi153.32 (6)
O3—Ca1—V2ix80.08 (5)O4—Ca1—O4vi111.59 (4)
O1iv—Ca1—V2ix134.57 (2)O4iii—Ca1—O4vi54.14 (4)
V1—Ca1—V2ix110.65 (3)O3iii—Ca1—O4vi25.81 (5)
V2v—Ca1—V2ix106.50 (3)O3—Ca1—O4vi92.32 (6)
V2vi—Ca1—V2ix46.175 (14)O1iv—Ca1—O4vi119.55 (3)
V1vii—Ca1—V2ix46.240 (15)V1—Ca1—O4vi87.17 (3)
O1viii—Ca1—V2ix59.99 (3)V2v—Ca1—O4vi106.49 (4)
V2i—Ca1—V2ix71.48 (2)V2vi—Ca1—O4vi23.48 (3)
V2ii—Ca1—V2ix124.29 (2)V1vii—Ca1—O4vi59.85 (3)
V1iv—Ca1—V2ix127.06 (2)O1viii—Ca1—O4vi85.17 (4)
V2—Ca1—V2ix148.75 (3)V2i—Ca1—O4vi75.92 (3)
V2iii—Ca1—V2ix82.73 (2)V2ii—Ca1—O4vi147.18 (3)
O2i—Ca1—V2vii127.65 (6)V1iv—Ca1—O4vi121.80 (3)
O2ii—Ca1—V2vii58.84 (5)V2—Ca1—O4vi132.46 (4)
O4—Ca1—V2vii79.53 (5)V2iii—Ca1—O4vi57.85 (3)
O4iii—Ca1—V2vii126.41 (6)V2ix—Ca1—O4vi25.73 (3)
O3iii—Ca1—V2vii80.08 (5)V2vii—Ca1—O4vi105.87 (3)
O3—Ca1—V2vii20.44 (5)O2—Ca1—O4vi153.95 (5)
O1iv—Ca1—V2vii134.57 (2)O2iii—Ca1—O4vi63.37 (4)
V1—Ca1—V2vii110.65 (3)O3x—Ca1—O4vi101.03 (4)
V2v—Ca1—V2vii46.175 (14)O3viii—Ca1—O4vi138.08 (4)
V2vi—Ca1—V2vii106.50 (3)O3xi—Ca1—O4vi112.55 (4)
V1vii—Ca1—V2vii46.240 (15)O3xii—Ca1—O4vi81.52 (4)
O1viii—Ca1—V2vii59.99 (3)O2ix—Ca1—O4vi38.31 (4)
V2i—Ca1—V2vii124.29 (2)O2vii—Ca1—O4vi119.73 (4)
V2ii—Ca1—V2vii71.48 (2)O2v—Ca1—O4vi88.20 (5)
V1iv—Ca1—V2vii127.06 (2)O2vi—Ca1—O4vi39.01 (4)
V2—Ca1—V2vii82.73 (2)O4x—Ca1—O4vi89.42 (4)
V2iii—Ca1—V2vii148.75 (3)O4viii—Ca1—O4vi120.72 (4)
V2ix—Ca1—V2vii87.40 (3)V1viii—Ca1—O4vi95.66 (3)
O2i—Ca1—O2132.45 (4)O4ix—Ca1—O4vi48.33 (4)
O2ii—Ca1—O251.77 (7)O4vii—Ca1—O4vi81.28 (3)
O4—Ca1—O245.12 (6)O3xiii—Ca1—O4vi127.13 (4)
O4iii—Ca1—O2100.58 (6)O3xiv—Ca1—O4vi32.51 (3)
O3iii—Ca1—O2149.35 (6)O2i—Ca1—O4v153.32 (6)
O3—Ca1—O289.04 (6)O2ii—Ca1—O4v60.39 (6)
O1iv—Ca1—O256.40 (4)O4—Ca1—O4v54.14 (4)
V1—Ca1—O266.81 (3)O4iii—Ca1—O4v111.59 (4)
V2v—Ca1—O262.21 (3)O3iii—Ca1—O4v92.32 (6)
V2vi—Ca1—O2130.81 (4)O3—Ca1—O4v25.81 (5)
V1vii—Ca1—O2122.62 (4)O1iv—Ca1—O4v119.55 (3)
O1viii—Ca1—O2119.89 (4)V1—Ca1—O4v87.17 (3)
V2i—Ca1—O2119.39 (4)V2v—Ca1—O4v23.48 (3)
V2ii—Ca1—O258.70 (3)V2vi—Ca1—O4v106.49 (4)
V1iv—Ca1—O264.21 (4)V1vii—Ca1—O4v59.85 (3)
V2—Ca1—O222.83 (3)O1viii—Ca1—O4v85.17 (4)
V2iii—Ca1—O2101.76 (4)V2i—Ca1—O4v147.18 (3)
V2ix—Ca1—O2168.64 (4)V2ii—Ca1—O4v75.92 (3)
V2vii—Ca1—O283.43 (4)V1iv—Ca1—O4v121.80 (3)
O2i—Ca1—O2iii51.77 (7)V2—Ca1—O4v57.85 (3)
O2ii—Ca1—O2iii132.45 (4)V2iii—Ca1—O4v132.46 (4)
O4—Ca1—O2iii100.58 (6)V2ix—Ca1—O4v105.87 (3)
O4iii—Ca1—O2iii45.12 (6)V2vii—Ca1—O4v25.73 (3)
O3iii—Ca1—O2iii89.04 (6)O2—Ca1—O4v63.37 (4)
O3—Ca1—O2iii149.35 (6)O2iii—Ca1—O4v153.95 (5)
O1iv—Ca1—O2iii56.40 (4)O3x—Ca1—O4v138.08 (4)
V1—Ca1—O2iii66.81 (3)O3viii—Ca1—O4v101.03 (4)
V2v—Ca1—O2iii130.81 (4)O3xi—Ca1—O4v81.52 (4)
V2vi—Ca1—O2iii62.21 (3)O3xii—Ca1—O4v112.55 (4)
V1vii—Ca1—O2iii122.62 (4)O2ix—Ca1—O4v119.73 (4)
O1viii—Ca1—O2iii119.89 (4)O2vii—Ca1—O4v38.31 (4)
V2i—Ca1—O2iii58.70 (3)O2v—Ca1—O4v39.01 (4)
V2ii—Ca1—O2iii119.39 (4)O2vi—Ca1—O4v88.20 (5)
V1iv—Ca1—O2iii64.21 (4)O4x—Ca1—O4v120.72 (4)
V2—Ca1—O2iii101.76 (4)O4viii—Ca1—O4v89.42 (4)
V2iii—Ca1—O2iii22.83 (3)V1viii—Ca1—O4v95.66 (3)
V2ix—Ca1—O2iii83.43 (4)O4ix—Ca1—O4v81.28 (3)
V2vii—Ca1—O2iii168.64 (4)O4vii—Ca1—O4v48.33 (4)
O2—Ca1—O2iii104.80 (7)O3xiii—Ca1—O4v32.51 (3)
O2i—Ca1—O3x41.91 (6)O3xiv—Ca1—O4v127.13 (4)
O2ii—Ca1—O3x77.70 (7)O4vi—Ca1—O4v116.38 (5)
O4—Ca1—O3x128.90 (6)O2i—Ca1—O1vii111.86 (6)
O4iii—Ca1—O3x105.24 (6)O2ii—Ca1—O1vii111.86 (6)
O3iii—Ca1—O3x119.24 (7)O4—Ca1—O1vii78.78 (6)
O3—Ca1—O3x148.06 (6)O4iii—Ca1—O1vii78.78 (6)
O1iv—Ca1—O3x44.38 (7)O3iii—Ca1—O1vii35.11 (5)
V1—Ca1—O3x114.13 (4)O3—Ca1—O1vii35.11 (5)
V2v—Ca1—O3x152.27 (3)O1iv—Ca1—O1vii160.19 (8)
V2vi—Ca1—O3x115.18 (3)V1—Ca1—O1vii85.48 (5)
V1vii—Ca1—O3x138.27 (3)V2v—Ca1—O1vii53.48 (3)
O1viii—Ca1—O3x79.57 (6)V2vi—Ca1—O1vii53.48 (3)
V2i—Ca1—O3x28.27 (3)V1vii—Ca1—O1vii16.80 (4)
V2ii—Ca1—O3x62.23 (4)O1viii—Ca1—O1vii79.95 (4)
V1iv—Ca1—O3x28.22 (3)V2i—Ca1—O1vii123.95 (3)
V2—Ca1—O3x109.66 (3)V2ii—Ca1—O1vii123.95 (3)
V2iii—Ca1—O3x82.79 (3)V1iv—Ca1—O1vii179.81 (4)
V2ix—Ca1—O3x99.74 (3)V2—Ca1—O1vii98.40 (3)
V2vii—Ca1—O3x128.22 (4)V2iii—Ca1—O1vii98.40 (3)
O2—Ca1—O3x91.22 (5)V2ix—Ca1—O1vii53.04 (2)
O2iii—Ca1—O3x60.39 (4)V2vii—Ca1—O1vii53.04 (2)
O2i—Ca1—O3viii77.70 (7)O2—Ca1—O1vii115.69 (4)
O2ii—Ca1—O3viii41.91 (6)O2iii—Ca1—O1vii115.69 (4)
O4—Ca1—O3viii105.24 (6)O3x—Ca1—O1vii151.92 (4)
O4iii—Ca1—O3viii128.90 (6)O3viii—Ca1—O1vii151.92 (4)
O3iii—Ca1—O3viii148.06 (6)O3xi—Ca1—O1vii103.75 (5)
O3—Ca1—O3viii119.24 (7)O3xii—Ca1—O1vii103.75 (5)
O1iv—Ca1—O3viii44.38 (7)O2ix—Ca1—O1vii73.57 (4)
V1—Ca1—O3viii114.13 (4)O2vii—Ca1—O1vii73.57 (4)
V2v—Ca1—O3viii115.18 (3)O2v—Ca1—O1vii40.56 (4)
V2vi—Ca1—O3viii152.27 (3)O2vi—Ca1—O1vii40.56 (4)
V1vii—Ca1—O3viii138.27 (3)O4x—Ca1—O1vii117.55 (5)
O1viii—Ca1—O3viii79.57 (6)O4viii—Ca1—O1vii117.55 (5)
V2i—Ca1—O3viii62.23 (4)V1viii—Ca1—O1vii99.92 (5)
V2ii—Ca1—O3viii28.27 (3)O4ix—Ca1—O1vii38.48 (4)
V1iv—Ca1—O3viii28.22 (3)O4vii—Ca1—O1vii38.48 (4)
V2—Ca1—O3viii82.79 (3)O3xiii—Ca1—O1vii77.28 (3)
V2iii—Ca1—O3viii109.66 (3)O3xiv—Ca1—O1vii77.28 (3)
V2ix—Ca1—O3viii128.22 (4)O4vi—Ca1—O1vii58.20 (3)
V2vii—Ca1—O3viii99.74 (3)O4v—Ca1—O1vii58.20 (3)
O2—Ca1—O3viii60.39 (4)O2i—Ca1—O1122.72 (6)
O2iii—Ca1—O3viii91.22 (5)O2ii—Ca1—O1122.72 (6)
O3x—Ca1—O3viii37.96 (6)O4—Ca1—O134.59 (5)
O2i—Ca1—O3xi124.92 (6)O4iii—Ca1—O134.59 (5)
O2ii—Ca1—O3xi93.57 (6)O3iii—Ca1—O182.73 (6)
O4—Ca1—O3xi29.66 (5)O3—Ca1—O182.73 (6)
O4iii—Ca1—O3xi58.78 (6)O1iv—Ca1—O189.75 (5)
O3iii—Ca1—O3xi120.74 (7)V1—Ca1—O115.04 (4)
O3—Ca1—O3xi99.51 (7)V2v—Ca1—O155.95 (3)
O1iv—Ca1—O3xi57.64 (7)V2vi—Ca1—O155.95 (3)
V1—Ca1—O3xi26.09 (3)V1vii—Ca1—O187.24 (5)
V2v—Ca1—O3xi64.45 (3)O1viii—Ca1—O1150.39 (7)
V2vi—Ca1—O3xi90.59 (3)V2i—Ca1—O1133.39 (2)
V1vii—Ca1—O3xi119.56 (4)V2ii—Ca1—O1133.39 (3)
O1viii—Ca1—O3xi161.28 (3)V1iv—Ca1—O1109.36 (5)
V2i—Ca1—O3xi123.67 (4)V2—Ca1—O153.13 (2)
V2ii—Ca1—O3xi98.98 (3)V2iii—Ca1—O153.13 (2)
V1iv—Ca1—O3xi76.06 (4)V2ix—Ca1—O1100.19 (3)
V2—Ca1—O3xi27.13 (3)V2vii—Ca1—O1100.19 (3)
V2iii—Ca1—O3xi63.50 (3)O2—Ca1—O174.96 (4)
V2ix—Ca1—O3xi136.71 (4)O2iii—Ca1—O174.96 (4)
V2vii—Ca1—O3xi107.23 (3)O3x—Ca1—O1128.02 (5)
O2—Ca1—O3xi41.80 (4)O3viii—Ca1—O1128.02 (5)
O2iii—Ca1—O3xi75.50 (5)O3xi—Ca1—O138.09 (4)
O3x—Ca1—O3xi101.82 (4)O3xii—Ca1—O138.09 (4)
O3viii—Ca1—O3xi90.09 (3)O2ix—Ca1—O1117.68 (4)
O2i—Ca1—O3xii93.57 (6)O2vii—Ca1—O1117.68 (4)
O2ii—Ca1—O3xii124.92 (6)O2v—Ca1—O145.05 (4)
O4—Ca1—O3xii58.78 (6)O2vi—Ca1—O145.05 (4)
O4iii—Ca1—O3xii29.66 (5)O4x—Ca1—O1159.84 (3)
O3iii—Ca1—O3xii99.51 (7)O4viii—Ca1—O1159.84 (3)
O3—Ca1—O3xii120.74 (7)V1viii—Ca1—O1170.37 (4)
O1iv—Ca1—O3xii57.64 (7)O4ix—Ca1—O1104.52 (5)
V1—Ca1—O3xii26.09 (3)O4vii—Ca1—O1104.52 (5)
V2v—Ca1—O3xii90.59 (3)O3xiii—Ca1—O158.50 (3)
V2vi—Ca1—O3xii64.45 (3)O3xiv—Ca1—O158.50 (3)
V1vii—Ca1—O3xii119.56 (4)O4vi—Ca1—O179.40 (3)
O1viii—Ca1—O3xii161.28 (3)O4v—Ca1—O179.40 (3)
V2i—Ca1—O3xii98.98 (3)O1vii—Ca1—O170.44 (5)
V2ii—Ca1—O3xii123.67 (4)O1—V1—O3xi109.23 (9)
V1iv—Ca1—O3xii76.06 (4)O1—V1—O3xii109.23 (9)
V2—Ca1—O3xii63.50 (3)O3xi—V1—O3xii86.69 (12)
V2iii—Ca1—O3xii27.13 (3)O1—V1—O4iii111.32 (9)
V2ix—Ca1—O3xii107.23 (3)O3xi—V1—O4iii139.45 (9)
V2vii—Ca1—O3xii136.71 (4)O3xii—V1—O4iii79.90 (8)
O2—Ca1—O3xii75.50 (5)O1—V1—O4111.32 (9)
O2iii—Ca1—O3xii41.80 (4)O3xi—V1—O479.90 (8)
O3x—Ca1—O3xii90.09 (3)O3xii—V1—O4139.45 (9)
O3viii—Ca1—O3xii101.82 (4)O4iii—V1—O485.88 (12)
O3xi—Ca1—O3xii36.41 (6)O1—V1—V2iii110.644 (18)
O2i—Ca1—O2ix39.48 (7)O3xi—V1—V2iii121.59 (7)
O2ii—Ca1—O2ix117.30 (4)O3xii—V1—V2iii40.46 (6)
O4—Ca1—O2ix147.70 (6)O4iii—V1—V2iii40.25 (6)
O4iii—Ca1—O2ix89.98 (6)O4—V1—V2iii120.77 (7)
O3iii—Ca1—O2ix42.16 (6)O1—V1—V2110.644 (18)
O3—Ca1—O2ix95.33 (6)O3xi—V1—V240.46 (6)
O1iv—Ca1—O2ix117.85 (5)O3xii—V1—V2121.59 (7)
V1—Ca1—O2ix124.70 (4)O4iii—V1—V2120.77 (7)
V2v—Ca1—O2ix126.25 (4)O4—V1—V240.25 (6)
V2vi—Ca1—O2ix61.73 (3)V2iii—V1—V2138.71 (4)
V1vii—Ca1—O2ix63.75 (3)O1—V1—Ca1132.28 (10)
O1viii—Ca1—O2ix50.67 (3)O3xi—V1—Ca1104.96 (6)
V2i—Ca1—O2ix50.41 (3)O3xii—V1—Ca1104.96 (6)
V2ii—Ca1—O2ix108.87 (4)O4iii—V1—Ca144.38 (6)
V1iv—Ca1—O2ix106.55 (4)O4—V1—Ca144.38 (6)
V2—Ca1—O2ix170.12 (4)V2iii—V1—Ca176.442 (17)
V2iii—Ca1—O2ix85.11 (4)V2—V1—Ca176.442 (17)
V2ix—Ca1—O2ix21.74 (3)O1—V1—Ca1xi125.44 (10)
V2vii—Ca1—O2ix96.45 (4)O3xi—V1—Ca1xi44.01 (6)
O2—Ca1—O2ix167.01 (6)O3xii—V1—Ca1xi44.01 (6)
O2iii—Ca1—O2ix77.31 (5)O4iii—V1—Ca1xi107.87 (6)
O3x—Ca1—O2ix78.61 (4)O4—V1—Ca1xi107.87 (6)
O3viii—Ca1—O2ix107.02 (5)V2iii—V1—Ca1xi78.025 (17)
O3xi—Ca1—O2ix148.05 (4)V2—V1—Ca1xi78.025 (17)
O3xii—Ca1—O2ix112.19 (4)Ca1—V1—Ca1xi102.28 (4)
O2i—Ca1—O2vii117.30 (4)O1—V1—Ca1xv31.95 (10)
O2ii—Ca1—O2vii39.48 (7)O3xi—V1—Ca1xv86.35 (6)
O4—Ca1—O2vii89.98 (6)O3xii—V1—Ca1xv86.35 (6)
O4iii—Ca1—O2vii147.70 (6)O4iii—V1—Ca1xv130.15 (6)
O3iii—Ca1—O2vii95.33 (6)O4—V1—Ca1xv130.15 (6)
O3—Ca1—O2vii42.16 (6)V2iii—V1—Ca1xv107.287 (17)
O1iv—Ca1—O2vii117.85 (5)V2—V1—Ca1xv107.287 (17)
V1—Ca1—O2vii124.70 (4)Ca1—V1—Ca1xv164.23 (3)
V2v—Ca1—O2vii61.73 (3)Ca1xi—V1—Ca1xv93.49 (3)
V2vi—Ca1—O2vii126.25 (4)O1—V1—Ca1xvi48.32 (10)
V1vii—Ca1—O2vii63.75 (3)O3xi—V1—Ca1xvi134.69 (6)
O1viii—Ca1—O2vii50.67 (3)O3xii—V1—Ca1xvi134.69 (6)
V2i—Ca1—O2vii108.87 (4)O4iii—V1—Ca1xvi76.54 (6)
V2ii—Ca1—O2vii50.41 (3)O4—V1—Ca1xvi76.54 (6)
V1iv—Ca1—O2vii106.55 (4)V2iii—V1—Ca1xvi103.723 (17)
V2—Ca1—O2vii85.11 (4)V2—V1—Ca1xvi103.723 (17)
V2iii—Ca1—O2vii170.12 (4)Ca1—V1—Ca1xvi83.96 (3)
V2ix—Ca1—O2vii96.45 (4)Ca1xi—V1—Ca1xvi173.76 (3)
V2vii—Ca1—O2vii21.74 (3)Ca1xv—V1—Ca1xvi80.27 (3)
O2—Ca1—O2vii77.31 (5)O1—V1—Ca1xiii75.643 (13)
O2iii—Ca1—O2vii167.01 (6)O3xi—V1—Ca1xiii54.58 (6)
O3x—Ca1—O2vii107.02 (5)O3xii—V1—Ca1xiii138.61 (6)
O3viii—Ca1—O2vii78.61 (4)O4iii—V1—Ca1xiii138.29 (6)
O3xi—Ca1—O2vii112.19 (4)O4—V1—Ca1xiii55.02 (6)
O3xii—Ca1—O2vii148.05 (4)V2iii—V1—Ca1xiii173.71 (2)
O2ix—Ca1—O2vii97.79 (6)V2—V1—Ca1xiii35.01 (2)
O2i—Ca1—O2v148.52 (6)Ca1—V1—Ca1xiii99.362 (14)
O2ii—Ca1—O2v97.84 (8)Ca1xi—V1—Ca1xiii98.532 (14)
O4—Ca1—O2v38.73 (6)Ca1xv—V1—Ca1xiii78.028 (13)
O4iii—Ca1—O2v73.28 (6)Ca1xvi—V1—Ca1xiii80.266 (12)
O3iii—Ca1—O2v72.32 (6)O2—V2—O4112.28 (10)
O3—Ca1—O2v37.87 (5)O2—V2—O4xiii108.90 (10)
O1iv—Ca1—O2v123.52 (7)O4—V2—O4xiii138.76 (5)
V1—Ca1—O2v57.44 (3)O2—V2—O3xiii106.18 (10)
V2v—Ca1—O2v18.95 (4)O4—V2—O3xiii81.35 (9)
V2vi—Ca1—O2v70.99 (4)O4xiii—V2—O3xiii89.57 (9)
V1vii—Ca1—O2v53.94 (3)O2—V2—O3xi114.56 (10)
O1viii—Ca1—O2v109.87 (5)O4—V2—O3xi80.01 (8)
V2i—Ca1—O2v163.47 (4)O4xiii—V2—O3xi81.17 (9)
V2ii—Ca1—O2v113.53 (4)O3xiii—V2—O3xi139.07 (4)
V1iv—Ca1—O2v139.30 (3)O2—V2—V2xiii120.50 (7)
V2—Ca1—O2v57.92 (3)O4—V2—V2xiii111.56 (6)
V2iii—Ca1—O2v95.29 (4)O4xiii—V2—V2xiii40.54 (6)
V2ix—Ca1—O2v92.23 (4)O3xiii—V2—V2xiii118.45 (7)
V2vii—Ca1—O2v55.43 (3)O3xi—V2—V2xiii40.66 (6)
O2—Ca1—O2v77.04 (4)O2—V2—V2v114.34 (7)
O2iii—Ca1—O2v118.10 (4)O4—V2—V2v40.57 (6)
O3x—Ca1—O2v167.51 (4)O4xiii—V2—V2v120.49 (7)
O3viii—Ca1—O2v133.70 (5)O3xiii—V2—V2v40.81 (6)
O3xi—Ca1—O2v66.56 (4)O3xi—V2—V2v113.34 (6)
O3xii—Ca1—O2v82.90 (4)V2xiii—V2—V2v125.15 (4)
O2ix—Ca1—O2v113.61 (4)O2—V2—V1127.50 (10)
O2vii—Ca1—O2v74.89 (5)O4—V2—V140.53 (6)
O2i—Ca1—O2vi97.84 (8)O4xiii—V2—V1108.81 (6)
O2ii—Ca1—O2vi148.52 (6)O3xiii—V2—V1109.26 (6)
O4—Ca1—O2vi73.28 (6)O3xi—V2—V140.29 (6)
O4iii—Ca1—O2vi38.73 (6)V2xiii—V2—V172.53 (2)
O3iii—Ca1—O2vi37.87 (5)V2v—V2—V174.09 (3)
O3—Ca1—O2vi72.32 (6)O2—V2—Ca1xiii118.17 (10)
O1iv—Ca1—O2vi123.52 (7)O4—V2—Ca1xiii113.33 (6)
V1—Ca1—O2vi57.44 (3)O4xiii—V2—Ca1xiii44.27 (6)
V2v—Ca1—O2vi70.99 (4)O3xiii—V2—Ca1xiii45.46 (6)
V2vi—Ca1—O2vi18.95 (4)O3xi—V2—Ca1xiii112.53 (6)
V1vii—Ca1—O2vi53.94 (3)V2xiii—V2—Ca1xiii76.61 (3)
O1viii—Ca1—O2vi109.87 (5)V2v—V2—Ca1xiii79.19 (3)
V2i—Ca1—O2vi113.53 (4)V1—V2—Ca1xiii114.32 (3)
V2ii—Ca1—O2vi163.47 (4)O2—V2—Ca1ii23.26 (9)
V1iv—Ca1—O2vi139.30 (3)O4—V2—Ca1ii123.87 (6)
V2—Ca1—O2vi95.29 (4)O4xiii—V2—Ca1ii95.54 (6)
V2iii—Ca1—O2vi57.92 (3)O3xiii—V2—Ca1ii87.49 (6)
V2ix—Ca1—O2vi55.43 (3)O3xi—V2—Ca1ii132.87 (6)
V2vii—Ca1—O2vi92.23 (4)V2xiii—V2—Ca1ii121.90 (3)
O2—Ca1—O2vi118.10 (4)V2v—V2—Ca1ii108.65 (3)
O2iii—Ca1—O2vi77.04 (4)V1—V2—Ca1ii150.06 (3)
O3x—Ca1—O2vi133.70 (5)Ca1xiii—V2—Ca1ii95.21 (2)
O3viii—Ca1—O2vi167.51 (4)O2—V2—Ca184.87 (9)
O3xi—Ca1—O2vi82.90 (4)O4—V2—Ca127.80 (6)
O3xii—Ca1—O2vi66.56 (4)O4xiii—V2—Ca1164.57 (6)
O2ix—Ca1—O2vi74.89 (5)O3xiii—V2—Ca193.24 (6)
O2vii—Ca1—O2vi113.61 (4)O3xi—V2—Ca186.82 (6)
O2v—Ca1—O2vi52.05 (7)V2xiii—V2—Ca1126.50 (3)
O2i—Ca1—O4x37.85 (6)V2v—V2—Ca156.13 (2)
O2ii—Ca1—O4x73.20 (7)V1—V2—Ca156.01 (2)
O4—Ca1—O4x158.64 (5)Ca1xiii—V2—Ca1135.30 (2)
O4iii—Ca1—O4x125.96 (7)Ca1ii—V2—Ca199.73 (2)
O3iii—Ca1—O4x94.52 (6)O2—V2—Ca1xi89.03 (9)
O3—Ca1—O4x114.72 (6)O4—V2—Ca1xi88.13 (6)
O1iv—Ca1—O4x81.18 (7)O4xiii—V2—Ca1xi90.40 (6)
V1—Ca1—O4x149.97 (3)O3xiii—V2—Ca1xi163.91 (6)
V2v—Ca1—O4x144.13 (3)O3xi—V2—Ca1xi25.57 (6)
V2vi—Ca1—O4x112.15 (3)V2xiii—V2—Ca1xi54.64 (2)
V1vii—Ca1—O4x101.68 (4)V2v—V2—Ca1xi127.96 (3)
O1viii—Ca1—O4x42.41 (5)V1—V2—Ca1xi55.73 (2)
V2i—Ca1—O4x26.46 (3)Ca1xiii—V2—Ca1xi131.23 (2)
V2ii—Ca1—O4x59.71 (4)Ca1ii—V2—Ca1xi108.52 (2)
V1iv—Ca1—O4x62.63 (4)Ca1—V2—Ca1xi82.73 (2)
V2—Ca1—O4x136.30 (3)V1—O1—Ca1xv128.44 (15)
V2iii—Ca1—O4x106.71 (3)V1—O1—Ca1xvi111.70 (13)
V2ix—Ca1—O4x74.48 (3)Ca1xv—O1—Ca1xvi119.86 (11)
V2vii—Ca1—O4x98.98 (3)V1—O1—Ca1xi37.76 (8)
O2—Ca1—O4x113.54 (5)Ca1xv—O1—Ca1xi90.67 (8)
O2iii—Ca1—O4x85.05 (4)Ca1xvi—O1—Ca1xi149.47 (9)
O3x—Ca1—O4x37.73 (4)V1—O1—Ca132.68 (8)
O3viii—Ca1—O4x53.73 (4)Ca1xv—O1—Ca1161.12 (10)
O3xi—Ca1—O4x138.67 (4)Ca1xvi—O1—Ca179.02 (6)
O3xii—Ca1—O4x124.01 (4)Ca1xi—O1—Ca170.44 (5)
O2ix—Ca1—O4x53.57 (4)V2—O2—Ca1ii141.03 (14)
O2vii—Ca1—O4x82.42 (4)V2—O2—Ca172.30 (9)
O2v—Ca1—O4x152.27 (4)Ca1ii—O2—Ca1128.23 (7)
O2vi—Ca1—O4x128.04 (4)V2—O2—Ca1xi69.23 (8)
O2i—Ca1—O4viii73.20 (7)Ca1ii—O2—Ca1xi140.52 (7)
O2ii—Ca1—O4viii37.85 (6)Ca1—O2—Ca1xi77.31 (5)
O4—Ca1—O4viii125.96 (7)V2—O2—Ca1xiii42.89 (7)
O4iii—Ca1—O4viii158.64 (5)Ca1ii—O2—Ca1xiii98.52 (8)
O3iii—Ca1—O4viii114.72 (6)Ca1—O2—Ca1xiii105.72 (5)
O3—Ca1—O4viii94.52 (6)Ca1xi—O2—Ca1xiii102.13 (5)
O1iv—Ca1—O4viii81.18 (7)V1vii—O3—V2v128.39 (11)
V1—Ca1—O4viii149.97 (3)V1vii—O3—V2vii99.25 (9)
V2v—Ca1—O4viii112.15 (3)V2v—O3—V2vii98.53 (9)
V2vi—Ca1—O4viii144.13 (3)V1vii—O3—Ca1101.92 (9)
V1vii—Ca1—O4viii101.68 (4)V2v—O3—Ca199.44 (8)
O1viii—Ca1—O4viii42.41 (5)V2vii—O3—Ca1133.99 (10)
V2i—Ca1—O4viii59.71 (4)V1vii—O3—Ca1xvi65.42 (6)
V2ii—Ca1—O4viii26.46 (3)V2v—O3—Ca1xvi64.24 (5)
V1iv—Ca1—O4viii62.63 (4)V2vii—O3—Ca1xvi123.08 (8)
V2—Ca1—O4viii106.71 (3)Ca1—O3—Ca1xvi102.87 (6)
V2iii—Ca1—O4viii136.30 (3)V1vii—O3—Ca1vii48.95 (5)
V2ix—Ca1—O4viii98.98 (3)V2v—O3—Ca1vii160.88 (9)
V2vii—Ca1—O4viii74.48 (3)V2vii—O3—Ca1vii66.05 (5)
O2—Ca1—O4viii85.05 (4)Ca1—O3—Ca1vii99.51 (7)
O2iii—Ca1—O4viii113.54 (5)Ca1xvi—O3—Ca1vii113.57 (5)
O3x—Ca1—O4viii53.73 (4)V1vii—O3—Ca1v104.64 (7)
O3viii—Ca1—O4viii37.73 (4)V2v—O3—Ca1v60.97 (6)
O3xi—Ca1—O4viii124.01 (4)V2vii—O3—Ca1v43.66 (5)
O3xii—Ca1—O4viii138.67 (4)Ca1—O3—Ca1v153.25 (7)
O2ix—Ca1—O4viii82.42 (4)Ca1xvi—O3—Ca1v85.44 (4)
O2vii—Ca1—O4viii53.57 (4)Ca1vii—O3—Ca1v100.26 (4)
O2v—Ca1—O4viii128.04 (4)V2—O4—V2v98.88 (9)
O2vi—Ca1—O4viii152.27 (4)V2—O4—V199.23 (9)
O4x—Ca1—O4viii35.70 (6)V2v—O4—V1132.46 (11)
O2i—Ca1—V1viii60.07 (6)V2—O4—Ca1129.74 (10)
O2ii—Ca1—V1viii60.07 (6)V2v—O4—Ca1100.84 (8)
O4—Ca1—V1viii145.69 (5)V1—O4—Ca1100.44 (9)
O4iii—Ca1—V1viii145.69 (5)V2—O4—Ca1xvi132.15 (8)
O3iii—Ca1—V1viii89.26 (5)V2v—O4—Ca1xvi58.00 (5)
O3—Ca1—V1viii89.26 (5)V1—O4—Ca1xvi77.51 (6)
O1iv—Ca1—V1viii99.89 (8)Ca1—O4—Ca1xvi97.21 (6)
V1—Ca1—V1viii174.60 (3)V2—O4—Ca1xi65.73 (5)
V2v—Ca1—V1viii118.66 (2)V2v—O4—Ca1xi161.85 (8)
V2vi—Ca1—V1viii118.66 (2)V1—O4—Ca1xi47.17 (5)
V1vii—Ca1—V1viii83.12 (3)Ca1—O4—Ca1xi96.66 (6)
O1viii—Ca1—V1viii19.97 (5)Ca1xvi—O4—Ca1xi124.52 (5)
V2i—Ca1—V1viii51.762 (18)V2—O4—Ca1xiii43.20 (5)
V2ii—Ca1—V1viii51.762 (18)V2v—O4—Ca1xiii63.87 (6)
V1iv—Ca1—V1viii80.27 (3)V1—O4—Ca1xiii104.03 (7)
V2—Ca1—V1viii130.780 (18)Ca1—O4—Ca1xiii155.39 (7)
V2iii—Ca1—V1viii130.780 (18)Ca1xvi—O4—Ca1xiii90.58 (4)
V2ix—Ca1—V1viii73.04 (2)Ca1xi—O4—Ca1xiii98.03 (4)
V2vii—Ca1—V1viii73.04 (2)V2—O4—Ca1ii37.49 (4)
O2—Ca1—V1viii110.38 (4)V2v—O4—Ca1ii90.42 (7)
O2iii—Ca1—V1viii110.38 (4)V1—O4—Ca1ii128.35 (7)
O3x—Ca1—V1viii60.84 (3)Ca1—O4—Ca1ii96.65 (6)
O3viii—Ca1—V1viii60.84 (3)Ca1xvi—O4—Ca1ii147.38 (5)
O3xi—Ca1—V1viii149.88 (3)Ca1xi—O4—Ca1ii82.77 (3)
O3xii—Ca1—V1viii149.88 (3)Ca1xiii—O4—Ca1ii65.90 (3)
O2ix—Ca1—V1viii57.60 (3)
Symmetry codes: (i) x, y1/2, z+1; (ii) x, y+1, z+1; (iii) x, y+1/2, z; (iv) x1/2, y, z+3/2; (v) x+1/2, y+1, z1/2; (vi) x+1/2, y1/2, z1/2; (vii) x, y, z1; (viii) x1/2, y, z+1/2; (ix) x, y+1/2, z1; (x) x1/2, y+1/2, z+1/2; (xi) x, y, z+1; (xii) x, y+1/2, z+1; (xiii) x+1/2, y+1, z+1/2; (xiv) x+1/2, y1/2, z+1/2; (xv) x+1/2, y, z+3/2; (xvi) x+1/2, y, z+1/2.
(CaV3O7_287K) top
Crystal data top
O7V3·CaF(000) = 580
Mr = 304.90Dx = 3.534 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2645 reflections
a = 10.444 (3) Åθ = 1.3–23.4°
b = 10.368 (2) ŵ = 5.67 mm1
c = 5.2927 (15) ÅT = 287 K
V = 573.1 (2) Å3, brown
Z = 40.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
403 independent reflections
Radiation source: fine-focus sealed tube363 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
Detector resolution: 0 pixels mm-1θmax = 23.0°, θmin = 3.9°
Rotation method scansh = 1111
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1010
Tmin = 0.319, Tmax = 0.471l = 55
2387 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020 w = 1/[σ2(Fo2) + (0.0439P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.052(Δ/σ)max < 0.001
S = 0.93Δρmax = 0.34 e Å3
403 reflectionsΔρmin = 0.40 e Å3
38 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0190 (15)
Crystal data top
O7V3·CaV = 573.1 (2) Å3
Mr = 304.90Z = 4
Orthorhombic, PnmaMo Kα radiation
a = 10.444 (3) ŵ = 5.67 mm1
b = 10.368 (2) ÅT = 287 K
c = 5.2927 (15) Å0.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
403 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
363 reflections with I > 2σ(I)
Tmin = 0.319, Tmax = 0.471Rint = 0.032
2387 measured reflectionsθmax = 23.0°
Refinement top
R[F2 > 2σ(F2)] = 0.02038 parameters
wR(F2) = 0.0520 restraints
S = 0.93Δρmax = 0.34 e Å3
403 reflectionsΔρmin = 0.40 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.08470 (9)0.25000.29962 (15)0.0080 (3)
V10.28858 (7)0.25000.79194 (13)0.0064 (3)
V20.18749 (5)0.52036 (5)0.78352 (9)0.0063 (3)
O10.4432 (3)0.25000.8081 (5)0.0136 (8)*
O20.0404 (2)0.5655 (3)0.7669 (4)0.0151 (6)*
O30.22026 (19)0.3799 (2)0.0258 (4)0.0076 (5)*
O40.22625 (19)0.3795 (2)0.5481 (4)0.0079 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0055 (5)0.0082 (6)0.0103 (5)0.0000.0003 (3)0.000
V10.0066 (5)0.0058 (5)0.0068 (5)0.0000.0002 (3)0.000
V20.0065 (4)0.0056 (4)0.0068 (4)0.0011 (2)0.0001 (2)0.00039 (19)
Geometric parameters (Å, º) top
Ca1—O2i2.343 (3)V1—Ca1xiii4.4009 (14)
Ca1—O2ii2.343 (3)V1—Ca1xiv5.3504 (11)
Ca1—O42.391 (2)V2—O21.608 (2)
Ca1—O4iii2.391 (2)V2—O4xiv1.962 (2)
Ca1—O32.433 (2)V2—O41.962 (2)
Ca1—O3iii2.433 (2)V2—O3xiv1.964 (2)
Ca1—O1iv2.548 (3)V2—O3x1.970 (2)
Ca1—V13.3651 (13)V2—V2xiv2.9810 (9)
Ca1—V2v3.3671 (11)V2—V2v2.9810 (9)
Ca1—V2vi3.3671 (11)V2—Ca1xiv3.3671 (11)
Ca1—V1vii3.4284 (13)V2—Ca1ii3.7342 (11)
Ca1—O1viii3.539 (3)V2—Ca1x4.0585 (10)
Ca1—V2i3.7342 (11)O1—Ca1xii2.548 (3)
Ca1—V2ii3.7342 (11)O1—Ca1xiii3.539 (3)
Ca1—V1iv3.7734 (14)O1—Ca1x4.560 (3)
Ca1—V23.9458 (10)O2—Ca1ii2.343 (3)
Ca1—V2iii3.9458 (10)O2—Ca1x4.343 (3)
Ca1—V2ix4.0585 (10)O2—Ca1xiv4.361 (3)
Ca1—V2vii4.0585 (10)O3—V2v1.964 (2)
Ca1—O24.127 (3)O3—V1vii1.964 (2)
V1—O11.617 (3)O3—V2vii1.970 (2)
V1—O3x1.964 (2)O3—Ca1xiii4.142 (2)
V1—O3xi1.964 (2)O3—Ca1vii4.312 (2)
V1—O4iii1.973 (2)O3—Ca1v4.506 (2)
V1—O41.973 (2)O4—V2v1.962 (2)
V1—V2iii2.9957 (8)O4—Ca1xiii4.382 (2)
V1—V22.9957 (8)O4—Ca1x4.451 (2)
V1—Ca1x3.4284 (13)O4—Ca1xiv4.520 (2)
V1—Ca1xii3.7734 (14)O4—Ca1ii5.094 (2)
O2i—Ca1—O2ii109.43 (12)O1—V1—O4111.35 (9)
O2i—Ca1—O4152.36 (8)O3x—V1—O479.96 (8)
O2ii—Ca1—O488.23 (7)O3xi—V1—O4139.41 (10)
O2i—Ca1—O4iii88.23 (7)O4iii—V1—O485.77 (12)
O2ii—Ca1—O4iii152.36 (8)O1—V1—V2iii110.656 (18)
O4—Ca1—O4iii68.32 (10)O3x—V1—V2iii121.55 (7)
O2i—Ca1—O3133.39 (7)O3xi—V1—V2iii40.49 (6)
O2ii—Ca1—O377.47 (7)O4iii—V1—V2iii40.29 (6)
O4—Ca1—O369.93 (7)O4—V1—V2iii120.71 (7)
O4iii—Ca1—O3106.18 (8)O1—V1—V2110.656 (18)
O2i—Ca1—O3iii77.47 (7)O3x—V1—V240.49 (6)
O2ii—Ca1—O3iii133.39 (7)O3xi—V1—V2121.55 (7)
O4—Ca1—O3iii106.18 (8)O4iii—V1—V2120.71 (7)
O4iii—Ca1—O3iii69.93 (7)O4—V1—V240.29 (6)
O3—Ca1—O3iii67.24 (10)V2iii—V1—V2138.69 (4)
O2i—Ca1—O1iv78.41 (7)O1—V1—Ca1132.28 (11)
O2ii—Ca1—O1iv78.41 (7)O3x—V1—Ca1104.96 (6)
O4—Ca1—O1iv84.86 (8)O3xi—V1—Ca1104.96 (6)
O4iii—Ca1—O1iv84.86 (8)O4iii—V1—Ca144.33 (6)
O3—Ca1—O1iv145.36 (5)O4—V1—Ca144.33 (6)
O3iii—Ca1—O1iv145.36 (5)V2iii—V1—Ca176.434 (17)
O2i—Ca1—V1117.99 (6)V2—V1—Ca176.434 (17)
O2ii—Ca1—V1117.99 (6)O1—V1—Ca1x125.37 (11)
O4—Ca1—V135.21 (5)O3x—V1—Ca1x43.97 (6)
O4iii—Ca1—V135.21 (5)O3xi—V1—Ca1x43.97 (6)
O3—Ca1—V195.33 (6)O4iii—V1—Ca1x107.93 (6)
O3iii—Ca1—V195.33 (6)O4—V1—Ca1x107.93 (6)
O1iv—Ca1—V174.69 (7)V2iii—V1—Ca1x78.039 (18)
O2i—Ca1—V2v165.36 (6)V2—V1—Ca1x78.039 (18)
O2ii—Ca1—V2v79.23 (6)Ca1—V1—Ca1x102.35 (4)
O4—Ca1—V2v34.91 (5)O1—V1—Ca1xii31.93 (10)
O4iii—Ca1—V2v88.51 (6)O3x—V1—Ca1xii86.37 (6)
O3—Ca1—V2v35.13 (5)O3xi—V1—Ca1xii86.37 (6)
O3iii—Ca1—V2v88.01 (6)O4iii—V1—Ca1xii130.18 (6)
O1iv—Ca1—V2v115.49 (5)O4—V1—Ca1xii130.18 (6)
V1—Ca1—V2v64.69 (2)V2iii—V1—Ca1xii107.302 (17)
O2i—Ca1—V2vi79.23 (6)V2—V1—Ca1xii107.302 (17)
O2ii—Ca1—V2vi165.36 (6)Ca1—V1—Ca1xii164.21 (3)
O4—Ca1—V2vi88.51 (6)Ca1x—V1—Ca1xii93.44 (3)
O4iii—Ca1—V2vi34.91 (5)O1—V1—Ca1xiii48.38 (10)
O3—Ca1—V2vi88.01 (6)O3x—V1—Ca1xiii134.74 (6)
O3iii—Ca1—V2vi35.13 (5)O3xi—V1—Ca1xiii134.74 (6)
O1iv—Ca1—V2vi115.49 (5)O4iii—V1—Ca1xiii76.49 (6)
V1—Ca1—V2vi64.69 (2)O4—V1—Ca1xiii76.49 (6)
V2v—Ca1—V2vi90.00 (3)V2iii—V1—Ca1xiii103.715 (17)
O2i—Ca1—V1vii103.22 (5)V2—V1—Ca1xiii103.715 (17)
O2ii—Ca1—V1vii103.22 (5)Ca1—V1—Ca1xiii83.90 (3)
O4—Ca1—V1vii92.69 (6)Ca1x—V1—Ca1xiii173.75 (3)
O4iii—Ca1—V1vii92.69 (6)Ca1xii—V1—Ca1xiii80.30 (3)
O3—Ca1—V1vii34.08 (5)O1—V1—Ca1xiv75.676 (13)
O3iii—Ca1—V1vii34.08 (5)O3x—V1—Ca1xiv54.58 (6)
O1iv—Ca1—V1vii177.04 (8)O3xi—V1—Ca1xiv138.57 (6)
V1—Ca1—V1vii102.35 (4)O4iii—V1—Ca1xiv138.24 (6)
V2v—Ca1—V1vii62.69 (2)O4—V1—Ca1xiv55.05 (6)
V2vi—Ca1—V1vii62.69 (2)V2iii—V1—Ca1xiv173.67 (3)
O2i—Ca1—O1viii68.32 (6)V2—V1—Ca1xiv34.984 (19)
O2ii—Ca1—O1viii68.32 (6)Ca1—V1—Ca1xiv99.346 (14)
O4—Ca1—O1viii139.27 (6)Ca1x—V1—Ca1xiv98.493 (14)
O4iii—Ca1—O1viii139.27 (6)Ca1xii—V1—Ca1xiv78.048 (13)
O3—Ca1—O1viii72.64 (7)Ca1xiii—V1—Ca1xiv80.304 (13)
O3iii—Ca1—O1viii72.64 (7)O2—V2—O4xiv108.87 (10)
O1iv—Ca1—O1viii119.89 (11)O2—V2—O4112.28 (10)
V1—Ca1—O1viii165.42 (6)O4xiv—V2—O4138.79 (5)
V2v—Ca1—O1viii105.78 (4)O2—V2—O3xiv106.10 (10)
V2vi—Ca1—O1viii105.78 (4)O4xiv—V2—O3xiv89.53 (9)
V1vii—Ca1—O1viii63.07 (6)O4—V2—O3xiv81.35 (9)
O2i—Ca1—V2i15.68 (6)O2—V2—O3x114.63 (11)
O2ii—Ca1—V2i94.48 (7)O4xiv—V2—O3x81.18 (9)
O4—Ca1—V2i153.32 (6)O4—V2—O3x80.07 (8)
O4iii—Ca1—V2i100.22 (5)O3xiv—V2—O3x139.10 (4)
O3—Ca1—V2i136.54 (5)O2—V2—V2xiv120.54 (7)
O3iii—Ca1—V2i91.14 (5)O4xiv—V2—V2xiv40.56 (6)
O1iv—Ca1—V2i69.79 (5)O4—V2—V2xiv111.59 (7)
V1—Ca1—V2i124.96 (2)O3xiv—V2—V2xiv118.43 (7)
V2v—Ca1—V2i170.35 (2)O3x—V2—V2xiv40.66 (6)
V2vi—Ca1—V2i94.83 (2)O2—V2—V2v114.28 (7)
V1vii—Ca1—V2i112.36 (2)O4xiv—V2—V2v120.49 (7)
O1viii—Ca1—V2i64.86 (4)O4—V2—V2v40.57 (6)
O2i—Ca1—V2ii94.48 (7)O3xiv—V2—V2v40.82 (6)
O2ii—Ca1—V2ii15.68 (6)O3x—V2—V2v113.40 (7)
O4—Ca1—V2ii100.22 (5)V2xiv—V2—V2v125.18 (4)
O4iii—Ca1—V2ii153.32 (6)O2—V2—V1127.59 (10)
O3—Ca1—V2ii91.14 (5)O4xiv—V2—V1108.82 (6)
O3iii—Ca1—V2ii136.54 (5)O4—V2—V140.56 (6)
O1iv—Ca1—V2ii69.79 (5)O3xiv—V2—V1109.27 (6)
V1—Ca1—V2ii124.96 (2)O3x—V2—V140.32 (6)
V2v—Ca1—V2ii94.83 (2)V2xiv—V2—V172.53 (2)
V2vi—Ca1—V2ii170.35 (2)V2v—V2—V174.12 (3)
V1vii—Ca1—V2ii112.36 (2)O2—V2—Ca1xiv118.06 (10)
O1viii—Ca1—V2ii64.86 (4)O4xiv—V2—Ca1xiv44.22 (6)
V2i—Ca1—V2ii79.23 (3)O4—V2—Ca1xiv113.37 (7)
O2i—Ca1—V1iv68.22 (6)O3xiv—V2—Ca1xiv45.47 (6)
O2ii—Ca1—V1iv68.22 (6)O3x—V2—Ca1xiv112.54 (7)
O4—Ca1—V1iv101.05 (6)V2xiv—V2—Ca1xiv76.59 (3)
O4iii—Ca1—V1iv101.05 (6)V2v—V2—Ca1xiv79.23 (3)
O3—Ca1—V1iv144.91 (5)V1—V2—Ca1xiv114.34 (3)
O3iii—Ca1—V1iv144.91 (5)O2—V2—Ca1ii23.18 (9)
O1iv—Ca1—V1iv19.61 (7)O4xiv—V2—Ca1ii95.53 (6)
V1—Ca1—V1iv94.30 (3)O4—V2—Ca1ii123.84 (6)
V2v—Ca1—V1iv126.42 (2)O3xiv—V2—Ca1ii87.48 (6)
V2vi—Ca1—V1iv126.42 (2)O3x—V2—Ca1ii132.85 (6)
V1vii—Ca1—V1iv163.35 (3)V2xiv—V2—Ca1ii121.90 (3)
O1viii—Ca1—V1iv100.28 (6)V2v—V2—Ca1ii108.61 (3)
V2i—Ca1—V1iv56.19 (2)V1—V2—Ca1ii150.08 (3)
V2ii—Ca1—V1iv56.19 (2)Ca1xiv—V2—Ca1ii95.17 (2)
O2i—Ca1—V2146.02 (6)O2—V2—Ca184.93 (9)
O2ii—Ca1—V270.70 (6)O4xiv—V2—Ca1164.58 (6)
O4—Ca1—V222.47 (5)O4—V2—Ca127.76 (6)
O4iii—Ca1—V282.75 (5)O3xiv—V2—Ca193.25 (6)
O3—Ca1—V280.50 (5)O3x—V2—Ca186.83 (6)
O3iii—Ca1—V2128.43 (6)V2xiv—V2—Ca1126.50 (3)
O1iv—Ca1—V268.22 (5)V2v—V2—Ca156.11 (2)
V1—Ca1—V247.564 (15)V1—V2—Ca156.00 (2)
V2v—Ca1—V247.299 (14)Ca1xiv—V2—Ca1135.32 (2)
V2vi—Ca1—V2109.06 (3)Ca1ii—V2—Ca199.749 (19)
V1vii—Ca1—V2109.86 (3)O2—V2—Ca1x89.16 (9)
O1viii—Ca1—V2134.700 (15)O4xiv—V2—Ca1x90.38 (6)
V2i—Ca1—V2137.44 (3)O4—V2—Ca1x88.16 (6)
V2ii—Ca1—V280.251 (19)O3xiv—V2—Ca1x163.89 (6)
V1iv—Ca1—V281.44 (2)O3x—V2—Ca1x25.50 (6)
O2i—Ca1—V2iii70.70 (6)V2xiv—V2—Ca1x54.59 (2)
O2ii—Ca1—V2iii146.02 (6)V2v—V2—Ca1x127.99 (3)
O4—Ca1—V2iii82.75 (5)V1—V2—Ca1x55.73 (2)
O4iii—Ca1—V2iii22.47 (5)Ca1xiv—V2—Ca1x131.17 (2)
O3—Ca1—V2iii128.43 (6)Ca1ii—V2—Ca1x108.56 (2)
O3iii—Ca1—V2iii80.50 (5)Ca1—V2—Ca1x82.77 (2)
O1iv—Ca1—V2iii68.22 (5)V1—O1—Ca1xii128.46 (15)
V1—Ca1—V2iii47.564 (15)V1—O1—Ca1xiii111.65 (13)
V2v—Ca1—V2iii109.06 (3)Ca1xii—O1—Ca1xiii119.89 (11)
V2vi—Ca1—V2iii47.299 (14)V1—O1—Ca1x37.82 (8)
V1vii—Ca1—V2iii109.86 (3)Ca1xii—O1—Ca1x90.65 (8)
O1viii—Ca1—V2iii134.700 (15)Ca1xiii—O1—Ca1x149.46 (9)
V2i—Ca1—V2iii80.251 (19)V1—O1—Ca132.68 (8)
V2ii—Ca1—V2iii137.44 (3)Ca1xii—O1—Ca1161.14 (11)
V1iv—Ca1—V2iii81.44 (2)Ca1xiii—O1—Ca178.97 (6)
V2—Ca1—V2iii90.54 (3)Ca1x—O1—Ca170.49 (5)
O2i—Ca1—V2ix58.84 (5)V2—O2—Ca1ii141.14 (14)
O2ii—Ca1—V2ix127.60 (6)V2—O2—Ca172.23 (8)
O4—Ca1—V2ix126.47 (6)Ca1ii—O2—Ca1128.28 (7)
O4iii—Ca1—V2ix79.56 (5)V2—O2—Ca1x69.11 (8)
O3—Ca1—V2ix80.07 (5)Ca1ii—O2—Ca1x140.51 (7)
O3iii—Ca1—V2ix20.41 (5)Ca1—O2—Ca1x77.29 (5)
O1iv—Ca1—V2ix134.57 (2)V2—O2—Ca1xiv42.95 (7)
V1—Ca1—V2ix110.72 (3)Ca1ii—O2—Ca1xiv98.56 (8)
V2v—Ca1—V2ix106.52 (3)Ca1—O2—Ca1xiv105.71 (5)
V2vi—Ca1—V2ix46.184 (14)Ca1x—O2—Ca1xiv102.06 (5)
V1vii—Ca1—V2ix46.229 (15)V2v—O3—V1vii128.36 (11)
O1viii—Ca1—V2ix59.92 (3)V2v—O3—V2vii98.52 (9)
V2i—Ca1—V2ix71.44 (2)V1vii—O3—V2vii99.19 (9)
V2ii—Ca1—V2ix124.23 (2)V2v—O3—Ca199.40 (8)
V1iv—Ca1—V2ix127.04 (2)V1vii—O3—Ca1101.95 (9)
V2—Ca1—V2ix148.82 (3)V2vii—O3—Ca1134.09 (10)
V2iii—Ca1—V2ix82.77 (2)V2v—O3—Ca1xiii64.25 (6)
O2i—Ca1—V2vii127.60 (6)V1vii—O3—Ca1xiii65.39 (6)
O2ii—Ca1—V2vii58.84 (5)V2vii—O3—Ca1xiii123.04 (8)
O4—Ca1—V2vii79.56 (5)Ca1—O3—Ca1xiii102.82 (6)
O4iii—Ca1—V2vii126.47 (6)V2v—O3—Ca1vii160.83 (9)
O3—Ca1—V2vii20.41 (5)V1vii—O3—Ca1vii48.94 (5)
O3iii—Ca1—V2vii80.07 (5)V2vii—O3—Ca1vii66.02 (5)
O1iv—Ca1—V2vii134.57 (2)Ca1—O3—Ca1vii99.61 (7)
V1—Ca1—V2vii110.72 (3)Ca1xiii—O3—Ca1vii113.51 (5)
V2v—Ca1—V2vii46.184 (14)V2v—O3—Ca1v60.96 (6)
V2vi—Ca1—V2vii106.52 (3)V1vii—O3—Ca1v104.62 (7)
V1vii—Ca1—V2vii46.229 (15)V2vii—O3—Ca1v43.64 (5)
O1viii—Ca1—V2vii59.92 (4)Ca1—O3—Ca1v153.23 (7)
V2i—Ca1—V2vii124.23 (2)Ca1xiii—O3—Ca1v85.46 (4)
V2ii—Ca1—V2vii71.440 (19)Ca1vii—O3—Ca1v100.23 (4)
V1iv—Ca1—V2vii127.04 (2)V2v—O4—V298.87 (9)
V2—Ca1—V2vii82.77 (2)V2v—O4—V1132.49 (11)
V2iii—Ca1—V2vii148.82 (3)V2—O4—V199.16 (9)
V2ix—Ca1—V2vii87.37 (3)V2v—O4—Ca1100.87 (8)
O2i—Ca1—O2132.42 (4)V2—O4—Ca1129.77 (10)
O2ii—Ca1—O251.72 (7)V1—O4—Ca1100.46 (9)
O4—Ca1—O245.14 (6)V2v—O4—Ca1xiii58.01 (5)
O4iii—Ca1—O2100.65 (6)V2—O4—Ca1xiii132.15 (8)
O3—Ca1—O289.04 (6)V1—O4—Ca1xiii77.54 (6)
O3iii—Ca1—O2149.43 (7)Ca1—O4—Ca1xiii97.19 (6)
O1iv—Ca1—O256.41 (4)V2v—O4—Ca1x161.78 (9)
V1—Ca1—O266.85 (3)V2—O4—Ca1x65.69 (5)
V2v—Ca1—O262.22 (3)V1—O4—Ca1x47.13 (5)
V2vi—Ca1—O2130.91 (4)Ca1—O4—Ca1x96.70 (6)
V1vii—Ca1—O2122.63 (4)Ca1xiii—O4—Ca1x124.51 (5)
O1viii—Ca1—O2119.85 (4)V2v—O4—Ca1xiv63.89 (6)
V2i—Ca1—O2119.39 (4)V2—O4—Ca1xiv43.15 (5)
V2ii—Ca1—O258.66 (3)V1—O4—Ca1xiv103.98 (7)
V1iv—Ca1—O264.20 (4)Ca1—O4—Ca1xiv155.42 (7)
V2—Ca1—O222.84 (3)Ca1xiii—O4—Ca1xiv90.62 (4)
V2iii—Ca1—O2101.81 (4)Ca1x—O4—Ca1xiv97.95 (4)
V2ix—Ca1—O2168.65 (4)V2v—O4—Ca1ii90.38 (7)
V2vii—Ca1—O283.43 (4)V2—O4—Ca1ii37.51 (5)
O1—V1—O3x109.25 (9)V1—O4—Ca1ii128.31 (7)
O1—V1—O3xi109.25 (9)Ca1—O4—Ca1ii96.68 (6)
O3x—V1—O3xi86.63 (12)Ca1xiii—O4—Ca1ii147.36 (5)
O1—V1—O4iii111.35 (9)Ca1x—O4—Ca1ii82.78 (3)
O3x—V1—O4iii139.41 (10)Ca1xiv—O4—Ca1ii65.86 (3)
O3xi—V1—O4iii79.96 (8)
Symmetry codes: (i) x, y1/2, z+1; (ii) x, y+1, z+1; (iii) x, y+1/2, z; (iv) x1/2, y, z+3/2; (v) x+1/2, y+1, z1/2; (vi) x+1/2, y1/2, z1/2; (vii) x, y, z1; (viii) x1/2, y, z+1/2; (ix) x, y+1/2, z1; (x) x, y, z+1; (xi) x, y+1/2, z+1; (xii) x+1/2, y, z+3/2; (xiii) x+1/2, y, z+1/2; (xiv) x+1/2, y+1, z+1/2.
(CaV3O7_275k) top
Crystal data top
O7V3·CaF(000) = 580
Mr = 304.90Dx = 3.535 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2678 reflections
a = 10.437 (3) Åθ = 1.3–23.4°
b = 10.367 (2) ŵ = 5.67 mm1
c = 5.2947 (15) ÅT = 275 K
V = 572.9 (3) Å3, brown
Z = 40.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
402 independent reflections
Radiation source: fine-focus sealed tube367 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
Detector resolution: 0 pixels mm-1θmax = 23.0°, θmin = 3.9°
Rotation method scansh = 1111
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1010
Tmin = 0.317, Tmax = 0.472l = 55
2416 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021 w = 1/[σ2(Fo2) + (0.0494P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.061(Δ/σ)max < 0.001
S = 0.98Δρmax = 0.34 e Å3
402 reflectionsΔρmin = 0.39 e Å3
38 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0187 (18)
Crystal data top
O7V3·CaV = 572.9 (3) Å3
Mr = 304.90Z = 4
Orthorhombic, PnmaMo Kα radiation
a = 10.437 (3) ŵ = 5.67 mm1
b = 10.367 (2) ÅT = 275 K
c = 5.2947 (15) Å0.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
402 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
367 reflections with I > 2σ(I)
Tmin = 0.317, Tmax = 0.472Rint = 0.038
2416 measured reflectionsθmax = 23.0°
Refinement top
R[F2 > 2σ(F2)] = 0.02138 parameters
wR(F2) = 0.0610 restraints
S = 0.98Δρmax = 0.34 e Å3
402 reflectionsΔρmin = 0.39 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.08465 (10)0.25000.29951 (17)0.0079 (4)
V10.28863 (8)0.25000.79215 (14)0.0063 (3)
V20.18747 (6)0.52036 (6)0.78364 (11)0.0063 (3)
O10.4432 (3)0.25000.8080 (6)0.0131 (9)*
O20.0402 (2)0.5657 (3)0.7667 (4)0.0141 (7)*
O30.2203 (2)0.3799 (2)0.0261 (4)0.0079 (6)*
O40.2267 (2)0.3796 (2)0.5485 (4)0.0078 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0057 (6)0.0080 (7)0.0099 (6)0.0000.0008 (4)0.000
V10.0063 (5)0.0063 (6)0.0065 (5)0.0000.0006 (3)0.000
V20.0065 (5)0.0058 (5)0.0066 (4)0.0010 (2)0.0000 (2)0.0001 (2)
Geometric parameters (Å, º) top
Ca1—O2i2.339 (3)V1—Ca1xiii4.4000 (16)
Ca1—O2ii2.339 (3)V1—Ca1xiv5.3499 (12)
Ca1—O42.396 (2)V2—O21.610 (3)
Ca1—O4iii2.396 (2)V2—O4xiv1.960 (2)
Ca1—O32.432 (2)V2—O3xiv1.963 (2)
Ca1—O3iii2.432 (2)V2—O41.961 (2)
Ca1—O1iv2.549 (4)V2—O3x1.971 (2)
Ca1—V2v3.3663 (12)V2—V2xiv2.9817 (9)
Ca1—V2vi3.3663 (12)V2—V2v2.9817 (9)
Ca1—V13.3669 (14)V2—Ca1xiv3.3663 (12)
Ca1—V1vii3.4276 (14)V2—Ca1ii3.7321 (12)
Ca1—O1viii3.539 (3)V2—Ca1x4.0581 (11)
Ca1—V2i3.7321 (12)O1—Ca1xii2.549 (4)
Ca1—V2ii3.7321 (12)O1—Ca1xiii3.539 (3)
Ca1—V1iv3.7710 (15)O1—Ca1x4.559 (4)
Ca1—V23.9470 (10)O2—Ca1ii2.339 (3)
Ca1—V2iii3.9470 (10)O2—Ca1x4.346 (3)
Ca1—V2ix4.0581 (11)O2—Ca1xiv4.361 (3)
Ca1—V2vii4.0581 (11)O3—V2v1.963 (2)
Ca1—O24.129 (3)O3—V1vii1.964 (2)
V1—O11.616 (4)O3—V2vii1.971 (2)
V1—O3x1.964 (2)O3—Ca1xiii4.138 (3)
V1—O3xi1.964 (2)O3—Ca1vii4.315 (3)
V1—O4iii1.972 (2)O3—Ca1v4.506 (2)
V1—O41.972 (2)O4—V2v1.960 (2)
V1—V2iii2.9955 (9)O4—Ca1xiii4.377 (3)
V1—V22.9955 (9)O4—Ca1x4.452 (2)
V1—Ca1x3.4276 (14)O4—Ca1xiv4.515 (3)
V1—Ca1xii3.7710 (15)O4—Ca1ii5.094 (2)
O2i—Ca1—O2ii109.55 (13)O1—V1—O4111.17 (11)
O2i—Ca1—O4152.29 (8)O3x—V1—O479.99 (9)
O2ii—Ca1—O488.22 (8)O3xi—V1—O4139.57 (11)
O2i—Ca1—O4iii88.22 (8)O4iii—V1—O485.93 (14)
O2ii—Ca1—O4iii152.29 (8)O1—V1—V2iii110.66 (2)
O4—Ca1—O4iii68.24 (11)O3x—V1—V2iii121.56 (8)
O2i—Ca1—O3133.43 (8)O3xi—V1—V2iii40.51 (7)
O2ii—Ca1—O377.45 (8)O4iii—V1—V2iii40.26 (7)
O4—Ca1—O369.91 (8)O4—V1—V2iii120.82 (7)
O4iii—Ca1—O3106.13 (9)O1—V1—V2110.66 (2)
O2i—Ca1—O3iii77.45 (8)O3x—V1—V240.51 (6)
O2ii—Ca1—O3iii133.43 (8)O3xi—V1—V2121.56 (8)
O4—Ca1—O3iii106.13 (9)O4iii—V1—V2120.82 (7)
O4iii—Ca1—O3iii69.91 (8)O4—V1—V240.26 (7)
O3—Ca1—O3iii67.25 (11)V2iii—V1—V2138.69 (4)
O2i—Ca1—O1iv78.45 (7)O1—V1—Ca1132.19 (12)
O2ii—Ca1—O1iv78.45 (7)O3x—V1—Ca1105.02 (7)
O4—Ca1—O1iv84.82 (9)O3xi—V1—Ca1105.02 (7)
O4iii—Ca1—O1iv84.82 (9)O4iii—V1—Ca144.43 (7)
O3—Ca1—O1iv145.33 (6)O4—V1—Ca144.43 (7)
O3iii—Ca1—O1iv145.33 (6)V2iii—V1—Ca176.436 (19)
O2i—Ca1—V2v165.36 (7)V2—V1—Ca176.436 (19)
O2ii—Ca1—V2v79.17 (7)O1—V1—Ca1x125.42 (12)
O4—Ca1—V2v34.90 (5)O3x—V1—Ca1x43.97 (7)
O4iii—Ca1—V2v88.47 (6)O3xi—V1—Ca1x43.97 (7)
O3—Ca1—V2v35.12 (5)O4iii—V1—Ca1x108.01 (7)
O3iii—Ca1—V2v88.02 (6)O4—V1—Ca1x108.01 (7)
O1iv—Ca1—V2v115.43 (5)V2iii—V1—Ca1x78.046 (19)
O2i—Ca1—V2vi79.17 (7)V2—V1—Ca1x78.046 (19)
O2ii—Ca1—V2vi165.36 (7)Ca1—V1—Ca1x102.38 (4)
O4—Ca1—V2vi88.47 (6)O1—V1—Ca1xii32.01 (11)
O4iii—Ca1—V2vi34.90 (5)O3x—V1—Ca1xii86.32 (7)
O3—Ca1—V2vi88.02 (6)O3xi—V1—Ca1xii86.32 (7)
O3iii—Ca1—V2vi35.12 (5)O4iii—V1—Ca1xii130.06 (7)
O1iv—Ca1—V2vi115.43 (5)O4—V1—Ca1xii130.06 (7)
V2v—Ca1—V2vi90.02 (4)V2iii—V1—Ca1xii107.302 (19)
O2i—Ca1—V1117.93 (6)V2—V1—Ca1xii107.302 (19)
O2ii—Ca1—V1117.93 (6)Ca1—V1—Ca1xii164.20 (4)
O4—Ca1—V135.18 (5)Ca1x—V1—Ca1xii93.42 (3)
O4iii—Ca1—V135.18 (5)O1—V1—Ca1xiii48.37 (11)
O3—Ca1—V195.33 (6)O3x—V1—Ca1xiii134.74 (7)
O3iii—Ca1—V195.33 (6)O3xi—V1—Ca1xiii134.74 (7)
O1iv—Ca1—V174.60 (8)O4iii—V1—Ca1xiii76.37 (7)
V2v—Ca1—V164.70 (2)O4—V1—Ca1xiii76.37 (7)
V2vi—Ca1—V164.70 (2)V2iii—V1—Ca1xiii103.697 (19)
O2i—Ca1—V1vii103.21 (6)V2—V1—Ca1xiii103.697 (19)
O2ii—Ca1—V1vii103.21 (6)Ca1—V1—Ca1xiii83.83 (3)
O4—Ca1—V1vii92.68 (6)Ca1x—V1—Ca1xiii173.79 (3)
O4iii—Ca1—V1vii92.68 (6)Ca1xii—V1—Ca1xiii80.38 (3)
O3—Ca1—V1vii34.09 (5)O1—V1—Ca1xiv75.684 (15)
O3iii—Ca1—V1vii34.09 (5)O3x—V1—Ca1xiv54.58 (7)
O1iv—Ca1—V1vii176.98 (9)O3xi—V1—Ca1xiv138.57 (7)
V2v—Ca1—V1vii62.72 (2)O4iii—V1—Ca1xiv138.26 (7)
V2vi—Ca1—V1vii62.72 (2)O4—V1—Ca1xiv54.93 (7)
V1—Ca1—V1vii102.38 (4)V2iii—V1—Ca1xiv173.66 (3)
O2i—Ca1—O1viii68.37 (6)V2—V1—Ca1xiv34.98 (2)
O2ii—Ca1—O1viii68.37 (6)Ca1—V1—Ca1xiv99.321 (16)
O4—Ca1—O1viii139.29 (6)Ca1x—V1—Ca1xiv98.502 (16)
O4iii—Ca1—O1viii139.29 (6)Ca1xii—V1—Ca1xiv78.069 (14)
O3—Ca1—O1viii72.65 (7)Ca1xiii—V1—Ca1xiv80.304 (14)
O3iii—Ca1—O1viii72.65 (7)O2—V2—O4xiv108.76 (11)
O1iv—Ca1—O1viii119.97 (12)O2—V2—O3xiv106.00 (11)
V2v—Ca1—O1viii105.78 (5)O4xiv—V2—O3xiv89.68 (10)
V2vi—Ca1—O1viii105.78 (5)O2—V2—O4112.41 (12)
V1—Ca1—O1viii165.43 (7)O4xiv—V2—O4138.77 (5)
V1vii—Ca1—O1viii63.05 (6)O3xiv—V2—O481.27 (10)
O2i—Ca1—V2i15.71 (6)O2—V2—O3x114.71 (12)
O2ii—Ca1—V2i94.56 (7)O4xiv—V2—O3x81.10 (10)
O4—Ca1—V2i153.32 (6)O3xiv—V2—O3x139.11 (5)
O4iii—Ca1—V2i100.25 (6)O4—V2—O3x80.08 (9)
O3—Ca1—V2i136.57 (6)O2—V2—V2xiv120.58 (8)
O3iii—Ca1—V2i91.12 (6)O4xiv—V2—V2xiv40.52 (7)
O1iv—Ca1—V2i69.85 (6)O3xiv—V2—V2xiv118.48 (8)
V2v—Ca1—V2i170.37 (3)O4—V2—V2xiv111.53 (7)
V2vi—Ca1—V2i94.79 (2)O3x—V2—V2xiv40.63 (7)
V1—Ca1—V2i124.93 (2)O2—V2—V2v114.20 (8)
V1vii—Ca1—V2i112.35 (3)O4xiv—V2—V2v120.66 (7)
O1viii—Ca1—V2i64.88 (4)O3xiv—V2—V2v40.82 (7)
O2i—Ca1—V2ii94.56 (7)O4—V2—V2v40.50 (7)
O2ii—Ca1—V2ii15.71 (6)O3x—V2—V2v113.42 (7)
O4—Ca1—V2ii100.25 (6)V2xiv—V2—V2v125.21 (5)
O4iii—Ca1—V2ii153.32 (6)O2—V2—V1127.63 (11)
O3—Ca1—V2ii91.12 (6)O4xiv—V2—V1108.84 (7)
O3iii—Ca1—V2ii136.57 (6)O3xiv—V2—V1109.29 (7)
O1iv—Ca1—V2ii69.85 (6)O4—V2—V140.53 (6)
V2v—Ca1—V2ii94.79 (2)O3x—V2—V140.33 (7)
V2vi—Ca1—V2ii170.37 (3)V2xiv—V2—V172.53 (3)
V1—Ca1—V2ii124.93 (2)V2v—V2—V174.13 (3)
V1vii—Ca1—V2ii112.35 (3)O2—V2—Ca1xiv118.00 (11)
O1viii—Ca1—V2ii64.88 (4)O4xiv—V2—Ca1xiv44.38 (7)
V2i—Ca1—V2ii79.27 (4)O3xiv—V2—Ca1xiv45.47 (7)
O2i—Ca1—V1iv68.26 (6)O4—V2—Ca1xiv113.23 (7)
O2ii—Ca1—V1iv68.26 (6)O3x—V2—Ca1xiv112.53 (7)
O4—Ca1—V1iv101.05 (6)V2xiv—V2—Ca1xiv76.62 (3)
O4iii—Ca1—V1iv101.05 (6)V2v—V2—Ca1xiv79.22 (3)
O3—Ca1—V1iv144.92 (6)V1—V2—Ca1xiv114.35 (3)
O3iii—Ca1—V1iv144.92 (6)O2—V2—Ca1ii23.16 (10)
O1iv—Ca1—V1iv19.64 (8)O4xiv—V2—Ca1ii95.44 (7)
V2v—Ca1—V1iv126.38 (2)O3xiv—V2—Ca1ii87.43 (7)
V2vi—Ca1—V1iv126.38 (2)O4—V2—Ca1ii123.95 (7)
V1—Ca1—V1iv94.24 (3)O3x—V2—Ca1ii132.88 (7)
V1vii—Ca1—V1iv163.38 (4)V2xiv—V2—Ca1ii121.88 (3)
O1viii—Ca1—V1iv100.33 (7)V2v—V2—Ca1ii108.59 (3)
V2i—Ca1—V1iv56.23 (2)V1—V2—Ca1ii150.10 (3)
V2ii—Ca1—V1iv56.23 (2)Ca1xiv—V2—Ca1ii95.13 (2)
O2i—Ca1—V2145.99 (6)O2—V2—Ca184.93 (10)
O2ii—Ca1—V270.65 (6)O4xiv—V2—Ca1164.64 (7)
O4—Ca1—V222.52 (5)O3xiv—V2—Ca193.21 (7)
O4iii—Ca1—V282.70 (6)O4—V2—Ca127.90 (7)
O3—Ca1—V280.50 (6)O3x—V2—Ca186.89 (7)
O3iii—Ca1—V2128.43 (7)V2xiv—V2—Ca1126.52 (4)
O1iv—Ca1—V268.16 (5)V2v—V2—Ca156.07 (3)
V2v—Ca1—V247.302 (15)V1—V2—Ca156.02 (2)
V2vi—Ca1—V2109.05 (3)Ca1xiv—V2—Ca1135.28 (3)
V1—Ca1—V247.542 (17)Ca1ii—V2—Ca199.76 (2)
V1vii—Ca1—V2109.88 (3)O2—V2—Ca1x89.23 (9)
O1viii—Ca1—V2134.721 (16)O4xiv—V2—Ca1x90.27 (7)
V2i—Ca1—V2137.44 (3)O3xiv—V2—Ca1x163.91 (7)
V2ii—Ca1—V280.24 (2)O4—V2—Ca1x88.21 (7)
V1iv—Ca1—V281.40 (2)O3x—V2—Ca1x25.52 (7)
O2i—Ca1—V2iii70.65 (6)V2xiv—V2—Ca1x54.58 (3)
O2ii—Ca1—V2iii145.99 (6)V2v—V2—Ca1x127.99 (3)
O4—Ca1—V2iii82.70 (6)V1—V2—Ca1x55.72 (2)
O4iii—Ca1—V2iii22.52 (5)Ca1xiv—V2—Ca1x131.19 (3)
O3—Ca1—V2iii128.43 (7)Ca1ii—V2—Ca1x108.59 (2)
O3iii—Ca1—V2iii80.50 (6)Ca1—V2—Ca1x82.80 (2)
O1iv—Ca1—V2iii68.16 (5)V1—O1—Ca1xii128.36 (17)
V2v—Ca1—V2iii109.05 (3)V1—O1—Ca1xiii111.67 (14)
V2vi—Ca1—V2iii47.302 (15)Ca1xii—O1—Ca1xiii119.97 (12)
V1—Ca1—V2iii47.542 (17)V1—O1—Ca1x37.79 (9)
V1vii—Ca1—V2iii109.88 (3)Ca1xii—O1—Ca1x90.57 (9)
O1viii—Ca1—V2iii134.721 (16)Ca1xiii—O1—Ca1x149.46 (10)
V2i—Ca1—V2iii80.24 (2)V1—O1—Ca132.75 (9)
V2ii—Ca1—V2iii137.44 (3)Ca1xii—O1—Ca1161.11 (12)
V1iv—Ca1—V2iii81.40 (2)Ca1xiii—O1—Ca178.92 (6)
V2—Ca1—V2iii90.49 (3)Ca1x—O1—Ca170.54 (6)
O2i—Ca1—V2ix58.81 (6)V2—O2—Ca1ii141.14 (16)
O2ii—Ca1—V2ix127.63 (6)V2—O2—Ca172.21 (9)
O4—Ca1—V2ix126.44 (6)Ca1ii—O2—Ca1128.34 (8)
O4iii—Ca1—V2ix79.58 (6)V2—O2—Ca1x69.02 (9)
O3—Ca1—V2ix80.09 (6)Ca1ii—O2—Ca1x140.54 (8)
O3iii—Ca1—V2ix20.43 (5)Ca1—O2—Ca1x77.28 (5)
O1iv—Ca1—V2ix134.58 (3)V2—O2—Ca1xiv42.97 (8)
V2v—Ca1—V2ix106.55 (3)Ca1ii—O2—Ca1xiv98.52 (8)
V2vi—Ca1—V2ix46.202 (16)Ca1—O2—Ca1xiv105.68 (5)
V1—Ca1—V2ix110.75 (3)Ca1x—O2—Ca1xiv102.02 (5)
V1vii—Ca1—V2ix46.232 (16)V2v—O3—V1vii128.42 (12)
O1viii—Ca1—V2ix59.90 (4)V2v—O3—V2vii98.55 (10)
V2i—Ca1—V2ix71.41 (2)V1vii—O3—V2vii99.16 (10)
V2ii—Ca1—V2ix124.23 (3)V2v—O3—Ca199.41 (9)
V1iv—Ca1—V2ix127.05 (2)V1vii—O3—Ca1101.94 (10)
V2—Ca1—V2ix148.84 (4)V2vii—O3—Ca1134.05 (11)
V2iii—Ca1—V2ix82.80 (2)V2v—O3—Ca1xiii64.28 (6)
O2i—Ca1—V2vii127.63 (6)V1vii—O3—Ca1xiii65.42 (6)
O2ii—Ca1—V2vii58.81 (6)V2vii—O3—Ca1xiii123.07 (9)
O4—Ca1—V2vii79.58 (6)Ca1—O3—Ca1xiii102.82 (7)
O4iii—Ca1—V2vii126.44 (6)V2v—O3—Ca1vii160.83 (10)
O3—Ca1—V2vii20.43 (5)V1vii—O3—Ca1vii48.91 (5)
O3iii—Ca1—V2vii80.09 (6)V2vii—O3—Ca1vii65.98 (6)
O1iv—Ca1—V2vii134.58 (3)Ca1—O3—Ca1vii99.59 (7)
V2v—Ca1—V2vii46.202 (16)Ca1xiii—O3—Ca1vii113.51 (5)
V2vi—Ca1—V2vii106.55 (3)V2v—O3—Ca1v61.00 (6)
V1—Ca1—V2vii110.75 (3)V1vii—O3—Ca1v104.61 (8)
V1vii—Ca1—V2vii46.232 (16)V2vii—O3—Ca1v43.64 (6)
O1viii—Ca1—V2vii59.90 (4)Ca1—O3—Ca1v153.26 (8)
V2i—Ca1—V2vii124.23 (3)Ca1xiii—O3—Ca1v85.50 (4)
V2ii—Ca1—V2vii71.41 (2)Ca1vii—O3—Ca1v100.18 (5)
V1iv—Ca1—V2vii127.05 (2)V2v—O4—V298.99 (11)
V2—Ca1—V2vii82.80 (2)V2v—O4—V1132.74 (12)
V2iii—Ca1—V2vii148.84 (4)V2—O4—V199.20 (10)
V2ix—Ca1—V2vii87.37 (3)V2v—O4—Ca1100.72 (9)
O2i—Ca1—O2132.43 (5)V2—O4—Ca1129.59 (11)
O2ii—Ca1—O251.66 (8)V1—O4—Ca1100.39 (10)
O4—Ca1—O245.20 (6)V2v—O4—Ca1xiii58.08 (6)
O4iii—Ca1—O2100.64 (7)V2—O4—Ca1xiii132.37 (9)
O3—Ca1—O289.03 (7)V1—O4—Ca1xiii77.67 (7)
O3iii—Ca1—O2149.44 (7)Ca1—O4—Ca1xiii97.14 (7)
O1iv—Ca1—O256.39 (5)V2v—O4—Ca1x161.94 (10)
V2v—Ca1—O262.21 (4)V2—O4—Ca1x65.66 (6)
V2vi—Ca1—O2130.92 (4)V1—O4—Ca1x47.07 (6)
V1—Ca1—O266.86 (4)Ca1—O4—Ca1x96.66 (7)
V1vii—Ca1—O2122.64 (4)Ca1xiii—O4—Ca1x124.58 (5)
O1viii—Ca1—O2119.84 (5)V2v—O4—Ca1xiv64.00 (7)
V2i—Ca1—O2119.39 (5)V2—O4—Ca1xiv43.25 (6)
V2ii—Ca1—O258.63 (4)V1—O4—Ca1xiv104.13 (8)
V1iv—Ca1—O264.17 (4)Ca1—O4—Ca1xiv155.33 (8)
V2—Ca1—O222.86 (4)Ca1xiii—O4—Ca1xiv90.74 (4)
V2iii—Ca1—O2101.79 (4)Ca1x—O4—Ca1xiv97.99 (5)
V2ix—Ca1—O2168.67 (5)V2v—O4—Ca1ii90.34 (7)
V2vii—Ca1—O283.42 (4)V2—O4—Ca1ii37.42 (5)
O1—V1—O3x109.25 (11)V1—O4—Ca1ii128.27 (8)
O1—V1—O3xi109.25 (11)Ca1—O4—Ca1ii96.60 (6)
O3x—V1—O3xi86.62 (14)Ca1xiii—O4—Ca1ii147.40 (5)
O1—V1—O4iii111.17 (10)Ca1x—O4—Ca1ii82.76 (4)
O3x—V1—O4iii139.57 (11)Ca1xiv—O4—Ca1ii65.84 (3)
O3xi—V1—O4iii79.99 (9)
Symmetry codes: (i) x, y1/2, z+1; (ii) x, y+1, z+1; (iii) x, y+1/2, z; (iv) x1/2, y, z+3/2; (v) x+1/2, y+1, z1/2; (vi) x+1/2, y1/2, z1/2; (vii) x, y, z1; (viii) x1/2, y, z+1/2; (ix) x, y+1/2, z1; (x) x, y, z+1; (xi) x, y+1/2, z+1; (xii) x+1/2, y, z+3/2; (xiii) x+1/2, y, z+1/2; (xiv) x+1/2, y+1, z+1/2.
(CaV3O7_262K) top
Crystal data top
O7V3·CaF(000) = 580
Mr = 304.90Dx = 3.535 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2683 reflections
a = 10.442 (3) Åθ = 1.3–23.4°
b = 10.367 (2) ŵ = 5.67 mm1
c = 5.2914 (15) ÅT = 262 K
V = 572.8 (2) Å3, brown
Z = 40.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
404 independent reflections
Radiation source: fine-focus sealed tube365 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
Detector resolution: 0 pixels mm-1θmax = 23.0°, θmin = 3.9°
Rotation method scansh = 1111
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1010
Tmin = 0.318, Tmax = 0.471l = 55
2427 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019 w = 1/[σ2(Fo2) + (0.0464P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055(Δ/σ)max < 0.001
S = 0.94Δρmax = 0.34 e Å3
404 reflectionsΔρmin = 0.40 e Å3
38 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0193 (16)
Crystal data top
O7V3·CaV = 572.8 (2) Å3
Mr = 304.90Z = 4
Orthorhombic, PnmaMo Kα radiation
a = 10.442 (3) ŵ = 5.67 mm1
b = 10.367 (2) ÅT = 262 K
c = 5.2914 (15) Å0.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
404 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
365 reflections with I > 2σ(I)
Tmin = 0.318, Tmax = 0.471Rint = 0.032
2427 measured reflectionsθmax = 23.0°
Refinement top
R[F2 > 2σ(F2)] = 0.01938 parameters
wR(F2) = 0.0550 restraints
S = 0.94Δρmax = 0.34 e Å3
404 reflectionsΔρmin = 0.40 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.08476 (10)0.25000.29971 (15)0.0077 (3)
V10.28862 (7)0.25000.79194 (13)0.0060 (3)
V20.18747 (6)0.52037 (6)0.78355 (10)0.0061 (3)
O10.4435 (3)0.25000.8080 (5)0.0122 (8)*
O20.0402 (2)0.5656 (3)0.7668 (4)0.0141 (6)*
O30.22014 (19)0.3799 (2)0.0261 (4)0.0074 (5)*
O40.22655 (19)0.3796 (2)0.5481 (4)0.0073 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0054 (5)0.0080 (6)0.0097 (6)0.0000.0001 (3)0.000
V10.0059 (5)0.0056 (6)0.0065 (5)0.0000.0005 (3)0.000
V20.0063 (4)0.0055 (4)0.0065 (4)0.0010 (2)0.0001 (2)0.0003 (2)
Geometric parameters (Å, º) top
Ca1—O2i2.341 (3)V1—Ca1xiii4.4004 (15)
Ca1—O2ii2.341 (3)V1—Ca1xiv5.3498 (11)
Ca1—O42.392 (2)V2—O21.611 (2)
Ca1—O4iii2.392 (2)V2—O4xiv1.960 (2)
Ca1—O3iii2.431 (2)V2—O41.962 (2)
Ca1—O32.431 (2)V2—O3xiv1.964 (2)
Ca1—O1iv2.547 (3)V2—O3x1.971 (2)
Ca1—V13.3638 (13)V2—V2v2.9805 (9)
Ca1—V2v3.3662 (11)V2—V2xiv2.9805 (9)
Ca1—V2vi3.3662 (11)V2—Ca1xiv3.3662 (11)
Ca1—V1vii3.4279 (13)V2—Ca1ii3.7340 (11)
Ca1—O1viii3.538 (3)V2—Ca1x4.0579 (10)
Ca1—V2i3.7340 (11)O1—Ca1xii2.547 (3)
Ca1—V2ii3.7340 (11)O1—Ca1xiii3.538 (3)
Ca1—V1iv3.7724 (14)O1—Ca1x4.561 (3)
Ca1—V23.9448 (10)O2—Ca1ii2.341 (3)
Ca1—V2iii3.9448 (10)O2—Ca1x4.344 (3)
Ca1—V2ix4.0579 (10)O2—Ca1xiv4.362 (3)
Ca1—V2vii4.0579 (10)O3—V1vii1.965 (2)
Ca1—O24.127 (3)O3—V2v1.964 (2)
V1—O11.619 (3)O3—V2vii1.971 (2)
V1—O3x1.965 (2)O3—Ca1xiii4.142 (2)
V1—O3xi1.965 (2)O3—Ca1vii4.311 (2)
V1—O4iii1.972 (2)O3—Ca1v4.506 (2)
V1—O41.972 (2)O4—V2v1.960 (2)
V1—V2iii2.9957 (9)O4—Ca1xiii4.380 (2)
V1—V22.9957 (9)O4—Ca1x4.451 (2)
V1—Ca1x3.4279 (13)O4—Ca1xiv4.517 (2)
V1—Ca1xii3.7724 (14)O4—Ca1ii5.095 (2)
O2i—Ca1—O2ii109.50 (12)O1—V1—O4111.25 (10)
O2i—Ca1—O4152.37 (8)O3x—V1—O479.99 (9)
O2ii—Ca1—O488.22 (8)O3xi—V1—O4139.45 (10)
O2i—Ca1—O4iii88.22 (8)O4iii—V1—O485.87 (12)
O2ii—Ca1—O4iii152.37 (8)O1—V1—V2iii110.663 (18)
O4—Ca1—O4iii68.32 (10)O3x—V1—V2iii121.49 (7)
O2i—Ca1—O3iii77.41 (7)O3xi—V1—V2iii40.51 (6)
O2ii—Ca1—O3iii133.39 (8)O4iii—V1—V2iii40.28 (6)
O4—Ca1—O3iii106.16 (8)O4—V1—V2iii120.78 (7)
O4iii—Ca1—O3iii69.89 (7)O1—V1—V2110.663 (18)
O2i—Ca1—O3133.39 (8)O3x—V1—V240.51 (6)
O2ii—Ca1—O377.41 (7)O3xi—V1—V2121.49 (7)
O4—Ca1—O369.89 (7)O4iii—V1—V2120.78 (7)
O4iii—Ca1—O3106.16 (8)O4—V1—V240.28 (6)
O3iii—Ca1—O367.29 (10)V2iii—V1—V2138.67 (4)
O2i—Ca1—O1iv78.45 (7)O1—V1—Ca1132.26 (11)
O2ii—Ca1—O1iv78.45 (7)O3x—V1—Ca1104.95 (6)
O4—Ca1—O1iv84.88 (8)O3xi—V1—Ca1104.95 (6)
O4iii—Ca1—O1iv84.88 (8)O4iii—V1—Ca144.39 (6)
O3iii—Ca1—O1iv145.33 (5)O4—V1—Ca144.39 (6)
O3—Ca1—O1iv145.33 (5)V2iii—V1—Ca176.432 (17)
O2i—Ca1—V1117.97 (6)V2—V1—Ca176.432 (17)
O2ii—Ca1—V1117.97 (6)O1—V1—Ca1x125.39 (11)
O4—Ca1—V135.22 (5)O3x—V1—Ca1x43.92 (6)
O4iii—Ca1—V135.22 (5)O3xi—V1—Ca1x43.92 (6)
O3iii—Ca1—V195.34 (6)O4iii—V1—Ca1x107.98 (7)
O3—Ca1—V195.34 (6)O4—V1—Ca1x107.98 (7)
O1iv—Ca1—V174.66 (7)V2iii—V1—Ca1x78.034 (18)
O2i—Ca1—V2v165.33 (6)V2—V1—Ca1x78.034 (18)
O2ii—Ca1—V2v79.18 (6)Ca1—V1—Ca1x102.35 (4)
O4—Ca1—V2v34.88 (5)O1—V1—Ca1xii31.94 (10)
O4iii—Ca1—V2v88.50 (6)O3x—V1—Ca1xii86.40 (6)
O3iii—Ca1—V2v88.04 (6)O3xi—V1—Ca1xii86.40 (6)
O3—Ca1—V2v35.13 (5)O4iii—V1—Ca1xii130.10 (6)
O1iv—Ca1—V2v115.47 (5)O4—V1—Ca1xii130.10 (6)
V1—Ca1—V2v64.69 (2)V2iii—V1—Ca1xii107.308 (17)
O2i—Ca1—V2vi79.18 (6)V2—V1—Ca1xii107.308 (17)
O2ii—Ca1—V2vi165.33 (6)Ca1—V1—Ca1xii164.20 (3)
O4—Ca1—V2vi88.50 (6)Ca1x—V1—Ca1xii93.45 (3)
O4iii—Ca1—V2vi34.88 (5)O1—V1—Ca1xiii48.35 (10)
O3iii—Ca1—V2vi35.13 (5)O3x—V1—Ca1xiii134.79 (6)
O3—Ca1—V2vi88.04 (6)O3xi—V1—Ca1xiii134.79 (6)
O1iv—Ca1—V2vi115.47 (5)O4iii—V1—Ca1xiii76.44 (6)
V1—Ca1—V2vi64.69 (2)O4—V1—Ca1xiii76.44 (6)
V2v—Ca1—V2vi90.02 (4)V2iii—V1—Ca1xiii103.723 (17)
O2i—Ca1—V1vii103.19 (6)V2—V1—Ca1xiii103.723 (17)
O2ii—Ca1—V1vii103.19 (6)Ca1—V1—Ca1xiii83.91 (3)
O4—Ca1—V1vii92.65 (6)Ca1x—V1—Ca1xiii173.74 (3)
O4iii—Ca1—V1vii92.65 (6)Ca1xii—V1—Ca1xiii80.30 (3)
O3iii—Ca1—V1vii34.10 (5)O1—V1—Ca1xiv75.688 (14)
O3—Ca1—V1vii34.10 (5)O3x—V1—Ca1xiv54.62 (6)
O1iv—Ca1—V1vii177.01 (8)O3xi—V1—Ca1xiv138.52 (6)
V1—Ca1—V1vii102.35 (4)O4iii—V1—Ca1xiv138.27 (6)
V2v—Ca1—V1vii62.70 (2)O4—V1—Ca1xiv54.99 (6)
V2vi—Ca1—V1vii62.70 (2)V2iii—V1—Ca1xiv173.65 (3)
O2i—Ca1—O1viii68.34 (6)V2—V1—Ca1xiv34.98 (2)
O2ii—Ca1—O1viii68.34 (6)Ca1—V1—Ca1xiv99.343 (15)
O4—Ca1—O1viii139.23 (6)Ca1x—V1—Ca1xiv98.479 (15)
O4iii—Ca1—O1viii139.23 (6)Ca1xii—V1—Ca1xiv78.054 (13)
O3iii—Ca1—O1viii72.62 (7)Ca1xiii—V1—Ca1xiv80.317 (13)
O3—Ca1—O1viii72.62 (7)O2—V2—O4xiv108.83 (10)
O1iv—Ca1—O1viii119.95 (11)O2—V2—O4112.35 (10)
V1—Ca1—O1viii165.39 (6)O4xiv—V2—O4138.76 (5)
V2v—Ca1—O1viii105.76 (4)O2—V2—O3xiv106.13 (10)
V2vi—Ca1—O1viii105.76 (4)O4xiv—V2—O3xiv89.52 (9)
V1vii—Ca1—O1viii63.04 (6)O4—V2—O3xiv81.32 (9)
O2i—Ca1—V2i15.72 (6)O2—V2—O3x114.59 (11)
O2ii—Ca1—V2i94.51 (7)O4xiv—V2—O3x81.18 (9)
O4—Ca1—V2i153.37 (6)O4—V2—O3x80.08 (9)
O4iii—Ca1—V2i100.25 (5)O3xiv—V2—O3x139.10 (5)
O3iii—Ca1—V2i91.10 (5)O2—V2—V2v114.26 (7)
O3—Ca1—V2i136.53 (6)O4xiv—V2—V2v120.55 (7)
O1iv—Ca1—V2i69.83 (6)O4—V2—V2v40.52 (6)
V1—Ca1—V2i124.97 (2)O3xiv—V2—V2v40.85 (6)
V2v—Ca1—V2i170.33 (3)O3x—V2—V2v113.42 (7)
V2vi—Ca1—V2i94.82 (2)O2—V2—V2xiv120.56 (8)
V1vii—Ca1—V2i112.35 (2)O4xiv—V2—V2xiv40.56 (6)
O1viii—Ca1—V2i64.86 (4)O4—V2—V2xiv111.54 (7)
O2i—Ca1—V2ii94.51 (7)O3xiv—V2—V2xiv118.37 (7)
O2ii—Ca1—V2ii15.72 (6)O3x—V2—V2xiv40.66 (6)
O4—Ca1—V2ii100.25 (5)V2v—V2—V2xiv125.16 (4)
O4iii—Ca1—V2ii153.37 (6)O2—V2—V1127.59 (10)
O3iii—Ca1—V2ii136.53 (6)O4xiv—V2—V1108.85 (7)
O3—Ca1—V2ii91.10 (5)O4—V2—V140.53 (6)
O1iv—Ca1—V2ii69.83 (6)O3xiv—V2—V1109.26 (7)
V1—Ca1—V2ii124.97 (2)O3x—V2—V140.36 (6)
V2v—Ca1—V2ii94.82 (2)V2v—V2—V174.10 (3)
V2vi—Ca1—V2ii170.33 (3)V2xiv—V2—V172.53 (3)
V1vii—Ca1—V2ii112.35 (2)O2—V2—Ca1xiv118.06 (10)
O1viii—Ca1—V2ii64.86 (4)O4xiv—V2—Ca1xiv44.27 (6)
V2i—Ca1—V2ii79.22 (3)O4—V2—Ca1xiv113.29 (7)
O2i—Ca1—V1iv68.25 (6)O3xiv—V2—Ca1xiv45.42 (6)
O2ii—Ca1—V1iv68.25 (6)O3x—V2—Ca1xiv112.57 (7)
O4—Ca1—V1iv101.10 (6)V2v—V2—Ca1xiv79.24 (3)
O4iii—Ca1—V1iv101.10 (6)V2xiv—V2—Ca1xiv76.59 (3)
O3iii—Ca1—V1iv144.88 (5)V1—V2—Ca1xiv114.35 (3)
O3—Ca1—V1iv144.88 (5)O2—V2—Ca1ii23.19 (9)
O1iv—Ca1—V1iv19.65 (7)O4xiv—V2—Ca1ii95.49 (6)
V1—Ca1—V1iv94.32 (3)O4—V2—Ca1ii123.90 (6)
V2v—Ca1—V1iv126.42 (2)O3xiv—V2—Ca1ii87.50 (6)
V2vi—Ca1—V1iv126.42 (2)O3x—V2—Ca1ii132.82 (6)
V1vii—Ca1—V1iv163.33 (3)V2v—V2—Ca1ii108.61 (3)
O1viii—Ca1—V1iv100.29 (6)V2xiv—V2—Ca1ii121.91 (3)
V2i—Ca1—V1iv56.19 (2)V1—V2—Ca1ii150.08 (3)
V2ii—Ca1—V1iv56.19 (2)Ca1xiv—V2—Ca1ii95.16 (2)
O2i—Ca1—V2146.03 (6)O2—V2—Ca184.92 (9)
O2ii—Ca1—V270.66 (6)O4xiv—V2—Ca1164.60 (7)
O4—Ca1—V222.52 (5)O4—V2—Ca127.84 (6)
O4iii—Ca1—V282.77 (5)O3xiv—V2—Ca193.30 (6)
O3iii—Ca1—V2128.47 (6)O3x—V2—Ca186.83 (7)
O3—Ca1—V280.49 (5)V2v—V2—Ca156.11 (2)
O1iv—Ca1—V268.19 (5)V2xiv—V2—Ca1126.48 (3)
V1—Ca1—V247.580 (15)V1—V2—Ca155.99 (2)
V2v—Ca1—V247.303 (14)Ca1xiv—V2—Ca1135.32 (3)
V2vi—Ca1—V2109.08 (3)Ca1ii—V2—Ca199.76 (2)
V1vii—Ca1—V2109.87 (3)O2—V2—Ca1x89.18 (9)
O1viii—Ca1—V2134.688 (15)O4xiv—V2—Ca1x90.34 (6)
V2i—Ca1—V2137.44 (3)O4—V2—Ca1x88.19 (6)
V2ii—Ca1—V280.24 (2)O3xiv—V2—Ca1x163.85 (7)
V1iv—Ca1—V281.44 (2)O3x—V2—Ca1x25.45 (6)
O2i—Ca1—V2iii70.66 (6)V2v—V2—Ca1x127.98 (3)
O2ii—Ca1—V2iii146.03 (6)V2xiv—V2—Ca1x54.58 (2)
O4—Ca1—V2iii82.77 (5)V1—V2—Ca1x55.73 (2)
O4iii—Ca1—V2iii22.52 (5)Ca1xiv—V2—Ca1x131.16 (2)
O3iii—Ca1—V2iii80.49 (5)Ca1ii—V2—Ca1x108.58 (2)
O3—Ca1—V2iii128.47 (6)Ca1—V2—Ca1x82.77 (2)
O1iv—Ca1—V2iii68.19 (5)V1—O1—Ca1xii128.40 (15)
V1—Ca1—V2iii47.580 (15)V1—O1—Ca1xiii111.65 (13)
V2v—Ca1—V2iii109.08 (3)Ca1xii—O1—Ca1xiii119.95 (11)
V2vi—Ca1—V2iii47.303 (14)V1—O1—Ca1x37.79 (8)
V1vii—Ca1—V2iii109.87 (3)Ca1xii—O1—Ca1x90.61 (8)
O1viii—Ca1—V2iii134.688 (15)Ca1xiii—O1—Ca1x149.44 (9)
V2i—Ca1—V2iii80.24 (2)V1—O1—Ca132.68 (8)
V2ii—Ca1—V2iii137.44 (3)Ca1xii—O1—Ca1161.08 (11)
V1iv—Ca1—V2iii81.44 (2)Ca1xiii—O1—Ca178.97 (6)
V2—Ca1—V2iii90.56 (3)Ca1x—O1—Ca170.47 (5)
O2i—Ca1—V2ix58.80 (6)V2—O2—Ca1ii141.10 (14)
O2ii—Ca1—V2ix127.60 (6)V2—O2—Ca172.20 (8)
O4—Ca1—V2ix126.44 (6)Ca1ii—O2—Ca1128.33 (7)
O4iii—Ca1—V2ix79.53 (5)V2—O2—Ca1x69.07 (8)
O3iii—Ca1—V2ix20.39 (5)Ca1ii—O2—Ca1x140.57 (8)
O3—Ca1—V2ix80.10 (6)Ca1—O2—Ca1x77.26 (5)
O1iv—Ca1—V2ix134.57 (3)V2—O2—Ca1xiv42.93 (7)
V1—Ca1—V2ix110.73 (3)Ca1ii—O2—Ca1xiv98.53 (8)
V2v—Ca1—V2ix106.54 (3)Ca1—O2—Ca1xiv105.67 (5)
V2vi—Ca1—V2ix46.183 (15)Ca1x—O2—Ca1xiv102.00 (5)
V1vii—Ca1—V2ix46.236 (15)V1vii—O3—V2v128.29 (11)
O1viii—Ca1—V2ix59.90 (4)V1vii—O3—V2vii99.13 (9)
V2i—Ca1—V2ix71.42 (2)V2v—O3—V2vii98.49 (10)
V2ii—Ca1—V2ix124.21 (3)V1vii—O3—Ca1101.98 (9)
V1iv—Ca1—V2ix127.03 (2)V2v—O3—Ca199.46 (8)
V2—Ca1—V2ix148.84 (3)V2vii—O3—Ca1134.16 (10)
V2iii—Ca1—V2ix82.77 (2)V1vii—O3—Ca1xiii65.35 (6)
O2i—Ca1—V2vii127.60 (6)V2v—O3—Ca1xiii64.23 (6)
O2ii—Ca1—V2vii58.80 (6)V2vii—O3—Ca1xiii122.97 (8)
O4—Ca1—V2vii79.53 (5)Ca1—O3—Ca1xiii102.82 (6)
O4iii—Ca1—V2vii126.44 (6)V1vii—O3—Ca1vii48.93 (5)
O3iii—Ca1—V2vii80.10 (6)V2v—O3—Ca1vii160.76 (9)
O3—Ca1—V2vii20.39 (5)V2vii—O3—Ca1vii66.01 (6)
O1iv—Ca1—V2vii134.57 (3)Ca1—O3—Ca1vii99.63 (7)
V1—Ca1—V2vii110.73 (3)Ca1xiii—O3—Ca1vii113.47 (5)
V2v—Ca1—V2vii46.183 (14)V1vii—O3—Ca1v104.56 (7)
V2vi—Ca1—V2vii106.54 (3)V2v—O3—Ca1v60.92 (6)
V1vii—Ca1—V2vii46.236 (15)V2vii—O3—Ca1v43.61 (5)
O1viii—Ca1—V2vii59.90 (4)Ca1—O3—Ca1v153.25 (7)
V2i—Ca1—V2vii124.21 (3)Ca1xiii—O3—Ca1v85.44 (4)
V2ii—Ca1—V2vii71.42 (2)Ca1vii—O3—Ca1v100.21 (4)
V1iv—Ca1—V2vii127.03 (2)V2v—O4—V298.92 (10)
V2—Ca1—V2vii82.77 (2)V2v—O4—V1132.62 (11)
V2iii—Ca1—V2vii148.84 (3)V2—O4—V199.19 (9)
V2ix—Ca1—V2vii87.38 (3)V2v—O4—Ca1100.85 (8)
O2i—Ca1—O2132.43 (4)V2—O4—Ca1129.63 (10)
O2ii—Ca1—O251.67 (7)V1—O4—Ca1100.39 (9)
O4—Ca1—O245.22 (6)V2v—O4—Ca1xiii58.06 (5)
O4iii—Ca1—O2100.72 (6)V2—O4—Ca1xiii132.27 (8)
O3iii—Ca1—O2149.50 (7)V1—O4—Ca1xiii77.60 (6)
O3—Ca1—O289.03 (6)Ca1—O4—Ca1xiii97.21 (6)
O1iv—Ca1—O256.39 (4)V2v—O4—Ca1x161.84 (9)
V1—Ca1—O266.90 (4)V2—O4—Ca1x65.67 (6)
V2v—Ca1—O262.24 (4)V1—O4—Ca1x47.10 (5)
V2vi—Ca1—O2130.97 (4)Ca1—O4—Ca1x96.63 (6)
V1vii—Ca1—O2122.65 (4)Ca1xiii—O4—Ca1x124.54 (5)
O1viii—Ca1—O2119.82 (4)V2v—O4—Ca1xiv63.94 (6)
V2i—Ca1—O2119.36 (4)V2—O4—Ca1xiv43.20 (5)
V2ii—Ca1—O258.62 (3)V1—O4—Ca1xiv104.06 (7)
V1iv—Ca1—O264.18 (4)Ca1—O4—Ca1xiv155.40 (7)
V2—Ca1—O222.87 (3)Ca1xiii—O4—Ca1xiv90.69 (4)
V2iii—Ca1—O2101.85 (4)Ca1x—O4—Ca1xiv97.95 (4)
V2ix—Ca1—O2168.69 (4)V2v—O4—Ca1ii90.36 (7)
V2vii—Ca1—O283.41 (4)V2—O4—Ca1ii37.46 (5)
O1—V1—O3x109.30 (10)V1—O4—Ca1ii128.29 (8)
O1—V1—O3xi109.30 (10)Ca1—O4—Ca1ii96.62 (6)
O3x—V1—O3xi86.53 (13)Ca1xiii—O4—Ca1ii147.40 (5)
O1—V1—O4iii111.25 (9)Ca1x—O4—Ca1ii82.76 (3)
O3x—V1—O4iii139.45 (10)Ca1xiv—O4—Ca1ii65.85 (3)
O3xi—V1—O4iii79.99 (9)
Symmetry codes: (i) x, y1/2, z+1; (ii) x, y+1, z+1; (iii) x, y+1/2, z; (iv) x1/2, y, z+3/2; (v) x+1/2, y+1, z1/2; (vi) x+1/2, y1/2, z1/2; (vii) x, y, z1; (viii) x1/2, y, z+1/2; (ix) x, y+1/2, z1; (x) x, y, z+1; (xi) x, y+1/2, z+1; (xii) x+1/2, y, z+3/2; (xiii) x+1/2, y, z+1/2; (xiv) x+1/2, y+1, z+1/2.
(CaV3O7_250K) top
Crystal data top
O7V3·CaF(000) = 580
Mr = 304.90Dx = 3.537 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2742 reflections
a = 10.436 (3) Åθ = 1.3–23.4°
b = 10.367 (2) ŵ = 5.67 mm1
c = 5.2921 (15) ÅT = 250 K
V = 572.6 (3) Å3, brown
Z = 40.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
403 independent reflections
Radiation source: fine-focus sealed tube366 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
Detector resolution: 0 pixels mm-1θmax = 23.0°, θmin = 3.9°
Rotation method scansh = 1111
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1010
Tmin = 0.317, Tmax = 0.471l = 55
2476 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019 w = 1/[σ2(Fo2) + (0.0472P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055(Δ/σ)max < 0.001
S = 0.94Δρmax = 0.35 e Å3
403 reflectionsΔρmin = 0.39 e Å3
38 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0175 (16)
Crystal data top
O7V3·CaV = 572.6 (3) Å3
Mr = 304.90Z = 4
Orthorhombic, PnmaMo Kα radiation
a = 10.436 (3) ŵ = 5.67 mm1
b = 10.367 (2) ÅT = 250 K
c = 5.2921 (15) Å0.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
403 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
366 reflections with I > 2σ(I)
Tmin = 0.317, Tmax = 0.471Rint = 0.034
2476 measured reflectionsθmax = 23.0°
Refinement top
R[F2 > 2σ(F2)] = 0.01938 parameters
wR(F2) = 0.0550 restraints
S = 0.94Δρmax = 0.35 e Å3
403 reflectionsΔρmin = 0.39 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.08473 (9)0.25000.29954 (15)0.0073 (3)
V10.28868 (7)0.25000.79217 (13)0.0058 (3)
V20.18742 (6)0.52032 (6)0.78363 (10)0.0058 (3)
O10.4435 (3)0.25000.8083 (5)0.0119 (8)*
O20.0401 (2)0.5658 (3)0.7668 (4)0.0134 (6)*
O30.22036 (19)0.3798 (2)0.0260 (4)0.0067 (5)*
O40.22672 (19)0.3796 (2)0.5482 (4)0.0071 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0055 (5)0.0071 (6)0.0092 (6)0.0000.0004 (3)0.000
V10.0060 (5)0.0052 (6)0.0060 (5)0.0000.0003 (3)0.000
V20.0060 (4)0.0054 (4)0.0061 (4)0.0009 (2)0.0000 (2)0.0000 (2)
Geometric parameters (Å, º) top
Ca1—O2i2.339 (3)V1—Ca1xiii4.3990 (15)
Ca1—O2ii2.339 (3)V1—Ca1xiv5.3493 (12)
Ca1—O42.394 (2)V2—O21.610 (2)
Ca1—O4iii2.394 (2)V2—O4xiv1.960 (2)
Ca1—O32.431 (2)V2—O3xiv1.964 (2)
Ca1—O3iii2.431 (2)V2—O41.962 (2)
Ca1—O1iv2.545 (3)V2—O3x1.971 (2)
Ca1—V13.3656 (13)V2—V2xiv2.9808 (9)
Ca1—V2v3.3662 (11)V2—V2v2.9808 (9)
Ca1—V2vi3.3662 (11)V2—Ca1xiv3.3662 (11)
Ca1—V1vii3.4264 (13)V2—Ca1ii3.7323 (11)
Ca1—O1viii3.538 (3)V2—Ca1x4.0566 (10)
Ca1—V2i3.7323 (11)O1—Ca1xii2.545 (3)
Ca1—V2ii3.7323 (11)O1—Ca1xiii3.538 (3)
Ca1—V1iv3.7702 (14)O1—Ca1x4.559 (3)
Ca1—V23.9452 (10)O2—Ca1ii2.339 (3)
Ca1—V2iii3.9452 (10)O2—Ca1x4.345 (3)
Ca1—V2ix4.0566 (10)O2—Ca1xiv4.359 (3)
Ca1—V2vii4.0566 (10)O3—V1vii1.962 (2)
Ca1—O24.129 (3)O3—V2v1.964 (2)
V1—O11.618 (3)O3—V2vii1.971 (2)
V1—O3x1.962 (2)O3—Ca1xiii4.138 (2)
V1—O3xi1.962 (2)O3—Ca1vii4.312 (2)
V1—O4iii1.972 (2)O3—Ca1v4.506 (2)
V1—O41.972 (2)O4—V2v1.960 (2)
V1—V2iii2.9953 (9)O4—Ca1xiii4.376 (2)
V1—V22.9953 (9)O4—Ca1x4.451 (2)
V1—Ca1x3.4264 (13)O4—Ca1xiv4.515 (2)
V1—Ca1xii3.7702 (14)O4—Ca1ii5.095 (2)
O2i—Ca1—O2ii109.51 (12)O1—V1—O4111.21 (10)
O2i—Ca1—O4152.33 (8)O3x—V1—O480.02 (9)
O2ii—Ca1—O488.23 (7)O3xi—V1—O4139.54 (10)
O2i—Ca1—O4iii88.23 (7)O4iii—V1—O485.87 (12)
O2ii—Ca1—O4iii152.33 (8)O1—V1—V2iii110.678 (18)
O4—Ca1—O4iii68.27 (10)O3x—V1—V2iii121.52 (7)
O2i—Ca1—O3133.41 (8)O3xi—V1—V2iii40.52 (6)
O2ii—Ca1—O377.47 (7)O4iii—V1—V2iii40.29 (6)
O4—Ca1—O369.90 (7)O4—V1—V2iii120.78 (7)
O4iii—Ca1—O3106.11 (8)O1—V1—V2110.678 (18)
O2i—Ca1—O3iii77.47 (7)O3x—V1—V240.52 (6)
O2ii—Ca1—O3iii133.41 (8)O3xi—V1—V2121.52 (7)
O4—Ca1—O3iii106.11 (8)O4iii—V1—V2120.78 (7)
O4iii—Ca1—O3iii69.90 (7)O4—V1—V240.29 (6)
O3—Ca1—O3iii67.22 (10)V2iii—V1—V2138.64 (4)
O2i—Ca1—O1iv78.45 (7)O1—V1—Ca1132.25 (11)
O2ii—Ca1—O1iv78.45 (7)O3x—V1—Ca1105.00 (6)
O4—Ca1—O1iv84.84 (8)O3xi—V1—Ca1105.00 (6)
O4iii—Ca1—O1iv84.84 (8)O4iii—V1—Ca144.40 (6)
O3—Ca1—O1iv145.35 (5)O4—V1—Ca144.40 (6)
O3iii—Ca1—O1iv145.35 (5)V2iii—V1—Ca176.419 (17)
O2i—Ca1—V1117.95 (6)V2—V1—Ca176.419 (17)
O2ii—Ca1—V1117.95 (6)O1—V1—Ca1x125.39 (11)
O4—Ca1—V135.20 (5)O3x—V1—Ca1x43.95 (6)
O4iii—Ca1—V135.20 (5)O3xi—V1—Ca1x43.95 (6)
O3—Ca1—V195.33 (6)O4iii—V1—Ca1x108.02 (7)
O3iii—Ca1—V195.33 (6)O4—V1—Ca1x108.02 (7)
O1iv—Ca1—V174.60 (7)V2iii—V1—Ca1x78.034 (18)
O2i—Ca1—V2v165.37 (6)V2—V1—Ca1x78.034 (18)
O2ii—Ca1—V2v79.18 (6)Ca1—V1—Ca1x102.37 (4)
O4—Ca1—V2v34.88 (5)O1—V1—Ca1xii31.95 (10)
O4iii—Ca1—V2v88.48 (6)O3x—V1—Ca1xii86.35 (6)
O3—Ca1—V2v35.14 (5)O3xi—V1—Ca1xii86.35 (6)
O3iii—Ca1—V2v88.01 (6)O4iii—V1—Ca1xii130.08 (6)
O1iv—Ca1—V2v115.43 (5)O4—V1—Ca1xii130.08 (6)
V1—Ca1—V2v64.70 (2)V2iii—V1—Ca1xii107.324 (17)
O2i—Ca1—V2vi79.18 (6)V2—V1—Ca1xii107.324 (17)
O2ii—Ca1—V2vi165.37 (6)Ca1—V1—Ca1xii164.20 (3)
O4—Ca1—V2vi88.48 (6)Ca1x—V1—Ca1xii93.44 (3)
O4iii—Ca1—V2vi34.88 (5)O1—V1—Ca1xiii48.40 (10)
O3—Ca1—V2vi88.01 (6)O3x—V1—Ca1xiii134.76 (6)
O3iii—Ca1—V2vi35.14 (5)O3xi—V1—Ca1xiii134.76 (6)
O1iv—Ca1—V2vi115.43 (5)O4iii—V1—Ca1xiii76.37 (6)
V1—Ca1—V2vi64.70 (2)O4—V1—Ca1xiii76.37 (6)
V2v—Ca1—V2vi90.04 (4)V2iii—V1—Ca1xiii103.712 (17)
O2i—Ca1—V1vii103.21 (6)V2—V1—Ca1xiii103.712 (17)
O2ii—Ca1—V1vii103.21 (6)Ca1—V1—Ca1xiii83.84 (3)
O4—Ca1—V1vii92.65 (6)Ca1x—V1—Ca1xiii173.79 (3)
O4iii—Ca1—V1vii92.65 (6)Ca1xii—V1—Ca1xiii80.35 (3)
O3—Ca1—V1vii34.07 (5)O1—V1—Ca1xiv75.699 (14)
O3iii—Ca1—V1vii34.07 (5)O3x—V1—Ca1xiv54.60 (6)
O1iv—Ca1—V1vii176.97 (8)O3xi—V1—Ca1xiv138.55 (6)
V1—Ca1—V1vii102.37 (4)O4iii—V1—Ca1xiv138.23 (6)
V2v—Ca1—V1vii62.71 (2)O4—V1—Ca1xiv54.95 (6)
V2vi—Ca1—V1vii62.71 (2)V2iii—V1—Ca1xiv173.62 (3)
O2i—Ca1—O1viii68.38 (6)V2—V1—Ca1xiv34.98 (2)
O2ii—Ca1—O1viii68.38 (6)Ca1—V1—Ca1xiv99.314 (15)
O4—Ca1—O1viii139.24 (6)Ca1x—V1—Ca1xiv98.495 (15)
O4iii—Ca1—O1viii139.24 (6)Ca1xii—V1—Ca1xiv78.078 (13)
O3—Ca1—O1viii72.61 (7)Ca1xiii—V1—Ca1xiv80.312 (13)
O3iii—Ca1—O1viii72.61 (7)O2—V2—O4xiv108.74 (10)
O1iv—Ca1—O1viii120.02 (11)O2—V2—O3xiv105.97 (10)
V1—Ca1—O1viii165.38 (6)O4xiv—V2—O3xiv89.58 (9)
V2v—Ca1—O1viii105.75 (4)O2—V2—O4112.45 (10)
V2vi—Ca1—O1viii105.75 (4)O4xiv—V2—O4138.76 (5)
V1vii—Ca1—O1viii63.02 (6)O3xiv—V2—O481.31 (9)
O2i—Ca1—V2i15.69 (6)O2—V2—O3x114.75 (11)
O2ii—Ca1—V2i94.55 (7)O4xiv—V2—O3x81.18 (9)
O4—Ca1—V2i153.35 (6)O3xiv—V2—O3x139.11 (4)
O4iii—Ca1—V2i100.24 (5)O4—V2—O3x80.05 (8)
O3—Ca1—V2i136.56 (6)O2—V2—V2xiv120.59 (7)
O3iii—Ca1—V2i91.14 (5)O4xiv—V2—V2xiv40.55 (6)
O1iv—Ca1—V2i69.86 (5)O3xiv—V2—V2xiv118.42 (7)
V1—Ca1—V2i124.93 (2)O4—V2—V2xiv111.53 (7)
V2v—Ca1—V2i170.36 (3)O3x—V2—V2xiv40.67 (6)
V2vi—Ca1—V2i94.78 (2)O2—V2—V2v114.24 (7)
V1vii—Ca1—V2i112.35 (2)O4xiv—V2—V2v120.58 (7)
O1viii—Ca1—V2i64.90 (4)O3xiv—V2—V2v40.86 (6)
O2i—Ca1—V2ii94.55 (7)O4—V2—V2v40.49 (6)
O2ii—Ca1—V2ii15.69 (6)O3x—V2—V2v113.38 (7)
O4—Ca1—V2ii100.24 (5)V2xiv—V2—V2v125.17 (4)
O4iii—Ca1—V2ii153.35 (6)O2—V2—V1127.69 (10)
O3—Ca1—V2ii91.14 (5)O4xiv—V2—V1108.86 (6)
O3iii—Ca1—V2ii136.56 (6)O3xiv—V2—V1109.32 (6)
O1iv—Ca1—V2ii69.86 (5)O4—V2—V140.55 (6)
V1—Ca1—V2ii124.93 (2)O3x—V2—V140.29 (6)
V2v—Ca1—V2ii94.78 (2)V2xiv—V2—V172.53 (3)
V2vi—Ca1—V2ii170.36 (3)V2v—V2—V174.13 (3)
V1vii—Ca1—V2ii112.35 (2)O2—V2—Ca1xiv117.96 (10)
O1viii—Ca1—V2ii64.90 (4)O4xiv—V2—Ca1xiv44.32 (6)
V2i—Ca1—V2ii79.28 (3)O3xiv—V2—Ca1xiv45.43 (6)
O2i—Ca1—V1iv68.24 (6)O4—V2—Ca1xiv113.22 (7)
O2ii—Ca1—V1iv68.24 (6)O3x—V2—Ca1xiv112.54 (7)
O4—Ca1—V1iv101.08 (6)V2xiv—V2—Ca1xiv76.60 (3)
O4iii—Ca1—V1iv101.08 (6)V2v—V2—Ca1xiv79.20 (3)
O3—Ca1—V1iv144.93 (5)V1—V2—Ca1xiv114.34 (3)
O3iii—Ca1—V1iv144.93 (5)O2—V2—Ca1ii23.13 (9)
O1iv—Ca1—V1iv19.66 (7)O4xiv—V2—Ca1ii95.42 (6)
V1—Ca1—V1iv94.26 (3)O3xiv—V2—Ca1ii87.40 (6)
V2v—Ca1—V1iv126.39 (2)O4—V2—Ca1ii123.96 (6)
V2vi—Ca1—V1iv126.39 (2)O3x—V2—Ca1ii132.91 (6)
V1vii—Ca1—V1iv163.37 (3)V2xiv—V2—Ca1ii121.89 (3)
O1viii—Ca1—V1iv100.35 (6)V2v—V2—Ca1ii108.60 (3)
V2i—Ca1—V1iv56.22 (2)V1—V2—Ca1ii150.13 (3)
V2ii—Ca1—V1iv56.22 (2)Ca1xiv—V2—Ca1ii95.12 (2)
O2i—Ca1—V2145.99 (6)O2—V2—Ca184.98 (9)
O2ii—Ca1—V270.65 (6)O4xiv—V2—Ca1164.64 (7)
O4—Ca1—V222.54 (5)O3xiv—V2—Ca193.27 (6)
O4iii—Ca1—V282.74 (5)O4—V2—Ca127.90 (6)
O3—Ca1—V280.52 (5)O3x—V2—Ca186.85 (7)
O3iii—Ca1—V2128.43 (6)V2xiv—V2—Ca1126.52 (3)
O1iv—Ca1—V268.15 (5)V2v—V2—Ca156.10 (2)
V1—Ca1—V247.561 (15)V1—V2—Ca156.02 (2)
V2v—Ca1—V247.305 (14)Ca1xiv—V2—Ca1135.28 (3)
V2vi—Ca1—V2109.07 (3)Ca1ii—V2—Ca199.78 (2)
V1vii—Ca1—V2109.88 (3)O2—V2—Ca1x89.27 (9)
O1viii—Ca1—V2134.708 (15)O4xiv—V2—Ca1x90.33 (6)
V2i—Ca1—V2137.43 (3)O3xiv—V2—Ca1x163.93 (7)
V2ii—Ca1—V280.22 (2)O4—V2—Ca1x88.22 (6)
V1iv—Ca1—V281.40 (2)O3x—V2—Ca1x25.52 (6)
O2i—Ca1—V2iii70.65 (6)V2xiv—V2—Ca1x54.60 (2)
O2ii—Ca1—V2iii145.99 (6)V2v—V2—Ca1x127.99 (3)
O4—Ca1—V2iii82.74 (5)V1—V2—Ca1x55.72 (2)
O4iii—Ca1—V2iii22.54 (5)Ca1xiv—V2—Ca1x131.18 (2)
O3—Ca1—V2iii128.43 (6)Ca1ii—V2—Ca1x108.60 (2)
O3iii—Ca1—V2iii80.52 (5)Ca1—V2—Ca1x82.79 (2)
O1iv—Ca1—V2iii68.15 (5)V1—O1—Ca1xii128.39 (15)
V1—Ca1—V2iii47.561 (16)V1—O1—Ca1xiii111.60 (13)
V2v—Ca1—V2iii109.07 (3)Ca1xii—O1—Ca1xiii120.02 (11)
V2vi—Ca1—V2iii47.305 (15)V1—O1—Ca1x37.79 (8)
V1vii—Ca1—V2iii109.88 (3)Ca1xii—O1—Ca1x90.60 (8)
O1viii—Ca1—V2iii134.708 (15)Ca1xiii—O1—Ca1x149.38 (9)
V2i—Ca1—V2iii80.22 (2)V1—O1—Ca132.70 (8)
V2ii—Ca1—V2iii137.43 (3)Ca1xii—O1—Ca1161.09 (11)
V1iv—Ca1—V2iii81.40 (2)Ca1xiii—O1—Ca178.90 (6)
V2—Ca1—V2iii90.52 (3)Ca1x—O1—Ca170.49 (5)
O2i—Ca1—V2ix58.81 (5)V2—O2—Ca1ii141.19 (14)
O2ii—Ca1—V2ix127.62 (6)V2—O2—Ca172.16 (8)
O4—Ca1—V2ix126.44 (6)Ca1ii—O2—Ca1128.35 (7)
O4iii—Ca1—V2ix79.56 (5)V2—O2—Ca1x68.99 (8)
O3—Ca1—V2ix80.08 (6)Ca1ii—O2—Ca1x140.56 (7)
O3iii—Ca1—V2ix20.45 (5)Ca1—O2—Ca1x77.25 (5)
O1iv—Ca1—V2ix134.57 (3)V2—O2—Ca1xiv43.00 (7)
V1—Ca1—V2ix110.75 (3)Ca1ii—O2—Ca1xiv98.54 (8)
V2v—Ca1—V2ix106.57 (3)Ca1—O2—Ca1xiv105.66 (5)
V2vi—Ca1—V2ix46.202 (15)Ca1x—O2—Ca1xiv102.01 (5)
V1vii—Ca1—V2ix46.248 (15)V1vii—O3—V2v128.41 (11)
O1viii—Ca1—V2ix59.88 (4)V1vii—O3—V2vii99.19 (9)
V2i—Ca1—V2ix71.40 (2)V2v—O3—V2vii98.48 (9)
V2ii—Ca1—V2ix124.22 (3)V1vii—O3—Ca1101.98 (9)
V1iv—Ca1—V2ix127.03 (2)V2v—O3—Ca199.44 (8)
V2—Ca1—V2ix148.87 (3)V2vii—O3—Ca1134.02 (10)
V2iii—Ca1—V2ix82.79 (2)V1vii—O3—Ca1xiii65.41 (6)
O2i—Ca1—V2vii127.62 (6)V2v—O3—Ca1xiii64.30 (6)
O2ii—Ca1—V2vii58.81 (5)V2vii—O3—Ca1xiii123.07 (8)
O4—Ca1—V2vii79.56 (5)Ca1—O3—Ca1xiii102.85 (6)
O4iii—Ca1—V2vii126.44 (6)V1vii—O3—Ca1vii48.93 (5)
O3—Ca1—V2vii20.45 (5)V2v—O3—Ca1vii160.78 (9)
O3iii—Ca1—V2vii80.08 (6)V2vii—O3—Ca1vii65.99 (6)
O1iv—Ca1—V2vii134.57 (3)Ca1—O3—Ca1vii99.61 (7)
V1—Ca1—V2vii110.75 (3)Ca1xiii—O3—Ca1vii113.52 (5)
V2v—Ca1—V2vii46.202 (15)V1vii—O3—Ca1v104.61 (7)
V2vi—Ca1—V2vii106.57 (3)V2v—O3—Ca1v60.94 (6)
V1vii—Ca1—V2vii46.248 (15)V2vii—O3—Ca1v43.63 (5)
O1viii—Ca1—V2vii59.88 (4)Ca1—O3—Ca1v153.22 (7)
V2i—Ca1—V2vii124.22 (3)Ca1xiii—O3—Ca1v85.49 (4)
V2ii—Ca1—V2vii71.40 (2)Ca1vii—O3—Ca1v100.18 (4)
V1iv—Ca1—V2vii127.03 (2)V2v—O4—V298.95 (10)
V2—Ca1—V2vii82.79 (2)V2v—O4—V1132.72 (11)
V2iii—Ca1—V2vii148.87 (3)V2—O4—V199.17 (9)
V2ix—Ca1—V2vii87.39 (3)V2v—O4—Ca1100.80 (8)
O2i—Ca1—O2132.42 (4)V2—O4—Ca1129.56 (10)
O2ii—Ca1—O251.65 (7)V1—O4—Ca1100.40 (9)
O4—Ca1—O245.23 (6)V2v—O4—Ca1xiii58.11 (5)
O4iii—Ca1—O2100.69 (6)V2—O4—Ca1xiii132.36 (8)
O3—Ca1—O289.05 (6)V1—O4—Ca1xiii77.66 (6)
O3iii—Ca1—O2149.44 (7)Ca1—O4—Ca1xiii97.18 (6)
O1iv—Ca1—O256.39 (4)V2v—O4—Ca1x161.87 (9)
V1—Ca1—O266.88 (3)V2—O4—Ca1x65.64 (6)
V2v—Ca1—O262.21 (3)V1—O4—Ca1x47.06 (5)
V2vi—Ca1—O2130.95 (4)Ca1—O4—Ca1x96.64 (6)
V1vii—Ca1—O2122.64 (4)Ca1xiii—O4—Ca1x124.56 (5)
O1viii—Ca1—O2119.84 (4)V2v—O4—Ca1xiv63.95 (6)
V2i—Ca1—O2119.38 (4)V2—O4—Ca1xiv43.25 (5)
V2ii—Ca1—O258.60 (3)V1—O4—Ca1xiv104.10 (7)
V1iv—Ca1—O264.18 (4)Ca1—O4—Ca1xiv155.35 (7)
V2—Ca1—O222.86 (3)Ca1xiii—O4—Ca1xiv90.74 (4)
V2iii—Ca1—O2101.82 (4)Ca1x—O4—Ca1xiv97.97 (4)
V2ix—Ca1—O2168.69 (4)V2v—O4—Ca1ii90.33 (7)
V2vii—Ca1—O283.40 (4)V2—O4—Ca1ii37.42 (5)
O1—V1—O3x109.25 (10)V1—O4—Ca1ii128.24 (8)
O1—V1—O3xi109.25 (10)Ca1—O4—Ca1ii96.60 (6)
O3x—V1—O3xi86.58 (12)Ca1xiii—O4—Ca1ii147.41 (5)
O1—V1—O4iii111.21 (10)Ca1x—O4—Ca1ii82.75 (3)
O3x—V1—O4iii139.54 (10)Ca1xiv—O4—Ca1ii65.83 (3)
O3xi—V1—O4iii80.02 (9)
Symmetry codes: (i) x, y1/2, z+1; (ii) x, y+1, z+1; (iii) x, y+1/2, z; (iv) x1/2, y, z+3/2; (v) x+1/2, y+1, z1/2; (vi) x+1/2, y1/2, z1/2; (vii) x, y, z1; (viii) x1/2, y, z+1/2; (ix) x, y+1/2, z1; (x) x, y, z+1; (xi) x, y+1/2, z+1; (xii) x+1/2, y, z+3/2; (xiii) x+1/2, y, z+1/2; (xiv) x+1/2, y+1, z+1/2.
(CaV3O7_237K) top
Crystal data top
O7V3·CaF(000) = 580
Mr = 304.90Dx = 3.537 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 2671 reflections
a = 10.436 (3) Åθ = 1.3–23.4°
b = 10.368 (2) ŵ = 5.67 mm1
c = 5.2911 (15) ÅT = 237 K
V = 572.5 (2) Å3, brown
Z = 40.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
404 independent reflections
Radiation source: fine-focus sealed tube367 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
Detector resolution: 0 pixels mm-1θmax = 23.0°, θmin = 3.9°
Rotation method scansh = 1111
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
k = 1010
Tmin = 0.317, Tmax = 0.471l = 55
2415 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019 w = 1/[σ2(Fo2) + (0.0477P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.054(Δ/σ)max < 0.001
S = 0.90Δρmax = 0.33 e Å3
404 reflectionsΔρmin = 0.36 e Å3
38 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0185 (15)
Crystal data top
O7V3·CaV = 572.5 (2) Å3
Mr = 304.90Z = 4
Orthorhombic, PnmaMo Kα radiation
a = 10.436 (3) ŵ = 5.67 mm1
b = 10.368 (2) ÅT = 237 K
c = 5.2911 (15) Å0.3 × 0.2 × 0.1 mm
Data collection top
STOE IPDS 2
diffractometer
404 independent reflections
Absorption correction: numerical
X-SHAPE (Stoe & Cie, 1996)
367 reflections with I > 2σ(I)
Tmin = 0.317, Tmax = 0.471Rint = 0.033
2415 measured reflectionsθmax = 23.0°
Refinement top
R[F2 > 2σ(F2)] = 0.01938 parameters
wR(F2) = 0.0540 restraints
S = 0.90Δρmax = 0.33 e Å3
404 reflectionsΔρmin = 0.36 e Å3
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.08481 (9)0.25000.29989 (14)0.0069 (3)
V10.28872 (7)0.25000.79216 (13)0.0052 (3)
V20.18744 (5)0.52030 (5)0.78363 (9)0.0053 (3)
O10.4435 (3)0.25000.8077 (5)0.0113 (8)*
O20.0400 (2)0.5653 (2)0.7667 (4)0.0125 (6)*
O30.22015 (19)0.3798 (2)0.0258 (4)0.0066 (5)*
O40.22661 (19)0.3795 (2)0.5483 (4)0.0065 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0046 (5)0.0071 (6)0.0089 (5)0.0000.0000 (3)0.000
V10.0047 (5)0.0050 (5)0.0061 (5)0.0000.0004 (3)0.000
V20.0051 (4)0.0050 (4)0.0059 (4)0.0008 (2)0.0001 (2)0.00021 (19)
Geometric parameters (Å, º) top
Ca1—O2i2.343 (3)V1—Ca1xiii4.4001 (14)
Ca1—O2ii2.343 (3)V1—Ca1xiv5.3497 (11)
Ca1—O42.392 (2)V2—O21.610 (2)
Ca1—O4iii2.392 (2)V2—O4xiv1.960 (2)
Ca1—O3iii2.431 (2)V2—O41.962 (2)
Ca1—O32.431 (2)V2—O3xiv1.966 (2)
Ca1—O1iv2.547 (3)V2—O3x1.970 (2)
Ca1—V13.3634 (12)V2—V2xiv2.9801 (9)
Ca1—V2v3.3658 (11)V2—V2v2.9801 (9)
Ca1—V2vi3.3658 (11)V2—Ca1xiv3.3658 (11)
Ca1—V1vii3.4271 (13)V2—Ca1ii3.7337 (11)
Ca1—O1viii3.537 (3)V2—Ca1x4.0574 (10)
Ca1—V2i3.7337 (11)O1—Ca1xii2.547 (3)
Ca1—V2ii3.7337 (11)O1—Ca1xiii3.537 (3)
Ca1—V1iv3.7693 (14)O1—Ca1x4.560 (3)
Ca1—V23.9437 (10)O2—Ca1ii2.343 (3)
Ca1—V2iii3.9437 (10)O2—Ca1x4.343 (2)
Ca1—V2ix4.0574 (10)O2—Ca1xiv4.362 (3)
Ca1—V2vii4.0574 (10)O3—V1vii1.962 (2)
Ca1—O24.124 (2)O3—V2v1.966 (2)
V1—O11.617 (3)O3—V2vii1.970 (2)
V1—O3x1.962 (2)O3—Ca1xiii4.141 (2)
V1—O3xi1.962 (2)O3—Ca1vii4.308 (2)
V1—O4iii1.972 (2)O3—Ca1v4.506 (2)
V1—O41.972 (2)O4—V2v1.960 (2)
V1—V2iii2.9956 (8)O4—Ca1xiii4.379 (2)
V1—V22.9956 (8)O4—Ca1x4.451 (2)
V1—Ca1x3.4271 (13)O4—Ca1xiv4.516 (2)
V1—Ca1xii3.7693 (14)O4—Ca1ii5.095 (2)
O2i—Ca1—O2ii109.66 (12)O1—V1—O4111.20 (9)
O2i—Ca1—O4152.33 (8)O3x—V1—O479.94 (8)
O2ii—Ca1—O488.14 (7)O3xi—V1—O4139.41 (10)
O2i—Ca1—O4iii88.14 (7)O4iii—V1—O485.85 (12)
O2ii—Ca1—O4iii152.33 (8)O1—V1—V2iii110.680 (18)
O4—Ca1—O4iii68.33 (10)O3x—V1—V2iii121.50 (7)
O2i—Ca1—O3iii77.34 (7)O3xi—V1—V2iii40.47 (6)
O2ii—Ca1—O3iii133.31 (7)O4iii—V1—V2iii40.27 (6)
O4—Ca1—O3iii106.22 (8)O4—V1—V2iii120.75 (7)
O4iii—Ca1—O3iii69.97 (7)O1—V1—V2110.680 (18)
O2i—Ca1—O3133.31 (7)O3x—V1—V240.47 (6)
O2ii—Ca1—O377.34 (7)O3xi—V1—V2121.50 (7)
O4—Ca1—O369.97 (7)O4iii—V1—V2120.75 (7)
O4iii—Ca1—O3106.22 (8)O4—V1—V240.27 (6)
O3iii—Ca1—O367.23 (10)V2iii—V1—V2138.64 (4)
O2i—Ca1—O1iv78.49 (7)O1—V1—Ca1132.17 (10)
O2ii—Ca1—O1iv78.49 (7)O3x—V1—Ca1104.90 (6)
O4—Ca1—O1iv84.86 (8)O3xi—V1—Ca1104.90 (6)
O4iii—Ca1—O1iv84.86 (8)O4iii—V1—Ca144.38 (6)
O3iii—Ca1—O1iv145.37 (5)O4—V1—Ca144.38 (6)
O3—Ca1—O1iv145.37 (5)V2iii—V1—Ca176.414 (17)
O2i—Ca1—V1117.92 (6)V2—V1—Ca176.414 (17)
O2ii—Ca1—V1117.92 (6)O1—V1—Ca1x125.46 (10)
O4—Ca1—V135.22 (5)O3x—V1—Ca1x43.93 (6)
O4iii—Ca1—V135.22 (5)O3xi—V1—Ca1x43.93 (6)
O3iii—Ca1—V195.42 (6)O4iii—V1—Ca1x107.99 (6)
O3—Ca1—V195.42 (6)O4—V1—Ca1x107.99 (6)
O1iv—Ca1—V174.64 (7)V2iii—V1—Ca1x78.037 (17)
O2i—Ca1—V2v165.29 (6)V2—V1—Ca1x78.037 (17)
O2ii—Ca1—V2v79.07 (6)Ca1—V1—Ca1x102.37 (4)
O4—Ca1—V2v34.90 (5)O1—V1—Ca1xii32.01 (10)
O4iii—Ca1—V2v88.54 (6)O3x—V1—Ca1xii86.46 (6)
O3iii—Ca1—V2v88.06 (6)O3xi—V1—Ca1xii86.46 (6)
O3—Ca1—V2v35.19 (5)O4iii—V1—Ca1xii130.10 (6)
O1iv—Ca1—V2v115.46 (5)O4—V1—Ca1xii130.10 (6)
V1—Ca1—V2v64.72 (2)V2iii—V1—Ca1xii107.330 (17)
O2i—Ca1—V2vi79.07 (6)V2—V1—Ca1xii107.330 (17)
O2ii—Ca1—V2vi165.29 (6)Ca1—V1—Ca1xii164.18 (3)
O4—Ca1—V2vi88.54 (6)Ca1x—V1—Ca1xii93.45 (3)
O4iii—Ca1—V2vi34.90 (5)O1—V1—Ca1xiii48.32 (10)
O3iii—Ca1—V2vi35.19 (5)O3x—V1—Ca1xiii134.79 (6)
O3—Ca1—V2vi88.06 (6)O3xi—V1—Ca1xiii134.79 (6)
O1iv—Ca1—V2vi115.46 (5)O4iii—V1—Ca1xiii76.41 (6)
V1—Ca1—V2vi64.72 (2)O4—V1—Ca1xiii76.41 (6)
V2v—Ca1—V2vi90.08 (3)V2iii—V1—Ca1xiii103.713 (17)
O2i—Ca1—V1vii103.15 (5)V2—V1—Ca1xiii103.713 (17)
O2ii—Ca1—V1vii103.15 (5)Ca1—V1—Ca1xiii83.86 (3)
O4—Ca1—V1vii92.67 (6)Ca1x—V1—Ca1xiii173.77 (3)
O4iii—Ca1—V1vii92.67 (6)Ca1xii—V1—Ca1xiii80.33 (3)
O3iii—Ca1—V1vii34.06 (5)O1—V1—Ca1xiv75.714 (13)
O3—Ca1—V1vii34.06 (5)O3x—V1—Ca1xiv54.59 (6)
O1iv—Ca1—V1vii177.01 (8)O3xi—V1—Ca1xiv138.57 (6)
V1—Ca1—V1vii102.37 (4)O4iii—V1—Ca1xiv138.25 (6)
V2v—Ca1—V1vii62.71 (2)O4—V1—Ca1xiv54.98 (6)
V2vi—Ca1—V1vii62.71 (2)V2iii—V1—Ca1xiv173.61 (2)
O2i—Ca1—O1viii68.38 (6)V2—V1—Ca1xiv34.970 (19)
O2ii—Ca1—O1viii68.38 (6)Ca1—V1—Ca1xiv99.323 (14)
O4—Ca1—O1viii139.23 (6)Ca1x—V1—Ca1xiv98.464 (14)
O4iii—Ca1—O1viii139.23 (6)Ca1xii—V1—Ca1xiv78.076 (13)
O3iii—Ca1—O1viii72.54 (6)Ca1xiii—V1—Ca1xiv80.340 (13)
O3—Ca1—O1viii72.54 (6)O2—V2—O4xiv108.87 (10)
O1iv—Ca1—O1viii119.96 (11)O2—V2—O4112.29 (10)
V1—Ca1—O1viii165.40 (6)O4xiv—V2—O4138.78 (5)
V2v—Ca1—O1viii105.74 (4)O2—V2—O3xiv106.10 (10)
V2vi—Ca1—O1viii105.74 (4)O4xiv—V2—O3xiv89.55 (9)
V1vii—Ca1—O1viii63.03 (6)O4—V2—O3xiv81.32 (9)
O2i—Ca1—V2i15.77 (6)O2—V2—O3x114.59 (10)
O2ii—Ca1—V2i94.62 (7)O4xiv—V2—O3x81.25 (9)
O4—Ca1—V2i153.39 (5)O4—V2—O3x80.02 (8)
O4iii—Ca1—V2i100.23 (5)O3xiv—V2—O3x139.12 (4)
O3iii—Ca1—V2i91.05 (5)O2—V2—V2xiv120.60 (7)
O3—Ca1—V2i136.44 (6)O4xiv—V2—V2xiv40.56 (6)
O1iv—Ca1—V2i69.86 (5)O4—V2—V2xiv111.54 (6)
V1—Ca1—V2i124.97 (2)O3xiv—V2—V2xiv118.40 (7)
V2v—Ca1—V2i170.30 (2)O3x—V2—V2xiv40.73 (6)
V2vi—Ca1—V2i94.76 (2)O2—V2—V2v114.21 (7)
V1vii—Ca1—V2i112.32 (2)O4xiv—V2—V2v120.56 (7)
O1viii—Ca1—V2i64.86 (4)O4—V2—V2v40.54 (6)
O2i—Ca1—V2ii94.62 (7)O3xiv—V2—V2v40.83 (6)
O2ii—Ca1—V2ii15.77 (6)O3x—V2—V2v113.39 (7)
O4—Ca1—V2ii100.23 (5)V2xiv—V2—V2v125.18 (4)
O4iii—Ca1—V2ii153.39 (5)O2—V2—V1127.52 (9)
O3iii—Ca1—V2ii136.44 (6)O4xiv—V2—V1108.87 (6)
O3—Ca1—V2ii91.05 (5)O4—V2—V140.53 (6)
O1iv—Ca1—V2ii69.86 (5)O3xiv—V2—V1109.29 (6)
V1—Ca1—V2ii124.97 (2)O3x—V2—V140.29 (6)
V2v—Ca1—V2ii94.76 (2)V2xiv—V2—V172.54 (2)
V2vi—Ca1—V2ii170.30 (2)V2v—V2—V174.14 (3)
V1vii—Ca1—V2ii112.32 (2)O2—V2—Ca1xiv118.11 (9)
O1viii—Ca1—V2ii64.86 (4)O4xiv—V2—Ca1xiv44.26 (6)
V2i—Ca1—V2ii79.27 (3)O4—V2—Ca1xiv113.30 (6)
O2i—Ca1—V1iv68.30 (6)O3xiv—V2—Ca1xiv45.45 (6)
O2ii—Ca1—V1iv68.30 (6)O3x—V2—Ca1xiv112.60 (7)
O4—Ca1—V1iv101.10 (5)V2xiv—V2—Ca1xiv76.58 (3)
O4iii—Ca1—V1iv101.10 (5)V2v—V2—Ca1xiv79.24 (3)
O3iii—Ca1—V1iv144.88 (5)V1—V2—Ca1xiv114.36 (3)
O3—Ca1—V1iv144.88 (5)O2—V2—Ca1ii23.29 (9)
O1iv—Ca1—V1iv19.67 (7)O4xiv—V2—Ca1ii95.44 (6)
V1—Ca1—V1iv94.31 (3)O4—V2—Ca1ii123.92 (6)
V2v—Ca1—V1iv126.408 (19)O3xiv—V2—Ca1ii87.43 (6)
V2vi—Ca1—V1iv126.408 (19)O3x—V2—Ca1ii132.89 (6)
V1vii—Ca1—V1iv163.32 (3)V2xiv—V2—Ca1ii121.91 (3)
O1viii—Ca1—V1iv100.29 (6)V2v—V2—Ca1ii108.57 (3)
V2i—Ca1—V1iv56.22 (2)V1—V2—Ca1ii150.12 (3)
V2ii—Ca1—V1iv56.22 (2)Ca1xiv—V2—Ca1ii95.11 (2)
O2i—Ca1—V2146.05 (6)O2—V2—Ca184.85 (8)
O2ii—Ca1—V270.59 (6)O4xiv—V2—Ca1164.63 (6)
O4—Ca1—V222.53 (5)O4—V2—Ca127.85 (6)
O4iii—Ca1—V282.79 (5)O3xiv—V2—Ca193.28 (6)
O3iii—Ca1—V2128.53 (6)O3x—V2—Ca186.77 (6)
O3—Ca1—V280.56 (5)V2xiv—V2—Ca1126.50 (3)
O1iv—Ca1—V268.17 (5)V2v—V2—Ca156.11 (2)
V1—Ca1—V247.590 (15)V1—V2—Ca156.00 (2)
V2v—Ca1—V247.309 (14)Ca1xiv—V2—Ca1135.33 (2)
V2vi—Ca1—V2109.13 (3)Ca1ii—V2—Ca199.777 (19)
V1vii—Ca1—V2109.88 (3)O2—V2—Ca1x89.17 (8)
O1viii—Ca1—V2134.680 (15)O4xiv—V2—Ca1x90.33 (6)
V2i—Ca1—V2137.46 (2)O4—V2—Ca1x88.20 (6)
V2ii—Ca1—V280.223 (19)O3xiv—V2—Ca1x163.88 (6)
V1iv—Ca1—V281.43 (2)O3x—V2—Ca1x25.45 (6)
O2i—Ca1—V2iii70.59 (6)V2xiv—V2—Ca1x54.58 (2)
O2ii—Ca1—V2iii146.05 (6)V2v—V2—Ca1x128.01 (3)
O4—Ca1—V2iii82.79 (5)V1—V2—Ca1x55.72 (2)
O4iii—Ca1—V2iii22.53 (5)Ca1xiv—V2—Ca1x131.14 (2)
O3iii—Ca1—V2iii80.56 (5)Ca1ii—V2—Ca1x108.63 (2)
O3—Ca1—V2iii128.53 (6)Ca1—V2—Ca1x82.78 (2)
O1iv—Ca1—V2iii68.17 (5)V1—O1—Ca1xii128.32 (15)
V1—Ca1—V2iii47.590 (15)V1—O1—Ca1xiii111.72 (13)
V2v—Ca1—V2iii109.13 (3)Ca1xii—O1—Ca1xiii119.96 (11)
V2vi—Ca1—V2iii47.309 (14)V1—O1—Ca1x37.75 (8)
V1vii—Ca1—V2iii109.88 (3)Ca1xii—O1—Ca1x90.57 (8)
O1viii—Ca1—V2iii134.680 (15)Ca1xiii—O1—Ca1x149.47 (9)
V2i—Ca1—V2iii80.223 (19)V1—O1—Ca132.75 (8)
V2ii—Ca1—V2iii137.46 (2)Ca1xii—O1—Ca1161.07 (10)
V1iv—Ca1—V2iii81.43 (2)Ca1xiii—O1—Ca178.97 (6)
V2—Ca1—V2iii90.57 (3)Ca1x—O1—Ca170.50 (5)
O2i—Ca1—V2ix58.73 (5)V2—O2—Ca1ii140.94 (14)
O2ii—Ca1—V2ix127.60 (6)V2—O2—Ca172.26 (8)
O4—Ca1—V2ix126.47 (6)Ca1ii—O2—Ca1128.39 (7)
O4iii—Ca1—V2ix79.56 (5)V2—O2—Ca1x69.07 (8)
O3iii—Ca1—V2ix20.38 (5)Ca1ii—O2—Ca1x140.60 (7)
O3—Ca1—V2ix80.06 (5)Ca1—O2—Ca1x