Temperature dependence of the AV₃O₇ (A = Ca, Sr) structure

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.

Computing details

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

(SrV3O7_315K)

Crystal data

O7V3·Sr	Dx = 3.945 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 10067 reflections
a = 5.2988 (9) Å	θ = 3.9–32.2°
b = 10.527 (2) Å	µ = 13.49 mm^−1
c = 5.3183 (9) Å	T = 315 K
V = 296.66 (10) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	336 independent reflections
Radiation source: fine-focus sealed tube	317 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.066
Detector resolution: 0 pixels mm^-1	θmax = 25.8°, θmin = 3.8°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.220, Tmax = 0.569	l = −6→6
5461 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.031	w = 1/[σ^2(Fo^2) + (0.0493P)^2 + 0.2079P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.080	(Δ/σ)max < 0.001
S = 1.21	Δρmax = 0.82 e Å^−3
336 reflections	Δρmin = −0.88 e Å^−3
24 parameters

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14871 (16)	0.0188 (3)
V1	0.2500	0.51544 (10)	0.62025 (19)	0.0150 (3)
V2	−0.2500	0.7500	0.5909 (3)	0.0149 (4)
O1	−0.2500	0.7500	−0.1058 (12)	0.0237 (15)*
O2	0.2500	0.5455 (4)	−0.0812 (9)	0.0245 (11)*
O3	−0.0120 (5)	0.6209 (3)	0.4635 (5)	0.0169 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0181 (5)	0.0162 (5)	0.0222 (5)	0.000	0.000	0.000
V1	0.0099 (5)	0.0128 (6)	0.0225 (6)	0.000	0.000	−0.0005 (4)
V2	0.0105 (7)	0.0126 (7)	0.0216 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.476 (5)	V2—V1^i	3.6250 (9)
Sr1—O2^i	2.476 (5)	V2—V1^xxi	3.6250 (9)
Sr1—O3^i	2.565 (3)	V2—V1^xxiv	3.6250 (9)
Sr1—O3^ii	2.565 (3)	V2—O1	3.706 (6)
Sr1—O3^iii	2.565 (3)	V2—O2^xix	3.833 (3)
Sr1—O3	2.565 (3)	V2—O2^xxv	3.833 (3)
Sr1—O1	2.975 (3)	V2—O2^v	3.833 (3)
Sr1—O1^iv	2.975 (3)	V2—O2^xxviii	3.833 (3)
Sr1—V1^i	3.5194 (13)	V2—Sr1^v	3.9773 (14)
Sr1—V1	3.5194 (13)	V2—Sr1^xxv	3.9773 (14)
Sr1—V2^iv	3.5427 (12)	V2—O2^xxvii	4.059 (5)
Sr1—V2	3.5427 (12)	V2—O2^vi	4.059 (5)
V1—O2^v	1.619 (5)	V2—O2^x	4.126 (5)
V1—O3^vi	1.962 (3)	V2—O2^xxix	4.126 (5)
V1—O3^vii	1.962 (3)	V2—O3^xiii	4.154 (3)
V1—O3^iii	1.963 (3)	V2—O3^xxx	4.154 (3)
V1—O3	1.963 (3)	V2—O3^vi	4.154 (3)
V1—V1^vi	2.9599 (10)	V2—O3^xxvii	4.154 (3)
V1—V1^viii	2.9599 (10)	V2—O3^xxi	4.314 (3)
V1—V2^vi	3.0117 (13)	V2—O3^i	4.314 (3)
V1—V2^iv	3.6250 (9)	V2—O3^xxxi	4.314 (3)
V1—V2	3.6250 (9)	V2—O3^iii	4.314 (3)
V1—O2^viii	3.666 (3)	V2—O2^xxi	4.943 (4)
V1—O2^vi	3.666 (3)	V2—O2^xxiv	4.943 (4)
V1—Sr1^v	3.7411 (13)	V2—O2	4.943 (4)
V1—O2	3.744 (5)	V2—O2^i	4.943 (4)
V1—O1^vi	3.805 (4)	V2—O3^xxxii	4.997 (3)
V1—O1^ix	3.904 (3)	V2—O3^xxviii	4.997 (3)
V1—O1^v	3.904 (3)	V2—O3^v	4.997 (3)
V1—O1^x	3.911 (5)	V2—O3^xxxiii	4.997 (3)
V1—O2^x	3.956 (4)	V2—V1^xxxiv	5.0406 (18)
V1—O2^xi	3.956 (4)	V2—V1^xviii	5.0406 (18)
V1—Sr1^vi	4.0420 (10)	V2—V2^iv	5.2988 (9)
V1—Sr1^viii	4.0420 (10)	V2—V2^xxi	5.2988 (9)
V1—O3^iv	4.150 (3)	V2—V2^xxii	5.3183 (9)
V1—O3^xii	4.150 (3)	V2—V2^v	5.3183 (9)
V1—O3^i	4.157 (3)	V2—Sr1^xxxv	5.4427 (12)
V1—O3^ii	4.157 (3)	V2—Sr1^vi	5.4427 (12)
V1—O3^xiii	4.308 (3)	V2—O3^xxxvi	5.534 (3)
V1—O3^viii	4.308 (3)	V2—O3^xxxvii	5.534 (3)
V1—O3^xiv	4.363 (3)	O1—V2^xxii	1.613 (6)
V1—O3^xv	4.363 (3)	O1—Sr1^xxi	2.975 (3)
V1—O3^xvi	4.824 (3)	O1—V1^xxvii	3.805 (4)
V1—O3^v	4.824 (3)	O1—V1^vi	3.805 (4)
V1—V1^xvii	4.8415 (18)	O1—V1^xxxviii	3.904 (2)
V1—V1^xviii	4.8415 (18)	O1—V1^xxxix	3.904 (2)
V1—O2^xix	4.887 (5)	O1—V1^xl	3.904 (2)
V1—V1^i	4.938 (2)	O1—V1^xxii	3.904 (2)
V1—V2^xviii	5.0406 (17)	O1—V1^x	3.911 (5)
V1—O3^xx	5.234 (3)	O1—V1^xxix	3.911 (5)
V1—O3^xviii	5.234 (3)	O2—V1^xxii	1.619 (5)
V1—O1	5.294 (5)	O2—V1^viii	3.666 (3)
V1—O1^iv	5.294 (5)	O2—V1^vi	3.666 (3)
V1—V1^xxi	5.2988 (9)	O2—V2^xli	3.833 (3)
V1—V1^iv	5.2988 (9)	O2—V2^xxii	3.833 (3)
V1—V1^xxii	5.3183 (9)	O2—V1^x	3.956 (4)
V1—O3^xxiii	5.536 (3)	O2—V1^xi	3.956 (4)
V1—O3^xxiv	5.536 (3)	O2—V2^vi	4.059 (5)
V1—O2^ix	5.5406 (17)	O2—V2^x	4.126 (5)
V1—O2^xxv	5.5406 (17)	O2—V1^xxxix	4.887 (5)
V1—V1^xxvi	5.589 (2)	O3—V1^vi	1.962 (3)
V2—O1^v	1.613 (6)	O3—V1^xxi	4.150 (3)
V2—O3^xii	1.974 (3)	O3—V2^vi	4.154 (3)
V2—O3^ii	1.974 (3)	O3—V1^i	4.157 (3)
V2—O3^xxiv	1.974 (3)	O3—V1^viii	4.308 (3)
V2—O3	1.974 (3)	O3—V2^iv	4.314 (3)
V2—V1^vi	3.0117 (13)	O3—V1^xxvii	4.363 (3)
V2—V1^xxvii	3.0117 (13)	O3—V1^xxii	4.824 (3)
V2—Sr1^xxi	3.5427 (12)	O3—V2^xxii	4.997 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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−1, y, z; (xxii) x, y, z−1; (xxiii) x+1, −y+3/2, z; (xxiv) −x−1/2, −y+3/2, z; (xxv) x−1, y, z+1; (xxvi) −x+1/2, −y+1/2, z; (xxvii) x−1/2, y+1/2, −z+1; (xxviii) −x−1/2, −y+3/2, z+1; (xxix) x−1/2, y+1/2, −z; (xxx) −x, y+1/2, −z+1; (xxxi) x−1, −y+3/2, z; (xxxii) x, −y+3/2, z+1; (xxxiii) −x−1/2, y, z+1; (xxxiv) x−1/2, y+1/2, −z+2; (xxxv) −x, −y+2, −z+1; (xxxvi) −x−1, −y+1, −z+1; (xxxvii) x+1/2, y+1/2, −z+1; (xxxviii) x−1, y, z−1; (xxxix) −x+1/2, −y+3/2, z−1; (xl) −x−1/2, −y+3/2, z−1; (xli) x+1, y, z−1.

(SrV3O7_298K)

Crystal data

O7V3·Sr	Dx = 3.949 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11182 reflections
a = 5.2979 (8) Å	θ = 3.8–32.1°
b = 10.529 (2) Å	µ = 13.51 mm^−1
c = 5.3139 (9) Å	T = 298 K
V = 296.41 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	331 independent reflections
Radiation source: fine-focus sealed tube	317 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.065
Detector resolution: 0 pixels mm^-1	θmax = 25.5°, θmin = 3.8°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.220, Tmax = 0.569	l = −6→6
5486 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.031	Secondary atom site location: difference Fourier map
wR(F^2) = 0.078	w = 1/[σ^2(Fo^2) + (0.0431P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.38	(Δ/σ)max < 0.001
331 reflections	Δρmax = 0.82 e Å^−3
24 parameters	Δρmin = −0.92 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14873 (15)	0.0184 (3)
V1	0.2500	0.51539 (10)	0.62054 (19)	0.0148 (3)
V2	0.7500	0.7500	0.5911 (3)	0.0143 (4)
O1	0.7500	0.7500	−0.1056 (12)	0.0233 (15)*
O2	0.2500	0.5455 (4)	−0.0809 (9)	0.0235 (10)*
O3	−0.0121 (5)	0.6206 (3)	0.4640 (5)	0.0166 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0172 (5)	0.0159 (5)	0.0219 (5)	0.000	0.000	0.000
V1	0.0095 (5)	0.0124 (6)	0.0226 (6)	0.000	0.000	−0.0004 (4)
V2	0.0108 (7)	0.0118 (7)	0.0204 (7)	0.000	0.000	0.000

Geometric parameters (Å, º)

Sr1—O2	2.475 (5)	V1—V1^viii	2.9603 (10)
Sr1—O2^i	2.475 (5)	V1—V2^viii	3.0120 (13)
Sr1—O3^i	2.567 (3)	V1—V2^i	3.6253 (8)
Sr1—O3^ii	2.567 (3)	V1—Sr1^v	3.7389 (12)
Sr1—O3	2.567 (3)	V2—O1^v	1.612 (6)
Sr1—O3^iii	2.567 (3)	V2—O3^ii	1.975 (3)
Sr1—O1^iv	2.974 (3)	V2—O3^ix	1.975 (3)
Sr1—O1	2.974 (3)	V2—O3^x	1.975 (3)
Sr1—V1^i	3.5195 (13)	V2—O3^i	1.975 (3)
Sr1—V1	3.5195 (13)	V2—V1^viii	3.0120 (13)
Sr1—V2	3.5415 (12)	V2—V1^xi	3.0120 (13)
Sr1—V2^i	3.5415 (12)	V2—Sr1^x	3.5415 (12)
V1—O2^v	1.618 (5)	O1—V2^xii	1.612 (6)
V1—O3^vi	1.960 (3)	O1—Sr1^x	2.974 (3)
V1—O3^vii	1.960 (3)	O2—V1^xii	1.618 (5)
V1—O3^ii	1.962 (3)	O3—V1^vi	1.960 (3)
V1—O3	1.962 (3)	O3—V2^i	1.975 (3)
V1—V1^vi	2.9603 (10)
O2—Sr1—O2^i	120.9 (2)	O3^ii—V1—V1^viii	40.97 (9)
O2—Sr1—O3^i	141.57 (8)	O3—V1—V1^viii	120.79 (10)
O2^i—Sr1—O3^i	81.97 (11)	V1^vi—V1—V1^viii	126.98 (7)
O2—Sr1—O3^ii	81.97 (11)	O2^v—V1—V2^viii	123.22 (16)
O2^i—Sr1—O3^ii	141.57 (8)	O3^vi—V1—V2^viii	40.23 (8)
O3^i—Sr1—O3^ii	64.09 (13)	O3^vii—V1—V2^viii	40.23 (8)
O2—Sr1—O3	81.97 (11)	O3^ii—V1—V2^viii	111.45 (9)
O2^i—Sr1—O3	141.57 (8)	O3—V1—V2^viii	111.45 (9)
O3^i—Sr1—O3	98.52 (13)	V1^vi—V1—V2^viii	74.74 (4)
O3^ii—Sr1—O3	65.49 (13)	V1^viii—V1—V2^viii	74.74 (4)
O2—Sr1—O3^iii	141.57 (8)	O2^v—V1—Sr1	124.12 (16)
O2^i—Sr1—O3^iii	81.97 (11)	O3^vi—V1—Sr1	110.46 (9)
O3^i—Sr1—O3^iii	65.49 (13)	O3^vii—V1—Sr1	110.46 (9)
O3^ii—Sr1—O3^iii	98.52 (13)	O3^ii—V1—Sr1	45.70 (9)
O3—Sr1—O3^iii	64.09 (13)	O3—V1—Sr1	45.70 (9)
O2—Sr1—O1^iv	77.05 (6)	V1^vi—V1—Sr1	76.62 (4)
O2^i—Sr1—O1^iv	77.05 (6)	V1^viii—V1—Sr1	76.62 (4)
O3^i—Sr1—O1^iv	141.12 (9)	V2^viii—V1—Sr1	112.65 (4)
O3^ii—Sr1—O1^iv	141.12 (9)	O2^v—V1—V2^i	84.77 (11)
O3—Sr1—O1^iv	79.33 (11)	O3^vi—V1—V2^i	91.04 (8)
O3^iii—Sr1—O1^iv	79.33 (11)	O3^vii—V1—V2^i	163.30 (9)
O2—Sr1—O1	77.05 (6)	O3^ii—V1—V2^i	96.55 (9)
O2^i—Sr1—O1	77.05 (6)	O3—V1—V2^i	23.01 (8)
O3^i—Sr1—O1	79.33 (11)	V1^vi—V1—V2^i	53.28 (3)
O3^ii—Sr1—O1	79.33 (11)	V1^viii—V1—V2^i	135.21 (6)
O3—Sr1—O1	141.12 (9)	V2^viii—V1—V2^i	128.022 (18)
O3^iii—Sr1—O1	141.12 (9)	Sr1—V1—V2^i	59.41 (3)
O1^iv—Sr1—O1	125.9 (2)	O2^v—V1—Sr1^v	30.05 (16)
O2—Sr1—V1^i	164.12 (11)	O3^vi—V1—Sr1^v	130.91 (8)
O2^i—Sr1—V1^i	74.97 (10)	O3^vii—V1—Sr1^v	130.91 (8)
O3^i—Sr1—V1^i	33.15 (6)	O3^ii—V1—Sr1^v	86.85 (9)
O3^ii—Sr1—V1^i	84.69 (7)	O3—V1—Sr1^v	86.85 (9)
O3—Sr1—V1^i	84.69 (7)	V1^vi—V1—Sr1^v	113.40 (4)
O3^iii—Sr1—V1^i	33.15 (6)	V1^viii—V1—Sr1^v	113.40 (4)
O1^iv—Sr1—V1^i	108.89 (7)	V2^viii—V1—Sr1^v	153.27 (4)
O1—Sr1—V1^i	108.89 (7)	Sr1—V1—Sr1^v	94.08 (3)
O2—Sr1—V1	74.97 (10)	V2^i—V1—Sr1^v	65.31 (3)
O2^i—Sr1—V1	164.12 (11)	O1^v—V2—O3^ii	109.99 (9)
O3^i—Sr1—V1	84.69 (7)	O1^v—V2—O3^ix	109.99 (9)
O3^ii—Sr1—V1	33.15 (6)	O3^ii—V2—O3^ix	140.02 (17)
O3—Sr1—V1	33.15 (6)	O1^v—V2—O3^x	109.99 (9)
O3^iii—Sr1—V1	84.69 (7)	O3^ii—V2—O3^x	79.32 (16)
O1^iv—Sr1—V1	108.89 (7)	O3^ix—V2—O3^x	87.22 (17)
O1—Sr1—V1	108.89 (7)	O1^v—V2—O3^i	109.99 (9)
V1^i—Sr1—V1	89.15 (4)	O3^ii—V2—O3^i	87.22 (17)
O2—Sr1—V2	109.11 (6)	O3^ix—V2—O3^i	79.32 (16)
O2^i—Sr1—V2	109.11 (6)	O3^x—V2—O3^i	140.02 (17)
O3^i—Sr1—V2	33.10 (6)	O1^v—V2—V1^viii	111.92 (3)
O3^ii—Sr1—V2	33.10 (6)	O3^ii—V2—V1^viii	39.87 (8)
O3—Sr1—V2	88.36 (7)	O3^ix—V2—V1^viii	120.81 (9)
O3^iii—Sr1—V2	88.36 (7)	O3^x—V2—V1^viii	39.87 (8)
O1^iv—Sr1—V2	165.45 (11)	O3^i—V2—V1^viii	120.81 (9)
O1—Sr1—V2	68.62 (11)	O1^v—V2—V1^xi	111.92 (3)
V1^i—Sr1—V2	61.784 (19)	O3^ii—V2—V1^xi	120.81 (9)
V1—Sr1—V2	61.784 (19)	O3^ix—V2—V1^xi	39.87 (8)
O2—Sr1—V2^i	109.11 (6)	O3^x—V2—V1^xi	120.81 (9)
O2^i—Sr1—V2^i	109.11 (6)	O3^i—V2—V1^xi	39.87 (8)
O3^i—Sr1—V2^i	88.36 (7)	V1^viii—V2—V1^xi	136.16 (6)
O3^ii—Sr1—V2^i	88.36 (7)	O1^v—V2—Sr1	131.58 (2)
O3—Sr1—V2^i	33.10 (6)	O3^ii—V2—Sr1	45.23 (9)
O3^iii—Sr1—V2^i	33.10 (6)	O3^ix—V2—Sr1	104.50 (9)
O1^iv—Sr1—V2^i	68.62 (11)	O3^x—V2—Sr1	104.50 (9)
O1—Sr1—V2^i	165.45 (11)	O3^i—V2—Sr1	45.23 (9)
V1^i—Sr1—V2^i	61.784 (19)	V1^viii—V2—Sr1	75.65 (2)
V1—Sr1—V2^i	61.784 (19)	V1^xi—V2—Sr1	75.65 (2)
V2—Sr1—V2^i	96.83 (4)	O1^v—V2—Sr1^x	131.58 (2)
O2^v—V1—O3^vi	111.59 (15)	O3^ii—V2—Sr1^x	104.50 (9)
O2^v—V1—O3^vii	111.59 (15)	O3^ix—V2—Sr1^x	45.23 (9)
O3^vi—V1—O3^vii	80.04 (17)	O3^x—V2—Sr1^x	45.23 (9)
O2^v—V1—O3^ii	107.76 (14)	O3^i—V2—Sr1^x	104.50 (9)
O3^vi—V1—O3^ii	140.42 (7)	V1^viii—V2—Sr1^x	75.65 (2)
O3^vii—V1—O3^ii	81.97 (13)	V1^xi—V2—Sr1^x	75.65 (2)
O2^v—V1—O3	107.76 (14)	Sr1—V2—Sr1^x	96.83 (4)
O3^vi—V1—O3	81.97 (13)	V2^xii—O1—Sr1^x	117.03 (11)
O3^vii—V1—O3	140.42 (7)	V2^xii—O1—Sr1	117.03 (11)
O3^ii—V1—O3	90.13 (17)	Sr1^x—O1—Sr1	125.9 (2)
O2^v—V1—V1^vi	116.48 (4)	V1^xii—O2—Sr1	130.8 (2)
O3^vi—V1—V1^vi	41.01 (9)	V1^vi—O3—V1	98.03 (13)
O3^vii—V1—V1^vi	113.34 (10)	V1^vi—O3—V2^i	99.90 (12)
O3^ii—V1—V1^vi	120.79 (10)	V1—O3—V2^i	134.15 (15)
O3—V1—V1^vi	40.97 (9)	V1^vi—O3—Sr1	125.86 (13)
O2^v—V1—V1^viii	116.48 (4)	V1—O3—Sr1	101.16 (11)
O3^vi—V1—V1^viii	113.34 (10)	V2^i—O3—Sr1	101.68 (12)
O3^vii—V1—V1^viii	41.01 (9)

Symmetry codes: (i) −x+1/2, −y+3/2, z; (ii) −x+1/2, y, z; (iii) x, −y+3/2, z; (iv) 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+3/2, z; (x) x+1, y, z; (xi) x+1/2, y+1/2, −z+1; (xii) x, y, z−1.

(SrV3O7_275K)

Crystal data

O7V3·Sr	Dx = 3.953 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11380 reflections
a = 5.2968 (8) Å	θ = 3.8–32.0°
b = 10.530 (2) Å	µ = 13.53 mm^−1
c = 5.3089 (9) Å	T = 275 K
V = 296.11 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	334 independent reflections
Radiation source: fine-focus sealed tube	322 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.067
Detector resolution: 0 pixels mm^-1	θmax = 25.6°, θmin = 3.8°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.219, Tmax = 0.569	l = −6→6
5445 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.033	Secondary atom site location: difference Fourier map
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0472P)^2 + 0.5886P] where P = (Fo^2 + 2Fc^2)/3
S = 1.22	(Δ/σ)max < 0.001
334 reflections	Δρmax = 0.74 e Å^−3
24 parameters	Δρmin = −0.92 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14876 (16)	0.0178 (3)
V1	0.2500	0.51541 (10)	0.6206 (2)	0.0146 (3)
V2	−0.2500	0.7500	0.5914 (3)	0.0140 (4)
O1	−0.2500	0.7500	−0.1044 (12)	0.0222 (16)*
O2	0.2500	0.5455 (5)	−0.0801 (9)	0.0229 (11)*
O3	−0.0119 (6)	0.6206 (3)	0.4640 (6)	0.0162 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0160 (5)	0.0158 (5)	0.0215 (5)	0.000	0.000	0.000
V1	0.0093 (6)	0.0123 (6)	0.0222 (6)	0.000	0.000	−0.0007 (4)
V2	0.0103 (7)	0.0117 (7)	0.0200 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.473 (5)	V2—V1^xxi	3.6249 (9)
Sr1—O2^i	2.473 (5)	V2—V1^i	3.6249 (9)
Sr1—O3^i	2.565 (3)	V2—V1^xxiv	3.6249 (9)
Sr1—O3^ii	2.565 (3)	V2—O1	3.694 (7)
Sr1—O3^iii	2.565 (3)	V2—O2^xix	3.833 (4)
Sr1—O3	2.565 (3)	V2—O2^xxv	3.833 (4)
Sr1—O1	2.970 (3)	V2—O2^v	3.833 (4)
Sr1—O1^iv	2.970 (3)	V2—O2^xxvii	3.833 (4)
Sr1—V1^i	3.5181 (14)	V2—Sr1^v	3.9712 (14)
Sr1—V1	3.5181 (14)	V2—Sr1^xxv	3.9712 (14)
Sr1—V2^iv	3.5405 (13)	V2—O2^xxvi	4.051 (5)
Sr1—V2	3.5405 (13)	V2—O2^vi	4.051 (5)
V1—O2^v	1.620 (5)	V2—O2^x	4.129 (5)
V1—O3^vi	1.961 (3)	V2—O2^xxviii	4.129 (5)
V1—O3^vii	1.961 (3)	V2—O3^xiii	4.152 (3)
V1—O3^iii	1.960 (3)	V2—O3^xxix	4.152 (3)
V1—O3	1.960 (3)	V2—O3^vi	4.152 (3)
V1—V1^vi	2.9596 (10)	V2—O3^xxvi	4.152 (3)
V1—V1^viii	2.9596 (10)	V2—O3^xxi	4.313 (3)
V1—V2^vi	3.0129 (14)	V2—O3^i	4.313 (3)
V1—V2^iv	3.6249 (9)	V2—O3^xxx	4.313 (3)
V1—V2	3.6249 (9)	V2—O3^iii	4.313 (3)
V1—O2^viii	3.657 (4)	V2—O2^xxi	4.935 (5)
V1—O2^vi	3.657 (4)	V2—O2	4.935 (4)
V1—O2	3.733 (5)	V2—O2^xxiv	4.935 (4)
V1—Sr1^v	3.7369 (13)	V2—O2^i	4.935 (5)
V1—O1^vi	3.796 (5)	V2—O3^xxxi	4.991 (3)
V1—O1^ix	3.905 (3)	V2—O3^v	4.991 (3)
V1—O1^v	3.905 (3)	V2—O3^xxvii	4.991 (3)
V1—O1^x	3.914 (5)	V2—O3^xxxii	4.991 (3)
V1—O2^x	3.957 (4)	V2—V1^xxxiii	5.0313 (18)
V1—O2^xi	3.957 (4)	V2—V1^xviii	5.0313 (18)
V1—Sr1^vi	4.0404 (10)	V2—V2^iv	5.2968 (8)
V1—Sr1^viii	4.0404 (10)	V2—V2^xxi	5.2968 (8)
V1—O3^iv	4.148 (3)	V2—V2^xxii	5.3089 (9)
V1—O3^xii	4.148 (3)	V2—V2^v	5.3089 (9)
V1—O3^i	4.160 (3)	V2—Sr1^xxxiv	5.4429 (12)
V1—O3^ii	4.160 (3)	V2—Sr1^vi	5.4429 (12)
V1—O3^xiii	4.306 (3)	V2—O1^ix	5.538 (2)
V1—O3^viii	4.306 (3)	V2—O1^xxv	5.538 (2)
V1—O3^xiv	4.368 (3)	O1—V2^xxii	1.615 (7)
V1—O3^xv	4.368 (3)	O1—Sr1^xxi	2.970 (3)
V1—O3^xvi	4.817 (3)	O1—V1^xxvi	3.796 (5)
V1—O3^v	4.817 (3)	O1—V1^vi	3.796 (5)
V1—V1^xvii	4.8319 (19)	O1—V1^xxxv	3.905 (3)
V1—V1^xviii	4.8319 (19)	O1—V1^xxxvi	3.905 (3)
V1—O2^xix	4.889 (5)	O1—V1^xxii	3.905 (3)
V1—V1^i	4.940 (2)	O1—V1^xxxvii	3.905 (3)
V1—V2^xviii	5.0313 (18)	O1—V1^x	3.914 (5)
V1—O3^xx	5.221 (3)	O1—V1^xxviii	3.914 (5)
V1—O3^xviii	5.221 (3)	O2—V1^xxii	1.620 (5)
V1—O1	5.285 (5)	O2—V1^viii	3.657 (4)
V1—O1^iv	5.285 (5)	O2—V1^vi	3.657 (4)
V1—V1^xxi	5.2968 (8)	O2—V2^xxxviii	3.833 (4)
V1—V1^iv	5.2968 (8)	O2—V2^xxii	3.833 (4)
V1—V1^xxii	5.3089 (9)	O2—V1^x	3.957 (4)
V1—V1^v	5.3089 (9)	O2—V1^xi	3.957 (4)
V1—O3^xxiii	5.538 (3)	O2—V2^vi	4.051 (5)
V1—O3^xxiv	5.538 (3)	O2—V2^x	4.129 (5)
V1—O2^ix	5.5391 (17)	O2—V1^xxxvi	4.889 (5)
V1—O2^xxv	5.5391 (17)	O3—V1^vi	1.961 (3)
V2—O1^v	1.615 (7)	O3—V1^xxi	4.148 (3)
V2—O3^xii	1.976 (3)	O3—V2^vi	4.152 (3)
V2—O3^ii	1.976 (3)	O3—V1^i	4.160 (3)
V2—O3	1.976 (3)	O3—V1^viii	4.306 (3)
V2—O3^xxiv	1.976 (3)	O3—V2^iv	4.313 (3)
V2—V1^vi	3.0129 (14)	O3—V1^xxvi	4.368 (3)
V2—V1^xxvi	3.0129 (14)	O3—V1^xxii	4.817 (3)
V2—Sr1^xxi	3.5405 (13)	O3—V2^xxii	4.991 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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−1, y, z; (xxii) x, y, z−1; (xxiii) x+1, −y+3/2, z; (xxiv) −x−1/2, −y+3/2, z; (xxv) x−1, y, z+1; (xxvi) x−1/2, y+1/2, −z+1; (xxvii) −x−1/2, −y+3/2, z+1; (xxviii) x−1/2, y+1/2, −z; (xxix) −x, y+1/2, −z+1; (xxx) x−1, −y+3/2, z; (xxxi) x, −y+3/2, z+1; (xxxii) −x−1/2, y, z+1; (xxxiii) x−1/2, y+1/2, −z+2; (xxxiv) −x, −y+2, −z+1; (xxxv) x−1, y, z−1; (xxxvi) −x+1/2, −y+3/2, z−1; (xxxvii) −x−1/2, −y+3/2, z−1; (xxxviii) x+1, y, z−1.

(SrV3O7_262K)

Crystal data

O7V3·Sr	Dx = 3.956 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11083 reflections
a = 5.2956 (8) Å	θ = 3.8–32.1°
b = 10.532 (2) Å	µ = 13.54 mm^−1
c = 5.3055 (9) Å	T = 262 K
V = 295.90 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	334 independent reflections
Radiation source: fine-focus sealed tube	321 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.067
Detector resolution: 0 pixels mm^-1	θmax = 25.6°, θmin = 3.8°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.218, Tmax = 0.568	l = −6→6
5436 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.032	Secondary atom site location: difference Fourier map
wR(F^2) = 0.078	w = 1/[σ^2(Fo^2) + (0.0397P)^2 + 0.8062P] where P = (Fo^2 + 2Fc^2)/3
S = 1.24	(Δ/σ)max < 0.001
334 reflections	Δρmax = 0.69 e Å^−3
24 parameters	Δρmin = −0.96 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14895 (17)	0.0174 (3)
V1	0.2500	0.51532 (10)	0.6207 (2)	0.0141 (3)
V2	−0.2500	0.7500	0.5915 (3)	0.0139 (4)
O1	−0.2500	0.7500	−0.1043 (12)	0.0215 (15)*
O2	0.2500	0.5452 (5)	−0.0804 (9)	0.0216 (11)*
O3	−0.0119 (6)	0.6205 (3)	0.4635 (6)	0.0158 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0160 (5)	0.0149 (5)	0.0212 (5)	0.000	0.000	0.000
V1	0.0089 (5)	0.0119 (6)	0.0214 (6)	0.000	0.000	−0.0003 (4)
V2	0.0103 (7)	0.0117 (7)	0.0198 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.477 (5)	V2—V1^i	3.6254 (9)
Sr1—O2^i	2.477 (5)	V2—V1^xxi	3.6254 (9)
Sr1—O3^i	2.563 (3)	V2—V1^xxv	3.6254 (9)
Sr1—O3^ii	2.563 (3)	V2—O1	3.692 (7)
Sr1—O3	2.563 (3)	V2—O2^xix	3.833 (4)
Sr1—O3^iii	2.563 (3)	V2—O2^xxvii	3.833 (4)
Sr1—O1	2.969 (3)	V2—O2^xxiii	3.833 (4)
Sr1—O1^iv	2.969 (3)	V2—O2^v	3.833 (4)
Sr1—V1^i	3.5175 (13)	V2—Sr1^v	3.9697 (14)
Sr1—V1	3.5175 (14)	V2—Sr1^xxiii	3.9697 (14)
Sr1—V2^iv	3.5388 (13)	V2—O2^xxvi	4.049 (5)
Sr1—V2	3.5388 (13)	V2—O2^vi	4.049 (5)
V1—O2^v	1.617 (5)	V2—O2^x	4.125 (5)
V1—O3^vi	1.958 (3)	V2—O2^xxviii	4.125 (5)
V1—O3^vii	1.958 (3)	V2—O3^xxix	4.151 (3)
V1—O3^iii	1.961 (3)	V2—O3^xxvi	4.151 (3)
V1—O3	1.961 (3)	V2—O3^xiii	4.151 (3)
V1—V1^vi	2.9589 (10)	V2—O3^vi	4.151 (3)
V1—V1^viii	2.9589 (10)	V2—O3^xxi	4.313 (3)
V1—V2^vi	3.0125 (14)	V2—O3^i	4.313 (3)
V1—V2^iv	3.6254 (9)	V2—O3^xxx	4.313 (3)
V1—V2	3.6254 (9)	V2—O3^iii	4.313 (3)
V1—O2^viii	3.656 (3)	V2—O2^xxi	4.937 (4)
V1—O2^vi	3.656 (3)	V2—O2^xxv	4.937 (4)
V1—O2	3.733 (5)	V2—O2	4.937 (4)
V1—Sr1^v	3.7369 (13)	V2—O2^i	4.937 (4)
V1—O1^vi	3.794 (5)	V2—O3^xxxi	4.986 (3)
V1—O1^ix	3.905 (3)	V2—O3^xxvii	4.986 (3)
V1—O1^v	3.905 (3)	V2—O3^v	4.986 (3)
V1—O1^x	3.913 (5)	V2—O3^xxxii	4.986 (3)
V1—O2^x	3.954 (4)	V2—V1^xxxiii	5.0279 (18)
V1—O2^xi	3.954 (4)	V2—V1^xviii	5.0279 (18)
V1—Sr1^vi	4.0389 (10)	V2—V2^iv	5.2956 (8)
V1—Sr1^viii	4.0389 (10)	V2—V2^xxi	5.2956 (8)
V1—O3^iv	4.147 (3)	V2—V2^v	5.3055 (9)
V1—O3^xii	4.147 (3)	V2—V2^xxii	5.3055 (9)
V1—O3^i	4.163 (3)	V2—Sr1^xxxiv	5.4431 (12)
V1—O3^ii	4.163 (3)	V2—Sr1^vi	5.4430 (12)
V1—O3^xiii	4.304 (3)	V2—O3^xxxv	5.530 (3)
V1—O3^viii	4.304 (3)	V2—O3^xxxvi	5.530 (3)
V1—O3^xiv	4.368 (3)	O1—V2^xxii	1.614 (7)
V1—O3^xv	4.368 (3)	O1—Sr1^xxi	2.969 (3)
V1—O3^xvi	4.811 (3)	O1—V1^xxvi	3.794 (5)
V1—O3^v	4.811 (3)	O1—V1^vi	3.794 (5)
V1—V1^xvii	4.8285 (19)	O1—V1^xxxvii	3.905 (3)
V1—V1^xviii	4.8285 (19)	O1—V1^xxxviii	3.905 (3)
V1—O2^xix	4.893 (5)	O1—V1^xxxix	3.905 (3)
V1—V1^i	4.943 (2)	O1—V1^xxii	3.905 (3)
V1—V2^xviii	5.0279 (18)	O1—V1^x	3.913 (5)
V1—O3^xx	5.219 (3)	O1—V1^xxviii	3.913 (5)
V1—O3^xviii	5.219 (3)	O2—V1^xxii	1.617 (5)
V1—O1	5.284 (5)	O2—V1^viii	3.656 (3)
V1—O1^iv	5.284 (5)	O2—V1^vi	3.656 (3)
V1—V1^xxi	5.2956 (8)	O2—V2^xl	3.833 (4)
V1—V1^iv	5.2956 (8)	O2—V2^xxii	3.833 (4)
V1—V1^xxii	5.3055 (9)	O2—V1^x	3.954 (4)
V1—V1^v	5.3055 (9)	O2—V1^xi	3.954 (4)
V1—O2^ix	5.5369 (16)	O2—V2^vi	4.049 (5)
V1—O2^xxiii	5.5369 (16)	O2—V2^x	4.125 (5)
V1—O3^xxiv	5.539 (3)	O2—V1^xxxviii	4.893 (5)
V1—O3^xxv	5.539 (3)	O3—V1^vi	1.958 (3)
V2—O1^v	1.614 (7)	O3—V1^xxi	4.147 (3)
V2—O3^ii	1.978 (3)	O3—V2^vi	4.151 (3)
V2—O3^xxv	1.978 (3)	O3—V1^i	4.163 (3)
V2—O3^xii	1.978 (3)	O3—V1^viii	4.304 (3)
V2—O3	1.978 (3)	O3—V2^iv	4.313 (3)
V2—V1^vi	3.0125 (14)	O3—V1^xxvi	4.368 (3)
V2—V1^xxvi	3.0125 (14)	O3—V1^xxii	4.811 (3)
V2—Sr1^xxi	3.5388 (13)	O3—V2^xxii	4.986 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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−1, y, z; (xxii) x, y, z−1; (xxiii) x−1, y, z+1; (xxiv) x+1, −y+3/2, z; (xxv) −x−1/2, −y+3/2, z; (xxvi) x−1/2, y+1/2, −z+1; (xxvii) −x−1/2, −y+3/2, z+1; (xxviii) x−1/2, y+1/2, −z; (xxix) −x, y+1/2, −z+1; (xxx) x−1, −y+3/2, z; (xxxi) x, −y+3/2, z+1; (xxxii) −x−1/2, y, z+1; (xxxiii) x−1/2, y+1/2, −z+2; (xxxiv) −x, −y+2, −z+1; (xxxv) x+1/2, y+1/2, −z+1; (xxxvi) −x−1, −y+1, −z+1; (xxxvii) x−1, y, z−1; (xxxviii) −x+1/2, −y+3/2, z−1; (xxxix) −x−1/2, −y+3/2, z−1; (xl) x+1, y, z−1.

(SrV3O7_250K)

Crystal data

O7V3·Sr	Dx = 3.958 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11262 reflections
a = 5.2959 (8) Å	θ = 3.8–32.1°
b = 10.534 (2) Å	µ = 13.54 mm^−1
c = 5.3014 (9) Å	T = 250 K
V = 295.74 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	332 independent reflections
Radiation source: fine-focus sealed tube	316 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.067
Detector resolution: 0 pixels mm^-1	θmax = 25.8°, θmin = 3.8°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.217, Tmax = 0.568	l = −6→6
5416 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.031	Secondary atom site location: difference Fourier map
wR(F^2) = 0.078	w = 1/[σ^2(Fo^2) + (0.0371P)^2 + 1.0548P] where P = (Fo^2 + 2Fc^2)/3
S = 1.24	(Δ/σ)max < 0.001
332 reflections	Δρmax = 0.69 e Å^−3
24 parameters	Δρmin = −0.99 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14883 (17)	0.0168 (3)
V1	0.2500	0.51530 (10)	0.6207 (2)	0.0139 (3)
V2	−0.2500	0.7500	0.5916 (3)	0.0136 (4)
O1	−0.2500	0.7500	−0.1042 (13)	0.0205 (16)*
O2	0.2500	0.5453 (5)	−0.0797 (9)	0.0216 (11)*
O3	−0.0120 (6)	0.6208 (3)	0.4640 (6)	0.0153 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0154 (5)	0.0144 (5)	0.0207 (5)	0.000	0.000	0.000
V1	0.0087 (6)	0.0119 (6)	0.0211 (6)	0.000	0.000	−0.0003 (4)
V2	0.0098 (8)	0.0109 (8)	0.0200 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.473 (5)	V2—V1^i	3.6259 (9)
Sr1—O2^i	2.473 (5)	V2—V1^xxi	3.6259 (9)
Sr1—O3^i	2.563 (3)	V2—V1^xxiv	3.6259 (9)
Sr1—O3	2.563 (3)	V2—O1	3.689 (7)
Sr1—O3^ii	2.563 (3)	V2—O2^xix	3.834 (4)
Sr1—O3^iii	2.563 (3)	V2—O2^xxv	3.834 (4)
Sr1—O1	2.968 (3)	V2—O2^v	3.834 (4)
Sr1—O1^iv	2.968 (3)	V2—O2^xxvii	3.834 (4)
Sr1—V1^i	3.5169 (14)	V2—Sr1^v	3.9672 (15)
Sr1—V1	3.5169 (14)	V2—Sr1^xxv	3.9672 (15)
Sr1—V2^iv	3.5385 (13)	V2—O2^xxvi	4.046 (5)
Sr1—V2	3.5385 (13)	V2—O2^vi	4.046 (5)
V1—O2^v	1.620 (5)	V2—O2^x	4.128 (5)
V1—O3^iii	1.962 (3)	V2—O2^xxviii	4.128 (5)
V1—O3	1.962 (3)	V2—O3^xiii	4.156 (3)
V1—O3^vi	1.961 (3)	V2—O3^xxix	4.156 (3)
V1—O3^vii	1.961 (3)	V2—O3^vi	4.156 (3)
V1—V1^vi	2.9584 (11)	V2—O3^xxvi	4.156 (3)
V1—V1^viii	2.9584 (11)	V2—O3^xxi	4.312 (3)
V1—V2^vi	3.0126 (14)	V2—O3^i	4.312 (3)
V1—V2^iv	3.6259 (9)	V2—O3^xxx	4.312 (3)
V1—V2	3.6259 (9)	V2—O3^iii	4.312 (3)
V1—O2^viii	3.652 (4)	V2—O2^xxi	4.932 (5)
V1—O2^vi	3.652 (4)	V2—O2^xxiv	4.932 (5)
V1—O2	3.726 (5)	V2—O2^i	4.932 (5)
V1—Sr1^v	3.7353 (14)	V2—O2	4.932 (5)
V1—O1^vi	3.792 (5)	V2—O3^xxxi	4.983 (3)
V1—O1^ix	3.905 (3)	V2—O3^xxvii	4.983 (3)
V1—O1^v	3.905 (3)	V2—O3^v	4.983 (3)
V1—O1^x	3.912 (5)	V2—O3^xxxii	4.983 (3)
V1—O2^x	3.955 (4)	V2—V1^xxxiii	5.0250 (18)
V1—O2^xi	3.955 (4)	V2—V1^xviii	5.0250 (19)
V1—Sr1^vi	4.0391 (10)	V2—V2^iv	5.2959 (8)
V1—Sr1^viii	4.0391 (10)	V2—V2^xxi	5.2959 (8)
V1—O3^iv	4.147 (3)	V2—V2^xxii	5.3014 (9)
V1—O3^xii	4.147 (3)	V2—V2^v	5.3014 (9)
V1—O3^i	4.160 (3)	V2—Sr1^xxxiv	5.4436 (12)
V1—O3^ii	4.160 (3)	V2—Sr1^vi	5.4436 (12)
V1—O3^xiii	4.306 (3)	V2—O3^xxxv	5.534 (3)
V1—O3^viii	4.306 (3)	V2—O3^xxxvi	5.534 (3)
V1—O3^xiv	4.365 (3)	O1—V2^xxii	1.613 (7)
V1—O3^xv	4.365 (3)	O1—Sr1^xxi	2.968 (3)
V1—O3^xvi	4.812 (3)	O1—V1^xxvi	3.792 (5)
V1—O3^v	4.812 (3)	O1—V1^vi	3.792 (5)
V1—V1^xvii	4.8263 (19)	O1—V1^xxxvii	3.905 (3)
V1—V1^xviii	4.826 (2)	O1—V1^xxxviii	3.905 (3)
V1—O2^xix	4.893 (5)	O1—V1^xxxix	3.905 (3)
V1—V1^i	4.944 (2)	O1—V1^xxii	3.905 (3)
V1—V2^xviii	5.0250 (18)	O1—V1^x	3.912 (5)
V1—O3^xx	5.214 (3)	O1—V1^xxviii	3.912 (5)
V1—O3^xviii	5.214 (3)	O2—V1^xxii	1.620 (5)
V1—O1	5.281 (5)	O2—V1^viii	3.652 (4)
V1—O1^iv	5.281 (5)	O2—V1^vi	3.652 (4)
V1—V1^xxi	5.2959 (8)	O2—V2^xl	3.834 (4)
V1—V1^iv	5.2959 (8)	O2—V2^xxii	3.834 (4)
V1—V1^xxii	5.3014 (9)	O2—V1^x	3.955 (4)
V1—V1^v	5.3014 (9)	O2—V1^xi	3.955 (4)
V1—O3^xxiii	5.537 (3)	O2—V2^vi	4.046 (5)
V1—O3^xxiv	5.537 (3)	O2—V2^x	4.128 (5)
V1—O2^ix	5.5381 (17)	O2—V1^xxxviii	4.893 (5)
V1—O2^xxv	5.5381 (17)	O3—V1^vi	1.961 (3)
V2—O1^v	1.613 (7)	O3—V1^xxi	4.147 (3)
V2—O3^xii	1.974 (3)	O3—V2^vi	4.156 (3)
V2—O3^ii	1.974 (3)	O3—V1^i	4.160 (3)
V2—O3^xxiv	1.974 (3)	O3—V1^viii	4.306 (3)
V2—O3	1.974 (3)	O3—V2^iv	4.312 (3)
V2—V1^vi	3.0126 (14)	O3—V1^xxvi	4.365 (3)
V2—V1^xxvi	3.0126 (14)	O3—V1^xxii	4.812 (3)
V2—Sr1^xxi	3.5385 (13)	O3—V2^xxii	4.983 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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−1, y, z; (xxii) x, y, z−1; (xxiii) x+1, −y+3/2, z; (xxiv) −x−1/2, −y+3/2, z; (xxv) x−1, y, z+1; (xxvi) x−1/2, y+1/2, −z+1; (xxvii) −x−1/2, −y+3/2, z+1; (xxviii) x−1/2, y+1/2, −z; (xxix) −x, y+1/2, −z+1; (xxx) x−1, −y+3/2, z; (xxxi) x, −y+3/2, z+1; (xxxii) −x−1/2, y, z+1; (xxxiii) x−1/2, y+1/2, −z+2; (xxxiv) −x, −y+2, −z+1; (xxxv) −x−1, −y+1, −z+1; (xxxvi) x+1/2, y+1/2, −z+1; (xxxvii) x−1, y, z−1; (xxxviii) −x+1/2, −y+3/2, z−1; (xxxix) −x−1/2, −y+3/2, z−1; (xl) x+1, y, z−1.

(SrV3O7_225K)

Crystal data

O7V3·Sr	Dx = 3.963 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11381 reflections
a = 5.2954 (8) Å	θ = 3.9–32.1°
b = 10.534 (2) Å	µ = 13.56 mm^−1
c = 5.2952 (9) Å	T = 225 K
V = 295.38 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	334 independent reflections
Radiation source: fine-focus sealed tube	320 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.067
Detector resolution: 0 pixels mm^-1	θmax = 25.8°, θmin = 3.9°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.218, Tmax = 0.568	l = −6→6
5414 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.033	Secondary atom site location: difference Fourier map
wR(F^2) = 0.077	w = 1/[σ^2(Fo^2) + (0.0346P)^2 + 0.5753P] where P = (Fo^2 + 2Fc^2)/3
S = 1.39	(Δ/σ)max < 0.001
334 reflections	Δρmax = 0.71 e Å^−3
24 parameters	Δρmin = −1.01 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14899 (17)	0.0162 (3)
V1	0.2500	0.51522 (10)	0.6210 (2)	0.0135 (3)
V2	−0.2500	0.7500	0.5921 (3)	0.0134 (4)
O1	−0.2500	0.7500	−0.1024 (12)	0.0200 (15)*
O2	0.2500	0.5452 (5)	−0.0795 (9)	0.0210 (11)*
O3	−0.0121 (6)	0.6207 (3)	0.4641 (6)	0.0146 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0145 (5)	0.0140 (5)	0.0201 (5)	0.000	0.000	0.000
V1	0.0087 (5)	0.0112 (6)	0.0205 (6)	0.000	0.000	−0.0003 (4)
V2	0.0098 (7)	0.0114 (7)	0.0190 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.474 (5)	V2—V1^i	3.6263 (9)
Sr1—O2^i	2.474 (5)	V2—V1^xxii	3.6263 (9)
Sr1—O3^i	2.562 (3)	V2—V1^xxiv	3.6263 (9)
Sr1—O3	2.562 (3)	V2—O1	3.677 (7)
Sr1—O3^ii	2.562 (3)	V2—O2^xix	3.833 (4)
Sr1—O3^iii	2.562 (3)	V2—O2^xxv	3.833 (4)
Sr1—O1	2.963 (3)	V2—O2^v	3.833 (4)
Sr1—O1^iv	2.963 (3)	V2—O2^xxvii	3.833 (4)
Sr1—V1^i	3.5161 (14)	V2—Sr1^v	3.9633 (14)
Sr1—V1	3.5161 (14)	V2—Sr1^xxv	3.9633 (14)
Sr1—V2^iv	3.5376 (13)	V2—O2^xxvi	4.041 (5)
Sr1—V2	3.5376 (13)	V2—O2^vi	4.041 (5)
V1—O2^v	1.617 (5)	V2—O2^x	4.127 (5)
V1—O3^vi	1.960 (3)	V2—O2^xxviii	4.127 (5)
V1—O3^vii	1.960 (3)	V2—O3^xxix	4.155 (3)
V1—O3^iii	1.962 (3)	V2—O3^xiii	4.155 (3)
V1—O3	1.962 (3)	V2—O3^xxvi	4.155 (3)
V1—V1^vi	2.9588 (10)	V2—O3^vi	4.155 (3)
V1—V1^viii	2.9588 (10)	V2—O3^xxii	4.313 (3)
V1—V2^vi	3.0131 (14)	V2—O3^i	4.313 (3)
V1—V2^iv	3.6263 (9)	V2—O3^xxx	4.313 (3)
V1—V2	3.6263 (9)	V2—O3^iii	4.313 (3)
V1—O2^viii	3.648 (3)	V2—O2^xxii	4.931 (4)
V1—O2^vi	3.648 (3)	V2—O2^xxiv	4.931 (4)
V1—O2	3.723 (5)	V2—O2	4.931 (4)
V1—Sr1^v	3.7328 (13)	V2—O2^i	4.931 (4)
V1—O1^vi	3.782 (4)	V2—O3^xxxi	4.976 (3)
V1—O1^ix	3.908 (3)	V2—O3^xxvii	4.976 (3)
V1—O1^v	3.908 (3)	V2—O3^v	4.976 (3)
V1—O1^x	3.917 (5)	V2—O3^xxxii	4.976 (3)
V1—O2^x	3.954 (4)	V2—V1^xxxiii	5.0171 (18)
V1—O2^xi	3.954 (4)	V2—V1^xviii	5.0171 (18)
V1—Sr1^vi	4.0373 (10)	V2—V2^v	5.2952 (9)
V1—Sr1^viii	4.0373 (10)	V2—V2^xxi	5.2952 (9)
V1—O3^iv	4.147 (3)	V2—V2^iv	5.2954 (8)
V1—O3^xii	4.147 (3)	V2—V2^xxii	5.2954 (8)
V1—O3^i	4.162 (3)	V2—Sr1^xxxiv	5.4427 (12)
V1—O3^ii	4.162 (3)	V2—Sr1^vi	5.4427 (12)
V1—O3^xiii	4.306 (3)	V2—O1^ix	5.537 (2)
V1—O3^viii	4.306 (3)	V2—O1^xxv	5.537 (2)
V1—O3^xiv	4.366 (3)	O1—V2^xxi	1.618 (7)
V1—O3^xv	4.366 (3)	O1—Sr1^xxii	2.963 (3)
V1—O3^xvi	4.805 (3)	O1—V1^xxvi	3.782 (4)
V1—O3^v	4.805 (3)	O1—V1^vi	3.782 (4)
V1—V1^xvii	4.8193 (19)	O1—V1^xxxv	3.908 (3)
V1—V1^xviii	4.8193 (19)	O1—V1^xxxvi	3.908 (3)
V1—O2^xix	4.895 (5)	O1—V1^xxxvii	3.908 (3)
V1—V1^i	4.946 (2)	O1—V1^xxi	3.908 (3)
V1—V2^xviii	5.0171 (18)	O1—V1^x	3.917 (5)
V1—O3^xx	5.207 (3)	O1—V1^xxviii	3.917 (5)
V1—O3^xviii	5.207 (3)	O2—V1^xxi	1.617 (5)
V1—O1	5.272 (5)	O2—V1^viii	3.648 (3)
V1—O1^iv	5.272 (5)	O2—V1^vi	3.648 (3)
V1—V1^v	5.2952 (9)	O2—V2^xxxviii	3.833 (4)
V1—V1^xxi	5.2952 (9)	O2—V2^xxi	3.833 (4)
V1—V1^xxii	5.2954 (8)	O2—V1^x	3.954 (4)
V1—V1^iv	5.2954 (8)	O2—V1^xi	3.954 (4)
V1—O3^xxiii	5.538 (3)	O2—V2^vi	4.041 (5)
V1—O3^xxiv	5.538 (3)	O2—V2^x	4.127 (5)
V1—O2^ix	5.5368 (16)	O2—V1^xxxvi	4.895 (5)
V1—O2^xxv	5.5368 (16)	O3—V1^vi	1.960 (3)
V2—O1^v	1.618 (7)	O3—V1^xxii	4.147 (3)
V2—O3^xii	1.975 (3)	O3—V2^vi	4.155 (3)
V2—O3^xxiv	1.975 (3)	O3—V1^i	4.162 (3)
V2—O3^ii	1.975 (3)	O3—V1^viii	4.306 (3)
V2—O3	1.975 (3)	O3—V2^iv	4.313 (3)
V2—V1^vi	3.0131 (14)	O3—V1^xxvi	4.366 (3)
V2—V1^xxvi	3.0131 (14)	O3—V1^xxi	4.805 (3)
V2—Sr1^xxii	3.5376 (13)	O3—V2^xxi	4.976 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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, z−1; (xxii) x−1, y, z; (xxiii) x+1, −y+3/2, z; (xxiv) −x−1/2, −y+3/2, z; (xxv) x−1, y, z+1; (xxvi) x−1/2, y+1/2, −z+1; (xxvii) −x−1/2, −y+3/2, z+1; (xxviii) x−1/2, y+1/2, −z; (xxix) −x, y+1/2, −z+1; (xxx) x−1, −y+3/2, z; (xxxi) x, −y+3/2, z+1; (xxxii) −x−1/2, y, z+1; (xxxiii) x−1/2, y+1/2, −z+2; (xxxiv) −x, −y+2, −z+1; (xxxv) x−1, y, z−1; (xxxvi) −x+1/2, −y+3/2, z−1; (xxxvii) −x−1/2, −y+3/2, z−1; (xxxviii) x+1, y, z−1.

(SrV3O7_200K)

Crystal data

O7V3·Sr	Dx = 3.968 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11571 reflections
a = 5.2934 (8) Å	θ = 3.9–32.1°
b = 10.537 (2) Å	µ = 13.58 mm^−1
c = 5.2889 (9) Å	T = 200 K
V = 294.99 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	335 independent reflections
Radiation source: fine-focus sealed tube	319 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.068
Detector resolution: 0 pixels mm^-1	θmax = 25.9°, θmin = 3.9°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.218, Tmax = 0.568	l = −6→6
5382 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.033	Secondary atom site location: difference Fourier map
wR(F^2) = 0.080	w = 1/[σ^2(Fo^2) + (0.0415P)^2 + 0.9218P] where P = (Fo^2 + 2Fc^2)/3
S = 1.23	(Δ/σ)max < 0.001
335 reflections	Δρmax = 0.61 e Å^−3
24 parameters	Δρmin = −0.86 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14897 (17)	0.0155 (3)
V1	0.2500	0.51518 (11)	0.6211 (2)	0.0131 (3)
V2	−0.2500	0.7500	0.5922 (3)	0.0132 (4)
O1	−0.2500	0.7500	−0.1024 (12)	0.0185 (15)*
O2	0.2500	0.5449 (5)	−0.0786 (9)	0.0195 (11)*
O3	−0.0116 (6)	0.6205 (3)	0.4639 (6)	0.0144 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0134 (5)	0.0134 (5)	0.0196 (5)	0.000	0.000	0.000
V1	0.0084 (6)	0.0117 (6)	0.0193 (6)	0.000	0.000	−0.0002 (4)
V2	0.0094 (8)	0.0112 (8)	0.0189 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.474 (5)	V2—V1^i	3.6263 (9)
Sr1—O2^i	2.474 (5)	V2—V1^xxii	3.6263 (9)
Sr1—O3^i	2.560 (3)	V2—V1^xxv	3.6263 (9)
Sr1—O3	2.560 (3)	V2—O1	3.674 (7)
Sr1—O3^ii	2.560 (3)	V2—O2^xix	3.835 (4)
Sr1—O3^iii	2.560 (3)	V2—O2^xxiii	3.835 (4)
Sr1—O1	2.962 (3)	V2—O2^v	3.835 (4)
Sr1—O1^iv	2.962 (3)	V2—O2^xxviii	3.835 (4)
Sr1—V1^i	3.5153 (14)	V2—Sr1^v	3.9592 (14)
Sr1—V1	3.5153 (14)	V2—Sr1^xxiii	3.9592 (14)
Sr1—V2^iv	3.5357 (13)	V2—O2^xxvii	4.033 (5)
Sr1—V2	3.5357 (13)	V2—O2^vi	4.033 (5)
V1—O2^v	1.619 (5)	V2—O2^x	4.127 (5)
V1—O3^iii	1.960 (3)	V2—O2^xxix	4.127 (5)
V1—O3	1.960 (3)	V2—O3^xiii	4.153 (3)
V1—O3^vi	1.959 (3)	V2—O3^xxx	4.153 (3)
V1—O3^vii	1.959 (3)	V2—O3^vi	4.153 (3)
V1—V1^vi	2.9578 (10)	V2—O3^xxvii	4.153 (3)
V1—V1^viii	2.9578 (10)	V2—O3^xxii	4.310 (3)
V1—V2^vi	3.0134 (14)	V2—O3^i	4.310 (3)
V1—V2^iv	3.6263 (9)	V2—O3^xxxi	4.310 (3)
V1—V2	3.6263 (9)	V2—O3^iii	4.310 (3)
V1—O2^viii	3.641 (3)	V2—O2^xxii	4.926 (4)
V1—O2^vi	3.641 (3)	V2—O2	4.926 (4)
V1—O2	3.714 (5)	V2—O2^xxv	4.926 (4)
V1—Sr1^v	3.7304 (14)	V2—O2^i	4.926 (4)
V1—O1^vi	3.780 (4)	V2—O3^xxxii	4.971 (3)
V1—O1^ix	3.907 (3)	V2—O3^xxviii	4.971 (3)
V1—O1^v	3.907 (3)	V2—O3^v	4.971 (3)
V1—O1^x	3.916 (5)	V2—O3^xxxiii	4.971 (3)
V1—O2^x	3.955 (4)	V2—V1^xxxiv	5.0116 (18)
V1—O2^xi	3.955 (4)	V2—V1^xviii	5.0116 (18)
V1—Sr1^vi	4.0362 (10)	V2—V2^xxi	5.2889 (9)
V1—Sr1^viii	4.0362 (10)	V2—V2^v	5.2889 (9)
V1—O3^iv	4.148 (3)	V2—V2^iv	5.2934 (8)
V1—O3^xii	4.148 (3)	V2—V2^xxii	5.2934 (8)
V1—O3^i	4.165 (3)	V2—Sr1^xxxv	5.4432 (12)
V1—O3^ii	4.165 (3)	V2—Sr1^vi	5.4432 (12)
V1—O3^xiii	4.301 (3)	V2—O3^xxxvi	5.532 (3)
V1—O3^viii	4.301 (3)	V2—O3^xxxvii	5.532 (3)
V1—O3^xiv	4.369 (3)	O1—V2^xxi	1.615 (7)
V1—O3^xv	4.369 (3)	O1—Sr1^xxii	2.962 (3)
V1—O3^xvi	4.798 (3)	O1—V1^xxvii	3.780 (4)
V1—O3^v	4.798 (3)	O1—V1^vi	3.780 (4)
V1—V1^xvii	4.8135 (19)	O1—V1^xxxviii	3.907 (3)
V1—V1^xviii	4.8135 (19)	O1—V1^xxxix	3.907 (3)
V1—O2^xix	4.900 (5)	O1—V1^xl	3.907 (3)
V1—V1^i	4.948 (2)	O1—V1^xxi	3.907 (3)
V1—V2^xviii	5.0116 (18)	O1—V1^x	3.916 (5)
V1—O3^xx	5.202 (3)	O1—V1^xxix	3.916 (5)
V1—O3^xviii	5.202 (3)	O2—V1^xxi	1.619 (5)
V1—O1	5.270 (5)	O2—V1^viii	3.641 (3)
V1—O1^iv	5.270 (5)	O2—V1^vi	3.641 (3)
V1—V1^xxi	5.2889 (9)	O2—V2^xli	3.835 (4)
V1—V1^xxii	5.2934 (8)	O2—V2^xxi	3.835 (4)
V1—V1^iv	5.2934 (8)	O2—V1^x	3.955 (4)
V1—O2^ix	5.5354 (17)	O2—V1^xi	3.955 (4)
V1—O2^xxiii	5.5354 (16)	O2—V2^vi	4.033 (5)
V1—O3^xxiv	5.541 (3)	O2—V2^x	4.127 (5)
V1—O3^xxv	5.541 (3)	O2—V1^xxxix	4.900 (5)
V1—V1^xxvi	5.588 (3)	O3—V1^vi	1.959 (3)
V2—O1^v	1.615 (7)	O3—V1^xxii	4.148 (3)
V2—O3^xii	1.979 (3)	O3—V2^vi	4.153 (3)
V2—O3^ii	1.979 (3)	O3—V1^i	4.165 (3)
V2—O3	1.979 (3)	O3—V1^viii	4.301 (3)
V2—O3^xxv	1.979 (3)	O3—V2^iv	4.310 (3)
V2—V1^vi	3.0134 (14)	O3—V1^xxvii	4.369 (3)
V2—V1^xxvii	3.0134 (14)	O3—V1^xxi	4.798 (3)
V2—Sr1^xxii	3.5357 (13)	O3—V2^xxi	4.971 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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, z−1; (xxii) x−1, y, z; (xxiii) x−1, y, z+1; (xxiv) x+1, −y+3/2, z; (xxv) −x−1/2, −y+3/2, z; (xxvi) −x+1/2, −y+1/2, z; (xxvii) x−1/2, y+1/2, −z+1; (xxviii) −x−1/2, −y+3/2, z+1; (xxix) x−1/2, y+1/2, −z; (xxx) −x, y+1/2, −z+1; (xxxi) x−1, −y+3/2, z; (xxxii) x, −y+3/2, z+1; (xxxiii) −x−1/2, y, z+1; (xxxiv) x−1/2, y+1/2, −z+2; (xxxv) −x, −y+2, −z+1; (xxxvi) −x−1, −y+1, −z+1; (xxxvii) x+1/2, y+1/2, −z+1; (xxxviii) x−1, y, z−1; (xxxix) −x+1/2, −y+3/2, z−1; (xl) −x−1/2, −y+3/2, z−1; (xli) x+1, y, z−1.

(SrV3O7_187K)

Crystal data

O7V3·Sr	Dx = 3.970 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11507 reflections
a = 5.2923 (8) Å	θ = 3.9–32.1°
b = 10.539 (2) Å	µ = 13.59 mm^−1
c = 5.2864 (9) Å	T = 187 K
V = 294.84 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	334 independent reflections
Radiation source: fine-focus sealed tube	317 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.070
Detector resolution: 0 pixels mm^-1	θmax = 25.8°, θmin = 3.9°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.217, Tmax = 0.567	l = −6→6
5376 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.033	Secondary atom site location: difference Fourier map
wR(F^2) = 0.079	w = 1/[σ^2(Fo^2) + (0.038P)^2 + 0.5256P] where P = (Fo^2 + 2Fc^2)/3
S = 1.34	(Δ/σ)max < 0.001
334 reflections	Δρmax = 0.68 e Å^−3
24 parameters	Δρmin = −1.08 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14884 (16)	0.0153 (3)
V1	0.2500	0.51513 (10)	0.6211 (2)	0.0129 (3)
V2	−0.2500	0.7500	0.5921 (3)	0.0128 (4)
O1	−0.2500	0.7500	−0.1020 (12)	0.0185 (15)*
O2	0.2500	0.5449 (4)	−0.0784 (9)	0.0187 (10)*
O3	−0.0119 (6)	0.6207 (3)	0.4642 (6)	0.0142 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0133 (5)	0.0133 (5)	0.0192 (5)	0.000	0.000	0.000
V1	0.0080 (6)	0.0111 (6)	0.0195 (6)	0.000	0.000	0.0000 (4)
V2	0.0090 (7)	0.0106 (7)	0.0187 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.473 (5)	V2—V1^i	3.6266 (9)
Sr1—O2^i	2.473 (5)	V2—V1^xxii	3.6266 (9)
Sr1—O3^i	2.561 (3)	V2—V1^xxv	3.6266 (9)
Sr1—O3^ii	2.561 (3)	V2—O1	3.669 (7)
Sr1—O3^iii	2.561 (3)	V2—O2^xix	3.835 (3)
Sr1—O3	2.561 (3)	V2—O2^xxiii	3.835 (3)
Sr1—O1	2.960 (3)	V2—O2^v	3.835 (3)
Sr1—O1^iv	2.960 (3)	V2—O2^xxvii	3.835 (3)
Sr1—V1^i	3.5156 (14)	V2—Sr1^v	3.9577 (14)
Sr1—V1	3.5156 (14)	V2—Sr1^xxiii	3.9577 (14)
Sr1—V2^iv	3.5346 (13)	V2—O2^xxvi	4.033 (5)
Sr1—V2	3.5346 (13)	V2—O2^vi	4.033 (5)
V1—O2^v	1.620 (5)	V2—O2^x	4.128 (5)
V1—O3^vi	1.960 (3)	V2—O2^xxviii	4.128 (5)
V1—O3^vii	1.960 (3)	V2—O3^xiii	4.156 (3)
V1—O3^iii	1.962 (3)	V2—O3^xxix	4.156 (3)
V1—O3	1.962 (3)	V2—O3^xxvi	4.156 (3)
V1—V1^vi	2.9568 (10)	V2—O3^vi	4.156 (3)
V1—V1^viii	2.9568 (10)	V2—O3^xxii	4.310 (3)
V1—V2^vi	3.0129 (14)	V2—O3^i	4.310 (3)
V1—V2^iv	3.6266 (9)	V2—O3^xxx	4.310 (3)
V1—V2	3.6266 (9)	V2—O3^iii	4.310 (3)
V1—O2^viii	3.640 (3)	V2—O2^xxii	4.923 (4)
V1—O2^vi	3.640 (3)	V2—O2^xxv	4.923 (4)
V1—O2	3.711 (5)	V2—O2	4.923 (4)
V1—Sr1^v	3.7296 (13)	V2—O2^i	4.923 (4)
V1—O1^vi	3.777 (4)	V2—O3^xxxi	4.969 (3)
V1—O1^ix	3.908 (3)	V2—O3^xxvii	4.969 (3)
V1—O1^v	3.908 (3)	V2—O3^v	4.969 (3)
V1—O1^x	3.916 (5)	V2—O3^xxxii	4.969 (3)
V1—O2^x	3.954 (4)	V2—V1^xxxiii	5.0107 (18)
V1—O2^xi	3.954 (4)	V2—V1^xviii	5.0107 (18)
V1—Sr1^vi	4.0359 (10)	V2—V2^v	5.2864 (9)
V1—Sr1^viii	4.0359 (10)	V2—V2^xxi	5.2864 (9)
V1—O3^iv	4.145 (3)	V2—V2^iv	5.2923 (8)
V1—O3^xii	4.145 (3)	V2—V2^xxii	5.2923 (8)
V1—O3^i	4.164 (3)	V2—Sr1^xxxiv	5.4444 (12)
V1—O3^ii	4.164 (3)	V2—Sr1^vi	5.4444 (12)
V1—O3^xiii	4.303 (3)	V2—O1^ix	5.534 (2)
V1—O3^viii	4.303 (3)	V2—O1^xxiii	5.534 (2)
V1—O3^xiv	4.367 (3)	O1—V2^xxi	1.617 (6)
V1—O3^xv	4.367 (3)	O1—Sr1^xxii	2.960 (3)
V1—O3^xvi	4.798 (3)	O1—V1^xxvi	3.777 (4)
V1—O3^v	4.798 (3)	O1—V1^vi	3.777 (4)
V1—V1^xvii	4.8117 (19)	O1—V1^xxxv	3.908 (3)
V1—V1^xviii	4.8117 (19)	O1—V1^xxxvi	3.908 (3)
V1—O2^xix	4.901 (5)	O1—V1^xxxvii	3.908 (3)
V1—V1^i	4.950 (2)	O1—V1^xxi	3.908 (3)
V1—V2^xviii	5.0107 (18)	O1—V1^x	3.916 (5)
V1—O3^xx	5.198 (3)	O1—V1^xxviii	3.916 (5)
V1—O3^xviii	5.198 (3)	O2—V1^xxi	1.620 (5)
V1—O1	5.267 (5)	O2—V1^viii	3.640 (3)
V1—O1^iv	5.267 (5)	O2—V1^vi	3.640 (3)
V1—V1^xxi	5.2864 (9)	O2—V2^xxxviii	3.835 (3)
V1—V1^v	5.2864 (9)	O2—V2^xxi	3.835 (3)
V1—V1^xxii	5.2923 (8)	O2—V1^x	3.954 (4)
V1—V1^iv	5.2923 (8)	O2—V1^xi	3.954 (4)
V1—O2^ix	5.5346 (16)	O2—V2^vi	4.033 (5)
V1—O2^xxiii	5.5346 (16)	O2—V2^x	4.128 (5)
V1—O3^xxiv	5.538 (3)	O2—V1^xxxvi	4.901 (5)
V1—O3^xxv	5.538 (3)	O3—V1^vi	1.960 (3)
V2—O1^v	1.617 (6)	O3—V1^xxii	4.145 (3)
V2—O3^xii	1.975 (3)	O3—V2^vi	4.156 (3)
V2—O3^ii	1.975 (3)	O3—V1^i	4.164 (3)
V2—O3	1.975 (3)	O3—V1^viii	4.303 (3)
V2—O3^xxv	1.975 (3)	O3—V2^iv	4.310 (3)
V2—V1^vi	3.0129 (14)	O3—V1^xxvi	4.367 (3)
V2—V1^xxvi	3.0129 (14)	O3—V1^xxi	4.798 (3)
V2—Sr1^xxii	3.5346 (13)	O3—V2^xxi	4.969 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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, z−1; (xxii) x−1, y, z; (xxiii) x−1, y, z+1; (xxiv) x+1, −y+3/2, z; (xxv) −x−1/2, −y+3/2, z; (xxvi) x−1/2, y+1/2, −z+1; (xxvii) −x−1/2, −y+3/2, z+1; (xxviii) x−1/2, y+1/2, −z; (xxix) −x, y+1/2, −z+1; (xxx) x−1, −y+3/2, z; (xxxi) x, −y+3/2, z+1; (xxxii) −x−1/2, y, z+1; (xxxiii) x−1/2, y+1/2, −z+2; (xxxiv) −x, −y+2, −z+1; (xxxv) x−1, y, z−1; (xxxvi) −x+1/2, −y+3/2, z−1; (xxxvii) −x−1/2, −y+3/2, z−1; (xxxviii) x+1, y, z−1.

(SrV3O7_175K)

Crystal data

O7V3·Sr	Dx = 3.973 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11566 reflections
a = 5.2914 (8) Å	θ = 3.9–32.1°
b = 10.539 (2) Å	µ = 13.60 mm^−1
c = 5.2828 (9) Å	T = 175 K
V = 294.60 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	333 independent reflections
Radiation source: fine-focus sealed tube	317 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.070
Detector resolution: 0 pixels mm^-1	θmax = 25.6°, θmin = 3.9°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.213, Tmax = 0.567	l = −6→6
5350 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.034	Secondary atom site location: difference Fourier map
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0452P)^2 + 0.7112P] where P = (Fo^2 + 2Fc^2)/3
S = 1.22	(Δ/σ)max < 0.001
333 reflections	Δρmax = 0.60 e Å^−3
24 parameters	Δρmin = −1.14 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14892 (16)	0.0151 (3)
V1	0.2500	0.51511 (11)	0.6211 (2)	0.0129 (3)
V2	−0.2500	0.7500	0.5923 (3)	0.0129 (4)
O1	−0.2500	0.7500	−0.1027 (12)	0.0177 (15)*
O2	0.2500	0.5448 (4)	−0.0779 (9)	0.0182 (10)*
O3	−0.0118 (6)	0.6208 (3)	0.4644 (6)	0.0143 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0123 (5)	0.0132 (5)	0.0197 (5)	0.000	0.000	0.000
V1	0.0083 (6)	0.0112 (6)	0.0191 (6)	0.000	0.000	−0.0002 (4)
V2	0.0092 (8)	0.0112 (8)	0.0182 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.473 (5)	V2—V1^i	3.6265 (9)
Sr1—O2^i	2.473 (5)	V2—V1^xxii	3.6265 (9)
Sr1—O3^i	2.560 (3)	V2—V1^xxv	3.6265 (9)
Sr1—O3^ii	2.560 (3)	V2—O1	3.671 (7)
Sr1—O3^iii	2.560 (3)	V2—O2^xix	3.836 (3)
Sr1—O3	2.560 (3)	V2—O2^xxvii	3.836 (3)
Sr1—O1	2.961 (3)	V2—O2^xxiii	3.836 (3)
Sr1—O1^iv	2.961 (3)	V2—O2^v	3.836 (3)
Sr1—V1^i	3.5144 (14)	V2—Sr1^v	3.9556 (14)
Sr1—V1	3.5144 (14)	V2—Sr1^xxiii	3.9556 (14)
Sr1—V2^iv	3.5335 (13)	V2—O2^xxvi	4.029 (5)
Sr1—V2	3.5335 (13)	V2—O2^vi	4.029 (5)
V1—O2^v	1.620 (5)	V2—O2^x	4.127 (5)
V1—O3^vi	1.961 (3)	V2—O2^xxviii	4.127 (5)
V1—O3^vii	1.961 (3)	V2—O3^xiii	4.157 (3)
V1—O3^iii	1.961 (3)	V2—O3^xxix	4.157 (3)
V1—O3	1.961 (3)	V2—O3^xxvi	4.157 (3)
V1—V1^vi	2.9562 (10)	V2—O3^vi	4.157 (3)
V1—V1^viii	2.9562 (10)	V2—O3^xxii	4.308 (3)
V1—V2^vi	3.0129 (14)	V2—O3^xxx	4.308 (3)
V1—V2^iv	3.6265 (9)	V2—O3^i	4.308 (3)
V1—V2	3.6265 (9)	V2—O3^iii	4.308 (3)
V1—O2^viii	3.636 (3)	V2—O2^xxii	4.921 (4)
V1—O2^vi	3.636 (3)	V2—O2^xxv	4.921 (4)
V1—O2	3.706 (5)	V2—O2	4.921 (4)
V1—Sr1^v	3.7286 (13)	V2—O2^i	4.921 (4)
V1—O1^vi	3.779 (4)	V2—O3^xxxi	4.967 (3)
V1—O1^ix	3.906 (3)	V2—O3^xxvii	4.967 (3)
V1—O1^v	3.906 (3)	V2—O3^v	4.967 (3)
V1—O1^x	3.912 (5)	V2—O3^xxxii	4.967 (3)
V1—O2^x	3.954 (4)	V2—V1^xxxiii	5.0074 (18)
V1—O2^xi	3.954 (4)	V2—V1^xviii	5.0074 (18)
V1—Sr1^vi	4.0351 (10)	V2—V2^xxi	5.2828 (9)
V1—Sr1^viii	4.0351 (10)	V2—V2^v	5.2828 (9)
V1—O3^iv	4.145 (3)	V2—V2^iv	5.2914 (8)
V1—O3^xii	4.145 (3)	V2—V2^xxii	5.2914 (8)
V1—O3^i	4.163 (3)	V2—Sr1^xxxiv	5.4440 (12)
V1—O3^ii	4.163 (3)	V2—Sr1^vi	5.4440 (12)
V1—O3^xiii	4.302 (3)	V2—O1^ix	5.531 (2)
V1—O3^viii	4.302 (3)	V2—O1^xxiii	5.531 (2)
V1—O3^xiv	4.366 (3)	O1—V2^xxi	1.611 (7)
V1—O3^xv	4.366 (3)	O1—Sr1^xxii	2.961 (3)
V1—O3^xvi	4.797 (3)	O1—V1^xxvi	3.779 (4)
V1—O3^v	4.797 (3)	O1—V1^vi	3.779 (4)
V1—V1^xvii	4.8088 (19)	O1—V1^xxxv	3.906 (3)
V1—V1^xviii	4.8088 (19)	O1—V1^xxxvi	3.906 (3)
V1—O2^xix	4.903 (5)	O1—V1^xxxvii	3.906 (3)
V1—V1^i	4.951 (2)	O1—V1^xxi	3.906 (3)
V1—V2^xviii	5.0074 (18)	O1—V1^x	3.912 (5)
V1—O3^xx	5.194 (3)	O1—V1^xxviii	3.912 (5)
V1—O3^xviii	5.194 (3)	O2—V1^xxi	1.620 (5)
V1—O1	5.268 (5)	O2—V1^viii	3.636 (3)
V1—O1^iv	5.268 (5)	O2—V1^vi	3.636 (3)
V1—V1^v	5.2828 (9)	O2—V2^xxxviii	3.836 (3)
V1—V1^xxi	5.2828 (9)	O2—V2^xxi	3.836 (3)
V1—V1^xxii	5.2914 (8)	O2—V1^x	3.954 (4)
V1—V1^iv	5.2914 (8)	O2—V1^xi	3.954 (4)
V1—O2^ix	5.5339 (16)	O2—V2^vi	4.029 (5)
V1—O2^xxiii	5.5339 (16)	O2—V2^x	4.127 (5)
V1—O3^xxiv	5.538 (3)	O2—V1^xxxvi	4.903 (5)
V1—O3^xxv	5.538 (3)	O3—V1^vi	1.961 (3)
V2—O1^v	1.611 (7)	O3—V1^xxii	4.145 (3)
V2—O3^xii	1.975 (3)	O3—V2^vi	4.157 (3)
V2—O3^xxv	1.975 (3)	O3—V1^i	4.163 (3)
V2—O3^ii	1.975 (3)	O3—V1^viii	4.302 (3)
V2—O3	1.975 (3)	O3—V2^iv	4.308 (3)
V2—V1^vi	3.0129 (14)	O3—V1^xxvi	4.366 (3)
V2—V1^xxvi	3.0129 (14)	O3—V1^xxi	4.797 (3)
V2—Sr1^xxii	3.5335 (13)	O3—V2^xxi	4.967 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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, z−1; (xxii) x−1, y, z; (xxiii) x−1, y, z+1; (xxiv) x+1, −y+3/2, z; (xxv) −x−1/2, −y+3/2, z; (xxvi) x−1/2, y+1/2, −z+1; (xxvii) −x−1/2, −y+3/2, z+1; (xxviii) x−1/2, y+1/2, −z; (xxix) −x, y+1/2, −z+1; (xxx) x−1, −y+3/2, z; (xxxi) x, −y+3/2, z+1; (xxxii) −x−1/2, y, z+1; (xxxiii) x−1/2, y+1/2, −z+2; (xxxiv) −x, −y+2, −z+1; (xxxv) x−1, y, z−1; (xxxvi) −x+1/2, −y+3/2, z−1; (xxxvii) −x−1/2, −y+3/2, z−1; (xxxviii) x+1, y, z−1.

(SrV3O7_150K)

Crystal data

O7V3·Sr	Dx = 3.977 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11695 reflections
a = 5.2909 (8) Å	θ = 3.9–32.1°
b = 10.544 (2) Å	µ = 13.61 mm^−1
c = 5.2763 (9) Å	T = 150 K
V = 294.34 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	334 independent reflections
Radiation source: fine-focus sealed tube	320 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.070
Detector resolution: 0 pixels mm^-1	θmax = 25.9°, θmin = 3.9°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.217, Tmax = 0.567	l = −6→6
5332 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.034	Secondary atom site location: difference Fourier map
wR(F^2) = 0.080	w = 1/[σ^2(Fo^2) + (0.041P)^2 + 0.4275P] where P = (Fo^2 + 2Fc^2)/3
S = 1.33	(Δ/σ)max < 0.001
334 reflections	Δρmax = 0.60 e Å^−3
24 parameters	Δρmin = −1.24 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14892 (16)	0.0144 (3)
V1	0.2500	0.51507 (10)	0.6213 (2)	0.0125 (3)
V2	−0.2500	0.7500	0.5928 (3)	0.0124 (4)
O1	−0.2500	0.7500	−0.1015 (12)	0.0168 (14)*
O2	0.2500	0.5447 (4)	−0.0776 (9)	0.0185 (10)*
O3	−0.0117 (5)	0.6207 (3)	0.4644 (6)	0.0137 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0117 (5)	0.0128 (5)	0.0188 (5)	0.000	0.000	0.000
V1	0.0079 (6)	0.0106 (6)	0.0190 (6)	0.000	0.000	−0.0003 (4)
V2	0.0088 (7)	0.0110 (8)	0.0174 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.473 (5)	V2—V1^i	3.6273 (9)
Sr1—O2^i	2.473 (5)	V2—V1^xxii	3.6273 (9)
Sr1—O3^i	2.559 (3)	V2—V1^xxv	3.6273 (9)
Sr1—O3^ii	2.559 (3)	V2—O1	3.663 (6)
Sr1—O3^iii	2.559 (3)	V2—O2^xix	3.835 (3)
Sr1—O3	2.559 (3)	V2—O2^xxiii	3.835 (3)
Sr1—O1	2.957 (3)	V2—O2^v	3.835 (3)
Sr1—O1^iv	2.957 (3)	V2—O2^xxvii	3.835 (3)
Sr1—V1^i	3.5140 (14)	V2—Sr1^v	3.9509 (14)
Sr1—V1	3.5140 (13)	V2—Sr1^xxiii	3.9509 (14)
Sr1—V2^iv	3.5331 (12)	V2—O2^xxvi	4.024 (5)
Sr1—V2	3.5331 (12)	V2—O2^vi	4.024 (5)
V1—O2^v	1.619 (5)	V2—O2^x	4.128 (5)
V1—O3^iii	1.960 (3)	V2—O2^xxviii	4.128 (5)
V1—O3	1.960 (3)	V2—O3^xiii	4.157 (3)
V1—O3^vi	1.960 (3)	V2—O3^xxix	4.157 (3)
V1—O3^vii	1.960 (3)	V2—O3^vi	4.157 (3)
V1—V1^vi	2.9560 (10)	V2—O3^xxvi	4.157 (3)
V1—V1^viii	2.9560 (10)	V2—O3^xxii	4.308 (3)
V1—V2^vi	3.0144 (14)	V2—O3^i	4.308 (3)
V1—V2^iv	3.6273 (9)	V2—O3^xxx	4.308 (3)
V1—V2	3.6273 (9)	V2—O3^iii	4.308 (3)
V1—O2^viii	3.632 (3)	V2—O2^xxii	4.919 (4)
V1—O2^vi	3.632 (3)	V2—O2^xxv	4.919 (4)
V1—O2	3.701 (5)	V2—O2	4.919 (4)
V1—Sr1^v	3.7264 (13)	V2—O2^i	4.919 (4)
V1—O1^vi	3.772 (4)	V2—O3^xxxi	4.960 (3)
V1—O1^ix	3.908 (2)	V2—O3^xxvii	4.960 (3)
V1—O1^v	3.908 (2)	V2—O3^v	4.960 (3)
V1—O1^x	3.916 (5)	V2—O3^xxxii	4.960 (3)
V1—O2^x	3.953 (4)	V2—V1^xxxiii	5.0007 (18)
V1—O2^xi	3.953 (4)	V2—V1^xviii	5.0007 (18)
V1—Sr1^vi	4.0347 (10)	V2—V2^v	5.2763 (9)
V1—Sr1^viii	4.0347 (10)	V2—V2^xxi	5.2763 (9)
V1—O3^iv	4.145 (3)	V2—V2^iv	5.2909 (8)
V1—O3^xii	4.145 (3)	V2—V2^xxii	5.2909 (8)
V1—O3^i	4.166 (3)	V2—Sr1^xxxiv	5.4452 (12)
V1—O3^ii	4.166 (3)	V2—Sr1^vi	5.4452 (12)
V1—O3^xiii	4.300 (3)	V2—O1^ix	5.531 (2)
V1—O3^viii	4.300 (3)	V2—O1^xxiii	5.531 (2)
V1—O3^xiv	4.369 (3)	O1—V2^xxi	1.613 (6)
V1—O3^xv	4.369 (3)	O1—Sr1^xxii	2.957 (3)
V1—O3^xvi	4.790 (3)	O1—V1^xxvi	3.772 (4)
V1—O3^v	4.790 (3)	O1—V1^vi	3.772 (4)
V1—V1^xvii	4.8030 (19)	O1—V1^xxxv	3.908 (2)
V1—V1^xviii	4.8030 (19)	O1—V1^xxxvi	3.908 (2)
V1—O2^xix	4.906 (5)	O1—V1^xxxvii	3.908 (2)
V1—V1^i	4.954 (2)	O1—V1^xxi	3.908 (2)
V1—V2^xviii	5.0007 (18)	O1—V1^x	3.916 (5)
V1—O3^xx	5.187 (3)	O1—V1^xxviii	3.916 (5)
V1—O3^xviii	5.187 (3)	O2—V1^xxi	1.619 (5)
V1—O1	5.261 (5)	O2—V1^viii	3.632 (3)
V1—O1^iv	5.261 (5)	O2—V1^vi	3.632 (3)
V1—V1^xxi	5.2763 (9)	O2—V2^xxxviii	3.835 (3)
V1—V1^v	5.2763 (9)	O2—V2^xxi	3.835 (3)
V1—V1^xxii	5.2909 (8)	O2—V1^x	3.953 (4)
V1—V1^iv	5.2909 (8)	O2—V1^xi	3.953 (4)
V1—O2^ix	5.5331 (16)	O2—V2^vi	4.024 (5)
V1—O2^xxiii	5.5331 (16)	O2—V2^x	4.128 (5)
V1—O3^xxiv	5.540 (3)	O2—V1^xxxvi	4.906 (5)
V1—O3^xxv	5.540 (3)	O3—V1^vi	1.960 (3)
V2—O1^v	1.613 (6)	O3—V1^xxii	4.145 (3)
V2—O3^xii	1.977 (3)	O3—V2^vi	4.157 (3)
V2—O3^ii	1.977 (3)	O3—V1^i	4.166 (3)
V2—O3	1.977 (3)	O3—V1^viii	4.300 (3)
V2—O3^xxv	1.977 (3)	O3—V2^iv	4.308 (3)
V2—V1^vi	3.0144 (14)	O3—V1^xxvi	4.369 (3)
V2—V1^xxvi	3.0144 (14)	O3—V1^xxi	4.790 (3)
V2—Sr1^xxii	3.5331 (12)	O3—V2^xxi	4.960 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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, z−1; (xxii) x−1, y, z; (xxiii) x−1, y, z+1; (xxiv) x+1, −y+3/2, z; (xxv) −x−1/2, −y+3/2, z; (xxvi) x−1/2, y+1/2, −z+1; (xxvii) −x−1/2, −y+3/2, z+1; (xxviii) x−1/2, y+1/2, −z; (xxix) −x, y+1/2, −z+1; (xxx) x−1, −y+3/2, z; (xxxi) x, −y+3/2, z+1; (xxxii) −x−1/2, y, z+1; (xxxiii) x−1/2, y+1/2, −z+2; (xxxiv) −x, −y+2, −z+1; (xxxv) x−1, y, z−1; (xxxvi) −x+1/2, −y+3/2, z−1; (xxxvii) −x−1/2, −y+3/2, z−1; (xxxviii) x+1, y, z−1.

(SrV3O7_125K)

Crystal data

O7V3·Sr	Dx = 3.981 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 11774 reflections
a = 5.2894 (8) Å	θ = 3.9–32.1°
b = 10.547 (2) Å	µ = 13.63 mm^−1
c = 5.2697 (9) Å	T = 125 K
V = 293.99 (9) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	331 independent reflections
Radiation source: fine-focus sealed tube	321 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.072
Detector resolution: 0 pixels mm^-1	θmax = 25.6°, θmin = 3.9°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.213, Tmax = 0.567	l = −6→6
5316 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.035	Secondary atom site location: difference Fourier map
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0404P)^2 + 0.623P] where P = (Fo^2 + 2Fc^2)/3
S = 1.34	(Δ/σ)max < 0.001
331 reflections	Δρmax = 0.63 e Å^−3
24 parameters	Δρmin = −0.91 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14880 (17)	0.0138 (3)
V1	0.2500	0.51499 (11)	0.6214 (2)	0.0120 (4)
V2	−0.2500	0.7500	0.5930 (3)	0.0123 (4)
O1	−0.2500	0.7500	−0.1008 (13)	0.0173 (15)*
O2	0.2500	0.5443 (5)	−0.0765 (9)	0.0170 (11)*
O3	−0.0119 (6)	0.6209 (3)	0.4646 (6)	0.0134 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0110 (5)	0.0124 (5)	0.0181 (5)	0.000	0.000	0.000
V1	0.0077 (6)	0.0107 (6)	0.0177 (7)	0.000	0.000	−0.0001 (4)
V2	0.0093 (8)	0.0105 (8)	0.0170 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.473 (5)	V2—V1^i	3.6278 (9)
Sr1—O2^i	2.473 (5)	V2—V1^xxii	3.6278 (9)
Sr1—O3^i	2.558 (3)	V2—V1^xxv	3.6278 (9)
Sr1—O3	2.558 (3)	V2—O1	3.656 (7)
Sr1—O3^ii	2.558 (3)	V2—O2^xix	3.839 (4)
Sr1—O3^iii	2.558 (3)	V2—O2^xxvii	3.839 (4)
Sr1—O1	2.954 (3)	V2—O2^xxiii	3.839 (4)
Sr1—O1^iv	2.954 (3)	V2—O2^v	3.839 (4)
Sr1—V1^i	3.5139 (14)	V2—Sr1^v	3.9462 (14)
Sr1—V1	3.5139 (14)	V2—Sr1^xxiii	3.9462 (14)
Sr1—V2^iv	3.5319 (13)	V2—O2^xxvi	4.015 (5)
Sr1—V2	3.5319 (13)	V2—O2^vi	4.015 (5)
V1—O2^v	1.622 (5)	V2—O2^x	4.128 (5)
V1—O3^vi	1.961 (3)	V2—O2^xxviii	4.128 (5)
V1—O3^vii	1.961 (3)	V2—O3^xxix	4.161 (3)
V1—O3^iii	1.962 (3)	V2—O3^xiii	4.161 (3)
V1—O3	1.962 (3)	V2—O3^xxvi	4.161 (3)
V1—V1^vi	2.9551 (11)	V2—O3^vi	4.161 (3)
V1—V1^viii	2.9551 (11)	V2—O3^xxii	4.307 (3)
V1—V2^vi	3.0147 (14)	V2—O3^i	4.307 (3)
V1—O2^viii	3.624 (3)	V2—O3^xxx	4.307 (3)
V1—O2^vi	3.624 (3)	V2—O3^iii	4.307 (3)
V1—V2^iv	3.6278 (9)	V2—O2^xxii	4.914 (4)
V1—V2	3.6278 (9)	V2—O2^xxv	4.914 (4)
V1—O2	3.691 (5)	V2—O2	4.914 (4)
V1—Sr1^v	3.7238 (14)	V2—O2^i	4.914 (4)
V1—O1^vi	3.767 (5)	V2—O3^xxxi	4.953 (3)
V1—O1^ix	3.909 (3)	V2—O3^xxvii	4.953 (3)
V1—O1^v	3.909 (3)	V2—O3^v	4.953 (3)
V1—O1^x	3.917 (5)	V2—O3^xxxii	4.953 (3)
V1—O2^x	3.954 (4)	V2—V1^xxxiii	4.9948 (18)
V1—O2^xi	3.954 (4)	V2—V1^xviii	4.9948 (18)
V1—Sr1^vi	4.0339 (10)	V2—V2^v	5.2697 (9)
V1—Sr1^viii	4.0339 (10)	V2—V2^xxi	5.2697 (9)
V1—O3^iv	4.144 (3)	V2—V2^iv	5.2894 (8)
V1—O3^xii	4.144 (3)	V2—V2^xxii	5.2894 (8)
V1—O3^i	4.166 (3)	V2—Sr1^xxxiv	5.4463 (12)
V1—O3^ii	4.166 (3)	V2—Sr1^vi	5.4463 (12)
V1—O3^xiii	4.301 (3)	V2—O1^ix	5.530 (2)
V1—O3^viii	4.301 (3)	V2—O1^xxiii	5.530 (2)
V1—O3^xiv	4.367 (3)	O1—V2^xxi	1.614 (7)
V1—O3^xv	4.367 (3)	O1—Sr1^xxii	2.954 (3)
V1—O3^xvi	4.786 (3)	O1—V1^xxvi	3.767 (4)
V1—O3^v	4.786 (3)	O1—V1^vi	3.767 (4)
V1—V1^xvii	4.797 (2)	O1—V1^xxxv	3.909 (3)
V1—V1^xviii	4.7972 (19)	O1—V1^xxxvi	3.909 (3)
V1—O2^xix	4.914 (5)	O1—V1^xxxvii	3.909 (3)
V1—V1^i	4.957 (3)	O1—V1^xxi	3.909 (3)
V1—V2^xviii	4.9948 (18)	O1—V1^x	3.917 (5)
V1—O3^xx	5.181 (3)	O1—V1^xxviii	3.917 (5)
V1—O3^xviii	5.181 (3)	O2—V1^xxi	1.622 (5)
V1—O1	5.256 (5)	O2—V1^viii	3.624 (3)
V1—O1^iv	5.256 (5)	O2—V1^vi	3.624 (3)
V1—V1^v	5.2697 (9)	O2—V2^xxxviii	3.839 (4)
V1—V1^xxi	5.2697 (9)	O2—V2^xxi	3.839 (4)
V1—V1^xxii	5.2894 (8)	O2—V1^x	3.954 (4)
V1—V1^iv	5.2894 (8)	O2—V1^xi	3.954 (4)
V1—O2^ix	5.5324 (16)	O2—V2^vi	4.015 (5)
V1—O2^xxiii	5.5324 (16)	O2—V2^x	4.128 (5)
V1—O3^xxiv	5.539 (3)	O2—V2^iv	4.914 (4)
V1—O3^xxv	5.539 (3)	O3—V1^vi	1.961 (3)
V2—O1^v	1.614 (7)	O3—V1^xxii	4.144 (3)
V2—O3^xii	1.975 (3)	O3—V2^vi	4.161 (3)
V2—O3^xxv	1.975 (3)	O3—V1^i	4.166 (3)
V2—O3^ii	1.975 (3)	O3—V1^viii	4.301 (3)
V2—O3	1.975 (3)	O3—V2^iv	4.307 (3)
V2—V1^vi	3.0147 (14)	O3—V1^xxvi	4.367 (3)
V2—V1^xxvi	3.0147 (14)	O3—V1^xxi	4.786 (3)
V2—Sr1^xxii	3.5319 (13)	O3—V2^xxi	4.953 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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, z−1; (xxii) x−1, y, z; (xxiii) x−1, y, z+1; (xxiv) x+1, −y+3/2, z; (xxv) −x−1/2, −y+3/2, z; (xxvi) x−1/2, y+1/2, −z+1; (xxvii) −x−1/2, −y+3/2, z+1; (xxviii) x−1/2, y+1/2, −z; (xxix) −x, y+1/2, −z+1; (xxx) x−1, −y+3/2, z; (xxxi) x, −y+3/2, z+1; (xxxii) −x−1/2, y, z+1; (xxxiii) x−1/2, y+1/2, −z+2; (xxxiv) −x, −y+2, −z+1; (xxxv) x−1, y, z−1; (xxxvi) −x+1/2, −y+3/2, z−1; (xxxvii) −x−1/2, −y+3/2, z−1; (xxxviii) x+1, y, z−1.

(SrV3O7_100K)

Crystal data

O7V3·Sr	Dx = 3.977 Mg m^−3
Mr = 352.44	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pmmn	Cell parameters from 10067 reflections
a = 5.2918 (12) Å	θ = 3.8–32.3°
b = 10.550 (3) Å	µ = 13.61 mm^−1
c = 5.2717 (14) Å	T = 100 K
V = 294.32 (14) Å^3	Needle, brown
Z = 2	0.15 × 0.1 × 0.02 mm
F(000) = 326

Data collection

STOE IPDS 2 diffractometer	321 independent reflections
Radiation source: fine-focus sealed tube	307 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.073
Detector resolution: 0 pixels mm^-1	θmax = 25.5°, θmin = 3.9°
Rotation method scans	h = −5→6
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −12→12
Tmin = 0.207, Tmax = 0.567	l = −6→6
5327 measured reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.032	Secondary atom site location: difference Fourier map
wR(F^2) = 0.079	w = 1/[σ^2(Fo^2) + (0.0396P)^2 + 1.0644P] where P = (Fo^2 + 2Fc^2)/3
S = 1.24	(Δ/σ)max < 0.001
321 reflections	Δρmax = 0.68 e Å^−3
24 parameters	Δρmin = −1.16 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Sr1	0.2500	0.7500	0.14894 (17)	0.0127 (3)
V1	0.2500	0.51497 (11)	0.6214 (2)	0.0114 (4)
V2	−0.2500	0.7500	0.5931 (3)	0.0114 (4)
O1	−0.2500	0.7500	−0.1003 (12)	0.0143 (15)*
O2	0.2500	0.5444 (5)	−0.0759 (9)	0.0156 (11)*
O3	−0.0117 (6)	0.6210 (3)	0.4651 (6)	0.0128 (7)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sr1	0.0095 (5)	0.0113 (5)	0.0175 (5)	0.000	0.000	0.000
V1	0.0073 (6)	0.0100 (6)	0.0168 (7)	0.000	0.000	0.0000 (4)
V2	0.0076 (8)	0.0096 (8)	0.0171 (8)	0.000	0.000	0.000

Bond lengths (Å)

Sr1—O2	2.472 (5)	V2—Sr1^xxii	3.5333 (14)
Sr1—O2^i	2.472 (5)	V2—V1^xxii	3.6293 (11)
Sr1—O3^i	2.559 (3)	V2—V1^i	3.6293 (11)
Sr1—O3^ii	2.559 (3)	V2—V1^xxv	3.6293 (11)
Sr1—O3^iii	2.559 (3)	V2—O1	3.656 (7)
Sr1—O3	2.559 (3)	V2—O2^xix	3.841 (4)
Sr1—O1	2.954 (3)	V2—O2^xxiii	3.841 (4)
Sr1—O1^iv	2.954 (3)	V2—O2^v	3.841 (4)
Sr1—V1^i	3.5144 (15)	V2—O2^xxviii	3.841 (4)
Sr1—V1	3.5144 (15)	V2—Sr1^v	3.9479 (16)
Sr1—V2^iv	3.5333 (14)	V2—Sr1^xxiii	3.9479 (16)
Sr1—V2	3.5333 (14)	V2—O2^xxvii	4.015 (5)
V1—O2^v	1.626 (5)	V2—O2^vi	4.015 (5)
V1—O3^iii	1.962 (3)	V2—O2^x	4.133 (5)
V1—O3	1.962 (3)	V2—O2^xxix	4.133 (5)
V1—O3^vi	1.963 (3)	V2—O3^xiii	4.163 (3)
V1—O3^vii	1.963 (3)	V2—O3^xxx	4.163 (3)
V1—V1^vi	2.9560 (11)	V2—O3^vi	4.163 (3)
V1—V1^viii	2.9560 (11)	V2—O3^xxvii	4.163 (3)
V1—V2^vi	3.0156 (16)	V2—O3^xxii	4.308 (3)
V1—O2^viii	3.624 (3)	V2—O3^i	4.308 (3)
V1—O2^vi	3.624 (3)	V2—O3^xxxi	4.308 (3)
V1—V2^iv	3.6293 (11)	V2—O3^iii	4.308 (3)
V1—V2	3.6293 (11)	V2—O2^xxii	4.914 (5)
V1—O2	3.689 (5)	V2—O2^xxv	4.914 (4)
V1—Sr1^v	3.7261 (15)	V2—O2	4.914 (4)
V1—O1^vi	3.767 (4)	V2—O2^i	4.914 (5)
V1—O1^ix	3.912 (3)	V2—O3^xxxii	4.957 (4)
V1—O1^v	3.912 (3)	V2—O3^xxviii	4.957 (4)
V1—O1^x	3.919 (5)	V2—O3^v	4.957 (4)
V1—O2^x	3.958 (4)	V2—O3^xxxiii	4.957 (4)
V1—O2^xi	3.958 (4)	V2—V1^xxxiv	4.996 (2)
V1—Sr1^vi	4.0352 (12)	V2—V1^xviii	4.996 (2)
V1—Sr1^viii	4.0352 (12)	V2—V2^v	5.2717 (14)
V1—O3^iv	4.146 (3)	V2—V2^xxi	5.2717 (14)
V1—O3^xii	4.146 (3)	V2—V2^iv	5.2918 (12)
V1—O3^i	4.165 (4)	V2—V2^xxii	5.2918 (12)
V1—O3^ii	4.165 (4)	V2—Sr1^xxxv	5.4477 (17)
V1—O3^xiii	4.303 (3)	V2—Sr1^vi	5.4477 (17)
V1—O3^viii	4.303 (3)	V2—O1^ix	5.533 (2)
V1—O3^xiv	4.368 (4)	V2—O1^xxiii	5.533 (2)
V1—O3^xv	4.368 (4)	O1—V2^xxi	1.616 (7)
V1—O3^xvi	4.791 (3)	O1—O3^xxxvi	2.948 (6)
V1—O3^v	4.791 (3)	O1—O3^xxxvii	2.948 (6)
V1—V1^xvii	4.800 (2)	O1—O3^xxi	2.948 (6)
V1—V1^xviii	4.800 (2)	O1—O3^xxxviii	2.948 (6)
V1—O2^xix	4.916 (5)	O1—Sr1^xxii	2.954 (3)
V1—V1^i	4.959 (3)	O1—O3^ii	3.511 (6)
V1—V2^xviii	4.996 (2)	O1—O3^xxv	3.511 (6)
V1—O3^xx	5.181 (4)	O1—O3	3.511 (6)
V1—O3^xviii	5.181 (4)	O1—O3^xii	3.511 (6)
V1—O1	5.256 (5)	O2—V1^xxi	1.626 (5)
V1—O1^iv	5.256 (5)	O2—O3^xxi	2.903 (5)
V1—V1^xxi	5.2717 (14)	O2—O3^xxxix	2.903 (5)
V1—V1^xxii	5.2918 (12)	O2—O3^x	2.974 (5)
V1—V1^iv	5.2918 (12)	O2—O3^xl	2.974 (5)
V1—O2^ix	5.5360 (19)	O2—O3^iii	3.272 (5)
V1—O2^xxiii	5.5360 (19)	O2—O3	3.272 (5)
V1—O3^xxiv	5.540 (3)	O2—V1^viii	3.624 (3)
V1—O3^xxv	5.540 (3)	O2—V1^vi	3.624 (3)
V1—V1^xxvi	5.591 (3)	O2—V2^xli	3.841 (4)
V2—O1^v	1.616 (7)	O3—V1^vi	1.963 (3)
V2—O3^xii	1.974 (3)	O3—O3^xii	2.522 (6)
V2—O3^ii	1.974 (3)	O3—O3^vi	2.582 (6)
V2—O3^xxv	1.974 (3)	O3—O3^ii	2.722 (6)
V2—O3	1.974 (3)	O3—O3^iii	2.770 (6)
V2—V1^vi	3.0156 (15)	O3—O2^v	2.903 (5)
V2—V1^xxvii	3.0156 (16)	O3—O1^v	2.948 (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) −x−1/2, y, z; (xiii) x−1/2, −y+1, −z+1; (xiv) −x, y−1/2, −z+1; (xv) x+1/2, y−1/2, −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, z−1; (xxii) x−1, y, z; (xxiii) x−1, y, z+1; (xxiv) x+1, −y+3/2, z; (xxv) −x−1/2, −y+3/2, z; (xxvi) −x+1/2, −y+1/2, z; (xxvii) x−1/2, y+1/2, −z+1; (xxviii) −x−1/2, −y+3/2, z+1; (xxix) x−1/2, y+1/2, −z; (xxx) −x, y+1/2, −z+1; (xxxi) x−1, −y+3/2, z; (xxxii) x, −y+3/2, z+1; (xxxiii) −x−1/2, y, z+1; (xxxiv) x−1/2, y+1/2, −z+2; (xxxv) −x, −y+2, −z+1; (xxxvi) −x−1/2, y, z−1; (xxxvii) −x−1/2, −y+3/2, z−1; (xxxviii) x, −y+3/2, z−1; (xxxix) −x+1/2, y, z−1; (xl) x+1/2, −y+1, −z; (xli) x+1, y, z−1.

(CaV3O7_297K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.537 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2764 reflections
a = 10.446 (3) Å	θ = 1.3–23.4°
b = 10.365 (2) Å	µ = 5.67 mm^−1
c = 5.2889 (15) Å	T = 297 K
V = 572.6 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	389 independent reflections
Radiation source: fine-focus sealed tube	365 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.030
Detector resolution: 0 pixels mm^-1	θmax = 22.9°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.319, Tmax = 0.471	l = −5→5
2489 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.0331P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.054	(Δ/σ)max < 0.001
S = 1.28	Δρmax = 0.36 e Å^−3
389 reflections	Δρmin = −0.31 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.020 (2)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08454 (9)	0.2500	0.29937 (14)	0.0090 (3)
V1	0.28850 (7)	0.2500	0.79190 (12)	0.0069 (3)
V2	0.18751 (5)	0.52039 (6)	0.78356 (9)	0.0071 (3)
O1	0.4431 (3)	0.2500	0.8079 (5)	0.0138 (8)*
O2	0.0405 (2)	0.5653 (3)	0.7673 (4)	0.0162 (6)*
O3	0.22034 (19)	0.3799 (2)	0.0257 (4)	0.0085 (5)*
O4	0.22625 (18)	0.3796 (2)	0.5483 (4)	0.0085 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0071 (5)	0.0093 (6)	0.0106 (5)	0.000	−0.0004 (3)	0.000
V1	0.0074 (5)	0.0066 (6)	0.0069 (5)	0.000	−0.0005 (3)	0.000
V2	0.0077 (4)	0.0066 (4)	0.0071 (4)	0.0010 (2)	0.0002 (2)	0.00028 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.344 (3)	Ca1—O1	4.611 (3)
Ca1—O2^ii	2.344 (3)	V1—O1	1.617 (3)
Ca1—O4	2.393 (2)	V1—O3^xi	1.962 (2)
Ca1—O4^iii	2.393 (2)	V1—O3^xii	1.962 (2)
Ca1—O3^iii	2.433 (2)	V1—O4^iii	1.972 (2)
Ca1—O3	2.433 (2)	V1—O4	1.972 (2)
Ca1—O1^iv	2.549 (3)	V1—V2^iii	2.9948 (9)
Ca1—V1	3.3653 (12)	V1—V2	2.9948 (9)
Ca1—V2^v	3.3676 (11)	V1—Ca1^xi	3.4268 (13)
Ca1—V2^vi	3.3676 (11)	V1—Ca1^xv	3.7732 (14)
Ca1—V1^vii	3.4268 (13)	V1—Ca1^xvi	4.3981 (14)
Ca1—O1^viii	3.536 (3)	V1—Ca1^xiii	5.3494 (12)
Ca1—V2^i	3.7326 (11)	V2—O2	1.607 (2)
Ca1—V2^ii	3.7326 (11)	V2—O4	1.960 (2)
Ca1—V1^iv	3.7732 (14)	V2—O4^xiii	1.961 (2)
Ca1—V2	3.9457 (10)	V2—O3^xiii	1.963 (2)
Ca1—V2^iii	3.9457 (10)	V2—O3^xi	1.969 (2)
Ca1—V2^ix	4.0562 (10)	V2—V2^xiii	2.9793 (9)
Ca1—V2^vii	4.0562 (10)	V2—V2^v	2.9793 (9)
Ca1—O2	4.125 (3)	V2—Ca1^xiii	3.3676 (11)
Ca1—O2^iii	4.125 (3)	V2—Ca1^ii	3.7326 (11)
Ca1—O3^x	4.141 (2)	V2—Ca1^xi	4.0562 (10)
Ca1—O3^viii	4.141 (2)	O1—Ca1^xv	2.549 (3)
Ca1—O3^xi	4.311 (2)	O1—Ca1^xvi	3.536 (3)
Ca1—O3^xii	4.311 (2)	O1—Ca1^xi	4.559 (3)
Ca1—O2^ix	4.337 (3)	O2—Ca1^ii	2.344 (3)
Ca1—O2^vii	4.337 (3)	O2—Ca1^xi	4.337 (3)
Ca1—O2^v	4.362 (3)	O2—Ca1^xiii	4.362 (3)
Ca1—O2^vi	4.362 (3)	O3—V1^vii	1.962 (2)
Ca1—O4^x	4.381 (2)	O3—V2^v	1.963 (2)
Ca1—O4^viii	4.381 (2)	O3—V2^vii	1.969 (2)
Ca1—V1^viii	4.3981 (14)	O3—Ca1^xvi	4.141 (2)
Ca1—O4^ix	4.447 (2)	O3—Ca1^vii	4.311 (2)
Ca1—O4^vii	4.447 (2)	O3—Ca1^v	4.505 (2)
Ca1—O3^xiii	4.505 (2)	O4—V2^v	1.961 (2)
Ca1—O3^xiv	4.505 (2)	O4—Ca1^xvi	4.381 (2)
Ca1—O4^vi	4.518 (2)	O4—Ca1^xi	4.447 (2)
Ca1—O4^v	4.518 (2)	O4—Ca1^xiii	4.518 (2)
Ca1—O1^vii	4.559 (3)	O4—Ca1^ii	5.092 (2)
O2^i—Ca1—O2^ii	109.47 (12)	O2^vii—Ca1—V1^viii	57.60 (3)
O2^i—Ca1—O4	152.33 (8)	O2^v—Ca1—V1^viii	127.13 (3)
O2^ii—Ca1—O4	88.24 (7)	O2^vi—Ca1—V1^viii	127.13 (3)
O2^i—Ca1—O4^iii	88.24 (7)	O4^x—Ca1—V1^viii	25.95 (3)
O2^ii—Ca1—O4^iii	152.33 (8)	O4^viii—Ca1—V1^viii	25.95 (3)
O4—Ca1—O4^iii	68.27 (10)	O2^i—Ca1—O4^ix	78.74 (6)
O2^i—Ca1—O3^iii	77.50 (7)	O2^ii—Ca1—O4^ix	107.33 (6)
O2^ii—Ca1—O3^iii	133.43 (8)	O4—Ca1—O4^ix	117.06 (7)
O4—Ca1—O3^iii	106.09 (8)	O4^iii—Ca1—O4^ix	96.66 (6)
O4^iii—Ca1—O3^iii	69.88 (7)	O3^iii—Ca1—O4^ix	26.81 (5)
O2^i—Ca1—O3	133.43 (8)	O3—Ca1—O4^ix	56.07 (6)
O2^ii—Ca1—O3	77.50 (7)	O1^iv—Ca1—O4^ix	157.05 (5)
O4—Ca1—O3	69.88 (7)	V1—Ca1—O4^ix	118.73 (4)
O4^iii—Ca1—O3	106.09 (8)	V2^v—Ca1—O4^ix	87.47 (3)
O3^iii—Ca1—O3	67.22 (10)	V2^vi—Ca1—O4^ix	61.90 (3)
O2^i—Ca1—O1^iv	78.42 (7)	V1^vii—Ca1—O4^ix	24.96 (3)
O2^ii—Ca1—O1^iv	78.42 (7)	O1^viii—Ca1—O4^ix	47.75 (6)
O4—Ca1—O1^iv	84.86 (8)	V2^i—Ca1—O4^ix	87.47 (3)
O4^iii—Ca1—O1^iv	84.86 (8)	V2^ii—Ca1—O4^ix	109.94 (3)
O3^iii—Ca1—O1^iv	145.35 (5)	V1^iv—Ca1—O4^ix	141.69 (3)
O3—Ca1—O1^iv	145.35 (5)	V2—Ca1—O4^ix	134.71 (3)
O2^i—Ca1—V1	117.99 (6)	V2^iii—Ca1—O4^ix	105.93 (3)
O2^ii—Ca1—V1	117.99 (6)	V2^ix—Ca1—O4^ix	26.14 (3)
O4—Ca1—V1	35.18 (5)	V2^vii—Ca1—O4^ix	61.29 (3)
O4^iii—Ca1—V1	35.18 (5)	O2—Ca1—O4^ix	144.32 (4)
O3^iii—Ca1—V1	95.24 (6)	O2^iii—Ca1—O4^ix	109.49 (4)
O3—Ca1—V1	95.24 (6)	O3^x—Ca1—O4^ix	114.03 (4)
O1^iv—Ca1—V1	74.71 (7)	O3^viii—Ca1—O4^ix	127.13 (4)
O2^i—Ca1—V2^v	165.34 (6)	O3^xi—Ca1—O4^ix	141.34 (5)
O2^ii—Ca1—V2^v	79.25 (6)	O3^xii—Ca1—O4^ix	126.31 (5)
O4—Ca1—V2^v	34.89 (5)	O2^ix—Ca1—O4^ix	39.48 (4)
O4^iii—Ca1—V2^v	88.45 (6)	O2^vii—Ca1—O4^ix	71.53 (4)
O3^iii—Ca1—V2^v	87.95 (6)	O2^v—Ca1—O4^ix	78.40 (4)
O3—Ca1—V2^v	35.10 (5)	O2^vi—Ca1—O4^ix	62.22 (4)
O1^iv—Ca1—V2^v	115.48 (5)	O4^x—Ca1—O4^ix	79.45 (3)
V1—Ca1—V2^v	64.63 (2)	O4^viii—Ca1—O4^ix	90.12 (3)
O2^i—Ca1—V2^vi	79.25 (6)	V1^viii—Ca1—O4^ix	66.35 (3)
O2^ii—Ca1—V2^vi	165.34 (6)	O2^i—Ca1—O4^vii	107.33 (6)
O4—Ca1—V2^vi	88.45 (6)	O2^ii—Ca1—O4^vii	78.74 (6)
O4^iii—Ca1—V2^vi	34.89 (5)	O4—Ca1—O4^vii	96.66 (6)
O3^iii—Ca1—V2^vi	35.10 (5)	O4^iii—Ca1—O4^vii	117.06 (7)
O3—Ca1—V2^vi	87.95 (6)	O3^iii—Ca1—O4^vii	56.07 (6)
O1^iv—Ca1—V2^vi	115.48 (5)	O3—Ca1—O4^vii	26.81 (5)
V1—Ca1—V2^vi	64.63 (2)	O1^iv—Ca1—O4^vii	157.05 (5)
V2^v—Ca1—V2^vi	89.93 (4)	V1—Ca1—O4^vii	118.73 (4)
O2^i—Ca1—V1^vii	103.23 (5)	V2^v—Ca1—O4^vii	61.90 (3)
O2^ii—Ca1—V1^vii	103.23 (5)	V2^vi—Ca1—O4^vii	87.47 (3)
O4—Ca1—V1^vii	92.65 (6)	V1^vii—Ca1—O4^vii	24.96 (3)
O4^iii—Ca1—V1^vii	92.65 (6)	O1^viii—Ca1—O4^vii	47.75 (6)
O3^iii—Ca1—V1^vii	34.07 (5)	V2^i—Ca1—O4^vii	109.94 (3)
O3—Ca1—V1^vii	34.07 (5)	V2^ii—Ca1—O4^vii	87.47 (3)
O1^iv—Ca1—V1^vii	176.99 (8)	V1^iv—Ca1—O4^vii	141.69 (3)
V1—Ca1—V1^vii	102.28 (4)	V2—Ca1—O4^vii	105.93 (3)
V2^v—Ca1—V1^vii	62.67 (2)	V2^iii—Ca1—O4^vii	134.71 (3)
V2^vi—Ca1—V1^vii	62.67 (2)	V2^ix—Ca1—O4^vii	61.29 (3)
O2^i—Ca1—O1^viii	68.31 (6)	V2^vii—Ca1—O4^vii	26.14 (3)
O2^ii—Ca1—O1^viii	68.31 (6)	O2—Ca1—O4^vii	109.49 (5)
O4—Ca1—O1^viii	139.31 (6)	O2^iii—Ca1—O4^vii	144.32 (4)
O4^iii—Ca1—O1^viii	139.31 (6)	O3^x—Ca1—O4^vii	127.13 (4)
O3^iii—Ca1—O1^viii	72.74 (6)	O3^viii—Ca1—O4^vii	114.03 (4)
O3—Ca1—O1^viii	72.74 (6)	O3^xi—Ca1—O4^vii	126.31 (5)
O1^iv—Ca1—O1^viii	119.86 (11)	O3^xii—Ca1—O4^vii	141.34 (5)
V1—Ca1—O1^viii	165.43 (6)	O2^ix—Ca1—O4^vii	71.53 (4)
V2^v—Ca1—O1^viii	105.84 (4)	O2^vii—Ca1—O4^vii	39.48 (4)
V2^vi—Ca1—O1^viii	105.84 (4)	O2^v—Ca1—O4^vii	62.22 (4)
V1^vii—Ca1—O1^viii	63.15 (6)	O2^vi—Ca1—O4^vii	78.40 (4)
O2^i—Ca1—V2^i	15.71 (6)	O4^x—Ca1—O4^vii	90.12 (3)
O2^ii—Ca1—V2^i	94.50 (7)	O4^viii—Ca1—O4^vii	79.45 (3)
O4—Ca1—V2^i	153.29 (5)	V1^viii—Ca1—O4^vii	66.35 (3)
O4^iii—Ca1—V2^i	100.24 (5)	O4^ix—Ca1—O4^vii	35.16 (5)
O3^iii—Ca1—V2^i	91.21 (5)	O2^i—Ca1—O3^xiii	170.83 (6)
O3—Ca1—V2^i	136.62 (6)	O2^ii—Ca1—O3^xiii	66.24 (7)
O1^iv—Ca1—V2^i	69.78 (5)	O4—Ca1—O3^xiii	25.35 (5)
V1—Ca1—V2^i	124.96 (2)	O4^iii—Ca1—O3^xiii	92.96 (6)
V2^v—Ca1—V2^i	170.40 (2)	O3^iii—Ca1—O3^xiii	111.44 (4)
V2^vi—Ca1—V2^i	94.87 (2)	O3—Ca1—O3^xiii	54.77 (4)
V1^vii—Ca1—V2^i	112.42 (2)	O1^iv—Ca1—O3^xiii	92.62 (5)
O1^viii—Ca1—V2^i	64.85 (4)	V1—Ca1—O3^xiii	60.52 (3)
O2^i—Ca1—V2^ii	94.50 (7)	V2^v—Ca1—O3^xiii	23.81 (3)
O2^ii—Ca1—V2^ii	15.71 (6)	V2^vi—Ca1—O3^xiii	106.76 (4)
O4—Ca1—V2^ii	100.24 (5)	V1^vii—Ca1—O3^xiii	85.80 (3)
O4^iii—Ca1—V2^ii	153.29 (5)	O1^viii—Ca1—O3^xiii	115.50 (3)
O3^iii—Ca1—V2^ii	136.62 (6)	V2^i—Ca1—O3^xiii	156.70 (3)
O3—Ca1—V2^ii	91.21 (5)	V2^ii—Ca1—O3^xiii	80.38 (3)
O1^iv—Ca1—V2^ii	69.78 (5)	V1^iv—Ca1—O3^xiii	102.63 (3)
V1—Ca1—V2^ii	124.96 (2)	V2—Ca1—O3^xiii	25.79 (3)
V2^v—Ca1—V2^ii	94.87 (2)	V2^iii—Ca1—O3^xiii	107.99 (3)
V2^vi—Ca1—V2^ii	170.40 (2)	V2^ix—Ca1—O3^xiii	130.31 (3)
V1^vii—Ca1—V2^ii	112.42 (2)	V2^vii—Ca1—O3^xiii	58.03 (3)
O1^viii—Ca1—V2^ii	64.85 (4)	O2—Ca1—O3^xiii	38.42 (4)
V2^i—Ca1—V2^ii	79.22 (3)	O2^iii—Ca1—O3^xiii	124.44 (5)
O2^i—Ca1—V1^iv	68.24 (6)	O3^x—Ca1—O3^xiii	129.29 (4)
O2^ii—Ca1—V1^iv	68.24 (6)	O3^viii—Ca1—O3^xiii	94.56 (4)
O4—Ca1—V1^iv	101.06 (5)	O3^xi—Ca1—O3^xiii	49.34 (4)
O4^iii—Ca1—V1^iv	101.06 (5)	O3^xii—Ca1—O3^xiii	83.13 (3)
O3^iii—Ca1—V1^iv	144.94 (5)	O2^ix—Ca1—O3^xiii	149.52 (4)
O3—Ca1—V1^iv	144.94 (5)	O2^vii—Ca1—O3^xiii	65.09 (4)
O1^iv—Ca1—V1^iv	19.61 (7)	O2^v—Ca1—O3^xiii	39.71 (4)
V1—Ca1—V1^iv	94.33 (3)	O2^vi—Ca1—O3^xiii	88.72 (5)
V2^v—Ca1—V1^iv	126.43 (2)	O4^x—Ca1—O3^xiii	139.38 (4)
V2^vi—Ca1—V1^iv	126.43 (2)	O4^viii—Ca1—O3^xiii	103.71 (4)
V1^vii—Ca1—V1^iv	163.40 (3)	V1^viii—Ca1—O3^xiii	120.47 (3)
O1^viii—Ca1—V1^iv	100.25 (6)	O4^ix—Ca1—O3^xiii	110.11 (4)
V2^i—Ca1—V1^iv	56.17 (2)	O4^vii—Ca1—O3^xiii	80.19 (4)
V2^ii—Ca1—V1^iv	56.17 (2)	O2^i—Ca1—O3^xiv	66.24 (7)
O2^i—Ca1—V2	146.04 (6)	O2^ii—Ca1—O3^xiv	170.83 (6)
O2^ii—Ca1—V2	70.71 (6)	O4—Ca1—O3^xiv	92.96 (6)
O4—Ca1—V2	22.46 (5)	O4^iii—Ca1—O3^xiv	25.35 (5)
O4^iii—Ca1—V2	82.70 (5)	O3^iii—Ca1—O3^xiv	54.77 (4)
O3^iii—Ca1—V2	128.33 (6)	O3—Ca1—O3^xiv	111.44 (4)
O3—Ca1—V2	80.44 (5)	O1^iv—Ca1—O3^xiv	92.62 (5)
O1^iv—Ca1—V2	68.24 (5)	V1—Ca1—O3^xiv	60.52 (3)
V1—Ca1—V2	47.548 (15)	V2^v—Ca1—O3^xiv	106.76 (4)
V2^v—Ca1—V2	47.268 (14)	V2^vi—Ca1—O3^xiv	23.81 (3)
V2^vi—Ca1—V2	108.98 (3)	V1^vii—Ca1—O3^xiv	85.80 (3)
V1^vii—Ca1—V2	109.81 (3)	O1^viii—Ca1—O3^xiv	115.50 (3)
O1^viii—Ca1—V2	134.712 (15)	V2^i—Ca1—O3^xiv	80.38 (3)
V2^i—Ca1—V2	137.45 (2)	V2^ii—Ca1—O3^xiv	156.70 (3)
V2^ii—Ca1—V2	80.27 (2)	V1^iv—Ca1—O3^xiv	102.63 (3)
V1^iv—Ca1—V2	81.47 (2)	V2—Ca1—O3^xiv	107.99 (3)
O2^i—Ca1—V2^iii	70.71 (6)	V2^iii—Ca1—O3^xiv	25.79 (3)
O2^ii—Ca1—V2^iii	146.04 (6)	V2^ix—Ca1—O3^xiv	58.03 (3)
O4—Ca1—V2^iii	82.70 (5)	V2^vii—Ca1—O3^xiv	130.31 (3)
O4^iii—Ca1—V2^iii	22.46 (5)	O2—Ca1—O3^xiv	124.44 (5)
O3^iii—Ca1—V2^iii	80.44 (5)	O2^iii—Ca1—O3^xiv	38.42 (4)
O3—Ca1—V2^iii	128.33 (6)	O3^x—Ca1—O3^xiv	94.56 (4)
O1^iv—Ca1—V2^iii	68.24 (5)	O3^viii—Ca1—O3^xiv	129.29 (4)
V1—Ca1—V2^iii	47.548 (15)	O3^xi—Ca1—O3^xiv	83.13 (3)
V2^v—Ca1—V2^iii	108.98 (3)	O3^xii—Ca1—O3^xiv	49.34 (4)
V2^vi—Ca1—V2^iii	47.268 (14)	O2^ix—Ca1—O3^xiv	65.09 (4)
V1^vii—Ca1—V2^iii	109.81 (3)	O2^vii—Ca1—O3^xiv	149.52 (4)
O1^viii—Ca1—V2^iii	134.712 (15)	O2^v—Ca1—O3^xiv	88.72 (5)
V2^i—Ca1—V2^iii	80.27 (2)	O2^vi—Ca1—O3^xiv	39.71 (4)
V2^ii—Ca1—V2^iii	137.45 (2)	O4^x—Ca1—O3^xiv	103.71 (4)
V1^iv—Ca1—V2^iii	81.47 (2)	O4^viii—Ca1—O3^xiv	139.38 (4)
V2—Ca1—V2^iii	90.51 (3)	V1^viii—Ca1—O3^xiv	120.47 (3)
O2^i—Ca1—V2^ix	58.84 (5)	O4^ix—Ca1—O3^xiv	80.19 (4)
O2^ii—Ca1—V2^ix	127.65 (6)	O4^vii—Ca1—O3^xiv	110.11 (4)
O4—Ca1—V2^ix	126.41 (6)	O3^xiii—Ca1—O3^xiv	116.71 (5)
O4^iii—Ca1—V2^ix	79.53 (5)	O2^i—Ca1—O4^vi	60.39 (6)
O3^iii—Ca1—V2^ix	20.44 (5)	O2^ii—Ca1—O4^vi	153.32 (6)
O3—Ca1—V2^ix	80.08 (5)	O4—Ca1—O4^vi	111.59 (4)
O1^iv—Ca1—V2^ix	134.57 (2)	O4^iii—Ca1—O4^vi	54.14 (4)
V1—Ca1—V2^ix	110.65 (3)	O3^iii—Ca1—O4^vi	25.81 (5)
V2^v—Ca1—V2^ix	106.50 (3)	O3—Ca1—O4^vi	92.32 (6)
V2^vi—Ca1—V2^ix	46.175 (14)	O1^iv—Ca1—O4^vi	119.55 (3)
V1^vii—Ca1—V2^ix	46.240 (15)	V1—Ca1—O4^vi	87.17 (3)
O1^viii—Ca1—V2^ix	59.99 (3)	V2^v—Ca1—O4^vi	106.49 (4)
V2^i—Ca1—V2^ix	71.48 (2)	V2^vi—Ca1—O4^vi	23.48 (3)
V2^ii—Ca1—V2^ix	124.29 (2)	V1^vii—Ca1—O4^vi	59.85 (3)
V1^iv—Ca1—V2^ix	127.06 (2)	O1^viii—Ca1—O4^vi	85.17 (4)
V2—Ca1—V2^ix	148.75 (3)	V2^i—Ca1—O4^vi	75.92 (3)
V2^iii—Ca1—V2^ix	82.73 (2)	V2^ii—Ca1—O4^vi	147.18 (3)
O2^i—Ca1—V2^vii	127.65 (6)	V1^iv—Ca1—O4^vi	121.80 (3)
O2^ii—Ca1—V2^vii	58.84 (5)	V2—Ca1—O4^vi	132.46 (4)
O4—Ca1—V2^vii	79.53 (5)	V2^iii—Ca1—O4^vi	57.85 (3)
O4^iii—Ca1—V2^vii	126.41 (6)	V2^ix—Ca1—O4^vi	25.73 (3)
O3^iii—Ca1—V2^vii	80.08 (5)	V2^vii—Ca1—O4^vi	105.87 (3)
O3—Ca1—V2^vii	20.44 (5)	O2—Ca1—O4^vi	153.95 (5)
O1^iv—Ca1—V2^vii	134.57 (2)	O2^iii—Ca1—O4^vi	63.37 (4)
V1—Ca1—V2^vii	110.65 (3)	O3^x—Ca1—O4^vi	101.03 (4)
V2^v—Ca1—V2^vii	46.175 (14)	O3^viii—Ca1—O4^vi	138.08 (4)
V2^vi—Ca1—V2^vii	106.50 (3)	O3^xi—Ca1—O4^vi	112.55 (4)
V1^vii—Ca1—V2^vii	46.240 (15)	O3^xii—Ca1—O4^vi	81.52 (4)
O1^viii—Ca1—V2^vii	59.99 (3)	O2^ix—Ca1—O4^vi	38.31 (4)
V2^i—Ca1—V2^vii	124.29 (2)	O2^vii—Ca1—O4^vi	119.73 (4)
V2^ii—Ca1—V2^vii	71.48 (2)	O2^v—Ca1—O4^vi	88.20 (5)
V1^iv—Ca1—V2^vii	127.06 (2)	O2^vi—Ca1—O4^vi	39.01 (4)
V2—Ca1—V2^vii	82.73 (2)	O4^x—Ca1—O4^vi	89.42 (4)
V2^iii—Ca1—V2^vii	148.75 (3)	O4^viii—Ca1—O4^vi	120.72 (4)
V2^ix—Ca1—V2^vii	87.40 (3)	V1^viii—Ca1—O4^vi	95.66 (3)
O2^i—Ca1—O2	132.45 (4)	O4^ix—Ca1—O4^vi	48.33 (4)
O2^ii—Ca1—O2	51.77 (7)	O4^vii—Ca1—O4^vi	81.28 (3)
O4—Ca1—O2	45.12 (6)	O3^xiii—Ca1—O4^vi	127.13 (4)
O4^iii—Ca1—O2	100.58 (6)	O3^xiv—Ca1—O4^vi	32.51 (3)
O3^iii—Ca1—O2	149.35 (6)	O2^i—Ca1—O4^v	153.32 (6)
O3—Ca1—O2	89.04 (6)	O2^ii—Ca1—O4^v	60.39 (6)
O1^iv—Ca1—O2	56.40 (4)	O4—Ca1—O4^v	54.14 (4)
V1—Ca1—O2	66.81 (3)	O4^iii—Ca1—O4^v	111.59 (4)
V2^v—Ca1—O2	62.21 (3)	O3^iii—Ca1—O4^v	92.32 (6)
V2^vi—Ca1—O2	130.81 (4)	O3—Ca1—O4^v	25.81 (5)
V1^vii—Ca1—O2	122.62 (4)	O1^iv—Ca1—O4^v	119.55 (3)
O1^viii—Ca1—O2	119.89 (4)	V1—Ca1—O4^v	87.17 (3)
V2^i—Ca1—O2	119.39 (4)	V2^v—Ca1—O4^v	23.48 (3)
V2^ii—Ca1—O2	58.70 (3)	V2^vi—Ca1—O4^v	106.49 (4)
V1^iv—Ca1—O2	64.21 (4)	V1^vii—Ca1—O4^v	59.85 (3)
V2—Ca1—O2	22.83 (3)	O1^viii—Ca1—O4^v	85.17 (4)
V2^iii—Ca1—O2	101.76 (4)	V2^i—Ca1—O4^v	147.18 (3)
V2^ix—Ca1—O2	168.64 (4)	V2^ii—Ca1—O4^v	75.92 (3)
V2^vii—Ca1—O2	83.43 (4)	V1^iv—Ca1—O4^v	121.80 (3)
O2^i—Ca1—O2^iii	51.77 (7)	V2—Ca1—O4^v	57.85 (3)
O2^ii—Ca1—O2^iii	132.45 (4)	V2^iii—Ca1—O4^v	132.46 (4)
O4—Ca1—O2^iii	100.58 (6)	V2^ix—Ca1—O4^v	105.87 (3)
O4^iii—Ca1—O2^iii	45.12 (6)	V2^vii—Ca1—O4^v	25.73 (3)
O3^iii—Ca1—O2^iii	89.04 (6)	O2—Ca1—O4^v	63.37 (4)
O3—Ca1—O2^iii	149.35 (6)	O2^iii—Ca1—O4^v	153.95 (5)
O1^iv—Ca1—O2^iii	56.40 (4)	O3^x—Ca1—O4^v	138.08 (4)
V1—Ca1—O2^iii	66.81 (3)	O3^viii—Ca1—O4^v	101.03 (4)
V2^v—Ca1—O2^iii	130.81 (4)	O3^xi—Ca1—O4^v	81.52 (4)
V2^vi—Ca1—O2^iii	62.21 (3)	O3^xii—Ca1—O4^v	112.55 (4)
V1^vii—Ca1—O2^iii	122.62 (4)	O2^ix—Ca1—O4^v	119.73 (4)
O1^viii—Ca1—O2^iii	119.89 (4)	O2^vii—Ca1—O4^v	38.31 (4)
V2^i—Ca1—O2^iii	58.70 (3)	O2^v—Ca1—O4^v	39.01 (4)
V2^ii—Ca1—O2^iii	119.39 (4)	O2^vi—Ca1—O4^v	88.20 (5)
V1^iv—Ca1—O2^iii	64.21 (4)	O4^x—Ca1—O4^v	120.72 (4)
V2—Ca1—O2^iii	101.76 (4)	O4^viii—Ca1—O4^v	89.42 (4)
V2^iii—Ca1—O2^iii	22.83 (3)	V1^viii—Ca1—O4^v	95.66 (3)
V2^ix—Ca1—O2^iii	83.43 (4)	O4^ix—Ca1—O4^v	81.28 (3)
V2^vii—Ca1—O2^iii	168.64 (4)	O4^vii—Ca1—O4^v	48.33 (4)
O2—Ca1—O2^iii	104.80 (7)	O3^xiii—Ca1—O4^v	32.51 (3)
O2^i—Ca1—O3^x	41.91 (6)	O3^xiv—Ca1—O4^v	127.13 (4)
O2^ii—Ca1—O3^x	77.70 (7)	O4^vi—Ca1—O4^v	116.38 (5)
O4—Ca1—O3^x	128.90 (6)	O2^i—Ca1—O1^vii	111.86 (6)
O4^iii—Ca1—O3^x	105.24 (6)	O2^ii—Ca1—O1^vii	111.86 (6)
O3^iii—Ca1—O3^x	119.24 (7)	O4—Ca1—O1^vii	78.78 (6)
O3—Ca1—O3^x	148.06 (6)	O4^iii—Ca1—O1^vii	78.78 (6)
O1^iv—Ca1—O3^x	44.38 (7)	O3^iii—Ca1—O1^vii	35.11 (5)
V1—Ca1—O3^x	114.13 (4)	O3—Ca1—O1^vii	35.11 (5)
V2^v—Ca1—O3^x	152.27 (3)	O1^iv—Ca1—O1^vii	160.19 (8)
V2^vi—Ca1—O3^x	115.18 (3)	V1—Ca1—O1^vii	85.48 (5)
V1^vii—Ca1—O3^x	138.27 (3)	V2^v—Ca1—O1^vii	53.48 (3)
O1^viii—Ca1—O3^x	79.57 (6)	V2^vi—Ca1—O1^vii	53.48 (3)
V2^i—Ca1—O3^x	28.27 (3)	V1^vii—Ca1—O1^vii	16.80 (4)
V2^ii—Ca1—O3^x	62.23 (4)	O1^viii—Ca1—O1^vii	79.95 (4)
V1^iv—Ca1—O3^x	28.22 (3)	V2^i—Ca1—O1^vii	123.95 (3)
V2—Ca1—O3^x	109.66 (3)	V2^ii—Ca1—O1^vii	123.95 (3)
V2^iii—Ca1—O3^x	82.79 (3)	V1^iv—Ca1—O1^vii	179.81 (4)
V2^ix—Ca1—O3^x	99.74 (3)	V2—Ca1—O1^vii	98.40 (3)
V2^vii—Ca1—O3^x	128.22 (4)	V2^iii—Ca1—O1^vii	98.40 (3)
O2—Ca1—O3^x	91.22 (5)	V2^ix—Ca1—O1^vii	53.04 (2)
O2^iii—Ca1—O3^x	60.39 (4)	V2^vii—Ca1—O1^vii	53.04 (2)
O2^i—Ca1—O3^viii	77.70 (7)	O2—Ca1—O1^vii	115.69 (4)
O2^ii—Ca1—O3^viii	41.91 (6)	O2^iii—Ca1—O1^vii	115.69 (4)
O4—Ca1—O3^viii	105.24 (6)	O3^x—Ca1—O1^vii	151.92 (4)
O4^iii—Ca1—O3^viii	128.90 (6)	O3^viii—Ca1—O1^vii	151.92 (4)
O3^iii—Ca1—O3^viii	148.06 (6)	O3^xi—Ca1—O1^vii	103.75 (5)
O3—Ca1—O3^viii	119.24 (7)	O3^xii—Ca1—O1^vii	103.75 (5)
O1^iv—Ca1—O3^viii	44.38 (7)	O2^ix—Ca1—O1^vii	73.57 (4)
V1—Ca1—O3^viii	114.13 (4)	O2^vii—Ca1—O1^vii	73.57 (4)
V2^v—Ca1—O3^viii	115.18 (3)	O2^v—Ca1—O1^vii	40.56 (4)
V2^vi—Ca1—O3^viii	152.27 (3)	O2^vi—Ca1—O1^vii	40.56 (4)
V1^vii—Ca1—O3^viii	138.27 (3)	O4^x—Ca1—O1^vii	117.55 (5)
O1^viii—Ca1—O3^viii	79.57 (6)	O4^viii—Ca1—O1^vii	117.55 (5)
V2^i—Ca1—O3^viii	62.23 (4)	V1^viii—Ca1—O1^vii	99.92 (5)
V2^ii—Ca1—O3^viii	28.27 (3)	O4^ix—Ca1—O1^vii	38.48 (4)
V1^iv—Ca1—O3^viii	28.22 (3)	O4^vii—Ca1—O1^vii	38.48 (4)
V2—Ca1—O3^viii	82.79 (3)	O3^xiii—Ca1—O1^vii	77.28 (3)
V2^iii—Ca1—O3^viii	109.66 (3)	O3^xiv—Ca1—O1^vii	77.28 (3)
V2^ix—Ca1—O3^viii	128.22 (4)	O4^vi—Ca1—O1^vii	58.20 (3)
V2^vii—Ca1—O3^viii	99.74 (3)	O4^v—Ca1—O1^vii	58.20 (3)
O2—Ca1—O3^viii	60.39 (4)	O2^i—Ca1—O1	122.72 (6)
O2^iii—Ca1—O3^viii	91.22 (5)	O2^ii—Ca1—O1	122.72 (6)
O3^x—Ca1—O3^viii	37.96 (6)	O4—Ca1—O1	34.59 (5)
O2^i—Ca1—O3^xi	124.92 (6)	O4^iii—Ca1—O1	34.59 (5)
O2^ii—Ca1—O3^xi	93.57 (6)	O3^iii—Ca1—O1	82.73 (6)
O4—Ca1—O3^xi	29.66 (5)	O3—Ca1—O1	82.73 (6)
O4^iii—Ca1—O3^xi	58.78 (6)	O1^iv—Ca1—O1	89.75 (5)
O3^iii—Ca1—O3^xi	120.74 (7)	V1—Ca1—O1	15.04 (4)
O3—Ca1—O3^xi	99.51 (7)	V2^v—Ca1—O1	55.95 (3)
O1^iv—Ca1—O3^xi	57.64 (7)	V2^vi—Ca1—O1	55.95 (3)
V1—Ca1—O3^xi	26.09 (3)	V1^vii—Ca1—O1	87.24 (5)
V2^v—Ca1—O3^xi	64.45 (3)	O1^viii—Ca1—O1	150.39 (7)
V2^vi—Ca1—O3^xi	90.59 (3)	V2^i—Ca1—O1	133.39 (2)
V1^vii—Ca1—O3^xi	119.56 (4)	V2^ii—Ca1—O1	133.39 (3)
O1^viii—Ca1—O3^xi	161.28 (3)	V1^iv—Ca1—O1	109.36 (5)
V2^i—Ca1—O3^xi	123.67 (4)	V2—Ca1—O1	53.13 (2)
V2^ii—Ca1—O3^xi	98.98 (3)	V2^iii—Ca1—O1	53.13 (2)
V1^iv—Ca1—O3^xi	76.06 (4)	V2^ix—Ca1—O1	100.19 (3)
V2—Ca1—O3^xi	27.13 (3)	V2^vii—Ca1—O1	100.19 (3)
V2^iii—Ca1—O3^xi	63.50 (3)	O2—Ca1—O1	74.96 (4)
V2^ix—Ca1—O3^xi	136.71 (4)	O2^iii—Ca1—O1	74.96 (4)
V2^vii—Ca1—O3^xi	107.23 (3)	O3^x—Ca1—O1	128.02 (5)
O2—Ca1—O3^xi	41.80 (4)	O3^viii—Ca1—O1	128.02 (5)
O2^iii—Ca1—O3^xi	75.50 (5)	O3^xi—Ca1—O1	38.09 (4)
O3^x—Ca1—O3^xi	101.82 (4)	O3^xii—Ca1—O1	38.09 (4)
O3^viii—Ca1—O3^xi	90.09 (3)	O2^ix—Ca1—O1	117.68 (4)
O2^i—Ca1—O3^xii	93.57 (6)	O2^vii—Ca1—O1	117.68 (4)
O2^ii—Ca1—O3^xii	124.92 (6)	O2^v—Ca1—O1	45.05 (4)
O4—Ca1—O3^xii	58.78 (6)	O2^vi—Ca1—O1	45.05 (4)
O4^iii—Ca1—O3^xii	29.66 (5)	O4^x—Ca1—O1	159.84 (3)
O3^iii—Ca1—O3^xii	99.51 (7)	O4^viii—Ca1—O1	159.84 (3)
O3—Ca1—O3^xii	120.74 (7)	V1^viii—Ca1—O1	170.37 (4)
O1^iv—Ca1—O3^xii	57.64 (7)	O4^ix—Ca1—O1	104.52 (5)
V1—Ca1—O3^xii	26.09 (3)	O4^vii—Ca1—O1	104.52 (5)
V2^v—Ca1—O3^xii	90.59 (3)	O3^xiii—Ca1—O1	58.50 (3)
V2^vi—Ca1—O3^xii	64.45 (3)	O3^xiv—Ca1—O1	58.50 (3)
V1^vii—Ca1—O3^xii	119.56 (4)	O4^vi—Ca1—O1	79.40 (3)
O1^viii—Ca1—O3^xii	161.28 (3)	O4^v—Ca1—O1	79.40 (3)
V2^i—Ca1—O3^xii	98.98 (3)	O1^vii—Ca1—O1	70.44 (5)
V2^ii—Ca1—O3^xii	123.67 (4)	O1—V1—O3^xi	109.23 (9)
V1^iv—Ca1—O3^xii	76.06 (4)	O1—V1—O3^xii	109.23 (9)
V2—Ca1—O3^xii	63.50 (3)	O3^xi—V1—O3^xii	86.69 (12)
V2^iii—Ca1—O3^xii	27.13 (3)	O1—V1—O4^iii	111.32 (9)
V2^ix—Ca1—O3^xii	107.23 (3)	O3^xi—V1—O4^iii	139.45 (9)
V2^vii—Ca1—O3^xii	136.71 (4)	O3^xii—V1—O4^iii	79.90 (8)
O2—Ca1—O3^xii	75.50 (5)	O1—V1—O4	111.32 (9)
O2^iii—Ca1—O3^xii	41.80 (4)	O3^xi—V1—O4	79.90 (8)
O3^x—Ca1—O3^xii	90.09 (3)	O3^xii—V1—O4	139.45 (9)
O3^viii—Ca1—O3^xii	101.82 (4)	O4^iii—V1—O4	85.88 (12)
O3^xi—Ca1—O3^xii	36.41 (6)	O1—V1—V2^iii	110.644 (18)
O2^i—Ca1—O2^ix	39.48 (7)	O3^xi—V1—V2^iii	121.59 (7)
O2^ii—Ca1—O2^ix	117.30 (4)	O3^xii—V1—V2^iii	40.46 (6)
O4—Ca1—O2^ix	147.70 (6)	O4^iii—V1—V2^iii	40.25 (6)
O4^iii—Ca1—O2^ix	89.98 (6)	O4—V1—V2^iii	120.77 (7)
O3^iii—Ca1—O2^ix	42.16 (6)	O1—V1—V2	110.644 (18)
O3—Ca1—O2^ix	95.33 (6)	O3^xi—V1—V2	40.46 (6)
O1^iv—Ca1—O2^ix	117.85 (5)	O3^xii—V1—V2	121.59 (7)
V1—Ca1—O2^ix	124.70 (4)	O4^iii—V1—V2	120.77 (7)
V2^v—Ca1—O2^ix	126.25 (4)	O4—V1—V2	40.25 (6)
V2^vi—Ca1—O2^ix	61.73 (3)	V2^iii—V1—V2	138.71 (4)
V1^vii—Ca1—O2^ix	63.75 (3)	O1—V1—Ca1	132.28 (10)
O1^viii—Ca1—O2^ix	50.67 (3)	O3^xi—V1—Ca1	104.96 (6)
V2^i—Ca1—O2^ix	50.41 (3)	O3^xii—V1—Ca1	104.96 (6)
V2^ii—Ca1—O2^ix	108.87 (4)	O4^iii—V1—Ca1	44.38 (6)
V1^iv—Ca1—O2^ix	106.55 (4)	O4—V1—Ca1	44.38 (6)
V2—Ca1—O2^ix	170.12 (4)	V2^iii—V1—Ca1	76.442 (17)
V2^iii—Ca1—O2^ix	85.11 (4)	V2—V1—Ca1	76.442 (17)
V2^ix—Ca1—O2^ix	21.74 (3)	O1—V1—Ca1^xi	125.44 (10)
V2^vii—Ca1—O2^ix	96.45 (4)	O3^xi—V1—Ca1^xi	44.01 (6)
O2—Ca1—O2^ix	167.01 (6)	O3^xii—V1—Ca1^xi	44.01 (6)
O2^iii—Ca1—O2^ix	77.31 (5)	O4^iii—V1—Ca1^xi	107.87 (6)
O3^x—Ca1—O2^ix	78.61 (4)	O4—V1—Ca1^xi	107.87 (6)
O3^viii—Ca1—O2^ix	107.02 (5)	V2^iii—V1—Ca1^xi	78.025 (17)
O3^xi—Ca1—O2^ix	148.05 (4)	V2—V1—Ca1^xi	78.025 (17)
O3^xii—Ca1—O2^ix	112.19 (4)	Ca1—V1—Ca1^xi	102.28 (4)
O2^i—Ca1—O2^vii	117.30 (4)	O1—V1—Ca1^xv	31.95 (10)
O2^ii—Ca1—O2^vii	39.48 (7)	O3^xi—V1—Ca1^xv	86.35 (6)
O4—Ca1—O2^vii	89.98 (6)	O3^xii—V1—Ca1^xv	86.35 (6)
O4^iii—Ca1—O2^vii	147.70 (6)	O4^iii—V1—Ca1^xv	130.15 (6)
O3^iii—Ca1—O2^vii	95.33 (6)	O4—V1—Ca1^xv	130.15 (6)
O3—Ca1—O2^vii	42.16 (6)	V2^iii—V1—Ca1^xv	107.287 (17)
O1^iv—Ca1—O2^vii	117.85 (5)	V2—V1—Ca1^xv	107.287 (17)
V1—Ca1—O2^vii	124.70 (4)	Ca1—V1—Ca1^xv	164.23 (3)
V2^v—Ca1—O2^vii	61.73 (3)	Ca1^xi—V1—Ca1^xv	93.49 (3)
V2^vi—Ca1—O2^vii	126.25 (4)	O1—V1—Ca1^xvi	48.32 (10)
V1^vii—Ca1—O2^vii	63.75 (3)	O3^xi—V1—Ca1^xvi	134.69 (6)
O1^viii—Ca1—O2^vii	50.67 (3)	O3^xii—V1—Ca1^xvi	134.69 (6)
V2^i—Ca1—O2^vii	108.87 (4)	O4^iii—V1—Ca1^xvi	76.54 (6)
V2^ii—Ca1—O2^vii	50.41 (3)	O4—V1—Ca1^xvi	76.54 (6)
V1^iv—Ca1—O2^vii	106.55 (4)	V2^iii—V1—Ca1^xvi	103.723 (17)
V2—Ca1—O2^vii	85.11 (4)	V2—V1—Ca1^xvi	103.723 (17)
V2^iii—Ca1—O2^vii	170.12 (4)	Ca1—V1—Ca1^xvi	83.96 (3)
V2^ix—Ca1—O2^vii	96.45 (4)	Ca1^xi—V1—Ca1^xvi	173.76 (3)
V2^vii—Ca1—O2^vii	21.74 (3)	Ca1^xv—V1—Ca1^xvi	80.27 (3)
O2—Ca1—O2^vii	77.31 (5)	O1—V1—Ca1^xiii	75.643 (13)
O2^iii—Ca1—O2^vii	167.01 (6)	O3^xi—V1—Ca1^xiii	54.58 (6)
O3^x—Ca1—O2^vii	107.02 (5)	O3^xii—V1—Ca1^xiii	138.61 (6)
O3^viii—Ca1—O2^vii	78.61 (4)	O4^iii—V1—Ca1^xiii	138.29 (6)
O3^xi—Ca1—O2^vii	112.19 (4)	O4—V1—Ca1^xiii	55.02 (6)
O3^xii—Ca1—O2^vii	148.05 (4)	V2^iii—V1—Ca1^xiii	173.71 (2)
O2^ix—Ca1—O2^vii	97.79 (6)	V2—V1—Ca1^xiii	35.01 (2)
O2^i—Ca1—O2^v	148.52 (6)	Ca1—V1—Ca1^xiii	99.362 (14)
O2^ii—Ca1—O2^v	97.84 (8)	Ca1^xi—V1—Ca1^xiii	98.532 (14)
O4—Ca1—O2^v	38.73 (6)	Ca1^xv—V1—Ca1^xiii	78.028 (13)
O4^iii—Ca1—O2^v	73.28 (6)	Ca1^xvi—V1—Ca1^xiii	80.266 (12)
O3^iii—Ca1—O2^v	72.32 (6)	O2—V2—O4	112.28 (10)
O3—Ca1—O2^v	37.87 (5)	O2—V2—O4^xiii	108.90 (10)
O1^iv—Ca1—O2^v	123.52 (7)	O4—V2—O4^xiii	138.76 (5)
V1—Ca1—O2^v	57.44 (3)	O2—V2—O3^xiii	106.18 (10)
V2^v—Ca1—O2^v	18.95 (4)	O4—V2—O3^xiii	81.35 (9)
V2^vi—Ca1—O2^v	70.99 (4)	O4^xiii—V2—O3^xiii	89.57 (9)
V1^vii—Ca1—O2^v	53.94 (3)	O2—V2—O3^xi	114.56 (10)
O1^viii—Ca1—O2^v	109.87 (5)	O4—V2—O3^xi	80.01 (8)
V2^i—Ca1—O2^v	163.47 (4)	O4^xiii—V2—O3^xi	81.17 (9)
V2^ii—Ca1—O2^v	113.53 (4)	O3^xiii—V2—O3^xi	139.07 (4)
V1^iv—Ca1—O2^v	139.30 (3)	O2—V2—V2^xiii	120.50 (7)
V2—Ca1—O2^v	57.92 (3)	O4—V2—V2^xiii	111.56 (6)
V2^iii—Ca1—O2^v	95.29 (4)	O4^xiii—V2—V2^xiii	40.54 (6)
V2^ix—Ca1—O2^v	92.23 (4)	O3^xiii—V2—V2^xiii	118.45 (7)
V2^vii—Ca1—O2^v	55.43 (3)	O3^xi—V2—V2^xiii	40.66 (6)
O2—Ca1—O2^v	77.04 (4)	O2—V2—V2^v	114.34 (7)
O2^iii—Ca1—O2^v	118.10 (4)	O4—V2—V2^v	40.57 (6)
O3^x—Ca1—O2^v	167.51 (4)	O4^xiii—V2—V2^v	120.49 (7)
O3^viii—Ca1—O2^v	133.70 (5)	O3^xiii—V2—V2^v	40.81 (6)
O3^xi—Ca1—O2^v	66.56 (4)	O3^xi—V2—V2^v	113.34 (6)
O3^xii—Ca1—O2^v	82.90 (4)	V2^xiii—V2—V2^v	125.15 (4)
O2^ix—Ca1—O2^v	113.61 (4)	O2—V2—V1	127.50 (10)
O2^vii—Ca1—O2^v	74.89 (5)	O4—V2—V1	40.53 (6)
O2^i—Ca1—O2^vi	97.84 (8)	O4^xiii—V2—V1	108.81 (6)
O2^ii—Ca1—O2^vi	148.52 (6)	O3^xiii—V2—V1	109.26 (6)
O4—Ca1—O2^vi	73.28 (6)	O3^xi—V2—V1	40.29 (6)
O4^iii—Ca1—O2^vi	38.73 (6)	V2^xiii—V2—V1	72.53 (2)
O3^iii—Ca1—O2^vi	37.87 (5)	V2^v—V2—V1	74.09 (3)
O3—Ca1—O2^vi	72.32 (6)	O2—V2—Ca1^xiii	118.17 (10)
O1^iv—Ca1—O2^vi	123.52 (7)	O4—V2—Ca1^xiii	113.33 (6)
V1—Ca1—O2^vi	57.44 (3)	O4^xiii—V2—Ca1^xiii	44.27 (6)
V2^v—Ca1—O2^vi	70.99 (4)	O3^xiii—V2—Ca1^xiii	45.46 (6)
V2^vi—Ca1—O2^vi	18.95 (4)	O3^xi—V2—Ca1^xiii	112.53 (6)
V1^vii—Ca1—O2^vi	53.94 (3)	V2^xiii—V2—Ca1^xiii	76.61 (3)
O1^viii—Ca1—O2^vi	109.87 (5)	V2^v—V2—Ca1^xiii	79.19 (3)
V2^i—Ca1—O2^vi	113.53 (4)	V1—V2—Ca1^xiii	114.32 (3)
V2^ii—Ca1—O2^vi	163.47 (4)	O2—V2—Ca1^ii	23.26 (9)
V1^iv—Ca1—O2^vi	139.30 (3)	O4—V2—Ca1^ii	123.87 (6)
V2—Ca1—O2^vi	95.29 (4)	O4^xiii—V2—Ca1^ii	95.54 (6)
V2^iii—Ca1—O2^vi	57.92 (3)	O3^xiii—V2—Ca1^ii	87.49 (6)
V2^ix—Ca1—O2^vi	55.43 (3)	O3^xi—V2—Ca1^ii	132.87 (6)
V2^vii—Ca1—O2^vi	92.23 (4)	V2^xiii—V2—Ca1^ii	121.90 (3)
O2—Ca1—O2^vi	118.10 (4)	V2^v—V2—Ca1^ii	108.65 (3)
O2^iii—Ca1—O2^vi	77.04 (4)	V1—V2—Ca1^ii	150.06 (3)
O3^x—Ca1—O2^vi	133.70 (5)	Ca1^xiii—V2—Ca1^ii	95.21 (2)
O3^viii—Ca1—O2^vi	167.51 (4)	O2—V2—Ca1	84.87 (9)
O3^xi—Ca1—O2^vi	82.90 (4)	O4—V2—Ca1	27.80 (6)
O3^xii—Ca1—O2^vi	66.56 (4)	O4^xiii—V2—Ca1	164.57 (6)
O2^ix—Ca1—O2^vi	74.89 (5)	O3^xiii—V2—Ca1	93.24 (6)
O2^vii—Ca1—O2^vi	113.61 (4)	O3^xi—V2—Ca1	86.82 (6)
O2^v—Ca1—O2^vi	52.05 (7)	V2^xiii—V2—Ca1	126.50 (3)
O2^i—Ca1—O4^x	37.85 (6)	V2^v—V2—Ca1	56.13 (2)
O2^ii—Ca1—O4^x	73.20 (7)	V1—V2—Ca1	56.01 (2)
O4—Ca1—O4^x	158.64 (5)	Ca1^xiii—V2—Ca1	135.30 (2)
O4^iii—Ca1—O4^x	125.96 (7)	Ca1^ii—V2—Ca1	99.73 (2)
O3^iii—Ca1—O4^x	94.52 (6)	O2—V2—Ca1^xi	89.03 (9)
O3—Ca1—O4^x	114.72 (6)	O4—V2—Ca1^xi	88.13 (6)
O1^iv—Ca1—O4^x	81.18 (7)	O4^xiii—V2—Ca1^xi	90.40 (6)
V1—Ca1—O4^x	149.97 (3)	O3^xiii—V2—Ca1^xi	163.91 (6)
V2^v—Ca1—O4^x	144.13 (3)	O3^xi—V2—Ca1^xi	25.57 (6)
V2^vi—Ca1—O4^x	112.15 (3)	V2^xiii—V2—Ca1^xi	54.64 (2)
V1^vii—Ca1—O4^x	101.68 (4)	V2^v—V2—Ca1^xi	127.96 (3)
O1^viii—Ca1—O4^x	42.41 (5)	V1—V2—Ca1^xi	55.73 (2)
V2^i—Ca1—O4^x	26.46 (3)	Ca1^xiii—V2—Ca1^xi	131.23 (2)
V2^ii—Ca1—O4^x	59.71 (4)	Ca1^ii—V2—Ca1^xi	108.52 (2)
V1^iv—Ca1—O4^x	62.63 (4)	Ca1—V2—Ca1^xi	82.73 (2)
V2—Ca1—O4^x	136.30 (3)	V1—O1—Ca1^xv	128.44 (15)
V2^iii—Ca1—O4^x	106.71 (3)	V1—O1—Ca1^xvi	111.70 (13)
V2^ix—Ca1—O4^x	74.48 (3)	Ca1^xv—O1—Ca1^xvi	119.86 (11)
V2^vii—Ca1—O4^x	98.98 (3)	V1—O1—Ca1^xi	37.76 (8)
O2—Ca1—O4^x	113.54 (5)	Ca1^xv—O1—Ca1^xi	90.67 (8)
O2^iii—Ca1—O4^x	85.05 (4)	Ca1^xvi—O1—Ca1^xi	149.47 (9)
O3^x—Ca1—O4^x	37.73 (4)	V1—O1—Ca1	32.68 (8)
O3^viii—Ca1—O4^x	53.73 (4)	Ca1^xv—O1—Ca1	161.12 (10)
O3^xi—Ca1—O4^x	138.67 (4)	Ca1^xvi—O1—Ca1	79.02 (6)
O3^xii—Ca1—O4^x	124.01 (4)	Ca1^xi—O1—Ca1	70.44 (5)
O2^ix—Ca1—O4^x	53.57 (4)	V2—O2—Ca1^ii	141.03 (14)
O2^vii—Ca1—O4^x	82.42 (4)	V2—O2—Ca1	72.30 (9)
O2^v—Ca1—O4^x	152.27 (4)	Ca1^ii—O2—Ca1	128.23 (7)
O2^vi—Ca1—O4^x	128.04 (4)	V2—O2—Ca1^xi	69.23 (8)
O2^i—Ca1—O4^viii	73.20 (7)	Ca1^ii—O2—Ca1^xi	140.52 (7)
O2^ii—Ca1—O4^viii	37.85 (6)	Ca1—O2—Ca1^xi	77.31 (5)
O4—Ca1—O4^viii	125.96 (7)	V2—O2—Ca1^xiii	42.89 (7)
O4^iii—Ca1—O4^viii	158.64 (5)	Ca1^ii—O2—Ca1^xiii	98.52 (8)
O3^iii—Ca1—O4^viii	114.72 (6)	Ca1—O2—Ca1^xiii	105.72 (5)
O3—Ca1—O4^viii	94.52 (6)	Ca1^xi—O2—Ca1^xiii	102.13 (5)
O1^iv—Ca1—O4^viii	81.18 (7)	V1^vii—O3—V2^v	128.39 (11)
V1—Ca1—O4^viii	149.97 (3)	V1^vii—O3—V2^vii	99.25 (9)
V2^v—Ca1—O4^viii	112.15 (3)	V2^v—O3—V2^vii	98.53 (9)
V2^vi—Ca1—O4^viii	144.13 (3)	V1^vii—O3—Ca1	101.92 (9)
V1^vii—Ca1—O4^viii	101.68 (4)	V2^v—O3—Ca1	99.44 (8)
O1^viii—Ca1—O4^viii	42.41 (5)	V2^vii—O3—Ca1	133.99 (10)
V2^i—Ca1—O4^viii	59.71 (4)	V1^vii—O3—Ca1^xvi	65.42 (6)
V2^ii—Ca1—O4^viii	26.46 (3)	V2^v—O3—Ca1^xvi	64.24 (5)
V1^iv—Ca1—O4^viii	62.63 (4)	V2^vii—O3—Ca1^xvi	123.08 (8)
V2—Ca1—O4^viii	106.71 (3)	Ca1—O3—Ca1^xvi	102.87 (6)
V2^iii—Ca1—O4^viii	136.30 (3)	V1^vii—O3—Ca1^vii	48.95 (5)
V2^ix—Ca1—O4^viii	98.98 (3)	V2^v—O3—Ca1^vii	160.88 (9)
V2^vii—Ca1—O4^viii	74.48 (3)	V2^vii—O3—Ca1^vii	66.05 (5)
O2—Ca1—O4^viii	85.05 (4)	Ca1—O3—Ca1^vii	99.51 (7)
O2^iii—Ca1—O4^viii	113.54 (5)	Ca1^xvi—O3—Ca1^vii	113.57 (5)
O3^x—Ca1—O4^viii	53.73 (4)	V1^vii—O3—Ca1^v	104.64 (7)
O3^viii—Ca1—O4^viii	37.73 (4)	V2^v—O3—Ca1^v	60.97 (6)
O3^xi—Ca1—O4^viii	124.01 (4)	V2^vii—O3—Ca1^v	43.66 (5)
O3^xii—Ca1—O4^viii	138.67 (4)	Ca1—O3—Ca1^v	153.25 (7)
O2^ix—Ca1—O4^viii	82.42 (4)	Ca1^xvi—O3—Ca1^v	85.44 (4)
O2^vii—Ca1—O4^viii	53.57 (4)	Ca1^vii—O3—Ca1^v	100.26 (4)
O2^v—Ca1—O4^viii	128.04 (4)	V2—O4—V2^v	98.88 (9)
O2^vi—Ca1—O4^viii	152.27 (4)	V2—O4—V1	99.23 (9)
O4^x—Ca1—O4^viii	35.70 (6)	V2^v—O4—V1	132.46 (11)
O2^i—Ca1—V1^viii	60.07 (6)	V2—O4—Ca1	129.74 (10)
O2^ii—Ca1—V1^viii	60.07 (6)	V2^v—O4—Ca1	100.84 (8)
O4—Ca1—V1^viii	145.69 (5)	V1—O4—Ca1	100.44 (9)
O4^iii—Ca1—V1^viii	145.69 (5)	V2—O4—Ca1^xvi	132.15 (8)
O3^iii—Ca1—V1^viii	89.26 (5)	V2^v—O4—Ca1^xvi	58.00 (5)
O3—Ca1—V1^viii	89.26 (5)	V1—O4—Ca1^xvi	77.51 (6)
O1^iv—Ca1—V1^viii	99.89 (8)	Ca1—O4—Ca1^xvi	97.21 (6)
V1—Ca1—V1^viii	174.60 (3)	V2—O4—Ca1^xi	65.73 (5)
V2^v—Ca1—V1^viii	118.66 (2)	V2^v—O4—Ca1^xi	161.85 (8)
V2^vi—Ca1—V1^viii	118.66 (2)	V1—O4—Ca1^xi	47.17 (5)
V1^vii—Ca1—V1^viii	83.12 (3)	Ca1—O4—Ca1^xi	96.66 (6)
O1^viii—Ca1—V1^viii	19.97 (5)	Ca1^xvi—O4—Ca1^xi	124.52 (5)
V2^i—Ca1—V1^viii	51.762 (18)	V2—O4—Ca1^xiii	43.20 (5)
V2^ii—Ca1—V1^viii	51.762 (18)	V2^v—O4—Ca1^xiii	63.87 (6)
V1^iv—Ca1—V1^viii	80.27 (3)	V1—O4—Ca1^xiii	104.03 (7)
V2—Ca1—V1^viii	130.780 (18)	Ca1—O4—Ca1^xiii	155.39 (7)
V2^iii—Ca1—V1^viii	130.780 (18)	Ca1^xvi—O4—Ca1^xiii	90.58 (4)
V2^ix—Ca1—V1^viii	73.04 (2)	Ca1^xi—O4—Ca1^xiii	98.03 (4)
V2^vii—Ca1—V1^viii	73.04 (2)	V2—O4—Ca1^ii	37.49 (4)
O2—Ca1—V1^viii	110.38 (4)	V2^v—O4—Ca1^ii	90.42 (7)
O2^iii—Ca1—V1^viii	110.38 (4)	V1—O4—Ca1^ii	128.35 (7)
O3^x—Ca1—V1^viii	60.84 (3)	Ca1—O4—Ca1^ii	96.65 (6)
O3^viii—Ca1—V1^viii	60.84 (3)	Ca1^xvi—O4—Ca1^ii	147.38 (5)
O3^xi—Ca1—V1^viii	149.88 (3)	Ca1^xi—O4—Ca1^ii	82.77 (3)
O3^xii—Ca1—V1^viii	149.88 (3)	Ca1^xiii—O4—Ca1^ii	65.90 (3)
O2^ix—Ca1—V1^viii	57.60 (3)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (x) x−1/2, −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, y−1/2, z+1/2; (xv) x+1/2, y, −z+3/2; (xvi) x+1/2, y, −z+1/2.

(CaV3O7_287K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.534 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2645 reflections
a = 10.444 (3) Å	θ = 1.3–23.4°
b = 10.368 (2) Å	µ = 5.67 mm^−1
c = 5.2927 (15) Å	T = 287 K
V = 573.1 (2) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	403 independent reflections
Radiation source: fine-focus sealed tube	363 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.319, Tmax = 0.471	l = −5→5
2387 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.0439P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.052	(Δ/σ)max < 0.001
S = 0.93	Δρmax = 0.34 e Å^−3
403 reflections	Δρmin = −0.40 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0190 (15)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08470 (9)	0.2500	0.29962 (15)	0.0080 (3)
V1	0.28858 (7)	0.2500	0.79194 (13)	0.0064 (3)
V2	0.18749 (5)	0.52036 (5)	0.78352 (9)	0.0063 (3)
O1	0.4432 (3)	0.2500	0.8081 (5)	0.0136 (8)*
O2	0.0404 (2)	0.5655 (3)	0.7669 (4)	0.0151 (6)*
O3	0.22026 (19)	0.3799 (2)	0.0258 (4)	0.0076 (5)*
O4	0.22625 (19)	0.3795 (2)	0.5481 (4)	0.0079 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0055 (5)	0.0082 (6)	0.0103 (5)	0.000	−0.0003 (3)	0.000
V1	0.0066 (5)	0.0058 (5)	0.0068 (5)	0.000	−0.0002 (3)	0.000
V2	0.0065 (4)	0.0056 (4)	0.0068 (4)	0.0011 (2)	0.0001 (2)	0.00039 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.343 (3)	V1—Ca1^xiii	4.4009 (14)
Ca1—O2^ii	2.343 (3)	V1—Ca1^xiv	5.3504 (11)
Ca1—O4	2.391 (2)	V2—O2	1.608 (2)
Ca1—O4^iii	2.391 (2)	V2—O4^xiv	1.962 (2)
Ca1—O3	2.433 (2)	V2—O4	1.962 (2)
Ca1—O3^iii	2.433 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.548 (3)	V2—O3^x	1.970 (2)
Ca1—V1	3.3651 (13)	V2—V2^xiv	2.9810 (9)
Ca1—V2^v	3.3671 (11)	V2—V2^v	2.9810 (9)
Ca1—V2^vi	3.3671 (11)	V2—Ca1^xiv	3.3671 (11)
Ca1—V1^vii	3.4284 (13)	V2—Ca1^ii	3.7342 (11)
Ca1—O1^viii	3.539 (3)	V2—Ca1^x	4.0585 (10)
Ca1—V2^i	3.7342 (11)	O1—Ca1^xii	2.548 (3)
Ca1—V2^ii	3.7342 (11)	O1—Ca1^xiii	3.539 (3)
Ca1—V1^iv	3.7734 (14)	O1—Ca1^x	4.560 (3)
Ca1—V2	3.9458 (10)	O2—Ca1^ii	2.343 (3)
Ca1—V2^iii	3.9458 (10)	O2—Ca1^x	4.343 (3)
Ca1—V2^ix	4.0585 (10)	O2—Ca1^xiv	4.361 (3)
Ca1—V2^vii	4.0585 (10)	O3—V2^v	1.964 (2)
Ca1—O2	4.127 (3)	O3—V1^vii	1.964 (2)
V1—O1	1.617 (3)	O3—V2^vii	1.970 (2)
V1—O3^x	1.964 (2)	O3—Ca1^xiii	4.142 (2)
V1—O3^xi	1.964 (2)	O3—Ca1^vii	4.312 (2)
V1—O4^iii	1.973 (2)	O3—Ca1^v	4.506 (2)
V1—O4	1.973 (2)	O4—V2^v	1.962 (2)
V1—V2^iii	2.9957 (8)	O4—Ca1^xiii	4.382 (2)
V1—V2	2.9957 (8)	O4—Ca1^x	4.451 (2)
V1—Ca1^x	3.4284 (13)	O4—Ca1^xiv	4.520 (2)
V1—Ca1^xii	3.7734 (14)	O4—Ca1^ii	5.094 (2)
O2^i—Ca1—O2^ii	109.43 (12)	O1—V1—O4	111.35 (9)
O2^i—Ca1—O4	152.36 (8)	O3^x—V1—O4	79.96 (8)
O2^ii—Ca1—O4	88.23 (7)	O3^xi—V1—O4	139.41 (10)
O2^i—Ca1—O4^iii	88.23 (7)	O4^iii—V1—O4	85.77 (12)
O2^ii—Ca1—O4^iii	152.36 (8)	O1—V1—V2^iii	110.656 (18)
O4—Ca1—O4^iii	68.32 (10)	O3^x—V1—V2^iii	121.55 (7)
O2^i—Ca1—O3	133.39 (7)	O3^xi—V1—V2^iii	40.49 (6)
O2^ii—Ca1—O3	77.47 (7)	O4^iii—V1—V2^iii	40.29 (6)
O4—Ca1—O3	69.93 (7)	O4—V1—V2^iii	120.71 (7)
O4^iii—Ca1—O3	106.18 (8)	O1—V1—V2	110.656 (18)
O2^i—Ca1—O3^iii	77.47 (7)	O3^x—V1—V2	40.49 (6)
O2^ii—Ca1—O3^iii	133.39 (7)	O3^xi—V1—V2	121.55 (7)
O4—Ca1—O3^iii	106.18 (8)	O4^iii—V1—V2	120.71 (7)
O4^iii—Ca1—O3^iii	69.93 (7)	O4—V1—V2	40.29 (6)
O3—Ca1—O3^iii	67.24 (10)	V2^iii—V1—V2	138.69 (4)
O2^i—Ca1—O1^iv	78.41 (7)	O1—V1—Ca1	132.28 (11)
O2^ii—Ca1—O1^iv	78.41 (7)	O3^x—V1—Ca1	104.96 (6)
O4—Ca1—O1^iv	84.86 (8)	O3^xi—V1—Ca1	104.96 (6)
O4^iii—Ca1—O1^iv	84.86 (8)	O4^iii—V1—Ca1	44.33 (6)
O3—Ca1—O1^iv	145.36 (5)	O4—V1—Ca1	44.33 (6)
O3^iii—Ca1—O1^iv	145.36 (5)	V2^iii—V1—Ca1	76.434 (17)
O2^i—Ca1—V1	117.99 (6)	V2—V1—Ca1	76.434 (17)
O2^ii—Ca1—V1	117.99 (6)	O1—V1—Ca1^x	125.37 (11)
O4—Ca1—V1	35.21 (5)	O3^x—V1—Ca1^x	43.97 (6)
O4^iii—Ca1—V1	35.21 (5)	O3^xi—V1—Ca1^x	43.97 (6)
O3—Ca1—V1	95.33 (6)	O4^iii—V1—Ca1^x	107.93 (6)
O3^iii—Ca1—V1	95.33 (6)	O4—V1—Ca1^x	107.93 (6)
O1^iv—Ca1—V1	74.69 (7)	V2^iii—V1—Ca1^x	78.039 (18)
O2^i—Ca1—V2^v	165.36 (6)	V2—V1—Ca1^x	78.039 (18)
O2^ii—Ca1—V2^v	79.23 (6)	Ca1—V1—Ca1^x	102.35 (4)
O4—Ca1—V2^v	34.91 (5)	O1—V1—Ca1^xii	31.93 (10)
O4^iii—Ca1—V2^v	88.51 (6)	O3^x—V1—Ca1^xii	86.37 (6)
O3—Ca1—V2^v	35.13 (5)	O3^xi—V1—Ca1^xii	86.37 (6)
O3^iii—Ca1—V2^v	88.01 (6)	O4^iii—V1—Ca1^xii	130.18 (6)
O1^iv—Ca1—V2^v	115.49 (5)	O4—V1—Ca1^xii	130.18 (6)
V1—Ca1—V2^v	64.69 (2)	V2^iii—V1—Ca1^xii	107.302 (17)
O2^i—Ca1—V2^vi	79.23 (6)	V2—V1—Ca1^xii	107.302 (17)
O2^ii—Ca1—V2^vi	165.36 (6)	Ca1—V1—Ca1^xii	164.21 (3)
O4—Ca1—V2^vi	88.51 (6)	Ca1^x—V1—Ca1^xii	93.44 (3)
O4^iii—Ca1—V2^vi	34.91 (5)	O1—V1—Ca1^xiii	48.38 (10)
O3—Ca1—V2^vi	88.01 (6)	O3^x—V1—Ca1^xiii	134.74 (6)
O3^iii—Ca1—V2^vi	35.13 (5)	O3^xi—V1—Ca1^xiii	134.74 (6)
O1^iv—Ca1—V2^vi	115.49 (5)	O4^iii—V1—Ca1^xiii	76.49 (6)
V1—Ca1—V2^vi	64.69 (2)	O4—V1—Ca1^xiii	76.49 (6)
V2^v—Ca1—V2^vi	90.00 (3)	V2^iii—V1—Ca1^xiii	103.715 (17)
O2^i—Ca1—V1^vii	103.22 (5)	V2—V1—Ca1^xiii	103.715 (17)
O2^ii—Ca1—V1^vii	103.22 (5)	Ca1—V1—Ca1^xiii	83.90 (3)
O4—Ca1—V1^vii	92.69 (6)	Ca1^x—V1—Ca1^xiii	173.75 (3)
O4^iii—Ca1—V1^vii	92.69 (6)	Ca1^xii—V1—Ca1^xiii	80.30 (3)
O3—Ca1—V1^vii	34.08 (5)	O1—V1—Ca1^xiv	75.676 (13)
O3^iii—Ca1—V1^vii	34.08 (5)	O3^x—V1—Ca1^xiv	54.58 (6)
O1^iv—Ca1—V1^vii	177.04 (8)	O3^xi—V1—Ca1^xiv	138.57 (6)
V1—Ca1—V1^vii	102.35 (4)	O4^iii—V1—Ca1^xiv	138.24 (6)
V2^v—Ca1—V1^vii	62.69 (2)	O4—V1—Ca1^xiv	55.05 (6)
V2^vi—Ca1—V1^vii	62.69 (2)	V2^iii—V1—Ca1^xiv	173.67 (3)
O2^i—Ca1—O1^viii	68.32 (6)	V2—V1—Ca1^xiv	34.984 (19)
O2^ii—Ca1—O1^viii	68.32 (6)	Ca1—V1—Ca1^xiv	99.346 (14)
O4—Ca1—O1^viii	139.27 (6)	Ca1^x—V1—Ca1^xiv	98.493 (14)
O4^iii—Ca1—O1^viii	139.27 (6)	Ca1^xii—V1—Ca1^xiv	78.048 (13)
O3—Ca1—O1^viii	72.64 (7)	Ca1^xiii—V1—Ca1^xiv	80.304 (13)
O3^iii—Ca1—O1^viii	72.64 (7)	O2—V2—O4^xiv	108.87 (10)
O1^iv—Ca1—O1^viii	119.89 (11)	O2—V2—O4	112.28 (10)
V1—Ca1—O1^viii	165.42 (6)	O4^xiv—V2—O4	138.79 (5)
V2^v—Ca1—O1^viii	105.78 (4)	O2—V2—O3^xiv	106.10 (10)
V2^vi—Ca1—O1^viii	105.78 (4)	O4^xiv—V2—O3^xiv	89.53 (9)
V1^vii—Ca1—O1^viii	63.07 (6)	O4—V2—O3^xiv	81.35 (9)
O2^i—Ca1—V2^i	15.68 (6)	O2—V2—O3^x	114.63 (11)
O2^ii—Ca1—V2^i	94.48 (7)	O4^xiv—V2—O3^x	81.18 (9)
O4—Ca1—V2^i	153.32 (6)	O4—V2—O3^x	80.07 (8)
O4^iii—Ca1—V2^i	100.22 (5)	O3^xiv—V2—O3^x	139.10 (4)
O3—Ca1—V2^i	136.54 (5)	O2—V2—V2^xiv	120.54 (7)
O3^iii—Ca1—V2^i	91.14 (5)	O4^xiv—V2—V2^xiv	40.56 (6)
O1^iv—Ca1—V2^i	69.79 (5)	O4—V2—V2^xiv	111.59 (7)
V1—Ca1—V2^i	124.96 (2)	O3^xiv—V2—V2^xiv	118.43 (7)
V2^v—Ca1—V2^i	170.35 (2)	O3^x—V2—V2^xiv	40.66 (6)
V2^vi—Ca1—V2^i	94.83 (2)	O2—V2—V2^v	114.28 (7)
V1^vii—Ca1—V2^i	112.36 (2)	O4^xiv—V2—V2^v	120.49 (7)
O1^viii—Ca1—V2^i	64.86 (4)	O4—V2—V2^v	40.57 (6)
O2^i—Ca1—V2^ii	94.48 (7)	O3^xiv—V2—V2^v	40.82 (6)
O2^ii—Ca1—V2^ii	15.68 (6)	O3^x—V2—V2^v	113.40 (7)
O4—Ca1—V2^ii	100.22 (5)	V2^xiv—V2—V2^v	125.18 (4)
O4^iii—Ca1—V2^ii	153.32 (6)	O2—V2—V1	127.59 (10)
O3—Ca1—V2^ii	91.14 (5)	O4^xiv—V2—V1	108.82 (6)
O3^iii—Ca1—V2^ii	136.54 (5)	O4—V2—V1	40.56 (6)
O1^iv—Ca1—V2^ii	69.79 (5)	O3^xiv—V2—V1	109.27 (6)
V1—Ca1—V2^ii	124.96 (2)	O3^x—V2—V1	40.32 (6)
V2^v—Ca1—V2^ii	94.83 (2)	V2^xiv—V2—V1	72.53 (2)
V2^vi—Ca1—V2^ii	170.35 (2)	V2^v—V2—V1	74.12 (3)
V1^vii—Ca1—V2^ii	112.36 (2)	O2—V2—Ca1^xiv	118.06 (10)
O1^viii—Ca1—V2^ii	64.86 (4)	O4^xiv—V2—Ca1^xiv	44.22 (6)
V2^i—Ca1—V2^ii	79.23 (3)	O4—V2—Ca1^xiv	113.37 (7)
O2^i—Ca1—V1^iv	68.22 (6)	O3^xiv—V2—Ca1^xiv	45.47 (6)
O2^ii—Ca1—V1^iv	68.22 (6)	O3^x—V2—Ca1^xiv	112.54 (7)
O4—Ca1—V1^iv	101.05 (6)	V2^xiv—V2—Ca1^xiv	76.59 (3)
O4^iii—Ca1—V1^iv	101.05 (6)	V2^v—V2—Ca1^xiv	79.23 (3)
O3—Ca1—V1^iv	144.91 (5)	V1—V2—Ca1^xiv	114.34 (3)
O3^iii—Ca1—V1^iv	144.91 (5)	O2—V2—Ca1^ii	23.18 (9)
O1^iv—Ca1—V1^iv	19.61 (7)	O4^xiv—V2—Ca1^ii	95.53 (6)
V1—Ca1—V1^iv	94.30 (3)	O4—V2—Ca1^ii	123.84 (6)
V2^v—Ca1—V1^iv	126.42 (2)	O3^xiv—V2—Ca1^ii	87.48 (6)
V2^vi—Ca1—V1^iv	126.42 (2)	O3^x—V2—Ca1^ii	132.85 (6)
V1^vii—Ca1—V1^iv	163.35 (3)	V2^xiv—V2—Ca1^ii	121.90 (3)
O1^viii—Ca1—V1^iv	100.28 (6)	V2^v—V2—Ca1^ii	108.61 (3)
V2^i—Ca1—V1^iv	56.19 (2)	V1—V2—Ca1^ii	150.08 (3)
V2^ii—Ca1—V1^iv	56.19 (2)	Ca1^xiv—V2—Ca1^ii	95.17 (2)
O2^i—Ca1—V2	146.02 (6)	O2—V2—Ca1	84.93 (9)
O2^ii—Ca1—V2	70.70 (6)	O4^xiv—V2—Ca1	164.58 (6)
O4—Ca1—V2	22.47 (5)	O4—V2—Ca1	27.76 (6)
O4^iii—Ca1—V2	82.75 (5)	O3^xiv—V2—Ca1	93.25 (6)
O3—Ca1—V2	80.50 (5)	O3^x—V2—Ca1	86.83 (6)
O3^iii—Ca1—V2	128.43 (6)	V2^xiv—V2—Ca1	126.50 (3)
O1^iv—Ca1—V2	68.22 (5)	V2^v—V2—Ca1	56.11 (2)
V1—Ca1—V2	47.564 (15)	V1—V2—Ca1	56.00 (2)
V2^v—Ca1—V2	47.299 (14)	Ca1^xiv—V2—Ca1	135.32 (2)
V2^vi—Ca1—V2	109.06 (3)	Ca1^ii—V2—Ca1	99.749 (19)
V1^vii—Ca1—V2	109.86 (3)	O2—V2—Ca1^x	89.16 (9)
O1^viii—Ca1—V2	134.700 (15)	O4^xiv—V2—Ca1^x	90.38 (6)
V2^i—Ca1—V2	137.44 (3)	O4—V2—Ca1^x	88.16 (6)
V2^ii—Ca1—V2	80.251 (19)	O3^xiv—V2—Ca1^x	163.89 (6)
V1^iv—Ca1—V2	81.44 (2)	O3^x—V2—Ca1^x	25.50 (6)
O2^i—Ca1—V2^iii	70.70 (6)	V2^xiv—V2—Ca1^x	54.59 (2)
O2^ii—Ca1—V2^iii	146.02 (6)	V2^v—V2—Ca1^x	127.99 (3)
O4—Ca1—V2^iii	82.75 (5)	V1—V2—Ca1^x	55.73 (2)
O4^iii—Ca1—V2^iii	22.47 (5)	Ca1^xiv—V2—Ca1^x	131.17 (2)
O3—Ca1—V2^iii	128.43 (6)	Ca1^ii—V2—Ca1^x	108.56 (2)
O3^iii—Ca1—V2^iii	80.50 (5)	Ca1—V2—Ca1^x	82.77 (2)
O1^iv—Ca1—V2^iii	68.22 (5)	V1—O1—Ca1^xii	128.46 (15)
V1—Ca1—V2^iii	47.564 (15)	V1—O1—Ca1^xiii	111.65 (13)
V2^v—Ca1—V2^iii	109.06 (3)	Ca1^xii—O1—Ca1^xiii	119.89 (11)
V2^vi—Ca1—V2^iii	47.299 (14)	V1—O1—Ca1^x	37.82 (8)
V1^vii—Ca1—V2^iii	109.86 (3)	Ca1^xii—O1—Ca1^x	90.65 (8)
O1^viii—Ca1—V2^iii	134.700 (15)	Ca1^xiii—O1—Ca1^x	149.46 (9)
V2^i—Ca1—V2^iii	80.251 (19)	V1—O1—Ca1	32.68 (8)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.14 (11)
V1^iv—Ca1—V2^iii	81.44 (2)	Ca1^xiii—O1—Ca1	78.97 (6)
V2—Ca1—V2^iii	90.54 (3)	Ca1^x—O1—Ca1	70.49 (5)
O2^i—Ca1—V2^ix	58.84 (5)	V2—O2—Ca1^ii	141.14 (14)
O2^ii—Ca1—V2^ix	127.60 (6)	V2—O2—Ca1	72.23 (8)
O4—Ca1—V2^ix	126.47 (6)	Ca1^ii—O2—Ca1	128.28 (7)
O4^iii—Ca1—V2^ix	79.56 (5)	V2—O2—Ca1^x	69.11 (8)
O3—Ca1—V2^ix	80.07 (5)	Ca1^ii—O2—Ca1^x	140.51 (7)
O3^iii—Ca1—V2^ix	20.41 (5)	Ca1—O2—Ca1^x	77.29 (5)
O1^iv—Ca1—V2^ix	134.57 (2)	V2—O2—Ca1^xiv	42.95 (7)
V1—Ca1—V2^ix	110.72 (3)	Ca1^ii—O2—Ca1^xiv	98.56 (8)
V2^v—Ca1—V2^ix	106.52 (3)	Ca1—O2—Ca1^xiv	105.71 (5)
V2^vi—Ca1—V2^ix	46.184 (14)	Ca1^x—O2—Ca1^xiv	102.06 (5)
V1^vii—Ca1—V2^ix	46.229 (15)	V2^v—O3—V1^vii	128.36 (11)
O1^viii—Ca1—V2^ix	59.92 (3)	V2^v—O3—V2^vii	98.52 (9)
V2^i—Ca1—V2^ix	71.44 (2)	V1^vii—O3—V2^vii	99.19 (9)
V2^ii—Ca1—V2^ix	124.23 (2)	V2^v—O3—Ca1	99.40 (8)
V1^iv—Ca1—V2^ix	127.04 (2)	V1^vii—O3—Ca1	101.95 (9)
V2—Ca1—V2^ix	148.82 (3)	V2^vii—O3—Ca1	134.09 (10)
V2^iii—Ca1—V2^ix	82.77 (2)	V2^v—O3—Ca1^xiii	64.25 (6)
O2^i—Ca1—V2^vii	127.60 (6)	V1^vii—O3—Ca1^xiii	65.39 (6)
O2^ii—Ca1—V2^vii	58.84 (5)	V2^vii—O3—Ca1^xiii	123.04 (8)
O4—Ca1—V2^vii	79.56 (5)	Ca1—O3—Ca1^xiii	102.82 (6)
O4^iii—Ca1—V2^vii	126.47 (6)	V2^v—O3—Ca1^vii	160.83 (9)
O3—Ca1—V2^vii	20.41 (5)	V1^vii—O3—Ca1^vii	48.94 (5)
O3^iii—Ca1—V2^vii	80.07 (5)	V2^vii—O3—Ca1^vii	66.02 (5)
O1^iv—Ca1—V2^vii	134.57 (2)	Ca1—O3—Ca1^vii	99.61 (7)
V1—Ca1—V2^vii	110.72 (3)	Ca1^xiii—O3—Ca1^vii	113.51 (5)
V2^v—Ca1—V2^vii	46.184 (14)	V2^v—O3—Ca1^v	60.96 (6)
V2^vi—Ca1—V2^vii	106.52 (3)	V1^vii—O3—Ca1^v	104.62 (7)
V1^vii—Ca1—V2^vii	46.229 (15)	V2^vii—O3—Ca1^v	43.64 (5)
O1^viii—Ca1—V2^vii	59.92 (4)	Ca1—O3—Ca1^v	153.23 (7)
V2^i—Ca1—V2^vii	124.23 (2)	Ca1^xiii—O3—Ca1^v	85.46 (4)
V2^ii—Ca1—V2^vii	71.440 (19)	Ca1^vii—O3—Ca1^v	100.23 (4)
V1^iv—Ca1—V2^vii	127.04 (2)	V2^v—O4—V2	98.87 (9)
V2—Ca1—V2^vii	82.77 (2)	V2^v—O4—V1	132.49 (11)
V2^iii—Ca1—V2^vii	148.82 (3)	V2—O4—V1	99.16 (9)
V2^ix—Ca1—V2^vii	87.37 (3)	V2^v—O4—Ca1	100.87 (8)
O2^i—Ca1—O2	132.42 (4)	V2—O4—Ca1	129.77 (10)
O2^ii—Ca1—O2	51.72 (7)	V1—O4—Ca1	100.46 (9)
O4—Ca1—O2	45.14 (6)	V2^v—O4—Ca1^xiii	58.01 (5)
O4^iii—Ca1—O2	100.65 (6)	V2—O4—Ca1^xiii	132.15 (8)
O3—Ca1—O2	89.04 (6)	V1—O4—Ca1^xiii	77.54 (6)
O3^iii—Ca1—O2	149.43 (7)	Ca1—O4—Ca1^xiii	97.19 (6)
O1^iv—Ca1—O2	56.41 (4)	V2^v—O4—Ca1^x	161.78 (9)
V1—Ca1—O2	66.85 (3)	V2—O4—Ca1^x	65.69 (5)
V2^v—Ca1—O2	62.22 (3)	V1—O4—Ca1^x	47.13 (5)
V2^vi—Ca1—O2	130.91 (4)	Ca1—O4—Ca1^x	96.70 (6)
V1^vii—Ca1—O2	122.63 (4)	Ca1^xiii—O4—Ca1^x	124.51 (5)
O1^viii—Ca1—O2	119.85 (4)	V2^v—O4—Ca1^xiv	63.89 (6)
V2^i—Ca1—O2	119.39 (4)	V2—O4—Ca1^xiv	43.15 (5)
V2^ii—Ca1—O2	58.66 (3)	V1—O4—Ca1^xiv	103.98 (7)
V1^iv—Ca1—O2	64.20 (4)	Ca1—O4—Ca1^xiv	155.42 (7)
V2—Ca1—O2	22.84 (3)	Ca1^xiii—O4—Ca1^xiv	90.62 (4)
V2^iii—Ca1—O2	101.81 (4)	Ca1^x—O4—Ca1^xiv	97.95 (4)
V2^ix—Ca1—O2	168.65 (4)	V2^v—O4—Ca1^ii	90.38 (7)
V2^vii—Ca1—O2	83.43 (4)	V2—O4—Ca1^ii	37.51 (5)
O1—V1—O3^x	109.25 (9)	V1—O4—Ca1^ii	128.31 (7)
O1—V1—O3^xi	109.25 (9)	Ca1—O4—Ca1^ii	96.68 (6)
O3^x—V1—O3^xi	86.63 (12)	Ca1^xiii—O4—Ca1^ii	147.36 (5)
O1—V1—O4^iii	111.35 (9)	Ca1^x—O4—Ca1^ii	82.78 (3)
O3^x—V1—O4^iii	139.41 (10)	Ca1^xiv—O4—Ca1^ii	65.86 (3)
O3^xi—V1—O4^iii	79.96 (8)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.535 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2678 reflections
a = 10.437 (3) Å	θ = 1.3–23.4°
b = 10.367 (2) Å	µ = 5.67 mm^−1
c = 5.2947 (15) Å	T = 275 K
V = 572.9 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	402 independent reflections
Radiation source: fine-focus sealed tube	367 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.038
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.472	l = −5→5
2416 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.021	w = 1/[σ^2(Fo^2) + (0.0494P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.061	(Δ/σ)max < 0.001
S = 0.98	Δρmax = 0.34 e Å^−3
402 reflections	Δρmin = −0.39 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0187 (18)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08465 (10)	0.2500	0.29951 (17)	0.0079 (4)
V1	0.28863 (8)	0.2500	0.79215 (14)	0.0063 (3)
V2	0.18747 (6)	0.52036 (6)	0.78364 (11)	0.0063 (3)
O1	0.4432 (3)	0.2500	0.8080 (6)	0.0131 (9)*
O2	0.0402 (2)	0.5657 (3)	0.7667 (4)	0.0141 (7)*
O3	0.2203 (2)	0.3799 (2)	0.0261 (4)	0.0079 (6)*
O4	0.2267 (2)	0.3796 (2)	0.5485 (4)	0.0078 (6)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0057 (6)	0.0080 (7)	0.0099 (6)	0.000	−0.0008 (4)	0.000
V1	0.0063 (5)	0.0063 (6)	0.0065 (5)	0.000	−0.0006 (3)	0.000
V2	0.0065 (5)	0.0058 (5)	0.0066 (4)	0.0010 (2)	0.0000 (2)	0.0001 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.339 (3)	V1—Ca1^xiii	4.4000 (16)
Ca1—O2^ii	2.339 (3)	V1—Ca1^xiv	5.3499 (12)
Ca1—O4	2.396 (2)	V2—O2	1.610 (3)
Ca1—O4^iii	2.396 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3	2.432 (2)	V2—O3^xiv	1.963 (2)
Ca1—O3^iii	2.432 (2)	V2—O4	1.961 (2)
Ca1—O1^iv	2.549 (4)	V2—O3^x	1.971 (2)
Ca1—V2^v	3.3663 (12)	V2—V2^xiv	2.9817 (9)
Ca1—V2^vi	3.3663 (12)	V2—V2^v	2.9817 (9)
Ca1—V1	3.3669 (14)	V2—Ca1^xiv	3.3663 (12)
Ca1—V1^vii	3.4276 (14)	V2—Ca1^ii	3.7321 (12)
Ca1—O1^viii	3.539 (3)	V2—Ca1^x	4.0581 (11)
Ca1—V2^i	3.7321 (12)	O1—Ca1^xii	2.549 (4)
Ca1—V2^ii	3.7321 (12)	O1—Ca1^xiii	3.539 (3)
Ca1—V1^iv	3.7710 (15)	O1—Ca1^x	4.559 (4)
Ca1—V2	3.9470 (10)	O2—Ca1^ii	2.339 (3)
Ca1—V2^iii	3.9470 (10)	O2—Ca1^x	4.346 (3)
Ca1—V2^ix	4.0581 (11)	O2—Ca1^xiv	4.361 (3)
Ca1—V2^vii	4.0581 (11)	O3—V2^v	1.963 (2)
Ca1—O2	4.129 (3)	O3—V1^vii	1.964 (2)
V1—O1	1.616 (4)	O3—V2^vii	1.971 (2)
V1—O3^x	1.964 (2)	O3—Ca1^xiii	4.138 (3)
V1—O3^xi	1.964 (2)	O3—Ca1^vii	4.315 (3)
V1—O4^iii	1.972 (2)	O3—Ca1^v	4.506 (2)
V1—O4	1.972 (2)	O4—V2^v	1.960 (2)
V1—V2^iii	2.9955 (9)	O4—Ca1^xiii	4.377 (3)
V1—V2	2.9955 (9)	O4—Ca1^x	4.452 (2)
V1—Ca1^x	3.4276 (14)	O4—Ca1^xiv	4.515 (3)
V1—Ca1^xii	3.7710 (15)	O4—Ca1^ii	5.094 (2)
O2^i—Ca1—O2^ii	109.55 (13)	O1—V1—O4	111.17 (11)
O2^i—Ca1—O4	152.29 (8)	O3^x—V1—O4	79.99 (9)
O2^ii—Ca1—O4	88.22 (8)	O3^xi—V1—O4	139.57 (11)
O2^i—Ca1—O4^iii	88.22 (8)	O4^iii—V1—O4	85.93 (14)
O2^ii—Ca1—O4^iii	152.29 (8)	O1—V1—V2^iii	110.66 (2)
O4—Ca1—O4^iii	68.24 (11)	O3^x—V1—V2^iii	121.56 (8)
O2^i—Ca1—O3	133.43 (8)	O3^xi—V1—V2^iii	40.51 (7)
O2^ii—Ca1—O3	77.45 (8)	O4^iii—V1—V2^iii	40.26 (7)
O4—Ca1—O3	69.91 (8)	O4—V1—V2^iii	120.82 (7)
O4^iii—Ca1—O3	106.13 (9)	O1—V1—V2	110.66 (2)
O2^i—Ca1—O3^iii	77.45 (8)	O3^x—V1—V2	40.51 (6)
O2^ii—Ca1—O3^iii	133.43 (8)	O3^xi—V1—V2	121.56 (8)
O4—Ca1—O3^iii	106.13 (9)	O4^iii—V1—V2	120.82 (7)
O4^iii—Ca1—O3^iii	69.91 (8)	O4—V1—V2	40.26 (7)
O3—Ca1—O3^iii	67.25 (11)	V2^iii—V1—V2	138.69 (4)
O2^i—Ca1—O1^iv	78.45 (7)	O1—V1—Ca1	132.19 (12)
O2^ii—Ca1—O1^iv	78.45 (7)	O3^x—V1—Ca1	105.02 (7)
O4—Ca1—O1^iv	84.82 (9)	O3^xi—V1—Ca1	105.02 (7)
O4^iii—Ca1—O1^iv	84.82 (9)	O4^iii—V1—Ca1	44.43 (7)
O3—Ca1—O1^iv	145.33 (6)	O4—V1—Ca1	44.43 (7)
O3^iii—Ca1—O1^iv	145.33 (6)	V2^iii—V1—Ca1	76.436 (19)
O2^i—Ca1—V2^v	165.36 (7)	V2—V1—Ca1	76.436 (19)
O2^ii—Ca1—V2^v	79.17 (7)	O1—V1—Ca1^x	125.42 (12)
O4—Ca1—V2^v	34.90 (5)	O3^x—V1—Ca1^x	43.97 (7)
O4^iii—Ca1—V2^v	88.47 (6)	O3^xi—V1—Ca1^x	43.97 (7)
O3—Ca1—V2^v	35.12 (5)	O4^iii—V1—Ca1^x	108.01 (7)
O3^iii—Ca1—V2^v	88.02 (6)	O4—V1—Ca1^x	108.01 (7)
O1^iv—Ca1—V2^v	115.43 (5)	V2^iii—V1—Ca1^x	78.046 (19)
O2^i—Ca1—V2^vi	79.17 (7)	V2—V1—Ca1^x	78.046 (19)
O2^ii—Ca1—V2^vi	165.36 (7)	Ca1—V1—Ca1^x	102.38 (4)
O4—Ca1—V2^vi	88.47 (6)	O1—V1—Ca1^xii	32.01 (11)
O4^iii—Ca1—V2^vi	34.90 (5)	O3^x—V1—Ca1^xii	86.32 (7)
O3—Ca1—V2^vi	88.02 (6)	O3^xi—V1—Ca1^xii	86.32 (7)
O3^iii—Ca1—V2^vi	35.12 (5)	O4^iii—V1—Ca1^xii	130.06 (7)
O1^iv—Ca1—V2^vi	115.43 (5)	O4—V1—Ca1^xii	130.06 (7)
V2^v—Ca1—V2^vi	90.02 (4)	V2^iii—V1—Ca1^xii	107.302 (19)
O2^i—Ca1—V1	117.93 (6)	V2—V1—Ca1^xii	107.302 (19)
O2^ii—Ca1—V1	117.93 (6)	Ca1—V1—Ca1^xii	164.20 (4)
O4—Ca1—V1	35.18 (5)	Ca1^x—V1—Ca1^xii	93.42 (3)
O4^iii—Ca1—V1	35.18 (5)	O1—V1—Ca1^xiii	48.37 (11)
O3—Ca1—V1	95.33 (6)	O3^x—V1—Ca1^xiii	134.74 (7)
O3^iii—Ca1—V1	95.33 (6)	O3^xi—V1—Ca1^xiii	134.74 (7)
O1^iv—Ca1—V1	74.60 (8)	O4^iii—V1—Ca1^xiii	76.37 (7)
V2^v—Ca1—V1	64.70 (2)	O4—V1—Ca1^xiii	76.37 (7)
V2^vi—Ca1—V1	64.70 (2)	V2^iii—V1—Ca1^xiii	103.697 (19)
O2^i—Ca1—V1^vii	103.21 (6)	V2—V1—Ca1^xiii	103.697 (19)
O2^ii—Ca1—V1^vii	103.21 (6)	Ca1—V1—Ca1^xiii	83.83 (3)
O4—Ca1—V1^vii	92.68 (6)	Ca1^x—V1—Ca1^xiii	173.79 (3)
O4^iii—Ca1—V1^vii	92.68 (6)	Ca1^xii—V1—Ca1^xiii	80.38 (3)
O3—Ca1—V1^vii	34.09 (5)	O1—V1—Ca1^xiv	75.684 (15)
O3^iii—Ca1—V1^vii	34.09 (5)	O3^x—V1—Ca1^xiv	54.58 (7)
O1^iv—Ca1—V1^vii	176.98 (9)	O3^xi—V1—Ca1^xiv	138.57 (7)
V2^v—Ca1—V1^vii	62.72 (2)	O4^iii—V1—Ca1^xiv	138.26 (7)
V2^vi—Ca1—V1^vii	62.72 (2)	O4—V1—Ca1^xiv	54.93 (7)
V1—Ca1—V1^vii	102.38 (4)	V2^iii—V1—Ca1^xiv	173.66 (3)
O2^i—Ca1—O1^viii	68.37 (6)	V2—V1—Ca1^xiv	34.98 (2)
O2^ii—Ca1—O1^viii	68.37 (6)	Ca1—V1—Ca1^xiv	99.321 (16)
O4—Ca1—O1^viii	139.29 (6)	Ca1^x—V1—Ca1^xiv	98.502 (16)
O4^iii—Ca1—O1^viii	139.29 (6)	Ca1^xii—V1—Ca1^xiv	78.069 (14)
O3—Ca1—O1^viii	72.65 (7)	Ca1^xiii—V1—Ca1^xiv	80.304 (14)
O3^iii—Ca1—O1^viii	72.65 (7)	O2—V2—O4^xiv	108.76 (11)
O1^iv—Ca1—O1^viii	119.97 (12)	O2—V2—O3^xiv	106.00 (11)
V2^v—Ca1—O1^viii	105.78 (5)	O4^xiv—V2—O3^xiv	89.68 (10)
V2^vi—Ca1—O1^viii	105.78 (5)	O2—V2—O4	112.41 (12)
V1—Ca1—O1^viii	165.43 (7)	O4^xiv—V2—O4	138.77 (5)
V1^vii—Ca1—O1^viii	63.05 (6)	O3^xiv—V2—O4	81.27 (10)
O2^i—Ca1—V2^i	15.71 (6)	O2—V2—O3^x	114.71 (12)
O2^ii—Ca1—V2^i	94.56 (7)	O4^xiv—V2—O3^x	81.10 (10)
O4—Ca1—V2^i	153.32 (6)	O3^xiv—V2—O3^x	139.11 (5)
O4^iii—Ca1—V2^i	100.25 (6)	O4—V2—O3^x	80.08 (9)
O3—Ca1—V2^i	136.57 (6)	O2—V2—V2^xiv	120.58 (8)
O3^iii—Ca1—V2^i	91.12 (6)	O4^xiv—V2—V2^xiv	40.52 (7)
O1^iv—Ca1—V2^i	69.85 (6)	O3^xiv—V2—V2^xiv	118.48 (8)
V2^v—Ca1—V2^i	170.37 (3)	O4—V2—V2^xiv	111.53 (7)
V2^vi—Ca1—V2^i	94.79 (2)	O3^x—V2—V2^xiv	40.63 (7)
V1—Ca1—V2^i	124.93 (2)	O2—V2—V2^v	114.20 (8)
V1^vii—Ca1—V2^i	112.35 (3)	O4^xiv—V2—V2^v	120.66 (7)
O1^viii—Ca1—V2^i	64.88 (4)	O3^xiv—V2—V2^v	40.82 (7)
O2^i—Ca1—V2^ii	94.56 (7)	O4—V2—V2^v	40.50 (7)
O2^ii—Ca1—V2^ii	15.71 (6)	O3^x—V2—V2^v	113.42 (7)
O4—Ca1—V2^ii	100.25 (6)	V2^xiv—V2—V2^v	125.21 (5)
O4^iii—Ca1—V2^ii	153.32 (6)	O2—V2—V1	127.63 (11)
O3—Ca1—V2^ii	91.12 (6)	O4^xiv—V2—V1	108.84 (7)
O3^iii—Ca1—V2^ii	136.57 (6)	O3^xiv—V2—V1	109.29 (7)
O1^iv—Ca1—V2^ii	69.85 (6)	O4—V2—V1	40.53 (6)
V2^v—Ca1—V2^ii	94.79 (2)	O3^x—V2—V1	40.33 (7)
V2^vi—Ca1—V2^ii	170.37 (3)	V2^xiv—V2—V1	72.53 (3)
V1—Ca1—V2^ii	124.93 (2)	V2^v—V2—V1	74.13 (3)
V1^vii—Ca1—V2^ii	112.35 (3)	O2—V2—Ca1^xiv	118.00 (11)
O1^viii—Ca1—V2^ii	64.88 (4)	O4^xiv—V2—Ca1^xiv	44.38 (7)
V2^i—Ca1—V2^ii	79.27 (4)	O3^xiv—V2—Ca1^xiv	45.47 (7)
O2^i—Ca1—V1^iv	68.26 (6)	O4—V2—Ca1^xiv	113.23 (7)
O2^ii—Ca1—V1^iv	68.26 (6)	O3^x—V2—Ca1^xiv	112.53 (7)
O4—Ca1—V1^iv	101.05 (6)	V2^xiv—V2—Ca1^xiv	76.62 (3)
O4^iii—Ca1—V1^iv	101.05 (6)	V2^v—V2—Ca1^xiv	79.22 (3)
O3—Ca1—V1^iv	144.92 (6)	V1—V2—Ca1^xiv	114.35 (3)
O3^iii—Ca1—V1^iv	144.92 (6)	O2—V2—Ca1^ii	23.16 (10)
O1^iv—Ca1—V1^iv	19.64 (8)	O4^xiv—V2—Ca1^ii	95.44 (7)
V2^v—Ca1—V1^iv	126.38 (2)	O3^xiv—V2—Ca1^ii	87.43 (7)
V2^vi—Ca1—V1^iv	126.38 (2)	O4—V2—Ca1^ii	123.95 (7)
V1—Ca1—V1^iv	94.24 (3)	O3^x—V2—Ca1^ii	132.88 (7)
V1^vii—Ca1—V1^iv	163.38 (4)	V2^xiv—V2—Ca1^ii	121.88 (3)
O1^viii—Ca1—V1^iv	100.33 (7)	V2^v—V2—Ca1^ii	108.59 (3)
V2^i—Ca1—V1^iv	56.23 (2)	V1—V2—Ca1^ii	150.10 (3)
V2^ii—Ca1—V1^iv	56.23 (2)	Ca1^xiv—V2—Ca1^ii	95.13 (2)
O2^i—Ca1—V2	145.99 (6)	O2—V2—Ca1	84.93 (10)
O2^ii—Ca1—V2	70.65 (6)	O4^xiv—V2—Ca1	164.64 (7)
O4—Ca1—V2	22.52 (5)	O3^xiv—V2—Ca1	93.21 (7)
O4^iii—Ca1—V2	82.70 (6)	O4—V2—Ca1	27.90 (7)
O3—Ca1—V2	80.50 (6)	O3^x—V2—Ca1	86.89 (7)
O3^iii—Ca1—V2	128.43 (7)	V2^xiv—V2—Ca1	126.52 (4)
O1^iv—Ca1—V2	68.16 (5)	V2^v—V2—Ca1	56.07 (3)
V2^v—Ca1—V2	47.302 (15)	V1—V2—Ca1	56.02 (2)
V2^vi—Ca1—V2	109.05 (3)	Ca1^xiv—V2—Ca1	135.28 (3)
V1—Ca1—V2	47.542 (17)	Ca1^ii—V2—Ca1	99.76 (2)
V1^vii—Ca1—V2	109.88 (3)	O2—V2—Ca1^x	89.23 (9)
O1^viii—Ca1—V2	134.721 (16)	O4^xiv—V2—Ca1^x	90.27 (7)
V2^i—Ca1—V2	137.44 (3)	O3^xiv—V2—Ca1^x	163.91 (7)
V2^ii—Ca1—V2	80.24 (2)	O4—V2—Ca1^x	88.21 (7)
V1^iv—Ca1—V2	81.40 (2)	O3^x—V2—Ca1^x	25.52 (7)
O2^i—Ca1—V2^iii	70.65 (6)	V2^xiv—V2—Ca1^x	54.58 (3)
O2^ii—Ca1—V2^iii	145.99 (6)	V2^v—V2—Ca1^x	127.99 (3)
O4—Ca1—V2^iii	82.70 (6)	V1—V2—Ca1^x	55.72 (2)
O4^iii—Ca1—V2^iii	22.52 (5)	Ca1^xiv—V2—Ca1^x	131.19 (3)
O3—Ca1—V2^iii	128.43 (7)	Ca1^ii—V2—Ca1^x	108.59 (2)
O3^iii—Ca1—V2^iii	80.50 (6)	Ca1—V2—Ca1^x	82.80 (2)
O1^iv—Ca1—V2^iii	68.16 (5)	V1—O1—Ca1^xii	128.36 (17)
V2^v—Ca1—V2^iii	109.05 (3)	V1—O1—Ca1^xiii	111.67 (14)
V2^vi—Ca1—V2^iii	47.302 (15)	Ca1^xii—O1—Ca1^xiii	119.97 (12)
V1—Ca1—V2^iii	47.542 (17)	V1—O1—Ca1^x	37.79 (9)
V1^vii—Ca1—V2^iii	109.88 (3)	Ca1^xii—O1—Ca1^x	90.57 (9)
O1^viii—Ca1—V2^iii	134.721 (16)	Ca1^xiii—O1—Ca1^x	149.46 (10)
V2^i—Ca1—V2^iii	80.24 (2)	V1—O1—Ca1	32.75 (9)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.11 (12)
V1^iv—Ca1—V2^iii	81.40 (2)	Ca1^xiii—O1—Ca1	78.92 (6)
V2—Ca1—V2^iii	90.49 (3)	Ca1^x—O1—Ca1	70.54 (6)
O2^i—Ca1—V2^ix	58.81 (6)	V2—O2—Ca1^ii	141.14 (16)
O2^ii—Ca1—V2^ix	127.63 (6)	V2—O2—Ca1	72.21 (9)
O4—Ca1—V2^ix	126.44 (6)	Ca1^ii—O2—Ca1	128.34 (8)
O4^iii—Ca1—V2^ix	79.58 (6)	V2—O2—Ca1^x	69.02 (9)
O3—Ca1—V2^ix	80.09 (6)	Ca1^ii—O2—Ca1^x	140.54 (8)
O3^iii—Ca1—V2^ix	20.43 (5)	Ca1—O2—Ca1^x	77.28 (5)
O1^iv—Ca1—V2^ix	134.58 (3)	V2—O2—Ca1^xiv	42.97 (8)
V2^v—Ca1—V2^ix	106.55 (3)	Ca1^ii—O2—Ca1^xiv	98.52 (8)
V2^vi—Ca1—V2^ix	46.202 (16)	Ca1—O2—Ca1^xiv	105.68 (5)
V1—Ca1—V2^ix	110.75 (3)	Ca1^x—O2—Ca1^xiv	102.02 (5)
V1^vii—Ca1—V2^ix	46.232 (16)	V2^v—O3—V1^vii	128.42 (12)
O1^viii—Ca1—V2^ix	59.90 (4)	V2^v—O3—V2^vii	98.55 (10)
V2^i—Ca1—V2^ix	71.41 (2)	V1^vii—O3—V2^vii	99.16 (10)
V2^ii—Ca1—V2^ix	124.23 (3)	V2^v—O3—Ca1	99.41 (9)
V1^iv—Ca1—V2^ix	127.05 (2)	V1^vii—O3—Ca1	101.94 (10)
V2—Ca1—V2^ix	148.84 (4)	V2^vii—O3—Ca1	134.05 (11)
V2^iii—Ca1—V2^ix	82.80 (2)	V2^v—O3—Ca1^xiii	64.28 (6)
O2^i—Ca1—V2^vii	127.63 (6)	V1^vii—O3—Ca1^xiii	65.42 (6)
O2^ii—Ca1—V2^vii	58.81 (6)	V2^vii—O3—Ca1^xiii	123.07 (9)
O4—Ca1—V2^vii	79.58 (6)	Ca1—O3—Ca1^xiii	102.82 (7)
O4^iii—Ca1—V2^vii	126.44 (6)	V2^v—O3—Ca1^vii	160.83 (10)
O3—Ca1—V2^vii	20.43 (5)	V1^vii—O3—Ca1^vii	48.91 (5)
O3^iii—Ca1—V2^vii	80.09 (6)	V2^vii—O3—Ca1^vii	65.98 (6)
O1^iv—Ca1—V2^vii	134.58 (3)	Ca1—O3—Ca1^vii	99.59 (7)
V2^v—Ca1—V2^vii	46.202 (16)	Ca1^xiii—O3—Ca1^vii	113.51 (5)
V2^vi—Ca1—V2^vii	106.55 (3)	V2^v—O3—Ca1^v	61.00 (6)
V1—Ca1—V2^vii	110.75 (3)	V1^vii—O3—Ca1^v	104.61 (8)
V1^vii—Ca1—V2^vii	46.232 (16)	V2^vii—O3—Ca1^v	43.64 (6)
O1^viii—Ca1—V2^vii	59.90 (4)	Ca1—O3—Ca1^v	153.26 (8)
V2^i—Ca1—V2^vii	124.23 (3)	Ca1^xiii—O3—Ca1^v	85.50 (4)
V2^ii—Ca1—V2^vii	71.41 (2)	Ca1^vii—O3—Ca1^v	100.18 (5)
V1^iv—Ca1—V2^vii	127.05 (2)	V2^v—O4—V2	98.99 (11)
V2—Ca1—V2^vii	82.80 (2)	V2^v—O4—V1	132.74 (12)
V2^iii—Ca1—V2^vii	148.84 (4)	V2—O4—V1	99.20 (10)
V2^ix—Ca1—V2^vii	87.37 (3)	V2^v—O4—Ca1	100.72 (9)
O2^i—Ca1—O2	132.43 (5)	V2—O4—Ca1	129.59 (11)
O2^ii—Ca1—O2	51.66 (8)	V1—O4—Ca1	100.39 (10)
O4—Ca1—O2	45.20 (6)	V2^v—O4—Ca1^xiii	58.08 (6)
O4^iii—Ca1—O2	100.64 (7)	V2—O4—Ca1^xiii	132.37 (9)
O3—Ca1—O2	89.03 (7)	V1—O4—Ca1^xiii	77.67 (7)
O3^iii—Ca1—O2	149.44 (7)	Ca1—O4—Ca1^xiii	97.14 (7)
O1^iv—Ca1—O2	56.39 (5)	V2^v—O4—Ca1^x	161.94 (10)
V2^v—Ca1—O2	62.21 (4)	V2—O4—Ca1^x	65.66 (6)
V2^vi—Ca1—O2	130.92 (4)	V1—O4—Ca1^x	47.07 (6)
V1—Ca1—O2	66.86 (4)	Ca1—O4—Ca1^x	96.66 (7)
V1^vii—Ca1—O2	122.64 (4)	Ca1^xiii—O4—Ca1^x	124.58 (5)
O1^viii—Ca1—O2	119.84 (5)	V2^v—O4—Ca1^xiv	64.00 (7)
V2^i—Ca1—O2	119.39 (5)	V2—O4—Ca1^xiv	43.25 (6)
V2^ii—Ca1—O2	58.63 (4)	V1—O4—Ca1^xiv	104.13 (8)
V1^iv—Ca1—O2	64.17 (4)	Ca1—O4—Ca1^xiv	155.33 (8)
V2—Ca1—O2	22.86 (4)	Ca1^xiii—O4—Ca1^xiv	90.74 (4)
V2^iii—Ca1—O2	101.79 (4)	Ca1^x—O4—Ca1^xiv	97.99 (5)
V2^ix—Ca1—O2	168.67 (5)	V2^v—O4—Ca1^ii	90.34 (7)
V2^vii—Ca1—O2	83.42 (4)	V2—O4—Ca1^ii	37.42 (5)
O1—V1—O3^x	109.25 (11)	V1—O4—Ca1^ii	128.27 (8)
O1—V1—O3^xi	109.25 (11)	Ca1—O4—Ca1^ii	96.60 (6)
O3^x—V1—O3^xi	86.62 (14)	Ca1^xiii—O4—Ca1^ii	147.40 (5)
O1—V1—O4^iii	111.17 (10)	Ca1^x—O4—Ca1^ii	82.76 (4)
O3^x—V1—O4^iii	139.57 (11)	Ca1^xiv—O4—Ca1^ii	65.84 (3)
O3^xi—V1—O4^iii	79.99 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.535 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2683 reflections
a = 10.442 (3) Å	θ = 1.3–23.4°
b = 10.367 (2) Å	µ = 5.67 mm^−1
c = 5.2914 (15) Å	T = 262 K
V = 572.8 (2) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	404 independent reflections
Radiation source: fine-focus sealed tube	365 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.318, Tmax = 0.471	l = −5→5
2427 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0464P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.055	(Δ/σ)max < 0.001
S = 0.94	Δρmax = 0.34 e Å^−3
404 reflections	Δρmin = −0.40 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0193 (16)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08476 (10)	0.2500	0.29971 (15)	0.0077 (3)
V1	0.28862 (7)	0.2500	0.79194 (13)	0.0060 (3)
V2	0.18747 (6)	0.52037 (6)	0.78355 (10)	0.0061 (3)
O1	0.4435 (3)	0.2500	0.8080 (5)	0.0122 (8)*
O2	0.0402 (2)	0.5656 (3)	0.7668 (4)	0.0141 (6)*
O3	0.22014 (19)	0.3799 (2)	0.0261 (4)	0.0074 (5)*
O4	0.22655 (19)	0.3796 (2)	0.5481 (4)	0.0073 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0054 (5)	0.0080 (6)	0.0097 (6)	0.000	−0.0001 (3)	0.000
V1	0.0059 (5)	0.0056 (6)	0.0065 (5)	0.000	−0.0005 (3)	0.000
V2	0.0063 (4)	0.0055 (4)	0.0065 (4)	0.0010 (2)	0.0001 (2)	0.0003 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.341 (3)	V1—Ca1^xiii	4.4004 (15)
Ca1—O2^ii	2.341 (3)	V1—Ca1^xiv	5.3498 (11)
Ca1—O4	2.392 (2)	V2—O2	1.611 (2)
Ca1—O4^iii	2.392 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3^iii	2.431 (2)	V2—O4	1.962 (2)
Ca1—O3	2.431 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.547 (3)	V2—O3^x	1.971 (2)
Ca1—V1	3.3638 (13)	V2—V2^v	2.9805 (9)
Ca1—V2^v	3.3662 (11)	V2—V2^xiv	2.9805 (9)
Ca1—V2^vi	3.3662 (11)	V2—Ca1^xiv	3.3662 (11)
Ca1—V1^vii	3.4279 (13)	V2—Ca1^ii	3.7340 (11)
Ca1—O1^viii	3.538 (3)	V2—Ca1^x	4.0579 (10)
Ca1—V2^i	3.7340 (11)	O1—Ca1^xii	2.547 (3)
Ca1—V2^ii	3.7340 (11)	O1—Ca1^xiii	3.538 (3)
Ca1—V1^iv	3.7724 (14)	O1—Ca1^x	4.561 (3)
Ca1—V2	3.9448 (10)	O2—Ca1^ii	2.341 (3)
Ca1—V2^iii	3.9448 (10)	O2—Ca1^x	4.344 (3)
Ca1—V2^ix	4.0579 (10)	O2—Ca1^xiv	4.362 (3)
Ca1—V2^vii	4.0579 (10)	O3—V1^vii	1.965 (2)
Ca1—O2	4.127 (3)	O3—V2^v	1.964 (2)
V1—O1	1.619 (3)	O3—V2^vii	1.971 (2)
V1—O3^x	1.965 (2)	O3—Ca1^xiii	4.142 (2)
V1—O3^xi	1.965 (2)	O3—Ca1^vii	4.311 (2)
V1—O4^iii	1.972 (2)	O3—Ca1^v	4.506 (2)
V1—O4	1.972 (2)	O4—V2^v	1.960 (2)
V1—V2^iii	2.9957 (9)	O4—Ca1^xiii	4.380 (2)
V1—V2	2.9957 (9)	O4—Ca1^x	4.451 (2)
V1—Ca1^x	3.4279 (13)	O4—Ca1^xiv	4.517 (2)
V1—Ca1^xii	3.7724 (14)	O4—Ca1^ii	5.095 (2)
O2^i—Ca1—O2^ii	109.50 (12)	O1—V1—O4	111.25 (10)
O2^i—Ca1—O4	152.37 (8)	O3^x—V1—O4	79.99 (9)
O2^ii—Ca1—O4	88.22 (8)	O3^xi—V1—O4	139.45 (10)
O2^i—Ca1—O4^iii	88.22 (8)	O4^iii—V1—O4	85.87 (12)
O2^ii—Ca1—O4^iii	152.37 (8)	O1—V1—V2^iii	110.663 (18)
O4—Ca1—O4^iii	68.32 (10)	O3^x—V1—V2^iii	121.49 (7)
O2^i—Ca1—O3^iii	77.41 (7)	O3^xi—V1—V2^iii	40.51 (6)
O2^ii—Ca1—O3^iii	133.39 (8)	O4^iii—V1—V2^iii	40.28 (6)
O4—Ca1—O3^iii	106.16 (8)	O4—V1—V2^iii	120.78 (7)
O4^iii—Ca1—O3^iii	69.89 (7)	O1—V1—V2	110.663 (18)
O2^i—Ca1—O3	133.39 (8)	O3^x—V1—V2	40.51 (6)
O2^ii—Ca1—O3	77.41 (7)	O3^xi—V1—V2	121.49 (7)
O4—Ca1—O3	69.89 (7)	O4^iii—V1—V2	120.78 (7)
O4^iii—Ca1—O3	106.16 (8)	O4—V1—V2	40.28 (6)
O3^iii—Ca1—O3	67.29 (10)	V2^iii—V1—V2	138.67 (4)
O2^i—Ca1—O1^iv	78.45 (7)	O1—V1—Ca1	132.26 (11)
O2^ii—Ca1—O1^iv	78.45 (7)	O3^x—V1—Ca1	104.95 (6)
O4—Ca1—O1^iv	84.88 (8)	O3^xi—V1—Ca1	104.95 (6)
O4^iii—Ca1—O1^iv	84.88 (8)	O4^iii—V1—Ca1	44.39 (6)
O3^iii—Ca1—O1^iv	145.33 (5)	O4—V1—Ca1	44.39 (6)
O3—Ca1—O1^iv	145.33 (5)	V2^iii—V1—Ca1	76.432 (17)
O2^i—Ca1—V1	117.97 (6)	V2—V1—Ca1	76.432 (17)
O2^ii—Ca1—V1	117.97 (6)	O1—V1—Ca1^x	125.39 (11)
O4—Ca1—V1	35.22 (5)	O3^x—V1—Ca1^x	43.92 (6)
O4^iii—Ca1—V1	35.22 (5)	O3^xi—V1—Ca1^x	43.92 (6)
O3^iii—Ca1—V1	95.34 (6)	O4^iii—V1—Ca1^x	107.98 (7)
O3—Ca1—V1	95.34 (6)	O4—V1—Ca1^x	107.98 (7)
O1^iv—Ca1—V1	74.66 (7)	V2^iii—V1—Ca1^x	78.034 (18)
O2^i—Ca1—V2^v	165.33 (6)	V2—V1—Ca1^x	78.034 (18)
O2^ii—Ca1—V2^v	79.18 (6)	Ca1—V1—Ca1^x	102.35 (4)
O4—Ca1—V2^v	34.88 (5)	O1—V1—Ca1^xii	31.94 (10)
O4^iii—Ca1—V2^v	88.50 (6)	O3^x—V1—Ca1^xii	86.40 (6)
O3^iii—Ca1—V2^v	88.04 (6)	O3^xi—V1—Ca1^xii	86.40 (6)
O3—Ca1—V2^v	35.13 (5)	O4^iii—V1—Ca1^xii	130.10 (6)
O1^iv—Ca1—V2^v	115.47 (5)	O4—V1—Ca1^xii	130.10 (6)
V1—Ca1—V2^v	64.69 (2)	V2^iii—V1—Ca1^xii	107.308 (17)
O2^i—Ca1—V2^vi	79.18 (6)	V2—V1—Ca1^xii	107.308 (17)
O2^ii—Ca1—V2^vi	165.33 (6)	Ca1—V1—Ca1^xii	164.20 (3)
O4—Ca1—V2^vi	88.50 (6)	Ca1^x—V1—Ca1^xii	93.45 (3)
O4^iii—Ca1—V2^vi	34.88 (5)	O1—V1—Ca1^xiii	48.35 (10)
O3^iii—Ca1—V2^vi	35.13 (5)	O3^x—V1—Ca1^xiii	134.79 (6)
O3—Ca1—V2^vi	88.04 (6)	O3^xi—V1—Ca1^xiii	134.79 (6)
O1^iv—Ca1—V2^vi	115.47 (5)	O4^iii—V1—Ca1^xiii	76.44 (6)
V1—Ca1—V2^vi	64.69 (2)	O4—V1—Ca1^xiii	76.44 (6)
V2^v—Ca1—V2^vi	90.02 (4)	V2^iii—V1—Ca1^xiii	103.723 (17)
O2^i—Ca1—V1^vii	103.19 (6)	V2—V1—Ca1^xiii	103.723 (17)
O2^ii—Ca1—V1^vii	103.19 (6)	Ca1—V1—Ca1^xiii	83.91 (3)
O4—Ca1—V1^vii	92.65 (6)	Ca1^x—V1—Ca1^xiii	173.74 (3)
O4^iii—Ca1—V1^vii	92.65 (6)	Ca1^xii—V1—Ca1^xiii	80.30 (3)
O3^iii—Ca1—V1^vii	34.10 (5)	O1—V1—Ca1^xiv	75.688 (14)
O3—Ca1—V1^vii	34.10 (5)	O3^x—V1—Ca1^xiv	54.62 (6)
O1^iv—Ca1—V1^vii	177.01 (8)	O3^xi—V1—Ca1^xiv	138.52 (6)
V1—Ca1—V1^vii	102.35 (4)	O4^iii—V1—Ca1^xiv	138.27 (6)
V2^v—Ca1—V1^vii	62.70 (2)	O4—V1—Ca1^xiv	54.99 (6)
V2^vi—Ca1—V1^vii	62.70 (2)	V2^iii—V1—Ca1^xiv	173.65 (3)
O2^i—Ca1—O1^viii	68.34 (6)	V2—V1—Ca1^xiv	34.98 (2)
O2^ii—Ca1—O1^viii	68.34 (6)	Ca1—V1—Ca1^xiv	99.343 (15)
O4—Ca1—O1^viii	139.23 (6)	Ca1^x—V1—Ca1^xiv	98.479 (15)
O4^iii—Ca1—O1^viii	139.23 (6)	Ca1^xii—V1—Ca1^xiv	78.054 (13)
O3^iii—Ca1—O1^viii	72.62 (7)	Ca1^xiii—V1—Ca1^xiv	80.317 (13)
O3—Ca1—O1^viii	72.62 (7)	O2—V2—O4^xiv	108.83 (10)
O1^iv—Ca1—O1^viii	119.95 (11)	O2—V2—O4	112.35 (10)
V1—Ca1—O1^viii	165.39 (6)	O4^xiv—V2—O4	138.76 (5)
V2^v—Ca1—O1^viii	105.76 (4)	O2—V2—O3^xiv	106.13 (10)
V2^vi—Ca1—O1^viii	105.76 (4)	O4^xiv—V2—O3^xiv	89.52 (9)
V1^vii—Ca1—O1^viii	63.04 (6)	O4—V2—O3^xiv	81.32 (9)
O2^i—Ca1—V2^i	15.72 (6)	O2—V2—O3^x	114.59 (11)
O2^ii—Ca1—V2^i	94.51 (7)	O4^xiv—V2—O3^x	81.18 (9)
O4—Ca1—V2^i	153.37 (6)	O4—V2—O3^x	80.08 (9)
O4^iii—Ca1—V2^i	100.25 (5)	O3^xiv—V2—O3^x	139.10 (5)
O3^iii—Ca1—V2^i	91.10 (5)	O2—V2—V2^v	114.26 (7)
O3—Ca1—V2^i	136.53 (6)	O4^xiv—V2—V2^v	120.55 (7)
O1^iv—Ca1—V2^i	69.83 (6)	O4—V2—V2^v	40.52 (6)
V1—Ca1—V2^i	124.97 (2)	O3^xiv—V2—V2^v	40.85 (6)
V2^v—Ca1—V2^i	170.33 (3)	O3^x—V2—V2^v	113.42 (7)
V2^vi—Ca1—V2^i	94.82 (2)	O2—V2—V2^xiv	120.56 (8)
V1^vii—Ca1—V2^i	112.35 (2)	O4^xiv—V2—V2^xiv	40.56 (6)
O1^viii—Ca1—V2^i	64.86 (4)	O4—V2—V2^xiv	111.54 (7)
O2^i—Ca1—V2^ii	94.51 (7)	O3^xiv—V2—V2^xiv	118.37 (7)
O2^ii—Ca1—V2^ii	15.72 (6)	O3^x—V2—V2^xiv	40.66 (6)
O4—Ca1—V2^ii	100.25 (5)	V2^v—V2—V2^xiv	125.16 (4)
O4^iii—Ca1—V2^ii	153.37 (6)	O2—V2—V1	127.59 (10)
O3^iii—Ca1—V2^ii	136.53 (6)	O4^xiv—V2—V1	108.85 (7)
O3—Ca1—V2^ii	91.10 (5)	O4—V2—V1	40.53 (6)
O1^iv—Ca1—V2^ii	69.83 (6)	O3^xiv—V2—V1	109.26 (7)
V1—Ca1—V2^ii	124.97 (2)	O3^x—V2—V1	40.36 (6)
V2^v—Ca1—V2^ii	94.82 (2)	V2^v—V2—V1	74.10 (3)
V2^vi—Ca1—V2^ii	170.33 (3)	V2^xiv—V2—V1	72.53 (3)
V1^vii—Ca1—V2^ii	112.35 (2)	O2—V2—Ca1^xiv	118.06 (10)
O1^viii—Ca1—V2^ii	64.86 (4)	O4^xiv—V2—Ca1^xiv	44.27 (6)
V2^i—Ca1—V2^ii	79.22 (3)	O4—V2—Ca1^xiv	113.29 (7)
O2^i—Ca1—V1^iv	68.25 (6)	O3^xiv—V2—Ca1^xiv	45.42 (6)
O2^ii—Ca1—V1^iv	68.25 (6)	O3^x—V2—Ca1^xiv	112.57 (7)
O4—Ca1—V1^iv	101.10 (6)	V2^v—V2—Ca1^xiv	79.24 (3)
O4^iii—Ca1—V1^iv	101.10 (6)	V2^xiv—V2—Ca1^xiv	76.59 (3)
O3^iii—Ca1—V1^iv	144.88 (5)	V1—V2—Ca1^xiv	114.35 (3)
O3—Ca1—V1^iv	144.88 (5)	O2—V2—Ca1^ii	23.19 (9)
O1^iv—Ca1—V1^iv	19.65 (7)	O4^xiv—V2—Ca1^ii	95.49 (6)
V1—Ca1—V1^iv	94.32 (3)	O4—V2—Ca1^ii	123.90 (6)
V2^v—Ca1—V1^iv	126.42 (2)	O3^xiv—V2—Ca1^ii	87.50 (6)
V2^vi—Ca1—V1^iv	126.42 (2)	O3^x—V2—Ca1^ii	132.82 (6)
V1^vii—Ca1—V1^iv	163.33 (3)	V2^v—V2—Ca1^ii	108.61 (3)
O1^viii—Ca1—V1^iv	100.29 (6)	V2^xiv—V2—Ca1^ii	121.91 (3)
V2^i—Ca1—V1^iv	56.19 (2)	V1—V2—Ca1^ii	150.08 (3)
V2^ii—Ca1—V1^iv	56.19 (2)	Ca1^xiv—V2—Ca1^ii	95.16 (2)
O2^i—Ca1—V2	146.03 (6)	O2—V2—Ca1	84.92 (9)
O2^ii—Ca1—V2	70.66 (6)	O4^xiv—V2—Ca1	164.60 (7)
O4—Ca1—V2	22.52 (5)	O4—V2—Ca1	27.84 (6)
O4^iii—Ca1—V2	82.77 (5)	O3^xiv—V2—Ca1	93.30 (6)
O3^iii—Ca1—V2	128.47 (6)	O3^x—V2—Ca1	86.83 (7)
O3—Ca1—V2	80.49 (5)	V2^v—V2—Ca1	56.11 (2)
O1^iv—Ca1—V2	68.19 (5)	V2^xiv—V2—Ca1	126.48 (3)
V1—Ca1—V2	47.580 (15)	V1—V2—Ca1	55.99 (2)
V2^v—Ca1—V2	47.303 (14)	Ca1^xiv—V2—Ca1	135.32 (3)
V2^vi—Ca1—V2	109.08 (3)	Ca1^ii—V2—Ca1	99.76 (2)
V1^vii—Ca1—V2	109.87 (3)	O2—V2—Ca1^x	89.18 (9)
O1^viii—Ca1—V2	134.688 (15)	O4^xiv—V2—Ca1^x	90.34 (6)
V2^i—Ca1—V2	137.44 (3)	O4—V2—Ca1^x	88.19 (6)
V2^ii—Ca1—V2	80.24 (2)	O3^xiv—V2—Ca1^x	163.85 (7)
V1^iv—Ca1—V2	81.44 (2)	O3^x—V2—Ca1^x	25.45 (6)
O2^i—Ca1—V2^iii	70.66 (6)	V2^v—V2—Ca1^x	127.98 (3)
O2^ii—Ca1—V2^iii	146.03 (6)	V2^xiv—V2—Ca1^x	54.58 (2)
O4—Ca1—V2^iii	82.77 (5)	V1—V2—Ca1^x	55.73 (2)
O4^iii—Ca1—V2^iii	22.52 (5)	Ca1^xiv—V2—Ca1^x	131.16 (2)
O3^iii—Ca1—V2^iii	80.49 (5)	Ca1^ii—V2—Ca1^x	108.58 (2)
O3—Ca1—V2^iii	128.47 (6)	Ca1—V2—Ca1^x	82.77 (2)
O1^iv—Ca1—V2^iii	68.19 (5)	V1—O1—Ca1^xii	128.40 (15)
V1—Ca1—V2^iii	47.580 (15)	V1—O1—Ca1^xiii	111.65 (13)
V2^v—Ca1—V2^iii	109.08 (3)	Ca1^xii—O1—Ca1^xiii	119.95 (11)
V2^vi—Ca1—V2^iii	47.303 (14)	V1—O1—Ca1^x	37.79 (8)
V1^vii—Ca1—V2^iii	109.87 (3)	Ca1^xii—O1—Ca1^x	90.61 (8)
O1^viii—Ca1—V2^iii	134.688 (15)	Ca1^xiii—O1—Ca1^x	149.44 (9)
V2^i—Ca1—V2^iii	80.24 (2)	V1—O1—Ca1	32.68 (8)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.08 (11)
V1^iv—Ca1—V2^iii	81.44 (2)	Ca1^xiii—O1—Ca1	78.97 (6)
V2—Ca1—V2^iii	90.56 (3)	Ca1^x—O1—Ca1	70.47 (5)
O2^i—Ca1—V2^ix	58.80 (6)	V2—O2—Ca1^ii	141.10 (14)
O2^ii—Ca1—V2^ix	127.60 (6)	V2—O2—Ca1	72.20 (8)
O4—Ca1—V2^ix	126.44 (6)	Ca1^ii—O2—Ca1	128.33 (7)
O4^iii—Ca1—V2^ix	79.53 (5)	V2—O2—Ca1^x	69.07 (8)
O3^iii—Ca1—V2^ix	20.39 (5)	Ca1^ii—O2—Ca1^x	140.57 (8)
O3—Ca1—V2^ix	80.10 (6)	Ca1—O2—Ca1^x	77.26 (5)
O1^iv—Ca1—V2^ix	134.57 (3)	V2—O2—Ca1^xiv	42.93 (7)
V1—Ca1—V2^ix	110.73 (3)	Ca1^ii—O2—Ca1^xiv	98.53 (8)
V2^v—Ca1—V2^ix	106.54 (3)	Ca1—O2—Ca1^xiv	105.67 (5)
V2^vi—Ca1—V2^ix	46.183 (15)	Ca1^x—O2—Ca1^xiv	102.00 (5)
V1^vii—Ca1—V2^ix	46.236 (15)	V1^vii—O3—V2^v	128.29 (11)
O1^viii—Ca1—V2^ix	59.90 (4)	V1^vii—O3—V2^vii	99.13 (9)
V2^i—Ca1—V2^ix	71.42 (2)	V2^v—O3—V2^vii	98.49 (10)
V2^ii—Ca1—V2^ix	124.21 (3)	V1^vii—O3—Ca1	101.98 (9)
V1^iv—Ca1—V2^ix	127.03 (2)	V2^v—O3—Ca1	99.46 (8)
V2—Ca1—V2^ix	148.84 (3)	V2^vii—O3—Ca1	134.16 (10)
V2^iii—Ca1—V2^ix	82.77 (2)	V1^vii—O3—Ca1^xiii	65.35 (6)
O2^i—Ca1—V2^vii	127.60 (6)	V2^v—O3—Ca1^xiii	64.23 (6)
O2^ii—Ca1—V2^vii	58.80 (6)	V2^vii—O3—Ca1^xiii	122.97 (8)
O4—Ca1—V2^vii	79.53 (5)	Ca1—O3—Ca1^xiii	102.82 (6)
O4^iii—Ca1—V2^vii	126.44 (6)	V1^vii—O3—Ca1^vii	48.93 (5)
O3^iii—Ca1—V2^vii	80.10 (6)	V2^v—O3—Ca1^vii	160.76 (9)
O3—Ca1—V2^vii	20.39 (5)	V2^vii—O3—Ca1^vii	66.01 (6)
O1^iv—Ca1—V2^vii	134.57 (3)	Ca1—O3—Ca1^vii	99.63 (7)
V1—Ca1—V2^vii	110.73 (3)	Ca1^xiii—O3—Ca1^vii	113.47 (5)
V2^v—Ca1—V2^vii	46.183 (14)	V1^vii—O3—Ca1^v	104.56 (7)
V2^vi—Ca1—V2^vii	106.54 (3)	V2^v—O3—Ca1^v	60.92 (6)
V1^vii—Ca1—V2^vii	46.236 (15)	V2^vii—O3—Ca1^v	43.61 (5)
O1^viii—Ca1—V2^vii	59.90 (4)	Ca1—O3—Ca1^v	153.25 (7)
V2^i—Ca1—V2^vii	124.21 (3)	Ca1^xiii—O3—Ca1^v	85.44 (4)
V2^ii—Ca1—V2^vii	71.42 (2)	Ca1^vii—O3—Ca1^v	100.21 (4)
V1^iv—Ca1—V2^vii	127.03 (2)	V2^v—O4—V2	98.92 (10)
V2—Ca1—V2^vii	82.77 (2)	V2^v—O4—V1	132.62 (11)
V2^iii—Ca1—V2^vii	148.84 (3)	V2—O4—V1	99.19 (9)
V2^ix—Ca1—V2^vii	87.38 (3)	V2^v—O4—Ca1	100.85 (8)
O2^i—Ca1—O2	132.43 (4)	V2—O4—Ca1	129.63 (10)
O2^ii—Ca1—O2	51.67 (7)	V1—O4—Ca1	100.39 (9)
O4—Ca1—O2	45.22 (6)	V2^v—O4—Ca1^xiii	58.06 (5)
O4^iii—Ca1—O2	100.72 (6)	V2—O4—Ca1^xiii	132.27 (8)
O3^iii—Ca1—O2	149.50 (7)	V1—O4—Ca1^xiii	77.60 (6)
O3—Ca1—O2	89.03 (6)	Ca1—O4—Ca1^xiii	97.21 (6)
O1^iv—Ca1—O2	56.39 (4)	V2^v—O4—Ca1^x	161.84 (9)
V1—Ca1—O2	66.90 (4)	V2—O4—Ca1^x	65.67 (6)
V2^v—Ca1—O2	62.24 (4)	V1—O4—Ca1^x	47.10 (5)
V2^vi—Ca1—O2	130.97 (4)	Ca1—O4—Ca1^x	96.63 (6)
V1^vii—Ca1—O2	122.65 (4)	Ca1^xiii—O4—Ca1^x	124.54 (5)
O1^viii—Ca1—O2	119.82 (4)	V2^v—O4—Ca1^xiv	63.94 (6)
V2^i—Ca1—O2	119.36 (4)	V2—O4—Ca1^xiv	43.20 (5)
V2^ii—Ca1—O2	58.62 (3)	V1—O4—Ca1^xiv	104.06 (7)
V1^iv—Ca1—O2	64.18 (4)	Ca1—O4—Ca1^xiv	155.40 (7)
V2—Ca1—O2	22.87 (3)	Ca1^xiii—O4—Ca1^xiv	90.69 (4)
V2^iii—Ca1—O2	101.85 (4)	Ca1^x—O4—Ca1^xiv	97.95 (4)
V2^ix—Ca1—O2	168.69 (4)	V2^v—O4—Ca1^ii	90.36 (7)
V2^vii—Ca1—O2	83.41 (4)	V2—O4—Ca1^ii	37.46 (5)
O1—V1—O3^x	109.30 (10)	V1—O4—Ca1^ii	128.29 (8)
O1—V1—O3^xi	109.30 (10)	Ca1—O4—Ca1^ii	96.62 (6)
O3^x—V1—O3^xi	86.53 (13)	Ca1^xiii—O4—Ca1^ii	147.40 (5)
O1—V1—O4^iii	111.25 (9)	Ca1^x—O4—Ca1^ii	82.76 (3)
O3^x—V1—O4^iii	139.45 (10)	Ca1^xiv—O4—Ca1^ii	65.85 (3)
O3^xi—V1—O4^iii	79.99 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.537 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2742 reflections
a = 10.436 (3) Å	θ = 1.3–23.4°
b = 10.367 (2) Å	µ = 5.67 mm^−1
c = 5.2921 (15) Å	T = 250 K
V = 572.6 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	403 independent reflections
Radiation source: fine-focus sealed tube	366 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.471	l = −5→5
2476 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0472P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.055	(Δ/σ)max < 0.001
S = 0.94	Δρmax = 0.35 e Å^−3
403 reflections	Δρmin = −0.39 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0175 (16)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08473 (9)	0.2500	0.29954 (15)	0.0073 (3)
V1	0.28868 (7)	0.2500	0.79217 (13)	0.0058 (3)
V2	0.18742 (6)	0.52032 (6)	0.78363 (10)	0.0058 (3)
O1	0.4435 (3)	0.2500	0.8083 (5)	0.0119 (8)*
O2	0.0401 (2)	0.5658 (3)	0.7668 (4)	0.0134 (6)*
O3	0.22036 (19)	0.3798 (2)	0.0260 (4)	0.0067 (5)*
O4	0.22672 (19)	0.3796 (2)	0.5482 (4)	0.0071 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0055 (5)	0.0071 (6)	0.0092 (6)	0.000	−0.0004 (3)	0.000
V1	0.0060 (5)	0.0052 (6)	0.0060 (5)	0.000	−0.0003 (3)	0.000
V2	0.0060 (4)	0.0054 (4)	0.0061 (4)	0.0009 (2)	0.0000 (2)	0.0000 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.339 (3)	V1—Ca1^xiii	4.3990 (15)
Ca1—O2^ii	2.339 (3)	V1—Ca1^xiv	5.3493 (12)
Ca1—O4	2.394 (2)	V2—O2	1.610 (2)
Ca1—O4^iii	2.394 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3	2.431 (2)	V2—O3^xiv	1.964 (2)
Ca1—O3^iii	2.431 (2)	V2—O4	1.962 (2)
Ca1—O1^iv	2.545 (3)	V2—O3^x	1.971 (2)
Ca1—V1	3.3656 (13)	V2—V2^xiv	2.9808 (9)
Ca1—V2^v	3.3662 (11)	V2—V2^v	2.9808 (9)
Ca1—V2^vi	3.3662 (11)	V2—Ca1^xiv	3.3662 (11)
Ca1—V1^vii	3.4264 (13)	V2—Ca1^ii	3.7323 (11)
Ca1—O1^viii	3.538 (3)	V2—Ca1^x	4.0566 (10)
Ca1—V2^i	3.7323 (11)	O1—Ca1^xii	2.545 (3)
Ca1—V2^ii	3.7323 (11)	O1—Ca1^xiii	3.538 (3)
Ca1—V1^iv	3.7702 (14)	O1—Ca1^x	4.559 (3)
Ca1—V2	3.9452 (10)	O2—Ca1^ii	2.339 (3)
Ca1—V2^iii	3.9452 (10)	O2—Ca1^x	4.345 (3)
Ca1—V2^ix	4.0566 (10)	O2—Ca1^xiv	4.359 (3)
Ca1—V2^vii	4.0566 (10)	O3—V1^vii	1.962 (2)
Ca1—O2	4.129 (3)	O3—V2^v	1.964 (2)
V1—O1	1.618 (3)	O3—V2^vii	1.971 (2)
V1—O3^x	1.962 (2)	O3—Ca1^xiii	4.138 (2)
V1—O3^xi	1.962 (2)	O3—Ca1^vii	4.312 (2)
V1—O4^iii	1.972 (2)	O3—Ca1^v	4.506 (2)
V1—O4	1.972 (2)	O4—V2^v	1.960 (2)
V1—V2^iii	2.9953 (9)	O4—Ca1^xiii	4.376 (2)
V1—V2	2.9953 (9)	O4—Ca1^x	4.451 (2)
V1—Ca1^x	3.4264 (13)	O4—Ca1^xiv	4.515 (2)
V1—Ca1^xii	3.7702 (14)	O4—Ca1^ii	5.095 (2)
O2^i—Ca1—O2^ii	109.51 (12)	O1—V1—O4	111.21 (10)
O2^i—Ca1—O4	152.33 (8)	O3^x—V1—O4	80.02 (9)
O2^ii—Ca1—O4	88.23 (7)	O3^xi—V1—O4	139.54 (10)
O2^i—Ca1—O4^iii	88.23 (7)	O4^iii—V1—O4	85.87 (12)
O2^ii—Ca1—O4^iii	152.33 (8)	O1—V1—V2^iii	110.678 (18)
O4—Ca1—O4^iii	68.27 (10)	O3^x—V1—V2^iii	121.52 (7)
O2^i—Ca1—O3	133.41 (8)	O3^xi—V1—V2^iii	40.52 (6)
O2^ii—Ca1—O3	77.47 (7)	O4^iii—V1—V2^iii	40.29 (6)
O4—Ca1—O3	69.90 (7)	O4—V1—V2^iii	120.78 (7)
O4^iii—Ca1—O3	106.11 (8)	O1—V1—V2	110.678 (18)
O2^i—Ca1—O3^iii	77.47 (7)	O3^x—V1—V2	40.52 (6)
O2^ii—Ca1—O3^iii	133.41 (8)	O3^xi—V1—V2	121.52 (7)
O4—Ca1—O3^iii	106.11 (8)	O4^iii—V1—V2	120.78 (7)
O4^iii—Ca1—O3^iii	69.90 (7)	O4—V1—V2	40.29 (6)
O3—Ca1—O3^iii	67.22 (10)	V2^iii—V1—V2	138.64 (4)
O2^i—Ca1—O1^iv	78.45 (7)	O1—V1—Ca1	132.25 (11)
O2^ii—Ca1—O1^iv	78.45 (7)	O3^x—V1—Ca1	105.00 (6)
O4—Ca1—O1^iv	84.84 (8)	O3^xi—V1—Ca1	105.00 (6)
O4^iii—Ca1—O1^iv	84.84 (8)	O4^iii—V1—Ca1	44.40 (6)
O3—Ca1—O1^iv	145.35 (5)	O4—V1—Ca1	44.40 (6)
O3^iii—Ca1—O1^iv	145.35 (5)	V2^iii—V1—Ca1	76.419 (17)
O2^i—Ca1—V1	117.95 (6)	V2—V1—Ca1	76.419 (17)
O2^ii—Ca1—V1	117.95 (6)	O1—V1—Ca1^x	125.39 (11)
O4—Ca1—V1	35.20 (5)	O3^x—V1—Ca1^x	43.95 (6)
O4^iii—Ca1—V1	35.20 (5)	O3^xi—V1—Ca1^x	43.95 (6)
O3—Ca1—V1	95.33 (6)	O4^iii—V1—Ca1^x	108.02 (7)
O3^iii—Ca1—V1	95.33 (6)	O4—V1—Ca1^x	108.02 (7)
O1^iv—Ca1—V1	74.60 (7)	V2^iii—V1—Ca1^x	78.034 (18)
O2^i—Ca1—V2^v	165.37 (6)	V2—V1—Ca1^x	78.034 (18)
O2^ii—Ca1—V2^v	79.18 (6)	Ca1—V1—Ca1^x	102.37 (4)
O4—Ca1—V2^v	34.88 (5)	O1—V1—Ca1^xii	31.95 (10)
O4^iii—Ca1—V2^v	88.48 (6)	O3^x—V1—Ca1^xii	86.35 (6)
O3—Ca1—V2^v	35.14 (5)	O3^xi—V1—Ca1^xii	86.35 (6)
O3^iii—Ca1—V2^v	88.01 (6)	O4^iii—V1—Ca1^xii	130.08 (6)
O1^iv—Ca1—V2^v	115.43 (5)	O4—V1—Ca1^xii	130.08 (6)
V1—Ca1—V2^v	64.70 (2)	V2^iii—V1—Ca1^xii	107.324 (17)
O2^i—Ca1—V2^vi	79.18 (6)	V2—V1—Ca1^xii	107.324 (17)
O2^ii—Ca1—V2^vi	165.37 (6)	Ca1—V1—Ca1^xii	164.20 (3)
O4—Ca1—V2^vi	88.48 (6)	Ca1^x—V1—Ca1^xii	93.44 (3)
O4^iii—Ca1—V2^vi	34.88 (5)	O1—V1—Ca1^xiii	48.40 (10)
O3—Ca1—V2^vi	88.01 (6)	O3^x—V1—Ca1^xiii	134.76 (6)
O3^iii—Ca1—V2^vi	35.14 (5)	O3^xi—V1—Ca1^xiii	134.76 (6)
O1^iv—Ca1—V2^vi	115.43 (5)	O4^iii—V1—Ca1^xiii	76.37 (6)
V1—Ca1—V2^vi	64.70 (2)	O4—V1—Ca1^xiii	76.37 (6)
V2^v—Ca1—V2^vi	90.04 (4)	V2^iii—V1—Ca1^xiii	103.712 (17)
O2^i—Ca1—V1^vii	103.21 (6)	V2—V1—Ca1^xiii	103.712 (17)
O2^ii—Ca1—V1^vii	103.21 (6)	Ca1—V1—Ca1^xiii	83.84 (3)
O4—Ca1—V1^vii	92.65 (6)	Ca1^x—V1—Ca1^xiii	173.79 (3)
O4^iii—Ca1—V1^vii	92.65 (6)	Ca1^xii—V1—Ca1^xiii	80.35 (3)
O3—Ca1—V1^vii	34.07 (5)	O1—V1—Ca1^xiv	75.699 (14)
O3^iii—Ca1—V1^vii	34.07 (5)	O3^x—V1—Ca1^xiv	54.60 (6)
O1^iv—Ca1—V1^vii	176.97 (8)	O3^xi—V1—Ca1^xiv	138.55 (6)
V1—Ca1—V1^vii	102.37 (4)	O4^iii—V1—Ca1^xiv	138.23 (6)
V2^v—Ca1—V1^vii	62.71 (2)	O4—V1—Ca1^xiv	54.95 (6)
V2^vi—Ca1—V1^vii	62.71 (2)	V2^iii—V1—Ca1^xiv	173.62 (3)
O2^i—Ca1—O1^viii	68.38 (6)	V2—V1—Ca1^xiv	34.98 (2)
O2^ii—Ca1—O1^viii	68.38 (6)	Ca1—V1—Ca1^xiv	99.314 (15)
O4—Ca1—O1^viii	139.24 (6)	Ca1^x—V1—Ca1^xiv	98.495 (15)
O4^iii—Ca1—O1^viii	139.24 (6)	Ca1^xii—V1—Ca1^xiv	78.078 (13)
O3—Ca1—O1^viii	72.61 (7)	Ca1^xiii—V1—Ca1^xiv	80.312 (13)
O3^iii—Ca1—O1^viii	72.61 (7)	O2—V2—O4^xiv	108.74 (10)
O1^iv—Ca1—O1^viii	120.02 (11)	O2—V2—O3^xiv	105.97 (10)
V1—Ca1—O1^viii	165.38 (6)	O4^xiv—V2—O3^xiv	89.58 (9)
V2^v—Ca1—O1^viii	105.75 (4)	O2—V2—O4	112.45 (10)
V2^vi—Ca1—O1^viii	105.75 (4)	O4^xiv—V2—O4	138.76 (5)
V1^vii—Ca1—O1^viii	63.02 (6)	O3^xiv—V2—O4	81.31 (9)
O2^i—Ca1—V2^i	15.69 (6)	O2—V2—O3^x	114.75 (11)
O2^ii—Ca1—V2^i	94.55 (7)	O4^xiv—V2—O3^x	81.18 (9)
O4—Ca1—V2^i	153.35 (6)	O3^xiv—V2—O3^x	139.11 (4)
O4^iii—Ca1—V2^i	100.24 (5)	O4—V2—O3^x	80.05 (8)
O3—Ca1—V2^i	136.56 (6)	O2—V2—V2^xiv	120.59 (7)
O3^iii—Ca1—V2^i	91.14 (5)	O4^xiv—V2—V2^xiv	40.55 (6)
O1^iv—Ca1—V2^i	69.86 (5)	O3^xiv—V2—V2^xiv	118.42 (7)
V1—Ca1—V2^i	124.93 (2)	O4—V2—V2^xiv	111.53 (7)
V2^v—Ca1—V2^i	170.36 (3)	O3^x—V2—V2^xiv	40.67 (6)
V2^vi—Ca1—V2^i	94.78 (2)	O2—V2—V2^v	114.24 (7)
V1^vii—Ca1—V2^i	112.35 (2)	O4^xiv—V2—V2^v	120.58 (7)
O1^viii—Ca1—V2^i	64.90 (4)	O3^xiv—V2—V2^v	40.86 (6)
O2^i—Ca1—V2^ii	94.55 (7)	O4—V2—V2^v	40.49 (6)
O2^ii—Ca1—V2^ii	15.69 (6)	O3^x—V2—V2^v	113.38 (7)
O4—Ca1—V2^ii	100.24 (5)	V2^xiv—V2—V2^v	125.17 (4)
O4^iii—Ca1—V2^ii	153.35 (6)	O2—V2—V1	127.69 (10)
O3—Ca1—V2^ii	91.14 (5)	O4^xiv—V2—V1	108.86 (6)
O3^iii—Ca1—V2^ii	136.56 (6)	O3^xiv—V2—V1	109.32 (6)
O1^iv—Ca1—V2^ii	69.86 (5)	O4—V2—V1	40.55 (6)
V1—Ca1—V2^ii	124.93 (2)	O3^x—V2—V1	40.29 (6)
V2^v—Ca1—V2^ii	94.78 (2)	V2^xiv—V2—V1	72.53 (3)
V2^vi—Ca1—V2^ii	170.36 (3)	V2^v—V2—V1	74.13 (3)
V1^vii—Ca1—V2^ii	112.35 (2)	O2—V2—Ca1^xiv	117.96 (10)
O1^viii—Ca1—V2^ii	64.90 (4)	O4^xiv—V2—Ca1^xiv	44.32 (6)
V2^i—Ca1—V2^ii	79.28 (3)	O3^xiv—V2—Ca1^xiv	45.43 (6)
O2^i—Ca1—V1^iv	68.24 (6)	O4—V2—Ca1^xiv	113.22 (7)
O2^ii—Ca1—V1^iv	68.24 (6)	O3^x—V2—Ca1^xiv	112.54 (7)
O4—Ca1—V1^iv	101.08 (6)	V2^xiv—V2—Ca1^xiv	76.60 (3)
O4^iii—Ca1—V1^iv	101.08 (6)	V2^v—V2—Ca1^xiv	79.20 (3)
O3—Ca1—V1^iv	144.93 (5)	V1—V2—Ca1^xiv	114.34 (3)
O3^iii—Ca1—V1^iv	144.93 (5)	O2—V2—Ca1^ii	23.13 (9)
O1^iv—Ca1—V1^iv	19.66 (7)	O4^xiv—V2—Ca1^ii	95.42 (6)
V1—Ca1—V1^iv	94.26 (3)	O3^xiv—V2—Ca1^ii	87.40 (6)
V2^v—Ca1—V1^iv	126.39 (2)	O4—V2—Ca1^ii	123.96 (6)
V2^vi—Ca1—V1^iv	126.39 (2)	O3^x—V2—Ca1^ii	132.91 (6)
V1^vii—Ca1—V1^iv	163.37 (3)	V2^xiv—V2—Ca1^ii	121.89 (3)
O1^viii—Ca1—V1^iv	100.35 (6)	V2^v—V2—Ca1^ii	108.60 (3)
V2^i—Ca1—V1^iv	56.22 (2)	V1—V2—Ca1^ii	150.13 (3)
V2^ii—Ca1—V1^iv	56.22 (2)	Ca1^xiv—V2—Ca1^ii	95.12 (2)
O2^i—Ca1—V2	145.99 (6)	O2—V2—Ca1	84.98 (9)
O2^ii—Ca1—V2	70.65 (6)	O4^xiv—V2—Ca1	164.64 (7)
O4—Ca1—V2	22.54 (5)	O3^xiv—V2—Ca1	93.27 (6)
O4^iii—Ca1—V2	82.74 (5)	O4—V2—Ca1	27.90 (6)
O3—Ca1—V2	80.52 (5)	O3^x—V2—Ca1	86.85 (7)
O3^iii—Ca1—V2	128.43 (6)	V2^xiv—V2—Ca1	126.52 (3)
O1^iv—Ca1—V2	68.15 (5)	V2^v—V2—Ca1	56.10 (2)
V1—Ca1—V2	47.561 (15)	V1—V2—Ca1	56.02 (2)
V2^v—Ca1—V2	47.305 (14)	Ca1^xiv—V2—Ca1	135.28 (3)
V2^vi—Ca1—V2	109.07 (3)	Ca1^ii—V2—Ca1	99.78 (2)
V1^vii—Ca1—V2	109.88 (3)	O2—V2—Ca1^x	89.27 (9)
O1^viii—Ca1—V2	134.708 (15)	O4^xiv—V2—Ca1^x	90.33 (6)
V2^i—Ca1—V2	137.43 (3)	O3^xiv—V2—Ca1^x	163.93 (7)
V2^ii—Ca1—V2	80.22 (2)	O4—V2—Ca1^x	88.22 (6)
V1^iv—Ca1—V2	81.40 (2)	O3^x—V2—Ca1^x	25.52 (6)
O2^i—Ca1—V2^iii	70.65 (6)	V2^xiv—V2—Ca1^x	54.60 (2)
O2^ii—Ca1—V2^iii	145.99 (6)	V2^v—V2—Ca1^x	127.99 (3)
O4—Ca1—V2^iii	82.74 (5)	V1—V2—Ca1^x	55.72 (2)
O4^iii—Ca1—V2^iii	22.54 (5)	Ca1^xiv—V2—Ca1^x	131.18 (2)
O3—Ca1—V2^iii	128.43 (6)	Ca1^ii—V2—Ca1^x	108.60 (2)
O3^iii—Ca1—V2^iii	80.52 (5)	Ca1—V2—Ca1^x	82.79 (2)
O1^iv—Ca1—V2^iii	68.15 (5)	V1—O1—Ca1^xii	128.39 (15)
V1—Ca1—V2^iii	47.561 (16)	V1—O1—Ca1^xiii	111.60 (13)
V2^v—Ca1—V2^iii	109.07 (3)	Ca1^xii—O1—Ca1^xiii	120.02 (11)
V2^vi—Ca1—V2^iii	47.305 (15)	V1—O1—Ca1^x	37.79 (8)
V1^vii—Ca1—V2^iii	109.88 (3)	Ca1^xii—O1—Ca1^x	90.60 (8)
O1^viii—Ca1—V2^iii	134.708 (15)	Ca1^xiii—O1—Ca1^x	149.38 (9)
V2^i—Ca1—V2^iii	80.22 (2)	V1—O1—Ca1	32.70 (8)
V2^ii—Ca1—V2^iii	137.43 (3)	Ca1^xii—O1—Ca1	161.09 (11)
V1^iv—Ca1—V2^iii	81.40 (2)	Ca1^xiii—O1—Ca1	78.90 (6)
V2—Ca1—V2^iii	90.52 (3)	Ca1^x—O1—Ca1	70.49 (5)
O2^i—Ca1—V2^ix	58.81 (5)	V2—O2—Ca1^ii	141.19 (14)
O2^ii—Ca1—V2^ix	127.62 (6)	V2—O2—Ca1	72.16 (8)
O4—Ca1—V2^ix	126.44 (6)	Ca1^ii—O2—Ca1	128.35 (7)
O4^iii—Ca1—V2^ix	79.56 (5)	V2—O2—Ca1^x	68.99 (8)
O3—Ca1—V2^ix	80.08 (6)	Ca1^ii—O2—Ca1^x	140.56 (7)
O3^iii—Ca1—V2^ix	20.45 (5)	Ca1—O2—Ca1^x	77.25 (5)
O1^iv—Ca1—V2^ix	134.57 (3)	V2—O2—Ca1^xiv	43.00 (7)
V1—Ca1—V2^ix	110.75 (3)	Ca1^ii—O2—Ca1^xiv	98.54 (8)
V2^v—Ca1—V2^ix	106.57 (3)	Ca1—O2—Ca1^xiv	105.66 (5)
V2^vi—Ca1—V2^ix	46.202 (15)	Ca1^x—O2—Ca1^xiv	102.01 (5)
V1^vii—Ca1—V2^ix	46.248 (15)	V1^vii—O3—V2^v	128.41 (11)
O1^viii—Ca1—V2^ix	59.88 (4)	V1^vii—O3—V2^vii	99.19 (9)
V2^i—Ca1—V2^ix	71.40 (2)	V2^v—O3—V2^vii	98.48 (9)
V2^ii—Ca1—V2^ix	124.22 (3)	V1^vii—O3—Ca1	101.98 (9)
V1^iv—Ca1—V2^ix	127.03 (2)	V2^v—O3—Ca1	99.44 (8)
V2—Ca1—V2^ix	148.87 (3)	V2^vii—O3—Ca1	134.02 (10)
V2^iii—Ca1—V2^ix	82.79 (2)	V1^vii—O3—Ca1^xiii	65.41 (6)
O2^i—Ca1—V2^vii	127.62 (6)	V2^v—O3—Ca1^xiii	64.30 (6)
O2^ii—Ca1—V2^vii	58.81 (5)	V2^vii—O3—Ca1^xiii	123.07 (8)
O4—Ca1—V2^vii	79.56 (5)	Ca1—O3—Ca1^xiii	102.85 (6)
O4^iii—Ca1—V2^vii	126.44 (6)	V1^vii—O3—Ca1^vii	48.93 (5)
O3—Ca1—V2^vii	20.45 (5)	V2^v—O3—Ca1^vii	160.78 (9)
O3^iii—Ca1—V2^vii	80.08 (6)	V2^vii—O3—Ca1^vii	65.99 (6)
O1^iv—Ca1—V2^vii	134.57 (3)	Ca1—O3—Ca1^vii	99.61 (7)
V1—Ca1—V2^vii	110.75 (3)	Ca1^xiii—O3—Ca1^vii	113.52 (5)
V2^v—Ca1—V2^vii	46.202 (15)	V1^vii—O3—Ca1^v	104.61 (7)
V2^vi—Ca1—V2^vii	106.57 (3)	V2^v—O3—Ca1^v	60.94 (6)
V1^vii—Ca1—V2^vii	46.248 (15)	V2^vii—O3—Ca1^v	43.63 (5)
O1^viii—Ca1—V2^vii	59.88 (4)	Ca1—O3—Ca1^v	153.22 (7)
V2^i—Ca1—V2^vii	124.22 (3)	Ca1^xiii—O3—Ca1^v	85.49 (4)
V2^ii—Ca1—V2^vii	71.40 (2)	Ca1^vii—O3—Ca1^v	100.18 (4)
V1^iv—Ca1—V2^vii	127.03 (2)	V2^v—O4—V2	98.95 (10)
V2—Ca1—V2^vii	82.79 (2)	V2^v—O4—V1	132.72 (11)
V2^iii—Ca1—V2^vii	148.87 (3)	V2—O4—V1	99.17 (9)
V2^ix—Ca1—V2^vii	87.39 (3)	V2^v—O4—Ca1	100.80 (8)
O2^i—Ca1—O2	132.42 (4)	V2—O4—Ca1	129.56 (10)
O2^ii—Ca1—O2	51.65 (7)	V1—O4—Ca1	100.40 (9)
O4—Ca1—O2	45.23 (6)	V2^v—O4—Ca1^xiii	58.11 (5)
O4^iii—Ca1—O2	100.69 (6)	V2—O4—Ca1^xiii	132.36 (8)
O3—Ca1—O2	89.05 (6)	V1—O4—Ca1^xiii	77.66 (6)
O3^iii—Ca1—O2	149.44 (7)	Ca1—O4—Ca1^xiii	97.18 (6)
O1^iv—Ca1—O2	56.39 (4)	V2^v—O4—Ca1^x	161.87 (9)
V1—Ca1—O2	66.88 (3)	V2—O4—Ca1^x	65.64 (6)
V2^v—Ca1—O2	62.21 (3)	V1—O4—Ca1^x	47.06 (5)
V2^vi—Ca1—O2	130.95 (4)	Ca1—O4—Ca1^x	96.64 (6)
V1^vii—Ca1—O2	122.64 (4)	Ca1^xiii—O4—Ca1^x	124.56 (5)
O1^viii—Ca1—O2	119.84 (4)	V2^v—O4—Ca1^xiv	63.95 (6)
V2^i—Ca1—O2	119.38 (4)	V2—O4—Ca1^xiv	43.25 (5)
V2^ii—Ca1—O2	58.60 (3)	V1—O4—Ca1^xiv	104.10 (7)
V1^iv—Ca1—O2	64.18 (4)	Ca1—O4—Ca1^xiv	155.35 (7)
V2—Ca1—O2	22.86 (3)	Ca1^xiii—O4—Ca1^xiv	90.74 (4)
V2^iii—Ca1—O2	101.82 (4)	Ca1^x—O4—Ca1^xiv	97.97 (4)
V2^ix—Ca1—O2	168.69 (4)	V2^v—O4—Ca1^ii	90.33 (7)
V2^vii—Ca1—O2	83.40 (4)	V2—O4—Ca1^ii	37.42 (5)
O1—V1—O3^x	109.25 (10)	V1—O4—Ca1^ii	128.24 (8)
O1—V1—O3^xi	109.25 (10)	Ca1—O4—Ca1^ii	96.60 (6)
O3^x—V1—O3^xi	86.58 (12)	Ca1^xiii—O4—Ca1^ii	147.41 (5)
O1—V1—O4^iii	111.21 (10)	Ca1^x—O4—Ca1^ii	82.75 (3)
O3^x—V1—O4^iii	139.54 (10)	Ca1^xiv—O4—Ca1^ii	65.83 (3)
O3^xi—V1—O4^iii	80.02 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.537 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2671 reflections
a = 10.436 (3) Å	θ = 1.3–23.4°
b = 10.368 (2) Å	µ = 5.67 mm^−1
c = 5.2911 (15) Å	T = 237 K
V = 572.5 (2) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	404 independent reflections
Radiation source: fine-focus sealed tube	367 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.471	l = −5→5
2415 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0477P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.054	(Δ/σ)max < 0.001
S = 0.90	Δρmax = 0.33 e Å^−3
404 reflections	Δρmin = −0.36 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0185 (15)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08481 (9)	0.2500	0.29989 (14)	0.0069 (3)
V1	0.28872 (7)	0.2500	0.79216 (13)	0.0052 (3)
V2	0.18744 (5)	0.52030 (5)	0.78363 (9)	0.0053 (3)
O1	0.4435 (3)	0.2500	0.8077 (5)	0.0113 (8)*
O2	0.0400 (2)	0.5653 (2)	0.7667 (4)	0.0125 (6)*
O3	0.22015 (19)	0.3798 (2)	0.0258 (4)	0.0066 (5)*
O4	0.22661 (19)	0.3795 (2)	0.5483 (4)	0.0065 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0046 (5)	0.0071 (6)	0.0089 (5)	0.000	0.0000 (3)	0.000
V1	0.0047 (5)	0.0050 (5)	0.0061 (5)	0.000	−0.0004 (3)	0.000
V2	0.0051 (4)	0.0050 (4)	0.0059 (4)	0.0008 (2)	0.0001 (2)	0.00021 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.343 (3)	V1—Ca1^xiii	4.4001 (14)
Ca1—O2^ii	2.343 (3)	V1—Ca1^xiv	5.3497 (11)
Ca1—O4	2.392 (2)	V2—O2	1.610 (2)
Ca1—O4^iii	2.392 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3^iii	2.431 (2)	V2—O4	1.962 (2)
Ca1—O3	2.431 (2)	V2—O3^xiv	1.966 (2)
Ca1—O1^iv	2.547 (3)	V2—O3^x	1.970 (2)
Ca1—V1	3.3634 (12)	V2—V2^xiv	2.9801 (9)
Ca1—V2^v	3.3658 (11)	V2—V2^v	2.9801 (9)
Ca1—V2^vi	3.3658 (11)	V2—Ca1^xiv	3.3658 (11)
Ca1—V1^vii	3.4271 (13)	V2—Ca1^ii	3.7337 (11)
Ca1—O1^viii	3.537 (3)	V2—Ca1^x	4.0574 (10)
Ca1—V2^i	3.7337 (11)	O1—Ca1^xii	2.547 (3)
Ca1—V2^ii	3.7337 (11)	O1—Ca1^xiii	3.537 (3)
Ca1—V1^iv	3.7693 (14)	O1—Ca1^x	4.560 (3)
Ca1—V2	3.9437 (10)	O2—Ca1^ii	2.343 (3)
Ca1—V2^iii	3.9437 (10)	O2—Ca1^x	4.343 (2)
Ca1—V2^ix	4.0574 (10)	O2—Ca1^xiv	4.362 (3)
Ca1—V2^vii	4.0574 (10)	O3—V1^vii	1.962 (2)
Ca1—O2	4.124 (2)	O3—V2^v	1.966 (2)
V1—O1	1.617 (3)	O3—V2^vii	1.970 (2)
V1—O3^x	1.962 (2)	O3—Ca1^xiii	4.141 (2)
V1—O3^xi	1.962 (2)	O3—Ca1^vii	4.308 (2)
V1—O4^iii	1.972 (2)	O3—Ca1^v	4.506 (2)
V1—O4	1.972 (2)	O4—V2^v	1.960 (2)
V1—V2^iii	2.9956 (8)	O4—Ca1^xiii	4.379 (2)
V1—V2	2.9956 (8)	O4—Ca1^x	4.451 (2)
V1—Ca1^x	3.4271 (13)	O4—Ca1^xiv	4.516 (2)
V1—Ca1^xii	3.7693 (14)	O4—Ca1^ii	5.095 (2)
O2^i—Ca1—O2^ii	109.66 (12)	O1—V1—O4	111.20 (9)
O2^i—Ca1—O4	152.33 (8)	O3^x—V1—O4	79.94 (8)
O2^ii—Ca1—O4	88.14 (7)	O3^xi—V1—O4	139.41 (10)
O2^i—Ca1—O4^iii	88.14 (7)	O4^iii—V1—O4	85.85 (12)
O2^ii—Ca1—O4^iii	152.33 (8)	O1—V1—V2^iii	110.680 (18)
O4—Ca1—O4^iii	68.33 (10)	O3^x—V1—V2^iii	121.50 (7)
O2^i—Ca1—O3^iii	77.34 (7)	O3^xi—V1—V2^iii	40.47 (6)
O2^ii—Ca1—O3^iii	133.31 (7)	O4^iii—V1—V2^iii	40.27 (6)
O4—Ca1—O3^iii	106.22 (8)	O4—V1—V2^iii	120.75 (7)
O4^iii—Ca1—O3^iii	69.97 (7)	O1—V1—V2	110.680 (18)
O2^i—Ca1—O3	133.31 (7)	O3^x—V1—V2	40.47 (6)
O2^ii—Ca1—O3	77.34 (7)	O3^xi—V1—V2	121.50 (7)
O4—Ca1—O3	69.97 (7)	O4^iii—V1—V2	120.75 (7)
O4^iii—Ca1—O3	106.22 (8)	O4—V1—V2	40.27 (6)
O3^iii—Ca1—O3	67.23 (10)	V2^iii—V1—V2	138.64 (4)
O2^i—Ca1—O1^iv	78.49 (7)	O1—V1—Ca1	132.17 (10)
O2^ii—Ca1—O1^iv	78.49 (7)	O3^x—V1—Ca1	104.90 (6)
O4—Ca1—O1^iv	84.86 (8)	O3^xi—V1—Ca1	104.90 (6)
O4^iii—Ca1—O1^iv	84.86 (8)	O4^iii—V1—Ca1	44.38 (6)
O3^iii—Ca1—O1^iv	145.37 (5)	O4—V1—Ca1	44.38 (6)
O3—Ca1—O1^iv	145.37 (5)	V2^iii—V1—Ca1	76.414 (17)
O2^i—Ca1—V1	117.92 (6)	V2—V1—Ca1	76.414 (17)
O2^ii—Ca1—V1	117.92 (6)	O1—V1—Ca1^x	125.46 (10)
O4—Ca1—V1	35.22 (5)	O3^x—V1—Ca1^x	43.93 (6)
O4^iii—Ca1—V1	35.22 (5)	O3^xi—V1—Ca1^x	43.93 (6)
O3^iii—Ca1—V1	95.42 (6)	O4^iii—V1—Ca1^x	107.99 (6)
O3—Ca1—V1	95.42 (6)	O4—V1—Ca1^x	107.99 (6)
O1^iv—Ca1—V1	74.64 (7)	V2^iii—V1—Ca1^x	78.037 (17)
O2^i—Ca1—V2^v	165.29 (6)	V2—V1—Ca1^x	78.037 (17)
O2^ii—Ca1—V2^v	79.07 (6)	Ca1—V1—Ca1^x	102.37 (4)
O4—Ca1—V2^v	34.90 (5)	O1—V1—Ca1^xii	32.01 (10)
O4^iii—Ca1—V2^v	88.54 (6)	O3^x—V1—Ca1^xii	86.46 (6)
O3^iii—Ca1—V2^v	88.06 (6)	O3^xi—V1—Ca1^xii	86.46 (6)
O3—Ca1—V2^v	35.19 (5)	O4^iii—V1—Ca1^xii	130.10 (6)
O1^iv—Ca1—V2^v	115.46 (5)	O4—V1—Ca1^xii	130.10 (6)
V1—Ca1—V2^v	64.72 (2)	V2^iii—V1—Ca1^xii	107.330 (17)
O2^i—Ca1—V2^vi	79.07 (6)	V2—V1—Ca1^xii	107.330 (17)
O2^ii—Ca1—V2^vi	165.29 (6)	Ca1—V1—Ca1^xii	164.18 (3)
O4—Ca1—V2^vi	88.54 (6)	Ca1^x—V1—Ca1^xii	93.45 (3)
O4^iii—Ca1—V2^vi	34.90 (5)	O1—V1—Ca1^xiii	48.32 (10)
O3^iii—Ca1—V2^vi	35.19 (5)	O3^x—V1—Ca1^xiii	134.79 (6)
O3—Ca1—V2^vi	88.06 (6)	O3^xi—V1—Ca1^xiii	134.79 (6)
O1^iv—Ca1—V2^vi	115.46 (5)	O4^iii—V1—Ca1^xiii	76.41 (6)
V1—Ca1—V2^vi	64.72 (2)	O4—V1—Ca1^xiii	76.41 (6)
V2^v—Ca1—V2^vi	90.08 (3)	V2^iii—V1—Ca1^xiii	103.713 (17)
O2^i—Ca1—V1^vii	103.15 (5)	V2—V1—Ca1^xiii	103.713 (17)
O2^ii—Ca1—V1^vii	103.15 (5)	Ca1—V1—Ca1^xiii	83.86 (3)
O4—Ca1—V1^vii	92.67 (6)	Ca1^x—V1—Ca1^xiii	173.77 (3)
O4^iii—Ca1—V1^vii	92.67 (6)	Ca1^xii—V1—Ca1^xiii	80.33 (3)
O3^iii—Ca1—V1^vii	34.06 (5)	O1—V1—Ca1^xiv	75.714 (13)
O3—Ca1—V1^vii	34.06 (5)	O3^x—V1—Ca1^xiv	54.59 (6)
O1^iv—Ca1—V1^vii	177.01 (8)	O3^xi—V1—Ca1^xiv	138.57 (6)
V1—Ca1—V1^vii	102.37 (4)	O4^iii—V1—Ca1^xiv	138.25 (6)
V2^v—Ca1—V1^vii	62.71 (2)	O4—V1—Ca1^xiv	54.98 (6)
V2^vi—Ca1—V1^vii	62.71 (2)	V2^iii—V1—Ca1^xiv	173.61 (2)
O2^i—Ca1—O1^viii	68.38 (6)	V2—V1—Ca1^xiv	34.970 (19)
O2^ii—Ca1—O1^viii	68.38 (6)	Ca1—V1—Ca1^xiv	99.323 (14)
O4—Ca1—O1^viii	139.23 (6)	Ca1^x—V1—Ca1^xiv	98.464 (14)
O4^iii—Ca1—O1^viii	139.23 (6)	Ca1^xii—V1—Ca1^xiv	78.076 (13)
O3^iii—Ca1—O1^viii	72.54 (6)	Ca1^xiii—V1—Ca1^xiv	80.340 (13)
O3—Ca1—O1^viii	72.54 (6)	O2—V2—O4^xiv	108.87 (10)
O1^iv—Ca1—O1^viii	119.96 (11)	O2—V2—O4	112.29 (10)
V1—Ca1—O1^viii	165.40 (6)	O4^xiv—V2—O4	138.78 (5)
V2^v—Ca1—O1^viii	105.74 (4)	O2—V2—O3^xiv	106.10 (10)
V2^vi—Ca1—O1^viii	105.74 (4)	O4^xiv—V2—O3^xiv	89.55 (9)
V1^vii—Ca1—O1^viii	63.03 (6)	O4—V2—O3^xiv	81.32 (9)
O2^i—Ca1—V2^i	15.77 (6)	O2—V2—O3^x	114.59 (10)
O2^ii—Ca1—V2^i	94.62 (7)	O4^xiv—V2—O3^x	81.25 (9)
O4—Ca1—V2^i	153.39 (5)	O4—V2—O3^x	80.02 (8)
O4^iii—Ca1—V2^i	100.23 (5)	O3^xiv—V2—O3^x	139.12 (4)
O3^iii—Ca1—V2^i	91.05 (5)	O2—V2—V2^xiv	120.60 (7)
O3—Ca1—V2^i	136.44 (6)	O4^xiv—V2—V2^xiv	40.56 (6)
O1^iv—Ca1—V2^i	69.86 (5)	O4—V2—V2^xiv	111.54 (6)
V1—Ca1—V2^i	124.97 (2)	O3^xiv—V2—V2^xiv	118.40 (7)
V2^v—Ca1—V2^i	170.30 (2)	O3^x—V2—V2^xiv	40.73 (6)
V2^vi—Ca1—V2^i	94.76 (2)	O2—V2—V2^v	114.21 (7)
V1^vii—Ca1—V2^i	112.32 (2)	O4^xiv—V2—V2^v	120.56 (7)
O1^viii—Ca1—V2^i	64.86 (4)	O4—V2—V2^v	40.54 (6)
O2^i—Ca1—V2^ii	94.62 (7)	O3^xiv—V2—V2^v	40.83 (6)
O2^ii—Ca1—V2^ii	15.77 (6)	O3^x—V2—V2^v	113.39 (7)
O4—Ca1—V2^ii	100.23 (5)	V2^xiv—V2—V2^v	125.18 (4)
O4^iii—Ca1—V2^ii	153.39 (5)	O2—V2—V1	127.52 (9)
O3^iii—Ca1—V2^ii	136.44 (6)	O4^xiv—V2—V1	108.87 (6)
O3—Ca1—V2^ii	91.05 (5)	O4—V2—V1	40.53 (6)
O1^iv—Ca1—V2^ii	69.86 (5)	O3^xiv—V2—V1	109.29 (6)
V1—Ca1—V2^ii	124.97 (2)	O3^x—V2—V1	40.29 (6)
V2^v—Ca1—V2^ii	94.76 (2)	V2^xiv—V2—V1	72.54 (2)
V2^vi—Ca1—V2^ii	170.30 (2)	V2^v—V2—V1	74.14 (3)
V1^vii—Ca1—V2^ii	112.32 (2)	O2—V2—Ca1^xiv	118.11 (9)
O1^viii—Ca1—V2^ii	64.86 (4)	O4^xiv—V2—Ca1^xiv	44.26 (6)
V2^i—Ca1—V2^ii	79.27 (3)	O4—V2—Ca1^xiv	113.30 (6)
O2^i—Ca1—V1^iv	68.30 (6)	O3^xiv—V2—Ca1^xiv	45.45 (6)
O2^ii—Ca1—V1^iv	68.30 (6)	O3^x—V2—Ca1^xiv	112.60 (7)
O4—Ca1—V1^iv	101.10 (5)	V2^xiv—V2—Ca1^xiv	76.58 (3)
O4^iii—Ca1—V1^iv	101.10 (5)	V2^v—V2—Ca1^xiv	79.24 (3)
O3^iii—Ca1—V1^iv	144.88 (5)	V1—V2—Ca1^xiv	114.36 (3)
O3—Ca1—V1^iv	144.88 (5)	O2—V2—Ca1^ii	23.29 (9)
O1^iv—Ca1—V1^iv	19.67 (7)	O4^xiv—V2—Ca1^ii	95.44 (6)
V1—Ca1—V1^iv	94.31 (3)	O4—V2—Ca1^ii	123.92 (6)
V2^v—Ca1—V1^iv	126.408 (19)	O3^xiv—V2—Ca1^ii	87.43 (6)
V2^vi—Ca1—V1^iv	126.408 (19)	O3^x—V2—Ca1^ii	132.89 (6)
V1^vii—Ca1—V1^iv	163.32 (3)	V2^xiv—V2—Ca1^ii	121.91 (3)
O1^viii—Ca1—V1^iv	100.29 (6)	V2^v—V2—Ca1^ii	108.57 (3)
V2^i—Ca1—V1^iv	56.22 (2)	V1—V2—Ca1^ii	150.12 (3)
V2^ii—Ca1—V1^iv	56.22 (2)	Ca1^xiv—V2—Ca1^ii	95.11 (2)
O2^i—Ca1—V2	146.05 (6)	O2—V2—Ca1	84.85 (8)
O2^ii—Ca1—V2	70.59 (6)	O4^xiv—V2—Ca1	164.63 (6)
O4—Ca1—V2	22.53 (5)	O4—V2—Ca1	27.85 (6)
O4^iii—Ca1—V2	82.79 (5)	O3^xiv—V2—Ca1	93.28 (6)
O3^iii—Ca1—V2	128.53 (6)	O3^x—V2—Ca1	86.77 (6)
O3—Ca1—V2	80.56 (5)	V2^xiv—V2—Ca1	126.50 (3)
O1^iv—Ca1—V2	68.17 (5)	V2^v—V2—Ca1	56.11 (2)
V1—Ca1—V2	47.590 (15)	V1—V2—Ca1	56.00 (2)
V2^v—Ca1—V2	47.309 (14)	Ca1^xiv—V2—Ca1	135.33 (2)
V2^vi—Ca1—V2	109.13 (3)	Ca1^ii—V2—Ca1	99.777 (19)
V1^vii—Ca1—V2	109.88 (3)	O2—V2—Ca1^x	89.17 (8)
O1^viii—Ca1—V2	134.680 (15)	O4^xiv—V2—Ca1^x	90.33 (6)
V2^i—Ca1—V2	137.46 (2)	O4—V2—Ca1^x	88.20 (6)
V2^ii—Ca1—V2	80.223 (19)	O3^xiv—V2—Ca1^x	163.88 (6)
V1^iv—Ca1—V2	81.43 (2)	O3^x—V2—Ca1^x	25.45 (6)
O2^i—Ca1—V2^iii	70.59 (6)	V2^xiv—V2—Ca1^x	54.58 (2)
O2^ii—Ca1—V2^iii	146.05 (6)	V2^v—V2—Ca1^x	128.01 (3)
O4—Ca1—V2^iii	82.79 (5)	V1—V2—Ca1^x	55.72 (2)
O4^iii—Ca1—V2^iii	22.53 (5)	Ca1^xiv—V2—Ca1^x	131.14 (2)
O3^iii—Ca1—V2^iii	80.56 (5)	Ca1^ii—V2—Ca1^x	108.63 (2)
O3—Ca1—V2^iii	128.53 (6)	Ca1—V2—Ca1^x	82.78 (2)
O1^iv—Ca1—V2^iii	68.17 (5)	V1—O1—Ca1^xii	128.32 (15)
V1—Ca1—V2^iii	47.590 (15)	V1—O1—Ca1^xiii	111.72 (13)
V2^v—Ca1—V2^iii	109.13 (3)	Ca1^xii—O1—Ca1^xiii	119.96 (11)
V2^vi—Ca1—V2^iii	47.309 (14)	V1—O1—Ca1^x	37.75 (8)
V1^vii—Ca1—V2^iii	109.88 (3)	Ca1^xii—O1—Ca1^x	90.57 (8)
O1^viii—Ca1—V2^iii	134.680 (15)	Ca1^xiii—O1—Ca1^x	149.47 (9)
V2^i—Ca1—V2^iii	80.223 (19)	V1—O1—Ca1	32.75 (8)
V2^ii—Ca1—V2^iii	137.46 (2)	Ca1^xii—O1—Ca1	161.07 (10)
V1^iv—Ca1—V2^iii	81.43 (2)	Ca1^xiii—O1—Ca1	78.97 (6)
V2—Ca1—V2^iii	90.57 (3)	Ca1^x—O1—Ca1	70.50 (5)
O2^i—Ca1—V2^ix	58.73 (5)	V2—O2—Ca1^ii	140.94 (14)
O2^ii—Ca1—V2^ix	127.60 (6)	V2—O2—Ca1	72.26 (8)
O4—Ca1—V2^ix	126.47 (6)	Ca1^ii—O2—Ca1	128.39 (7)
O4^iii—Ca1—V2^ix	79.56 (5)	V2—O2—Ca1^x	69.07 (8)
O3^iii—Ca1—V2^ix	20.38 (5)	Ca1^ii—O2—Ca1^x	140.60 (7)
O3—Ca1—V2^ix	80.06 (5)	Ca1—O2—Ca1^x	77.30 (5)
O1^iv—Ca1—V2^ix	134.56 (2)	V2—O2—Ca1^xiv	42.89 (7)
V1—Ca1—V2^ix	110.75 (3)	Ca1^ii—O2—Ca1^xiv	98.41 (7)
V2^v—Ca1—V2^ix	106.57 (3)	Ca1—O2—Ca1^xiv	105.69 (5)
V2^vi—Ca1—V2^ix	46.183 (14)	Ca1^x—O2—Ca1^xiv	101.98 (5)
V1^vii—Ca1—V2^ix	46.241 (15)	V1^vii—O3—V2^v	128.29 (11)
O1^viii—Ca1—V2^ix	59.88 (3)	V1^vii—O3—V2^vii	99.24 (9)
V2^i—Ca1—V2^ix	71.37 (2)	V2^v—O3—V2^vii	98.44 (9)
V2^ii—Ca1—V2^ix	124.18 (2)	V1^vii—O3—Ca1	102.00 (9)
V1^iv—Ca1—V2^ix	127.01 (2)	V2^v—O3—Ca1	99.36 (8)
V2—Ca1—V2^ix	148.88 (3)	V2^vii—O3—Ca1	134.17 (10)
V2^iii—Ca1—V2^ix	82.78 (2)	V1^vii—O3—Ca1^xiii	65.31 (6)
O2^i—Ca1—V2^vii	127.60 (6)	V2^v—O3—Ca1^xiii	64.26 (6)
O2^ii—Ca1—V2^vii	58.73 (5)	V2^vii—O3—Ca1^xiii	122.99 (8)
O4—Ca1—V2^vii	79.56 (5)	Ca1—O3—Ca1^xiii	102.78 (6)
O4^iii—Ca1—V2^vii	126.47 (6)	V1^vii—O3—Ca1^vii	48.98 (5)
O3^iii—Ca1—V2^vii	80.06 (5)	V2^v—O3—Ca1^vii	160.78 (9)
O3—Ca1—V2^vii	20.38 (5)	V2^vii—O3—Ca1^vii	66.06 (5)
O1^iv—Ca1—V2^vii	134.56 (2)	Ca1—O3—Ca1^vii	99.70 (7)
V1—Ca1—V2^vii	110.75 (3)	Ca1^xiii—O3—Ca1^vii	113.48 (5)
V2^v—Ca1—V2^vii	46.183 (14)	V1^vii—O3—Ca1^v	104.62 (7)
V2^vi—Ca1—V2^vii	106.57 (3)	V2^v—O3—Ca1^v	60.90 (6)
V1^vii—Ca1—V2^vii	46.241 (15)	V2^vii—O3—Ca1^v	43.60 (5)
O1^viii—Ca1—V2^vii	59.88 (3)	Ca1—O3—Ca1^v	153.16 (7)
V2^i—Ca1—V2^vii	124.18 (2)	Ca1^xiii—O3—Ca1^v	85.46 (4)
V2^ii—Ca1—V2^vii	71.37 (2)	Ca1^vii—O3—Ca1^v	100.24 (4)
V1^iv—Ca1—V2^vii	127.01 (2)	V2^v—O4—V2	98.90 (9)
V2—Ca1—V2^vii	82.78 (2)	V2^v—O4—V1	132.67 (11)
V2^iii—Ca1—V2^vii	148.88 (3)	V2—O4—V1	99.19 (9)
V2^ix—Ca1—V2^vii	87.37 (3)	V2^v—O4—Ca1	100.84 (8)
O2^i—Ca1—O2	132.45 (4)	V2—O4—Ca1	129.62 (10)
O2^ii—Ca1—O2	51.61 (7)	V1—O4—Ca1	100.39 (9)
O4—Ca1—O2	45.25 (6)	V2^v—O4—Ca1^xiii	58.09 (5)
O4^iii—Ca1—O2	100.73 (6)	V2—O4—Ca1^xiii	132.32 (8)
O3^iii—Ca1—O2	149.55 (6)	V1—O4—Ca1^xiii	77.63 (6)
O3—Ca1—O2	89.10 (6)	Ca1—O4—Ca1^xiii	97.17 (6)
O1^iv—Ca1—O2	56.36 (4)	V2^v—O4—Ca1^x	161.83 (8)
V1—Ca1—O2	66.92 (3)	V2—O4—Ca1^x	65.67 (5)
V2^v—Ca1—O2	62.25 (3)	V1—O4—Ca1^x	47.09 (5)
V2^vi—Ca1—O2	131.02 (4)	Ca1—O4—Ca1^x	96.65 (6)
V1^vii—Ca1—O2	122.68 (4)	Ca1^xiii—O4—Ca1^x	124.56 (5)
O1^viii—Ca1—O2	119.81 (4)	V2^v—O4—Ca1^xiv	63.94 (6)
V2^i—Ca1—O2	119.36 (4)	V2—O4—Ca1^xiv	43.19 (5)
V2^ii—Ca1—O2	58.59 (3)	V1—O4—Ca1^xiv	104.07 (7)
V1^iv—Ca1—O2	64.15 (3)	Ca1—O4—Ca1^xiv	155.38 (7)
V2—Ca1—O2	22.89 (3)	Ca1^xiii—O4—Ca1^xiv	90.74 (4)
V2^iii—Ca1—O2	101.86 (4)	Ca1^x—O4—Ca1^xiv	97.94 (4)
V2^ix—Ca1—O2	168.72 (4)	V2^v—O4—Ca1^ii	90.29 (7)
V2^vii—Ca1—O2	83.43 (4)	V2—O4—Ca1^ii	37.45 (4)
O1—V1—O3^x	109.39 (9)	V1—O4—Ca1^ii	128.31 (7)
O1—V1—O3^xi	109.39 (9)	Ca1—O4—Ca1^ii	96.62 (6)
O3^x—V1—O3^xi	86.60 (12)	Ca1^xiii—O4—Ca1^ii	147.37 (5)
O1—V1—O4^iii	111.20 (9)	Ca1^x—O4—Ca1^ii	82.79 (3)
O3^x—V1—O4^iii	139.41 (10)	Ca1^xiv—O4—Ca1^ii	65.82 (3)
O3^xi—V1—O4^iii	79.94 (8)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_225K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.540 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2716 reflections
a = 10.431 (3) Å	θ = 1.3–23.4°
b = 10.366 (2) Å	µ = 5.68 mm^−1
c = 5.2918 (15) Å	T = 225 K
V = 572.2 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	403 independent reflections
Radiation source: fine-focus sealed tube	371 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.471	l = −5→5
2451 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.0506P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.058	(Δ/σ)max < 0.001
S = 0.93	Δρmax = 0.36 e Å^−3
403 reflections	Δρmin = −0.41 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0185 (16)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08481 (10)	0.2500	0.29970 (15)	0.0069 (3)
V1	0.28872 (8)	0.2500	0.79230 (13)	0.0055 (3)
V2	0.18743 (6)	0.52027 (6)	0.78360 (10)	0.0055 (3)
O1	0.4437 (3)	0.2500	0.8086 (6)	0.0109 (8)*
O2	0.0400 (2)	0.5655 (3)	0.7667 (4)	0.0124 (6)*
O3	0.2204 (2)	0.3800 (2)	0.0261 (4)	0.0066 (5)*
O4	0.2267 (2)	0.3797 (2)	0.5483 (4)	0.0069 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0051 (6)	0.0068 (6)	0.0087 (6)	0.000	−0.0002 (4)	0.000
V1	0.0052 (5)	0.0053 (6)	0.0059 (5)	0.000	−0.0002 (3)	0.000
V2	0.0055 (4)	0.0051 (5)	0.0059 (4)	0.0010 (2)	0.0000 (2)	0.0000 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.340 (3)	V1—Ca1^xiii	4.3991 (15)
Ca1—O2^ii	2.340 (3)	V1—Ca1^xiv	5.3483 (12)
Ca1—O4	2.393 (2)	V2—O2	1.610 (2)
Ca1—O4^iii	2.393 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3^iii	2.432 (2)	V2—O4	1.960 (2)
Ca1—O3	2.432 (2)	V2—O3^xiv	1.962 (2)
Ca1—O1^iv	2.542 (3)	V2—O3^x	1.970 (2)
Ca1—V2^v	3.3648 (11)	V2—V2^xiv	2.9802 (9)
Ca1—V2^vi	3.3648 (11)	V2—V2^v	2.9802 (9)
Ca1—V1	3.3643 (13)	V2—Ca1^xiv	3.3648 (11)
Ca1—V1^vii	3.4254 (14)	V2—Ca1^ii	3.7321 (12)
Ca1—O1^viii	3.540 (3)	V2—Ca1^x	4.0563 (11)
Ca1—V2^i	3.7321 (12)	O1—Ca1^xii	2.542 (3)
Ca1—V2^ii	3.7321 (12)	O1—Ca1^xiii	3.540 (3)
Ca1—V1^iv	3.7683 (14)	O1—Ca1^x	4.557 (3)
Ca1—V2	3.9436 (10)	O2—Ca1^ii	2.340 (3)
Ca1—V2^iii	3.9436 (10)	O2—Ca1^x	4.344 (3)
Ca1—V2^ix	4.0563 (11)	O2—Ca1^xiv	4.359 (3)
Ca1—V2^vii	4.0563 (11)	O3—V2^v	1.962 (2)
Ca1—O2	4.126 (3)	O3—V1^vii	1.963 (2)
V1—O1	1.619 (3)	O3—V2^vii	1.970 (2)
V1—O3^x	1.963 (2)	O3—Ca1^xiii	4.136 (2)
V1—O3^xi	1.963 (2)	O3—Ca1^vii	4.312 (2)
V1—O4^iii	1.973 (2)	O3—Ca1^v	4.502 (2)
V1—O4	1.973 (2)	O4—V2^v	1.960 (2)
V1—V2	2.9946 (9)	O4—Ca1^xiii	4.376 (2)
V1—V2^iii	2.9946 (9)	O4—Ca1^x	4.451 (2)
V1—Ca1^x	3.4254 (14)	O4—Ca1^xiv	4.514 (2)
V1—Ca1^xii	3.7683 (14)	O4—Ca1^ii	5.093 (2)
O2^i—Ca1—O2^ii	109.62 (12)	O1—V1—O4	111.25 (10)
O2^i—Ca1—O4	152.32 (8)	O3^x—V1—O4	79.97 (9)
O2^ii—Ca1—O4	88.14 (8)	O3^xi—V1—O4	139.56 (10)
O2^i—Ca1—O4^iii	88.14 (8)	O4^iii—V1—O4	85.88 (13)
O2^ii—Ca1—O4^iii	152.32 (8)	O1—V1—V2	110.680 (19)
O4—Ca1—O4^iii	68.34 (10)	O3^x—V1—V2	40.49 (6)
O2^i—Ca1—O3^iii	77.38 (7)	O3^xi—V1—V2	121.59 (7)
O2^ii—Ca1—O3^iii	133.40 (8)	O4^iii—V1—V2	120.77 (7)
O4—Ca1—O3^iii	106.19 (8)	O4—V1—V2	40.26 (6)
O4^iii—Ca1—O3^iii	69.90 (7)	O1—V1—V2^iii	110.680 (19)
O2^i—Ca1—O3	133.40 (8)	O3^x—V1—V2^iii	121.59 (7)
O2^ii—Ca1—O3	77.38 (7)	O3^xi—V1—V2^iii	40.49 (6)
O4—Ca1—O3	69.90 (7)	O4^iii—V1—V2^iii	40.26 (6)
O4^iii—Ca1—O3	106.19 (8)	O4—V1—V2^iii	120.77 (7)
O3^iii—Ca1—O3	67.29 (10)	V2—V1—V2^iii	138.64 (4)
O2^i—Ca1—O1^iv	78.48 (7)	O1—V1—Ca1	132.27 (11)
O2^ii—Ca1—O1^iv	78.48 (7)	O3^x—V1—Ca1	105.01 (7)
O4—Ca1—O1^iv	84.83 (8)	O3^xi—V1—Ca1	105.01 (7)
O4^iii—Ca1—O1^iv	84.83 (8)	O4^iii—V1—Ca1	44.40 (6)
O3^iii—Ca1—O1^iv	145.32 (5)	O4—V1—Ca1	44.40 (6)
O3—Ca1—O1^iv	145.32 (5)	V2—V1—Ca1	76.411 (18)
O2^i—Ca1—V2^v	165.34 (6)	V2^iii—V1—Ca1	76.411 (18)
O2^ii—Ca1—V2^v	79.09 (6)	O1—V1—Ca1^x	125.32 (11)
O4—Ca1—V2^v	34.90 (5)	O3^x—V1—Ca1^x	44.00 (7)
O4^iii—Ca1—V2^v	88.56 (6)	O3^xi—V1—Ca1^x	44.00 (7)
O3^iii—Ca1—V2^v	88.07 (6)	O4^iii—V1—Ca1^x	108.02 (7)
O3—Ca1—V2^v	35.12 (5)	O4—V1—Ca1^x	108.02 (7)
O1^iv—Ca1—V2^v	115.43 (5)	V2—V1—Ca1^x	78.051 (18)
O2^i—Ca1—V2^vi	79.09 (6)	V2^iii—V1—Ca1^x	78.051 (18)
O2^ii—Ca1—V2^vi	165.34 (6)	Ca1—V1—Ca1^x	102.40 (4)
O4—Ca1—V2^vi	88.56 (6)	O1—V1—Ca1^xii	31.90 (11)
O4^iii—Ca1—V2^vi	34.90 (5)	O3^x—V1—Ca1^xii	86.35 (7)
O3^iii—Ca1—V2^vi	35.12 (5)	O3^xi—V1—Ca1^xii	86.35 (7)
O3—Ca1—V2^vi	88.07 (6)	O4^iii—V1—Ca1^xii	130.08 (7)
O1^iv—Ca1—V2^vi	115.43 (5)	O4—V1—Ca1^xii	130.08 (7)
V2^v—Ca1—V2^vi	90.10 (4)	V2—V1—Ca1^xii	107.336 (18)
O2^i—Ca1—V1	117.91 (6)	V2^iii—V1—Ca1^xii	107.336 (18)
O2^ii—Ca1—V1	117.91 (6)	Ca1—V1—Ca1^xii	164.17 (3)
O4—Ca1—V1	35.23 (5)	Ca1^x—V1—Ca1^xii	93.43 (3)
O4^iii—Ca1—V1	35.23 (5)	O1—V1—Ca1^xiii	48.47 (11)
O3^iii—Ca1—V1	95.37 (6)	O3^x—V1—Ca1^xiii	134.71 (7)
O3—Ca1—V1	95.37 (6)	O3^xi—V1—Ca1^xiii	134.71 (7)
O1^iv—Ca1—V1	74.59 (8)	O4^iii—V1—Ca1^xiii	76.36 (6)
V2^v—Ca1—V1	64.74 (2)	O4—V1—Ca1^xiii	76.36 (6)
V2^vi—Ca1—V1	64.74 (2)	V2—V1—Ca1^xiii	103.696 (18)
O2^i—Ca1—V1^vii	103.17 (6)	V2^iii—V1—Ca1^xiii	103.696 (18)
O2^ii—Ca1—V1^vii	103.17 (6)	Ca1—V1—Ca1^xiii	83.80 (3)
O4—Ca1—V1^vii	92.69 (6)	Ca1^x—V1—Ca1^xiii	173.79 (3)
O4^iii—Ca1—V1^vii	92.69 (6)	Ca1^xii—V1—Ca1^xiii	80.36 (3)
O3^iii—Ca1—V1^vii	34.11 (5)	O1—V1—Ca1^xiv	75.718 (14)
O3—Ca1—V1^vii	34.11 (5)	O3^x—V1—Ca1^xiv	54.52 (7)
O1^iv—Ca1—V1^vii	176.99 (8)	O3^xi—V1—Ca1^xiv	138.60 (6)
V2^v—Ca1—V1^vii	62.73 (2)	O4^iii—V1—Ca1^xiv	138.24 (6)
V2^vi—Ca1—V1^vii	62.73 (2)	O4—V1—Ca1^xiv	54.94 (6)
V1—Ca1—V1^vii	102.40 (4)	V2—V1—Ca1^xiv	34.97 (2)
O2^i—Ca1—O1^viii	68.42 (6)	V2^iii—V1—Ca1^xiv	173.60 (3)
O2^ii—Ca1—O1^viii	68.42 (6)	Ca1—V1—Ca1^xiv	99.300 (15)
O4—Ca1—O1^viii	139.20 (6)	Ca1^x—V1—Ca1^xiv	98.477 (15)
O4^iii—Ca1—O1^viii	139.20 (6)	Ca1^xii—V1—Ca1^xiv	78.091 (13)
O3^iii—Ca1—O1^viii	72.56 (7)	Ca1^xiii—V1—Ca1^xiv	80.332 (13)
O3—Ca1—O1^viii	72.56 (7)	O2—V2—O4^xiv	108.79 (11)
O1^iv—Ca1—O1^viii	120.05 (12)	O2—V2—O4	112.38 (11)
V2^v—Ca1—O1^viii	105.70 (4)	O4^xiv—V2—O4	138.77 (5)
V2^vi—Ca1—O1^viii	105.70 (4)	O2—V2—O3^xiv	105.99 (11)
V1—Ca1—O1^viii	165.36 (6)	O4^xiv—V2—O3^xiv	89.63 (10)
V1^vii—Ca1—O1^viii	62.95 (6)	O4—V2—O3^xiv	81.27 (9)
O2^i—Ca1—V2^i	15.73 (6)	O2—V2—O3^x	114.74 (11)
O2^ii—Ca1—V2^i	94.61 (7)	O4^xiv—V2—O3^x	81.10 (9)
O4—Ca1—V2^i	153.36 (6)	O4—V2—O3^x	80.12 (9)
O4^iii—Ca1—V2^i	100.20 (5)	O3^xiv—V2—O3^x	139.10 (5)
O3^iii—Ca1—V2^i	91.08 (5)	O2—V2—V2^xiv	120.59 (8)
O3—Ca1—V2^i	136.54 (6)	O4^xiv—V2—V2^xiv	40.52 (6)
O1^iv—Ca1—V2^i	69.87 (6)	O4—V2—V2^xiv	111.57 (7)
V2^v—Ca1—V2^i	170.33 (3)	O3^xiv—V2—V2^xiv	118.46 (7)
V2^vi—Ca1—V2^i	94.74 (2)	O3^x—V2—V2^xiv	40.62 (6)
V1—Ca1—V2^i	124.93 (2)	O2—V2—V2^v	114.20 (8)
V1^vii—Ca1—V2^i	112.32 (2)	O4^xiv—V2—V2^v	120.59 (7)
O1^viii—Ca1—V2^i	64.93 (4)	O4—V2—V2^v	40.51 (6)
O2^i—Ca1—V2^ii	94.61 (7)	O3^xiv—V2—V2^v	40.81 (6)
O2^ii—Ca1—V2^ii	15.73 (6)	O3^x—V2—V2^v	113.43 (7)
O4—Ca1—V2^ii	100.20 (5)	V2^xiv—V2—V2^v	125.21 (4)
O4^iii—Ca1—V2^ii	153.36 (6)	O2—V2—V1	127.62 (10)
O3^iii—Ca1—V2^ii	136.54 (6)	O4^xiv—V2—V1	108.84 (7)
O3—Ca1—V2^ii	91.08 (5)	O4—V2—V1	40.58 (6)
O1^iv—Ca1—V2^ii	69.87 (6)	O3^xiv—V2—V1	109.32 (7)
V2^v—Ca1—V2^ii	94.74 (2)	O3^x—V2—V1	40.32 (6)
V2^vi—Ca1—V2^ii	170.33 (3)	V2^xiv—V2—V1	72.54 (3)
V1—Ca1—V2^ii	124.93 (2)	V2^v—V2—V1	74.17 (3)
V1^vii—Ca1—V2^ii	112.32 (2)	O2—V2—Ca1^xiv	117.99 (10)
O1^viii—Ca1—V2^ii	64.93 (4)	O4^xiv—V2—Ca1^xiv	44.32 (6)
V2^i—Ca1—V2^ii	79.30 (3)	O4—V2—Ca1^xiv	113.26 (7)
O2^i—Ca1—V1^iv	68.28 (6)	O3^xiv—V2—Ca1^xiv	45.48 (7)
O2^ii—Ca1—V1^iv	68.28 (6)	O3^x—V2—Ca1^xiv	112.49 (7)
O4—Ca1—V1^iv	101.06 (6)	V2^xiv—V2—Ca1^xiv	76.59 (3)
O4^iii—Ca1—V1^iv	101.06 (6)	V2^v—V2—Ca1^xiv	79.22 (3)
O3^iii—Ca1—V1^iv	144.88 (5)	V1—V2—Ca1^xiv	114.37 (3)
O3—Ca1—V1^iv	144.88 (5)	O2—V2—Ca1^ii	23.20 (9)
O1^iv—Ca1—V1^iv	19.67 (7)	O4^xiv—V2—Ca1^ii	95.43 (7)
V2^v—Ca1—V1^iv	126.38 (2)	O4—V2—Ca1^ii	123.94 (6)
V2^vi—Ca1—V1^iv	126.38 (2)	O3^xiv—V2—Ca1^ii	87.38 (7)
V1—Ca1—V1^iv	94.26 (3)	O3^x—V2—Ca1^ii	132.93 (7)
V1^vii—Ca1—V1^iv	163.34 (3)	V2^xiv—V2—Ca1^ii	121.88 (3)
O1^viii—Ca1—V1^iv	100.39 (6)	V2^v—V2—Ca1^ii	108.56 (3)
V2^i—Ca1—V1^iv	56.23 (2)	V1—V2—Ca1^ii	150.14 (3)
V2^ii—Ca1—V1^iv	56.23 (2)	Ca1^xiv—V2—Ca1^ii	95.08 (2)
O2^i—Ca1—V2	146.00 (6)	O2—V2—Ca1	84.93 (9)
O2^ii—Ca1—V2	70.60 (6)	O4^xiv—V2—Ca1	164.62 (7)
O4—Ca1—V2	22.51 (5)	O4—V2—Ca1	27.87 (6)
O4^iii—Ca1—V2	82.78 (6)	O3^xiv—V2—Ca1	93.23 (7)
O3^iii—Ca1—V2	128.49 (6)	O3^x—V2—Ca1	86.90 (7)
O3—Ca1—V2	80.51 (5)	V2^xiv—V2—Ca1	126.53 (3)
O1^iv—Ca1—V2	68.14 (5)	V2^v—V2—Ca1	56.10 (3)
V2^v—Ca1—V2	47.315 (15)	V1—V2—Ca1	56.02 (2)
V2^vi—Ca1—V2	109.12 (3)	Ca1^xiv—V2—Ca1	135.30 (3)
V1—Ca1—V2	47.569 (16)	Ca1^ii—V2—Ca1	99.79 (2)
V1^vii—Ca1—V2	109.91 (3)	O2—V2—Ca1^x	89.24 (9)
O1^viii—Ca1—V2	134.700 (15)	O4^xiv—V2—Ca1^x	90.29 (7)
V2^i—Ca1—V2	137.44 (3)	O4—V2—Ca1^x	88.24 (7)
V2^ii—Ca1—V2	80.21 (2)	O3^xiv—V2—Ca1^x	163.92 (7)
V1^iv—Ca1—V2	81.40 (2)	O3^x—V2—Ca1^x	25.53 (6)
O2^i—Ca1—V2^iii	70.60 (6)	V2^xiv—V2—Ca1^x	54.58 (3)
O2^ii—Ca1—V2^iii	146.00 (6)	V2^v—V2—Ca1^x	128.02 (3)
O4—Ca1—V2^iii	82.78 (6)	V1—V2—Ca1^x	55.71 (2)
O4^iii—Ca1—V2^iii	22.51 (5)	Ca1^xiv—V2—Ca1^x	131.15 (3)
O3^iii—Ca1—V2^iii	80.51 (5)	Ca1^ii—V2—Ca1^x	108.63 (2)
O3—Ca1—V2^iii	128.49 (6)	Ca1—V2—Ca1^x	82.81 (2)
O1^iv—Ca1—V2^iii	68.14 (5)	V1—O1—Ca1^xii	128.44 (16)
V2^v—Ca1—V2^iii	109.12 (3)	V1—O1—Ca1^xiii	111.51 (13)
V2^vi—Ca1—V2^iii	47.315 (15)	Ca1^xii—O1—Ca1^xiii	120.05 (12)
V1—Ca1—V2^iii	47.569 (16)	V1—O1—Ca1^x	37.83 (8)
V1^vii—Ca1—V2^iii	109.91 (3)	Ca1^xii—O1—Ca1^x	90.61 (8)
O1^viii—Ca1—V2^iii	134.700 (15)	Ca1^xiii—O1—Ca1^x	149.34 (9)
V2^i—Ca1—V2^iii	80.21 (2)	V1—O1—Ca1	32.67 (8)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.11 (11)
V1^iv—Ca1—V2^iii	81.40 (2)	Ca1^xiii—O1—Ca1	78.84 (6)
V2—Ca1—V2^iii	90.54 (3)	Ca1^x—O1—Ca1	70.50 (5)
O2^i—Ca1—V2^ix	58.76 (6)	V2—O2—Ca1^ii	141.07 (15)
O2^ii—Ca1—V2^ix	127.60 (6)	V2—O2—Ca1	72.19 (9)
O4—Ca1—V2^ix	126.50 (6)	Ca1^ii—O2—Ca1	128.39 (7)
O4^iii—Ca1—V2^ix	79.57 (5)	V2—O2—Ca1^x	69.00 (8)
O3^iii—Ca1—V2^ix	20.43 (5)	Ca1^ii—O2—Ca1^x	140.59 (8)
O3—Ca1—V2^ix	80.11 (6)	Ca1—O2—Ca1^x	77.28 (5)
O1^iv—Ca1—V2^ix	134.57 (3)	V2—O2—Ca1^xiv	42.97 (7)
V2^v—Ca1—V2^ix	106.59 (3)	Ca1^ii—O2—Ca1^xiv	98.46 (8)
V2^vi—Ca1—V2^ix	46.199 (15)	Ca1—O2—Ca1^xiv	105.67 (5)
V1—Ca1—V2^ix	110.78 (3)	Ca1^x—O2—Ca1^xiv	101.98 (5)
V1^vii—Ca1—V2^ix	46.241 (16)	V2^v—O3—V1^vii	128.45 (11)
O1^viii—Ca1—V2^ix	59.83 (4)	V2^v—O3—V2^vii	98.57 (10)
V2^i—Ca1—V2^ix	71.37 (2)	V1^vii—O3—V2^vii	99.19 (9)
V2^ii—Ca1—V2^ix	124.19 (3)	V2^v—O3—Ca1	99.40 (9)
V1^iv—Ca1—V2^ix	127.02 (2)	V1^vii—O3—Ca1	101.89 (9)
V2—Ca1—V2^ix	148.90 (3)	V2^vii—O3—Ca1	134.04 (10)
V2^iii—Ca1—V2^ix	82.81 (2)	V2^v—O3—Ca1^xiii	64.33 (6)
O2^i—Ca1—V2^vii	127.60 (6)	V1^vii—O3—Ca1^xiii	65.39 (6)
O2^ii—Ca1—V2^vii	58.76 (6)	V2^vii—O3—Ca1^xiii	123.12 (8)
O4—Ca1—V2^vii	79.57 (5)	Ca1—O3—Ca1^xiii	102.79 (6)
O4^iii—Ca1—V2^vii	126.50 (6)	V2^v—O3—Ca1^vii	160.83 (9)
O3^iii—Ca1—V2^vii	80.11 (6)	V1^vii—O3—Ca1^vii	48.91 (5)
O3—Ca1—V2^vii	20.43 (5)	V2^vii—O3—Ca1^vii	65.96 (6)
O1^iv—Ca1—V2^vii	134.57 (3)	Ca1—O3—Ca1^vii	99.60 (7)
V2^v—Ca1—V2^vii	46.199 (15)	Ca1^xiii—O3—Ca1^vii	113.48 (5)
V2^vi—Ca1—V2^vii	106.59 (3)	V2^v—O3—Ca1^v	60.98 (6)
V1—Ca1—V2^vii	110.78 (3)	V1^vii—O3—Ca1^v	104.68 (8)
V1^vii—Ca1—V2^vii	46.241 (16)	V2^vii—O3—Ca1^v	43.67 (5)
O1^viii—Ca1—V2^vii	59.83 (4)	Ca1—O3—Ca1^v	153.24 (8)
V2^i—Ca1—V2^vii	124.19 (3)	Ca1^xiii—O3—Ca1^v	85.54 (4)
V2^ii—Ca1—V2^vii	71.37 (2)	Ca1^vii—O3—Ca1^v	100.20 (5)
V1^iv—Ca1—V2^vii	127.02 (2)	V2^v—O4—V2	98.98 (10)
V2—Ca1—V2^vii	82.81 (2)	V2^v—O4—V1	132.72 (11)
V2^iii—Ca1—V2^vii	148.90 (3)	V2—O4—V1	99.17 (9)
V2^ix—Ca1—V2^vii	87.37 (3)	V2^v—O4—Ca1	100.78 (8)
O2^i—Ca1—O2	132.43 (4)	V2—O4—Ca1	129.62 (10)
O2^ii—Ca1—O2	51.61 (7)	V1—O4—Ca1	100.36 (9)
O4—Ca1—O2	45.22 (6)	V2^v—O4—Ca1^xiii	58.10 (6)
O4^iii—Ca1—O2	100.73 (6)	V2—O4—Ca1^xiii	132.37 (9)
O3^iii—Ca1—O2	149.52 (7)	V1—O4—Ca1^xiii	77.65 (6)
O3—Ca1—O2	89.04 (6)	Ca1—O4—Ca1^xiii	97.12 (6)
O1^iv—Ca1—O2	56.36 (4)	V2^v—O4—Ca1^x	161.88 (9)
V2^v—Ca1—O2	62.23 (4)	V2—O4—Ca1^x	65.64 (6)
V2^vi—Ca1—O2	131.01 (4)	V1—O4—Ca1^x	47.05 (5)
V1—Ca1—O2	66.90 (4)	Ca1—O4—Ca1^x	96.65 (7)
V1^vii—Ca1—O2	122.67 (4)	Ca1^xiii—O4—Ca1^x	124.54 (5)
O1^viii—Ca1—O2	119.84 (4)	V2^v—O4—Ca1^xiv	63.98 (6)
V2^i—Ca1—O2	119.37 (4)	V2—O4—Ca1^xiv	43.23 (5)
V2^ii—Ca1—O2	58.58 (4)	V1—O4—Ca1^xiv	104.10 (7)
V1^iv—Ca1—O2	64.15 (4)	Ca1—O4—Ca1^xiv	155.38 (7)
V2—Ca1—O2	22.88 (3)	Ca1^xiii—O4—Ca1^xiv	90.77 (4)
V2^iii—Ca1—O2	101.83 (4)	Ca1^x—O4—Ca1^xiv	97.95 (4)
V2^ix—Ca1—O2	168.72 (4)	V2^v—O4—Ca1^ii	90.32 (7)
V2^vii—Ca1—O2	83.43 (4)	V2—O4—Ca1^ii	37.44 (5)
O1—V1—O3^x	109.19 (10)	V1—O4—Ca1^ii	128.27 (8)
O1—V1—O3^xi	109.19 (10)	Ca1—O4—Ca1^ii	96.64 (6)
O3^x—V1—O3^xi	86.70 (13)	Ca1^xiii—O4—Ca1^ii	147.40 (5)
O1—V1—O4^iii	111.25 (10)	Ca1^x—O4—Ca1^ii	82.79 (3)
O3^x—V1—O4^iii	139.56 (10)	Ca1^xiv—O4—Ca1^ii	65.81 (3)
O3^xi—V1—O4^iii	79.97 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_219K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.539 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2697 reflections
a = 10.442 (3) Å	θ = 1.3–23.4°
b = 10.367 (2) Å	µ = 5.67 mm^−1
c = 5.2860 (16) Å	T = 219 K
V = 572.2 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	404 independent reflections
Radiation source: fine-focus sealed tube	370 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.036
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.318, Tmax = 0.471	l = −5→5
2433 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.0674P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.063	(Δ/σ)max < 0.001
S = 0.79	Δρmax = 0.42 e Å^−3
404 reflections	Δρmin = −0.43 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0191 (18)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08488 (10)	0.2500	0.29968 (16)	0.0066 (4)
V1	0.28882 (8)	0.2500	0.79221 (14)	0.0052 (4)
V2	0.18749 (6)	0.52026 (6)	0.78361 (11)	0.0052 (3)
O1	0.4440 (3)	0.2500	0.8079 (6)	0.0100 (8)*
O2	0.0397 (2)	0.5653 (3)	0.7666 (4)	0.0121 (6)*
O3	0.2205 (2)	0.3799 (2)	0.0255 (4)	0.0066 (5)*
O4	0.2268 (2)	0.3796 (2)	0.5480 (4)	0.0064 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0051 (6)	0.0068 (7)	0.0079 (6)	0.000	0.0002 (4)	0.000
V1	0.0046 (5)	0.0051 (6)	0.0058 (5)	0.000	−0.0003 (3)	0.000
V2	0.0049 (5)	0.0050 (5)	0.0057 (4)	0.0006 (2)	0.0002 (2)	0.0002 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.341 (3)	V1—Ca1^xiii	4.3985 (16)
Ca1—O2^ii	2.341 (3)	V1—Ca1^xiv	5.3489 (12)
Ca1—O4	2.392 (2)	V2—O2	1.615 (2)
Ca1—O4^iii	2.392 (2)	V2—O4^xiv	1.958 (2)
Ca1—O3^iii	2.433 (2)	V2—O4	1.961 (2)
Ca1—O3	2.433 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.543 (3)	V2—O3^x	1.967 (2)
Ca1—V1	3.3635 (13)	V2—V2^v	2.9776 (9)
Ca1—V2^v	3.3659 (12)	V2—V2^xiv	2.9776 (9)
Ca1—V2^vi	3.3659 (12)	V2—Ca1^xiv	3.3659 (12)
Ca1—V1^vii	3.4250 (14)	V2—Ca1^ii	3.7358 (12)
Ca1—O1^viii	3.532 (3)	V2—Ca1^x	4.0546 (11)
Ca1—V2^i	3.7358 (12)	O1—Ca1^xii	2.543 (3)
Ca1—V2^ii	3.7358 (12)	O1—Ca1^xiii	3.532 (3)
Ca1—V1^iv	3.7698 (15)	O1—Ca1^x	4.563 (4)
Ca1—V2	3.9423 (10)	O2—Ca1^ii	2.341 (3)
Ca1—V2^iii	3.9423 (10)	O2—Ca1^x	4.341 (3)
Ca1—V2^ix	4.0546 (11)	O2—Ca1^xiv	4.366 (3)
Ca1—V2^vii	4.0546 (11)	O3—V1^vii	1.961 (2)
Ca1—O2	4.123 (3)	O3—V2^v	1.964 (2)
V1—O1	1.623 (4)	O3—V2^vii	1.967 (2)
V1—O3^x	1.961 (2)	O3—Ca1^xiii	4.141 (3)
V1—O3^xi	1.961 (2)	O3—Ca1^vii	4.306 (2)
V1—O4^iii	1.973 (2)	O3—Ca1^v	4.503 (2)
V1—O4	1.973 (2)	O4—V2^v	1.958 (2)
V1—V2^iii	2.9953 (9)	O4—Ca1^xiii	4.378 (2)
V1—V2	2.9953 (9)	O4—Ca1^x	4.449 (2)
V1—Ca1^x	3.4250 (14)	O4—Ca1^xiv	4.515 (2)
V1—Ca1^xii	3.7698 (15)	O4—Ca1^ii	5.097 (2)
O2^i—Ca1—O2^ii	109.75 (13)	O1—V1—O4	111.19 (10)
O2^i—Ca1—O4	152.32 (8)	O3^x—V1—O4	79.87 (9)
O2^ii—Ca1—O4	88.09 (8)	O3^xi—V1—O4	139.45 (10)
O2^i—Ca1—O4^iii	88.09 (8)	O4^iii—V1—O4	85.85 (13)
O2^ii—Ca1—O4^iii	152.32 (8)	O1—V1—V2^iii	110.705 (19)
O4—Ca1—O4^iii	68.34 (10)	O3^x—V1—V2^iii	121.57 (7)
O2^i—Ca1—O3^iii	77.38 (7)	O3^xi—V1—V2^iii	40.39 (6)
O2^ii—Ca1—O3^iii	133.40 (8)	O4^iii—V1—V2^iii	40.27 (6)
O4—Ca1—O3^iii	106.10 (9)	O4—V1—V2^iii	120.74 (7)
O4^iii—Ca1—O3^iii	69.85 (8)	O1—V1—V2	110.705 (19)
O2^i—Ca1—O3	133.40 (8)	O3^x—V1—V2	40.39 (6)
O2^ii—Ca1—O3	77.38 (7)	O3^xi—V1—V2	121.57 (7)
O4—Ca1—O3	69.85 (8)	O4^iii—V1—V2	120.74 (7)
O4^iii—Ca1—O3	106.10 (9)	O4—V1—V2	40.27 (6)
O3^iii—Ca1—O3	67.23 (10)	V2^iii—V1—V2	138.59 (4)
O2^i—Ca1—O1^iv	78.50 (7)	O1—V1—Ca1	132.21 (11)
O2^ii—Ca1—O1^iv	78.50 (7)	O3^x—V1—Ca1	104.85 (7)
O4—Ca1—O1^iv	84.88 (8)	O3^xi—V1—Ca1	104.85 (7)
O4^iii—Ca1—O1^iv	84.88 (8)	O4^iii—V1—Ca1	44.40 (7)
O3^iii—Ca1—O1^iv	145.34 (5)	O4—V1—Ca1	44.40 (7)
O3—Ca1—O1^iv	145.34 (5)	V2^iii—V1—Ca1	76.385 (18)
O2^i—Ca1—V1	117.87 (6)	V2—V1—Ca1	76.385 (18)
O2^ii—Ca1—V1	117.87 (6)	O1—V1—Ca1^x	125.52 (11)
O4—Ca1—V1	35.24 (5)	O3^x—V1—Ca1^x	44.03 (7)
O4^iii—Ca1—V1	35.24 (5)	O3^xi—V1—Ca1^x	44.03 (7)
O3^iii—Ca1—V1	95.32 (6)	O4^iii—V1—Ca1^x	107.96 (7)
O3—Ca1—V1	95.32 (6)	O4—V1—Ca1^x	107.96 (7)
O1^iv—Ca1—V1	74.62 (8)	V2^iii—V1—Ca1^x	78.010 (19)
O2^i—Ca1—V2^v	165.31 (6)	V2—V1—Ca1^x	78.010 (19)
O2^ii—Ca1—V2^v	79.04 (6)	Ca1—V1—Ca1^x	102.27 (4)
O4—Ca1—V2^v	34.82 (5)	O1—V1—Ca1^xii	31.98 (11)
O4^iii—Ca1—V2^v	88.51 (6)	O3^x—V1—Ca1^xii	86.48 (7)
O3^iii—Ca1—V2^v	88.04 (6)	O3^xi—V1—Ca1^xii	86.48 (7)
O3—Ca1—V2^v	35.14 (5)	O4^iii—V1—Ca1^xii	130.08 (7)
O1^iv—Ca1—V2^v	115.41 (5)	O4—V1—Ca1^xii	130.08 (7)
V1—Ca1—V2^v	64.69 (2)	V2^iii—V1—Ca1^xii	107.360 (18)
O2^i—Ca1—V2^vi	79.04 (6)	V2—V1—Ca1^xii	107.360 (18)
O2^ii—Ca1—V2^vi	165.31 (6)	Ca1—V1—Ca1^xii	164.19 (3)
O4—Ca1—V2^vi	88.51 (6)	Ca1^x—V1—Ca1^xii	93.54 (3)
O4^iii—Ca1—V2^vi	34.82 (5)	O1—V1—Ca1^xiii	48.27 (11)
O3^iii—Ca1—V2^vi	35.14 (5)	O3^x—V1—Ca1^xiii	134.69 (7)
O3—Ca1—V2^vi	88.04 (6)	O3^xi—V1—Ca1^xiii	134.69 (7)
O1^iv—Ca1—V2^vi	115.41 (5)	O4^iii—V1—Ca1^xiii	76.43 (6)
V1—Ca1—V2^vi	64.69 (2)	O4—V1—Ca1^xiii	76.43 (6)
V2^v—Ca1—V2^vi	90.08 (4)	V2^iii—V1—Ca1^xiii	103.738 (18)
O2^i—Ca1—V1^vii	103.20 (6)	V2—V1—Ca1^xiii	103.738 (18)
O2^ii—Ca1—V1^vii	103.20 (6)	Ca1—V1—Ca1^xiii	83.94 (3)
O4—Ca1—V1^vii	92.56 (6)	Ca1^x—V1—Ca1^xiii	173.79 (3)
O4^iii—Ca1—V1^vii	92.56 (6)	Ca1^xii—V1—Ca1^xiii	80.25 (3)
O3^iii—Ca1—V1^vii	34.07 (5)	O1—V1—Ca1^xiv	75.723 (15)
O3—Ca1—V1^vii	34.07 (5)	O3^x—V1—Ca1^xiv	54.51 (7)
O1^iv—Ca1—V1^vii	176.90 (8)	O3^xi—V1—Ca1^xiv	138.66 (7)
V1—Ca1—V1^vii	102.27 (4)	O4^iii—V1—Ca1^xiv	138.23 (7)
V2^v—Ca1—V1^vii	62.69 (2)	O4—V1—Ca1^xiv	54.96 (7)
V2^vi—Ca1—V1^vii	62.69 (2)	V2^iii—V1—Ca1^xiv	173.57 (3)
O2^i—Ca1—O1^viii	68.45 (6)	V2—V1—Ca1^xiv	34.99 (2)
O2^ii—Ca1—O1^viii	68.45 (6)	Ca1—V1—Ca1^xiv	99.312 (15)
O4—Ca1—O1^viii	139.17 (6)	Ca1^x—V1—Ca1^xiv	98.483 (16)
O4^iii—Ca1—O1^viii	139.17 (6)	Ca1^xii—V1—Ca1^xiv	78.087 (14)
O3^iii—Ca1—O1^viii	72.59 (7)	Ca1^xiii—V1—Ca1^xiv	80.326 (14)
O3—Ca1—O1^viii	72.59 (7)	O2—V2—O4^xiv	108.89 (11)
O1^iv—Ca1—O1^viii	120.05 (12)	O2—V2—O4	112.29 (11)
V1—Ca1—O1^viii	165.33 (7)	O4^xiv—V2—O4	138.77 (5)
V2^v—Ca1—O1^viii	105.73 (4)	O2—V2—O3^xiv	106.06 (11)
V2^vi—Ca1—O1^viii	105.73 (4)	O4^xiv—V2—O3^xiv	89.58 (10)
V1^vii—Ca1—O1^viii	63.06 (6)	O4—V2—O3^xiv	81.27 (9)
O2^i—Ca1—V2^i	15.83 (6)	O2—V2—O3^x	114.67 (11)
O2^ii—Ca1—V2^i	94.64 (7)	O4^xiv—V2—O3^x	81.27 (9)
O4—Ca1—V2^i	153.41 (6)	O4—V2—O3^x	80.00 (9)
O4^iii—Ca1—V2^i	100.26 (5)	O3^xiv—V2—O3^x	139.08 (5)
O3^iii—Ca1—V2^i	91.14 (5)	O2—V2—V2^v	114.22 (8)
O3—Ca1—V2^i	136.54 (6)	O4^xiv—V2—V2^v	120.52 (7)
O1^iv—Ca1—V2^i	69.86 (6)	O4—V2—V2^v	40.51 (6)
V1—Ca1—V2^i	124.98 (2)	O3^xiv—V2—V2^v	40.80 (6)
V2^v—Ca1—V2^i	170.33 (3)	O3^x—V2—V2^v	113.32 (7)
V2^vi—Ca1—V2^i	94.79 (2)	O2—V2—V2^xiv	120.62 (8)
V1^vii—Ca1—V2^i	112.40 (3)	O4^xiv—V2—V2^xiv	40.60 (6)
O1^viii—Ca1—V2^i	64.90 (4)	O4—V2—V2^xiv	111.55 (7)
O2^i—Ca1—V2^ii	94.64 (7)	O3^xiv—V2—V2^xiv	118.46 (7)
O2^ii—Ca1—V2^ii	15.83 (6)	O3^x—V2—V2^xiv	40.71 (6)
O4—Ca1—V2^ii	100.26 (5)	V2^v—V2—V2^xiv	125.16 (5)
O4^iii—Ca1—V2^ii	153.41 (6)	O2—V2—V1	127.50 (10)
O3^iii—Ca1—V2^ii	136.53 (6)	O4^xiv—V2—V1	108.88 (7)
O3—Ca1—V2^ii	91.14 (5)	O4—V2—V1	40.56 (6)
O1^iv—Ca1—V2^ii	69.86 (6)	O3^xiv—V2—V1	109.31 (7)
V1—Ca1—V2^ii	124.98 (2)	O3^x—V2—V1	40.23 (6)
V2^v—Ca1—V2^ii	94.79 (2)	V2^v—V2—V1	74.14 (3)
V2^vi—Ca1—V2^ii	170.33 (3)	V2^xiv—V2—V1	72.52 (3)
V1^vii—Ca1—V2^ii	112.40 (3)	O2—V2—Ca1^xiv	118.15 (10)
O1^viii—Ca1—V2^ii	64.90 (4)	O4^xiv—V2—Ca1^xiv	44.25 (6)
V2^i—Ca1—V2^ii	79.22 (4)	O4—V2—Ca1^xiv	113.24 (7)
O2^i—Ca1—V1^iv	68.28 (6)	O3^xiv—V2—Ca1^xiv	45.49 (7)
O2^ii—Ca1—V1^iv	68.28 (6)	O3^x—V2—Ca1^xiv	112.54 (7)
O4—Ca1—V1^iv	101.18 (6)	V2^v—V2—Ca1^xiv	79.20 (3)
O4^iii—Ca1—V1^iv	101.18 (6)	V2^xiv—V2—Ca1^xiv	76.58 (3)
O3^iii—Ca1—V1^iv	144.90 (5)	V1—V2—Ca1^xiv	114.34 (3)
O3—Ca1—V1^iv	144.90 (5)	O2—V2—Ca1^ii	23.30 (10)
O1^iv—Ca1—V1^iv	19.75 (7)	O4^xiv—V2—Ca1^ii	95.41 (7)
V1—Ca1—V1^iv	94.37 (3)	O4—V2—Ca1^ii	123.94 (7)
V2^v—Ca1—V1^iv	126.41 (2)	O3^xiv—V2—Ca1^ii	87.41 (7)
V2^vi—Ca1—V1^iv	126.41 (2)	O3^x—V2—Ca1^ii	132.95 (7)
V1^vii—Ca1—V1^iv	163.35 (3)	V2^v—V2—Ca1^ii	108.61 (3)
O1^viii—Ca1—V1^iv	100.30 (6)	V2^xiv—V2—Ca1^ii	121.89 (3)
V2^i—Ca1—V1^iv	56.16 (2)	V1—V2—Ca1^ii	150.12 (3)
V2^ii—Ca1—V1^iv	56.16 (2)	Ca1^xiv—V2—Ca1^ii	95.13 (2)
O2^i—Ca1—V2	146.03 (6)	O2—V2—Ca1	84.81 (9)
O2^ii—Ca1—V2	70.53 (6)	O4^xiv—V2—Ca1	164.67 (7)
O4—Ca1—V2	22.56 (5)	O4—V2—Ca1	27.90 (6)
O4^iii—Ca1—V2	82.81 (6)	O3^xiv—V2—Ca1	93.25 (7)
O3^iii—Ca1—V2	128.45 (6)	O3^x—V2—Ca1	86.77 (7)
O3—Ca1—V2	80.50 (6)	V2^v—V2—Ca1	56.15 (3)
O1^iv—Ca1—V2	68.16 (5)	V2^xiv—V2—Ca1	126.50 (3)
V1—Ca1—V2	47.598 (16)	V1—V2—Ca1	56.02 (2)
V2^v—Ca1—V2	47.278 (15)	Ca1^xiv—V2—Ca1	135.33 (3)
V2^vi—Ca1—V2	109.11 (3)	Ca1^ii—V2—Ca1	99.77 (2)
V1^vii—Ca1—V2	109.83 (3)	O2—V2—Ca1^x	89.13 (9)
O1^viii—Ca1—V2	134.677 (16)	O4^xiv—V2—Ca1^x	90.41 (7)
V2^i—Ca1—V2	137.43 (3)	O4—V2—Ca1^x	88.21 (7)
V2^ii—Ca1—V2	80.23 (2)	O3^xiv—V2—Ca1^x	163.94 (7)
V1^iv—Ca1—V2	81.46 (2)	O3^x—V2—Ca1^x	25.57 (7)
O2^i—Ca1—V2^iii	70.53 (6)	V2^v—V2—Ca1^x	127.99 (3)
O2^ii—Ca1—V2^iii	146.03 (6)	V2^xiv—V2—Ca1^x	54.63 (3)
O4—Ca1—V2^iii	82.81 (6)	V1—V2—Ca1^x	55.72 (2)
O4^iii—Ca1—V2^iii	22.56 (5)	Ca1^xiv—V2—Ca1^x	131.19 (3)
O3^iii—Ca1—V2^iii	80.50 (6)	Ca1^ii—V2—Ca1^x	108.58 (2)
O3—Ca1—V2^iii	128.45 (6)	Ca1—V2—Ca1^x	82.74 (2)
O1^iv—Ca1—V2^iii	68.16 (5)	V1—O1—Ca1^xii	128.27 (16)
V1—Ca1—V2^iii	47.598 (16)	V1—O1—Ca1^xiii	111.69 (14)
V2^v—Ca1—V2^iii	109.11 (3)	Ca1^xii—O1—Ca1^xiii	120.05 (12)
V2^vi—Ca1—V2^iii	47.278 (15)	V1—O1—Ca1^x	37.66 (9)
V1^vii—Ca1—V2^iii	109.83 (3)	Ca1^xii—O1—Ca1^x	90.61 (8)
O1^viii—Ca1—V2^iii	134.677 (16)	Ca1^xiii—O1—Ca1^x	149.34 (9)
V2^i—Ca1—V2^iii	80.23 (2)	V1—O1—Ca1	32.69 (8)
V2^ii—Ca1—V2^iii	137.43 (3)	Ca1^xii—O1—Ca1	160.96 (11)
V1^iv—Ca1—V2^iii	81.46 (2)	Ca1^xiii—O1—Ca1	78.99 (6)
V2—Ca1—V2^iii	90.58 (3)	Ca1^x—O1—Ca1	70.35 (6)
O2^i—Ca1—V2^ix	58.74 (6)	V2—O2—Ca1^ii	140.87 (15)
O2^ii—Ca1—V2^ix	127.69 (6)	V2—O2—Ca1	72.23 (9)
O4—Ca1—V2^ix	126.41 (6)	Ca1^ii—O2—Ca1	128.50 (8)
O4^iii—Ca1—V2^ix	79.47 (6)	V2—O2—Ca1^x	69.04 (8)
O3^iii—Ca1—V2^ix	20.42 (5)	Ca1^ii—O2—Ca1^x	140.64 (8)
O3—Ca1—V2^ix	80.10 (6)	Ca1—O2—Ca1^x	77.25 (5)
O1^iv—Ca1—V2^ix	134.56 (3)	V2—O2—Ca1^xiv	42.82 (8)
V1—Ca1—V2^ix	110.70 (3)	Ca1^ii—O2—Ca1^xiv	98.40 (8)
V2^v—Ca1—V2^ix	106.58 (3)	Ca1—O2—Ca1^xiv	105.60 (5)
V2^vi—Ca1—V2^ix	46.167 (16)	Ca1^x—O2—Ca1^xiv	101.92 (5)
V1^vii—Ca1—V2^ix	46.271 (16)	V1^vii—O3—V2^v	128.38 (11)
O1^viii—Ca1—V2^ix	59.89 (4)	V1^vii—O3—V2^vii	99.38 (9)
V2^i—Ca1—V2^ix	71.42 (2)	V2^v—O3—V2^vii	98.48 (10)
V2^ii—Ca1—V2^ix	124.23 (3)	V1^vii—O3—Ca1	101.90 (9)
V1^iv—Ca1—V2^ix	126.99 (2)	V2^v—O3—Ca1	99.36 (9)
V2—Ca1—V2^ix	148.85 (4)	V2^vii—O3—Ca1	134.01 (11)
V2^iii—Ca1—V2^ix	82.74 (2)	V1^vii—O3—Ca1^xiii	65.32 (6)
O2^i—Ca1—V2^vii	127.69 (6)	V2^v—O3—Ca1^xiii	64.32 (6)
O2^ii—Ca1—V2^vii	58.74 (6)	V2^vii—O3—Ca1^xiii	123.12 (8)
O4—Ca1—V2^vii	79.47 (6)	Ca1—O3—Ca1^xiii	102.81 (7)
O4^iii—Ca1—V2^vii	126.41 (6)	V1^vii—O3—Ca1^vii	49.03 (5)
O3^iii—Ca1—V2^vii	80.10 (6)	V2^v—O3—Ca1^vii	160.89 (9)
O3—Ca1—V2^vii	20.42 (5)	V2^vii—O3—Ca1^vii	66.09 (6)
O1^iv—Ca1—V2^vii	134.56 (3)	Ca1—O3—Ca1^vii	99.57 (7)
V1—Ca1—V2^vii	110.70 (3)	Ca1^xiii—O3—Ca1^vii	113.53 (5)
V2^v—Ca1—V2^vii	46.167 (16)	V1^vii—O3—Ca1^v	104.73 (8)
V2^vi—Ca1—V2^vii	106.58 (3)	V2^v—O3—Ca1^v	60.94 (6)
V1^vii—Ca1—V2^vii	46.271 (16)	V2^vii—O3—Ca1^v	43.66 (5)
O1^viii—Ca1—V2^vii	59.89 (4)	Ca1—O3—Ca1^v	153.16 (8)
V2^i—Ca1—V2^vii	124.23 (3)	Ca1^xiii—O3—Ca1^v	85.50 (4)
V2^ii—Ca1—V2^vii	71.42 (2)	Ca1^vii—O3—Ca1^v	100.30 (5)
V1^iv—Ca1—V2^vii	126.99 (2)	V2^v—O4—V2	98.90 (10)
V2—Ca1—V2^vii	82.74 (2)	V2^v—O4—V1	132.69 (11)
V2^iii—Ca1—V2^vii	148.85 (4)	V2—O4—V1	99.17 (9)
V2^ix—Ca1—V2^vii	87.42 (3)	V2^v—O4—Ca1	100.92 (9)
O2^i—Ca1—O2	132.41 (4)	V2—O4—Ca1	129.54 (10)
O2^ii—Ca1—O2	51.50 (8)	V1—O4—Ca1	100.37 (9)
O4—Ca1—O2	45.34 (6)	V2^v—O4—Ca1^xiii	58.16 (6)
O4^iii—Ca1—O2	100.82 (7)	V2—O4—Ca1^xiii	132.33 (9)
O3^iii—Ca1—O2	149.56 (7)	V1—O4—Ca1^xiii	77.59 (6)
O3—Ca1—O2	89.10 (6)	Ca1—O4—Ca1^xiii	97.26 (6)
O1^iv—Ca1—O2	56.32 (4)	V2^v—O4—Ca1^x	161.83 (9)
V1—Ca1—O2	66.99 (4)	V2—O4—Ca1^x	65.64 (6)
V2^v—Ca1—O2	62.28 (4)	V1—O4—Ca1^x	47.09 (5)
V2^vi—Ca1—O2	131.07 (4)	Ca1—O4—Ca1^x	96.56 (7)
V1^vii—Ca1—O2	122.68 (4)	Ca1^xiii—O4—Ca1^x	124.52 (5)
O1^viii—Ca1—O2	119.77 (4)	V2^v—O4—Ca1^xiv	63.90 (6)
V2^i—Ca1—O2	119.27 (5)	V2—O4—Ca1^xiv	43.24 (5)
V2^ii—Ca1—O2	58.53 (4)	V1—O4—Ca1^xiv	104.08 (8)
V1^iv—Ca1—O2	64.13 (4)	Ca1—O4—Ca1^xiv	155.39 (8)
V2—Ca1—O2	22.96 (3)	Ca1^xiii—O4—Ca1^xiv	90.72 (4)
V2^iii—Ca1—O2	101.90 (4)	Ca1^x—O4—Ca1^xiv	97.97 (5)
V2^ix—Ca1—O2	168.77 (4)	V2^v—O4—Ca1^ii	90.30 (7)
V2^vii—Ca1—O2	83.40 (4)	V2—O4—Ca1^ii	37.44 (5)
O1—V1—O3^x	109.36 (10)	V1—O4—Ca1^ii	128.27 (8)
O1—V1—O3^xi	109.36 (10)	Ca1—O4—Ca1^ii	96.57 (6)
O3^x—V1—O3^xi	86.78 (13)	Ca1^xiii—O4—Ca1^ii	147.44 (5)
O1—V1—O4^iii	111.19 (10)	Ca1^x—O4—Ca1^ii	82.75 (3)
O3^x—V1—O4^iii	139.45 (10)	Ca1^xiv—O4—Ca1^ii	65.85 (3)
O3^xi—V1—O4^iii	79.87 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_212K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.540 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2699 reflections
a = 10.423 (3) Å	θ = 1.3–23.4°
b = 10.366 (3) Å	µ = 5.68 mm^−1
c = 5.2958 (19) Å	T = 212 K
V = 572.2 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	403 independent reflections
Radiation source: fine-focus sealed tube	370 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.471	l = −5→5
2436 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	w = 1/[σ^2(Fo^2) + (0.0346P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.050	(Δ/σ)max < 0.001
S = 1.09	Δρmax = 0.32 e Å^−3
403 reflections	Δρmin = −0.41 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0172 (13)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08485 (9)	0.2500	0.29987 (14)	0.0066 (3)
V1	0.28882 (7)	0.2500	0.79221 (12)	0.0052 (3)
V2	0.18741 (5)	0.52024 (5)	0.78355 (9)	0.0052 (3)
O1	0.4438 (3)	0.2500	0.8084 (5)	0.0106 (7)*
O2	0.0400 (2)	0.5656 (2)	0.7667 (4)	0.0117 (6)*
O3	0.22029 (19)	0.3799 (2)	0.0261 (3)	0.0062 (5)*
O4	0.22667 (19)	0.3795 (2)	0.5483 (3)	0.0065 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0045 (5)	0.0069 (6)	0.0084 (5)	0.000	−0.0002 (3)	0.000
V1	0.0047 (5)	0.0049 (5)	0.0060 (4)	0.000	−0.0004 (3)	0.000
V2	0.0051 (4)	0.0048 (4)	0.0057 (3)	0.0009 (2)	−0.0001 (2)	0.00015 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.339 (3)	V1—Ca1^xiii	4.3991 (16)
Ca1—O2^ii	2.339 (3)	V1—Ca1^xiv	5.3476 (14)
Ca1—O4	2.392 (2)	V2—O2	1.610 (2)
Ca1—O4^iii	2.392 (2)	V2—O4^xiv	1.961 (2)
Ca1—O3^iii	2.430 (2)	V2—O4	1.961 (2)
Ca1—O3	2.430 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.543 (3)	V2—O3^x	1.971 (2)
Ca1—V2^v	3.3636 (11)	V2—V2^v	2.9816 (10)
Ca1—V2^vi	3.3636 (11)	V2—V2^xiv	2.9816 (10)
Ca1—V1	3.3642 (13)	V2—Ca1^xiv	3.3636 (11)
Ca1—V1^vii	3.4275 (14)	V2—Ca1^ii	3.7309 (12)
Ca1—O1^viii	3.541 (3)	V2—Ca1^x	4.0578 (11)
Ca1—V2^i	3.7309 (12)	O1—Ca1^xii	2.543 (3)
Ca1—V2^ii	3.7309 (12)	O1—Ca1^xiii	3.541 (3)
Ca1—V1^iv	3.7666 (15)	O1—Ca1^x	4.558 (3)
Ca1—V2	3.9434 (11)	O2—Ca1^ii	2.339 (3)
Ca1—V2^iii	3.9434 (11)	O2—Ca1^x	4.346 (3)
Ca1—V2^ix	4.0578 (11)	O2—Ca1^xiv	4.357 (3)
Ca1—V2^vii	4.0578 (11)	O3—V1^vii	1.964 (2)
Ca1—O2	4.127 (2)	O3—V2^v	1.964 (2)
V1—O1	1.618 (3)	O3—V2^vii	1.971 (2)
V1—O3^x	1.964 (2)	O3—Ca1^xiii	4.135 (3)
V1—O3^xi	1.964 (2)	O3—Ca1^vii	4.313 (2)
V1—O4^iii	1.973 (2)	O3—Ca1^v	4.503 (2)
V1—O4	1.973 (2)	O4—V2^v	1.961 (2)
V1—V2^iii	2.9944 (9)	O4—Ca1^xiii	4.375 (2)
V1—V2	2.9944 (9)	O4—Ca1^x	4.453 (2)
V1—Ca1^x	3.4275 (14)	O4—Ca1^xiv	4.514 (2)
V1—Ca1^xii	3.7666 (15)	O4—Ca1^ii	5.093 (2)
O2^i—Ca1—O2^ii	109.64 (12)	O1—V1—O4	111.26 (9)
O2^i—Ca1—O4	152.32 (7)	O3^x—V1—O4	80.04 (8)
O2^ii—Ca1—O4	88.15 (7)	O3^xi—V1—O4	139.48 (10)
O2^i—Ca1—O4^iii	88.15 (7)	O4^iii—V1—O4	85.80 (12)
O2^ii—Ca1—O4^iii	152.32 (7)	O1—V1—V2^iii	110.691 (18)
O4—Ca1—O4^iii	68.32 (10)	O3^x—V1—V2^iii	121.50 (7)
O2^i—Ca1—O3^iii	77.32 (7)	O3^xi—V1—V2^iii	40.54 (6)
O2^ii—Ca1—O3^iii	133.30 (7)	O4^iii—V1—V2^iii	40.29 (6)
O4—Ca1—O3^iii	106.27 (8)	O4—V1—V2^iii	120.72 (7)
O4^iii—Ca1—O3^iii	70.01 (7)	O1—V1—V2	110.691 (18)
O2^i—Ca1—O3	133.30 (7)	O3^x—V1—V2	40.54 (6)
O2^ii—Ca1—O3	77.32 (7)	O3^xi—V1—V2	121.50 (7)
O4—Ca1—O3	70.01 (7)	O4^iii—V1—V2	120.72 (7)
O4^iii—Ca1—O3	106.27 (8)	O4—V1—V2	40.29 (6)
O3^iii—Ca1—O3	67.26 (10)	V2^iii—V1—V2	138.62 (4)
O2^i—Ca1—O1^iv	78.55 (6)	O1—V1—Ca1	132.23 (10)
O2^ii—Ca1—O1^iv	78.55 (6)	O3^x—V1—Ca1	105.01 (6)
O4—Ca1—O1^iv	84.75 (8)	O3^xi—V1—Ca1	105.01 (7)
O4^iii—Ca1—O1^iv	84.75 (8)	O4^iii—V1—Ca1	44.36 (6)
O3^iii—Ca1—O1^iv	145.34 (5)	O4—V1—Ca1	44.36 (6)
O3—Ca1—O1^iv	145.34 (5)	V2^iii—V1—Ca1	76.412 (18)
O2^i—Ca1—V2^v	165.30 (6)	V2—V1—Ca1	76.412 (17)
O2^ii—Ca1—V2^v	79.04 (6)	O1—V1—Ca1^x	125.30 (10)
O4—Ca1—V2^v	34.95 (5)	O3^x—V1—Ca1^x	43.91 (6)
O4^iii—Ca1—V2^v	88.59 (6)	O3^xi—V1—Ca1^x	43.91 (6)
O3^iii—Ca1—V2^v	88.10 (6)	O4^iii—V1—Ca1^x	108.05 (7)
O3—Ca1—V2^v	35.17 (5)	O4—V1—Ca1^x	108.05 (7)
O1^iv—Ca1—V2^v	115.40 (5)	V2^iii—V1—Ca1^x	78.056 (18)
O2^i—Ca1—V2^vi	79.04 (6)	V2—V1—Ca1^x	78.056 (18)
O2^ii—Ca1—V2^vi	165.30 (6)	Ca1—V1—Ca1^x	102.47 (4)
O4—Ca1—V2^vi	88.59 (6)	O1—V1—Ca1^xii	31.97 (10)
O4^iii—Ca1—V2^vi	34.95 (5)	O3^x—V1—Ca1^xii	86.34 (6)
O3^iii—Ca1—V2^vi	35.17 (5)	O3^xi—V1—Ca1^xii	86.34 (6)
O3—Ca1—V2^vi	88.10 (6)	O4^iii—V1—Ca1^xii	130.13 (6)
O1^iv—Ca1—V2^vi	115.40 (5)	O4—V1—Ca1^xii	130.13 (6)
V2^v—Ca1—V2^vi	90.15 (4)	V2^iii—V1—Ca1^xii	107.335 (17)
O2^i—Ca1—V1	117.92 (5)	V2—V1—Ca1^xii	107.335 (17)
O2^ii—Ca1—V1	117.92 (5)	Ca1—V1—Ca1^xii	164.19 (3)
O4—Ca1—V1	35.22 (5)	Ca1^x—V1—Ca1^xii	93.34 (3)
O4^iii—Ca1—V1	35.22 (5)	O1—V1—Ca1^xiii	48.49 (10)
O3^iii—Ca1—V1	95.46 (6)	O3^x—V1—Ca1^xiii	134.81 (6)
O3—Ca1—V1	95.46 (6)	O3^xi—V1—Ca1^xiii	134.81 (6)
O1^iv—Ca1—V1	74.51 (7)	O4^iii—V1—Ca1^xiii	76.33 (6)
V2^v—Ca1—V1	64.78 (2)	O4—V1—Ca1^xiii	76.33 (6)
V2^vi—Ca1—V1	64.78 (2)	V2^iii—V1—Ca1^xiii	103.692 (17)
O2^i—Ca1—V1^vii	103.11 (5)	V2—V1—Ca1^xiii	103.692 (17)
O2^ii—Ca1—V1^vii	103.11 (5)	Ca1—V1—Ca1^xiii	83.73 (3)
O4—Ca1—V1^vii	92.76 (6)	Ca1^x—V1—Ca1^xiii	173.80 (3)
O4^iii—Ca1—V1^vii	92.76 (6)	Ca1^xii—V1—Ca1^xiii	80.46 (3)
O3^iii—Ca1—V1^vii	34.09 (5)	O1—V1—Ca1^xiv	75.742 (14)
O3—Ca1—V1^vii	34.09 (5)	O3^x—V1—Ca1^xiv	54.58 (6)
O1^iv—Ca1—V1^vii	176.98 (7)	O3^xi—V1—Ca1^xiv	138.51 (6)
V2^v—Ca1—V1^vii	62.75 (2)	O4^iii—V1—Ca1^xiv	138.21 (6)
V2^vi—Ca1—V1^vii	62.75 (2)	O4—V1—Ca1^xiv	54.97 (6)
V1—Ca1—V1^vii	102.47 (4)	V2^iii—V1—Ca1^xiv	173.57 (2)
O2^i—Ca1—O1^viii	68.41 (5)	V2—V1—Ca1^xiv	34.95 (2)
O2^ii—Ca1—O1^viii	68.41 (5)	Ca1—V1—Ca1^xiv	99.293 (14)
O4—Ca1—O1^viii	139.21 (6)	Ca1^x—V1—Ca1^xiv	98.440 (15)
O4^iii—Ca1—O1^viii	139.21 (6)	Ca1^xii—V1—Ca1^xiv	78.109 (13)
O3^iii—Ca1—O1^viii	72.45 (7)	Ca1^xiii—V1—Ca1^xiv	80.369 (13)
O3—Ca1—O1^viii	72.45 (7)	O2—V2—O4^xiv	108.73 (10)
O1^iv—Ca1—O1^viii	120.15 (11)	O2—V2—O4	112.40 (10)
V2^v—Ca1—O1^viii	105.64 (4)	O4^xiv—V2—O4	138.82 (5)
V2^vi—Ca1—O1^viii	105.64 (4)	O2—V2—O3^xiv	105.98 (10)
V1—Ca1—O1^viii	165.34 (6)	O4^xiv—V2—O3^xiv	89.62 (9)
V1^vii—Ca1—O1^viii	62.87 (6)	O4—V2—O3^xiv	81.31 (9)
O2^i—Ca1—V2^i	15.73 (6)	O2—V2—O3^x	114.69 (10)
O2^ii—Ca1—V2^i	94.64 (7)	O4^xiv—V2—O3^x	81.12 (9)
O4—Ca1—V2^i	153.34 (5)	O4—V2—O3^x	80.14 (8)
O4^iii—Ca1—V2^i	100.19 (5)	O3^xiv—V2—O3^x	139.16 (4)
O3^iii—Ca1—V2^i	91.01 (5)	O2—V2—V2^v	114.19 (7)
O3—Ca1—V2^i	136.45 (6)	O4^xiv—V2—V2^v	120.64 (7)
O1^iv—Ca1—V2^i	69.93 (5)	O4—V2—V2^v	40.53 (6)
V2^v—Ca1—V2^i	170.29 (2)	O3^xiv—V2—V2^v	40.83 (6)
V2^vi—Ca1—V2^i	94.69 (3)	O3^x—V2—V2^v	113.50 (7)
V1—Ca1—V2^i	124.92 (2)	O2—V2—V2^xiv	120.54 (7)
V1^vii—Ca1—V2^i	112.27 (2)	O4^xiv—V2—V2^xiv	40.52 (6)
O1^viii—Ca1—V2^i	64.94 (4)	O4—V2—V2^xiv	111.60 (7)
O2^i—Ca1—V2^ii	94.64 (7)	O3^xiv—V2—V2^xiv	118.45 (7)
O2^ii—Ca1—V2^ii	15.73 (6)	O3^x—V2—V2^xiv	40.64 (6)
O4—Ca1—V2^ii	100.19 (5)	V2^v—V2—V2^xiv	125.26 (4)
O4^iii—Ca1—V2^ii	153.34 (5)	O2—V2—V1	127.66 (9)
O3^iii—Ca1—V2^ii	136.45 (6)	O4^xiv—V2—V1	108.86 (6)
O3—Ca1—V2^ii	91.01 (5)	O4—V2—V1	40.57 (6)
O1^iv—Ca1—V2^ii	69.93 (5)	O3^xiv—V2—V1	109.33 (6)
V2^v—Ca1—V2^ii	94.69 (3)	O3^x—V2—V1	40.36 (6)
V2^vi—Ca1—V2^ii	170.29 (2)	V2^v—V2—V1	74.18 (3)
V1—Ca1—V2^ii	124.92 (2)	V2^xiv—V2—V1	72.56 (2)
V1^vii—Ca1—V2^ii	112.27 (2)	O2—V2—Ca1^xiv	117.95 (9)
O1^viii—Ca1—V2^ii	64.94 (4)	O4^xiv—V2—Ca1^xiv	44.31 (6)
V2^i—Ca1—V2^ii	79.33 (3)	O4—V2—Ca1^xiv	113.30 (7)
O2^i—Ca1—V1^iv	68.34 (6)	O3^xiv—V2—Ca1^xiv	45.47 (6)
O2^ii—Ca1—V1^iv	68.34 (6)	O3^x—V2—Ca1^xiv	112.53 (7)
O4—Ca1—V1^iv	101.00 (6)	V2^v—V2—Ca1^xiv	79.26 (3)
O4^iii—Ca1—V1^iv	101.00 (6)	V2^xiv—V2—Ca1^xiv	76.59 (3)
O3^iii—Ca1—V1^iv	144.88 (5)	V1—V2—Ca1^xiv	114.38 (3)
O3—Ca1—V1^iv	144.88 (5)	O2—V2—Ca1^ii	23.20 (9)
O1^iv—Ca1—V1^iv	19.68 (7)	O4^xiv—V2—Ca1^ii	95.39 (6)
V2^v—Ca1—V1^iv	126.36 (2)	O4—V2—Ca1^ii	123.93 (6)
V2^vi—Ca1—V1^iv	126.36 (2)	O3^xiv—V2—Ca1^ii	87.35 (6)
V1—Ca1—V1^iv	94.20 (3)	O3^x—V2—Ca1^ii	132.90 (6)
V1^vii—Ca1—V1^iv	163.33 (3)	V2^v—V2—Ca1^ii	108.51 (3)
O1^viii—Ca1—V1^iv	100.47 (6)	V2^xiv—V2—Ca1^ii	121.86 (3)
V2^i—Ca1—V1^iv	56.28 (2)	V1—V2—Ca1^ii	150.17 (2)
V2^ii—Ca1—V1^iv	56.28 (2)	Ca1^xiv—V2—Ca1^ii	95.04 (3)
O2^i—Ca1—V2	146.02 (6)	O2—V2—Ca1	84.98 (8)
O2^ii—Ca1—V2	70.61 (6)	O4^xiv—V2—Ca1	164.65 (6)
O4—Ca1—V2	22.52 (5)	O4—V2—Ca1	27.84 (6)
O4^iii—Ca1—V2	82.76 (5)	O3^xiv—V2—Ca1	93.24 (6)
O3^iii—Ca1—V2	128.57 (6)	O3^x—V2—Ca1	86.91 (7)
O3—Ca1—V2	80.59 (5)	V2^v—V2—Ca1	56.07 (3)
O1^iv—Ca1—V2	68.08 (5)	V2^xiv—V2—Ca1	126.55 (3)
V2^v—Ca1—V2	47.347 (16)	V1—V2—Ca1	56.02 (2)
V2^vi—Ca1—V2	109.17 (3)	Ca1^xiv—V2—Ca1	135.31 (3)
V1—Ca1—V2	47.568 (17)	Ca1^ii—V2—Ca1	99.81 (2)
V1^vii—Ca1—V2	109.96 (3)	O2—V2—Ca1^x	89.27 (8)
O1^viii—Ca1—V2	134.706 (16)	O4^xiv—V2—Ca1^x	90.24 (6)
V2^i—Ca1—V2	137.44 (3)	O4—V2—Ca1^x	88.26 (6)
V2^ii—Ca1—V2	80.19 (2)	O3^xiv—V2—Ca1^x	163.92 (7)
V1^iv—Ca1—V2	81.34 (2)	O3^x—V2—Ca1^x	25.45 (6)
O2^i—Ca1—V2^iii	70.61 (6)	V2^v—V2—Ca1^x	128.06 (3)
O2^ii—Ca1—V2^iii	146.02 (6)	V2^xiv—V2—Ca1^x	54.53 (3)
O4—Ca1—V2^iii	82.76 (5)	V1—V2—Ca1^x	55.73 (2)
O4^iii—Ca1—V2^iii	22.52 (5)	Ca1^xiv—V2—Ca1^x	131.10 (3)
O3^iii—Ca1—V2^iii	80.59 (5)	Ca1^ii—V2—Ca1^x	108.67 (2)
O3—Ca1—V2^iii	128.57 (6)	Ca1—V2—Ca1^x	82.87 (3)
O1^iv—Ca1—V2^iii	68.08 (5)	V1—O1—Ca1^xii	128.35 (14)
V2^v—Ca1—V2^iii	109.17 (3)	V1—O1—Ca1^xiii	111.50 (12)
V2^vi—Ca1—V2^iii	47.347 (16)	Ca1^xii—O1—Ca1^xiii	120.15 (11)
V1—Ca1—V2^iii	47.568 (17)	V1—O1—Ca1^x	37.86 (8)
V1^vii—Ca1—V2^iii	109.96 (3)	Ca1^xii—O1—Ca1^x	90.49 (8)
O1^viii—Ca1—V2^iii	134.706 (16)	Ca1^xiii—O1—Ca1^x	149.36 (9)
V2^i—Ca1—V2^iii	80.19 (2)	V1—O1—Ca1	32.71 (7)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.06 (10)
V1^iv—Ca1—V2^iii	81.34 (2)	Ca1^xiii—O1—Ca1	78.79 (6)
V2—Ca1—V2^iii	90.53 (3)	Ca1^x—O1—Ca1	70.57 (5)
O2^i—Ca1—V2^ix	58.72 (5)	V2—O2—Ca1^ii	141.07 (14)
O2^ii—Ca1—V2^ix	127.53 (6)	V2—O2—Ca1	72.16 (8)
O4—Ca1—V2^ix	126.55 (6)	Ca1^ii—O2—Ca1	128.36 (7)
O4^iii—Ca1—V2^ix	79.65 (5)	V2—O2—Ca1^x	68.99 (8)
O3^iii—Ca1—V2^ix	20.40 (5)	Ca1^ii—O2—Ca1^x	140.61 (7)
O3—Ca1—V2^ix	80.06 (6)	Ca1—O2—Ca1^x	77.32 (5)
O1^iv—Ca1—V2^ix	134.60 (3)	V2—O2—Ca1^xiv	43.00 (7)
V2^v—Ca1—V2^ix	106.59 (3)	Ca1^ii—O2—Ca1^xiv	98.43 (7)
V2^vi—Ca1—V2^ix	46.213 (15)	Ca1—O2—Ca1^xiv	105.68 (5)
V1—Ca1—V2^ix	110.84 (3)	Ca1^x—O2—Ca1^xiv	101.97 (5)
V1^vii—Ca1—V2^ix	46.216 (16)	V1^vii—O3—V2^v	128.40 (11)
O1^viii—Ca1—V2^ix	59.76 (4)	V1^vii—O3—V2^vii	99.10 (9)
V2^i—Ca1—V2^ix	71.33 (2)	V2^v—O3—V2^vii	98.53 (9)
V2^ii—Ca1—V2^ix	124.14 (3)	V1^vii—O3—Ca1	102.00 (9)
V1^iv—Ca1—V2^ix	127.03 (2)	V2^v—O3—Ca1	99.36 (8)
V2—Ca1—V2^ix	148.94 (3)	V2^vii—O3—Ca1	134.16 (10)
V2^iii—Ca1—V2^ix	82.87 (3)	V1^vii—O3—Ca1^xiii	65.37 (6)
O2^i—Ca1—V2^vii	127.53 (6)	V2^v—O3—Ca1^xiii	64.33 (6)
O2^ii—Ca1—V2^vii	58.72 (5)	V2^vii—O3—Ca1^xiii	123.05 (8)
O4—Ca1—V2^vii	79.65 (5)	Ca1—O3—Ca1^xiii	102.74 (6)
O4^iii—Ca1—V2^vii	126.55 (6)	V1^vii—O3—Ca1^vii	48.89 (5)
O3^iii—Ca1—V2^vii	80.06 (6)	V2^v—O3—Ca1^vii	160.75 (9)
O3—Ca1—V2^vii	20.40 (5)	V2^vii—O3—Ca1^vii	65.94 (5)
O1^iv—Ca1—V2^vii	134.60 (3)	Ca1—O3—Ca1^vii	99.73 (7)
V2^v—Ca1—V2^vii	46.213 (15)	Ca1^xiii—O3—Ca1^vii	113.45 (5)
V2^vi—Ca1—V2^vii	106.59 (3)	V1^vii—O3—Ca1^v	104.60 (7)
V1—Ca1—V2^vii	110.84 (3)	V2^v—O3—Ca1^v	60.96 (6)
V1^vii—Ca1—V2^vii	46.216 (16)	V2^vii—O3—Ca1^v	43.62 (5)
O1^viii—Ca1—V2^vii	59.76 (4)	Ca1—O3—Ca1^v	153.19 (7)
V2^i—Ca1—V2^vii	124.14 (3)	Ca1^xiii—O3—Ca1^v	85.54 (4)
V2^ii—Ca1—V2^vii	71.33 (2)	Ca1^vii—O3—Ca1^v	100.15 (4)
V1^iv—Ca1—V2^vii	127.03 (2)	V2^v—O4—V2	98.95 (10)
V2—Ca1—V2^vii	82.87 (3)	V2^v—O4—V1	132.74 (11)
V2^iii—Ca1—V2^vii	148.94 (3)	V2—O4—V1	99.14 (9)
V2^ix—Ca1—V2^vii	87.31 (3)	V2^v—O4—Ca1	100.74 (8)
O2^i—Ca1—O2	132.46 (4)	V2—O4—Ca1	129.64 (10)
O2^ii—Ca1—O2	51.64 (7)	V1—O4—Ca1	100.43 (9)
O4—Ca1—O2	45.21 (6)	V2^v—O4—Ca1^xiii	58.10 (5)
O4^iii—Ca1—O2	100.69 (6)	V2—O4—Ca1^xiii	132.38 (8)
O3^iii—Ca1—O2	149.57 (6)	V1—O4—Ca1^xiii	77.69 (6)
O3—Ca1—O2	89.10 (6)	Ca1—O4—Ca1^xiii	97.08 (6)
O1^iv—Ca1—O2	56.33 (4)	V2^v—O4—Ca1^x	161.85 (8)
V2^v—Ca1—O2	62.24 (3)	V2—O4—Ca1^x	65.62 (5)
V2^vi—Ca1—O2	131.04 (4)	V1—O4—Ca1^x	47.04 (5)
V1—Ca1—O2	66.88 (3)	Ca1—O4—Ca1^x	96.73 (6)
V1^vii—Ca1—O2	122.70 (4)	Ca1^xiii—O4—Ca1^x	124.57 (5)
O1^viii—Ca1—O2	119.86 (4)	V2^v—O4—Ca1^xiv	64.01 (6)
V2^i—Ca1—O2	119.38 (4)	V2—O4—Ca1^xiv	43.18 (5)
V2^ii—Ca1—O2	58.58 (3)	V1—O4—Ca1^xiv	104.06 (7)
V1^iv—Ca1—O2	64.12 (3)	Ca1—O4—Ca1^xiv	155.36 (7)
V2—Ca1—O2	22.86 (3)	Ca1^xiii—O4—Ca1^xiv	90.81 (4)
V2^iii—Ca1—O2	101.81 (4)	Ca1^x—O4—Ca1^xiv	97.89 (4)
V2^ix—Ca1—O2	168.73 (4)	V2^v—O4—Ca1^ii	90.27 (7)
V2^vii—Ca1—O2	83.48 (4)	V2—O4—Ca1^ii	37.43 (5)
O1—V1—O3^x	109.26 (9)	V1—O4—Ca1^ii	128.27 (7)
O1—V1—O3^xi	109.26 (9)	Ca1—O4—Ca1^ii	96.67 (6)
O3^x—V1—O3^xi	86.53 (12)	Ca1^xiii—O4—Ca1^ii	147.36 (5)
O1—V1—O4^iii	111.26 (9)	Ca1^x—O4—Ca1^ii	82.80 (3)
O3^x—V1—O4^iii	139.48 (10)	Ca1^xiv—O4—Ca1^ii	65.76 (3)
O3^xi—V1—O4^iii	80.04 (8)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_206K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.540 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2711 reflections
a = 10.427 (3) Å	θ = 1.3–23.4°
b = 10.370 (2) Å	µ = 5.68 mm^−1
c = 5.2904 (15) Å	T = 206 K
V = 572.0 (2) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	403 independent reflections
Radiation source: fine-focus sealed tube	367 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.471	l = −5→5
2452 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0672P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.063	(Δ/σ)max < 0.001
S = 0.80	Δρmax = 0.33 e Å^−3
403 reflections	Δρmin = −0.41 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0188 (19)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08488 (10)	0.2500	0.29988 (16)	0.0064 (4)
V1	0.28880 (8)	0.2500	0.79212 (14)	0.0051 (4)
V2	0.18739 (6)	0.52027 (6)	0.78355 (11)	0.0051 (3)
O1	0.4437 (3)	0.2500	0.8085 (6)	0.0105 (8)*
O2	0.0398 (2)	0.5651 (3)	0.7666 (4)	0.0116 (6)*
O3	0.2205 (2)	0.3798 (2)	0.0257 (4)	0.0066 (5)*
O4	0.2268 (2)	0.3796 (2)	0.5484 (4)	0.0058 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0041 (6)	0.0069 (7)	0.0081 (6)	0.000	−0.0002 (4)	0.000
V1	0.0046 (5)	0.0048 (6)	0.0059 (5)	0.000	−0.0002 (3)	0.000
V2	0.0048 (5)	0.0049 (5)	0.0057 (4)	0.0010 (2)	−0.0001 (2)	0.0002 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.343 (3)	V1—Ca1^xiii	4.3978 (15)
Ca1—O2^ii	2.343 (3)	V1—Ca1^xiv	5.3497 (11)
Ca1—O4	2.393 (2)	V2—O2	1.610 (2)
Ca1—O4^iii	2.393 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3^iii	2.432 (2)	V2—O4	1.961 (2)
Ca1—O3	2.432 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.542 (3)	V2—O3^x	1.971 (2)
Ca1—V1	3.3620 (13)	V2—V2^xiv	2.9797 (9)
Ca1—V2^v	3.3647 (12)	V2—V2^v	2.9797 (9)
Ca1—V2^vi	3.3647 (12)	V2—Ca1^xiv	3.3647 (12)
Ca1—V1^vii	3.4260 (14)	V2—Ca1^ii	3.7323 (12)
Ca1—O1^viii	3.539 (3)	V2—Ca1^x	4.0569 (11)
Ca1—V2^i	3.7323 (12)	O1—Ca1^xii	2.542 (3)
Ca1—V2^ii	3.7323 (12)	O1—Ca1^xiii	3.539 (3)
Ca1—V1^iv	3.7670 (15)	O1—Ca1^x	4.556 (4)
Ca1—V2	3.9427 (10)	O2—Ca1^ii	2.343 (3)
Ca1—V2^iii	3.9427 (10)	O2—Ca1^x	4.343 (3)
Ca1—V2^ix	4.0569 (11)	O2—Ca1^xiv	4.361 (3)
Ca1—V2^vii	4.0569 (11)	O3—V1^vii	1.961 (2)
Ca1—O2	4.122 (3)	O3—V2^v	1.964 (2)
V1—O1	1.617 (4)	O3—V2^vii	1.971 (2)
V1—O3^x	1.961 (2)	O3—Ca1^xiii	4.135 (3)
V1—O3^xi	1.961 (2)	O3—Ca1^vii	4.308 (2)
V1—O4^iii	1.971 (2)	O3—Ca1^v	4.504 (2)
V1—O4	1.971 (2)	O4—V2^v	1.960 (2)
V1—V2^iii	2.9958 (9)	O4—Ca1^xiii	4.375 (2)
V1—V2	2.9958 (9)	O4—Ca1^x	4.450 (2)
V1—Ca1^x	3.4260 (14)	O4—Ca1^xiv	4.514 (2)
V1—Ca1^xii	3.7670 (15)	O4—Ca1^ii	5.095 (2)
O2^i—Ca1—O2^ii	109.81 (13)	O1—V1—O4	111.24 (10)
O2^i—Ca1—O4	152.28 (8)	O3^x—V1—O4	79.94 (9)
O2^ii—Ca1—O4	88.07 (8)	O3^xi—V1—O4	139.55 (10)
O2^i—Ca1—O4^iii	88.07 (8)	O4^iii—V1—O4	85.95 (13)
O2^ii—Ca1—O4^iii	152.28 (8)	O1—V1—V2^iii	110.688 (19)
O4—Ca1—O4^iii	68.33 (10)	O3^x—V1—V2^iii	121.56 (7)
O2^i—Ca1—O3^iii	77.32 (7)	O3^xi—V1—V2^iii	40.48 (6)
O2^ii—Ca1—O3^iii	133.31 (8)	O4^iii—V1—V2^iii	40.24 (6)
O4—Ca1—O3^iii	106.18 (9)	O4—V1—V2^iii	120.80 (7)
O4^iii—Ca1—O3^iii	69.96 (8)	O1—V1—V2	110.688 (19)
O2^i—Ca1—O3	133.31 (8)	O3^x—V1—V2	40.48 (6)
O2^ii—Ca1—O3	77.32 (7)	O3^xi—V1—V2	121.56 (7)
O4—Ca1—O3	69.96 (8)	O4^iii—V1—V2	120.80 (7)
O4^iii—Ca1—O3	106.18 (9)	O4—V1—V2	40.24 (6)
O3^iii—Ca1—O3	67.19 (10)	V2^iii—V1—V2	138.62 (4)
O2^i—Ca1—O1^iv	78.51 (7)	O1—V1—Ca1	132.30 (11)
O2^ii—Ca1—O1^iv	78.51 (7)	O3^x—V1—Ca1	104.98 (7)
O4—Ca1—O1^iv	84.86 (8)	O3^xi—V1—Ca1	104.98 (7)
O4^iii—Ca1—O1^iv	84.86 (8)	O4^iii—V1—Ca1	44.44 (7)
O3^iii—Ca1—O1^iv	145.39 (5)	O4—V1—Ca1	44.44 (7)
O3—Ca1—O1^iv	145.39 (5)	V2^iii—V1—Ca1	76.411 (18)
O2^i—Ca1—V1	117.86 (6)	V2—V1—Ca1	76.411 (18)
O2^ii—Ca1—V1	117.86 (6)	O1—V1—Ca1^x	125.30 (11)
O4—Ca1—V1	35.22 (5)	O3^x—V1—Ca1^x	43.98 (7)
O4^iii—Ca1—V1	35.22 (5)	O3^xi—V1—Ca1^x	43.98 (7)
O3^iii—Ca1—V1	95.40 (6)	O4^iii—V1—Ca1^x	108.02 (7)
O3—Ca1—V1	95.40 (6)	O4—V1—Ca1^x	108.02 (7)
O1^iv—Ca1—V1	74.63 (8)	V2^iii—V1—Ca1^x	78.041 (18)
O2^i—Ca1—V2^v	165.27 (6)	V2—V1—Ca1^x	78.041 (19)
O2^ii—Ca1—V2^v	78.96 (6)	Ca1—V1—Ca1^x	102.40 (4)
O4—Ca1—V2^v	34.91 (5)	O1—V1—Ca1^xii	31.89 (11)
O4^iii—Ca1—V2^v	88.57 (6)	O3^x—V1—Ca1^xii	86.36 (7)
O3^iii—Ca1—V2^v	88.05 (6)	O3^xi—V1—Ca1^xii	86.36 (7)
O3—Ca1—V2^v	35.17 (5)	O4^iii—V1—Ca1^xii	130.05 (7)
O1^iv—Ca1—V2^v	115.45 (5)	O4—V1—Ca1^xii	130.05 (7)
V1—Ca1—V2^v	64.76 (2)	V2^iii—V1—Ca1^xii	107.334 (18)
O2^i—Ca1—V2^vi	78.96 (6)	V2—V1—Ca1^xii	107.334 (18)
O2^ii—Ca1—V2^vi	165.27 (6)	Ca1—V1—Ca1^xii	164.19 (4)
O4—Ca1—V2^vi	88.57 (6)	Ca1^x—V1—Ca1^xii	93.40 (3)
O4^iii—Ca1—V2^vi	34.91 (5)	O1—V1—Ca1^xiii	48.48 (11)
O3^iii—Ca1—V2^vi	35.17 (5)	O3^x—V1—Ca1^xiii	134.73 (7)
O3—Ca1—V2^vi	88.05 (6)	O3^xi—V1—Ca1^xiii	134.73 (7)
O1^iv—Ca1—V2^vi	115.45 (5)	O4^iii—V1—Ca1^xiii	76.37 (6)
V1—Ca1—V2^vi	64.76 (2)	O4—V1—Ca1^xiii	76.37 (6)
V2^v—Ca1—V2^vi	90.15 (4)	V2^iii—V1—Ca1^xiii	103.711 (18)
O2^i—Ca1—V1^vii	103.11 (6)	V2—V1—Ca1^xiii	103.711 (18)
O2^ii—Ca1—V1^vii	103.11 (6)	Ca1—V1—Ca1^xiii	83.82 (3)
O4—Ca1—V1^vii	92.69 (6)	Ca1^x—V1—Ca1^xiii	173.77 (3)
O4^iii—Ca1—V1^vii	92.69 (6)	Ca1^xii—V1—Ca1^xiii	80.37 (3)
O3^iii—Ca1—V1^vii	34.05 (5)	O1—V1—Ca1^xiv	75.743 (14)
O3—Ca1—V1^vii	34.05 (5)	O3^x—V1—Ca1^xiv	54.51 (7)
O1^iv—Ca1—V1^vii	177.04 (8)	O3^xi—V1—Ca1^xiv	138.56 (7)
V1—Ca1—V1^vii	102.40 (4)	O4^iii—V1—Ca1^xiv	138.28 (7)
V2^v—Ca1—V1^vii	62.73 (2)	O4—V1—Ca1^xiv	54.90 (6)
V2^vi—Ca1—V1^vii	62.73 (2)	V2^iii—V1—Ca1^xiv	173.57 (3)
O2^i—Ca1—O1^viii	68.45 (6)	V2—V1—Ca1^xiv	34.95 (2)
O2^ii—Ca1—O1^viii	68.45 (6)	Ca1—V1—Ca1^xiv	99.304 (15)
O4—Ca1—O1^viii	139.21 (6)	Ca1^x—V1—Ca1^xiv	98.441 (15)
O4^iii—Ca1—O1^viii	139.21 (6)	Ca1^xii—V1—Ca1^xiv	78.101 (13)
O3^iii—Ca1—O1^viii	72.52 (7)	Ca1^xiii—V1—Ca1^xiv	80.364 (13)
O3—Ca1—O1^viii	72.52 (7)	O2—V2—O4^xiv	108.84 (11)
O1^iv—Ca1—O1^viii	120.02 (12)	O2—V2—O4	112.34 (11)
V1—Ca1—O1^viii	165.35 (7)	O4^xiv—V2—O4	138.77 (5)
V2^v—Ca1—O1^viii	105.68 (4)	O2—V2—O3^xiv	106.02 (11)
V2^vi—Ca1—O1^viii	105.68 (4)	O4^xiv—V2—O3^xiv	89.64 (10)
V1^vii—Ca1—O1^viii	62.95 (6)	O4—V2—O3^xiv	81.35 (9)
O2^i—Ca1—V2^i	15.81 (6)	O2—V2—O3^x	114.67 (11)
O2^ii—Ca1—V2^i	94.72 (7)	O4^xiv—V2—O3^x	81.20 (9)
O4—Ca1—V2^i	153.38 (6)	O4—V2—O3^x	79.95 (9)
O4^iii—Ca1—V2^i	100.20 (5)	O3^xiv—V2—O3^x	139.12 (5)
O3^iii—Ca1—V2^i	91.07 (5)	O2—V2—V2^xiv	120.60 (8)
O3—Ca1—V2^i	136.46 (6)	O4^xiv—V2—V2^xiv	40.55 (6)
O1^iv—Ca1—V2^i	69.87 (6)	O4—V2—V2^xiv	111.49 (7)
V1—Ca1—V2^i	124.94 (2)	O3^xiv—V2—V2^xiv	118.47 (7)
V2^v—Ca1—V2^i	170.30 (3)	O3^x—V2—V2^xiv	40.69 (6)
V2^vi—Ca1—V2^i	94.70 (2)	O2—V2—V2^v	114.21 (8)
V1^vii—Ca1—V2^i	112.30 (2)	O4^xiv—V2—V2^v	120.62 (7)
O1^viii—Ca1—V2^i	64.91 (4)	O4—V2—V2^v	40.53 (6)
O2^i—Ca1—V2^ii	94.72 (7)	O3^xiv—V2—V2^v	40.86 (7)
O2^ii—Ca1—V2^ii	15.81 (6)	O3^x—V2—V2^v	113.33 (7)
O4—Ca1—V2^ii	100.20 (5)	V2^xiv—V2—V2^v	125.18 (5)
O4^iii—Ca1—V2^ii	153.38 (6)	O2—V2—V1	127.48 (10)
O3^iii—Ca1—V2^ii	136.46 (6)	O4^xiv—V2—V1	108.89 (7)
O3—Ca1—V2^ii	91.07 (5)	O4—V2—V1	40.49 (6)
O1^iv—Ca1—V2^ii	69.87 (6)	O3^xiv—V2—V1	109.37 (7)
V1—Ca1—V2^ii	124.94 (2)	O3^x—V2—V1	40.24 (6)
V2^v—Ca1—V2^ii	94.70 (2)	V2^xiv—V2—V1	72.54 (3)
V2^vi—Ca1—V2^ii	170.30 (3)	V2^v—V2—V1	74.14 (3)
V1^vii—Ca1—V2^ii	112.30 (2)	O2—V2—Ca1^xiv	118.12 (10)
O1^viii—Ca1—V2^ii	64.91 (4)	O4^xiv—V2—Ca1^xiv	44.31 (6)
V2^i—Ca1—V2^ii	79.33 (4)	O4—V2—Ca1^xiv	113.27 (7)
O2^i—Ca1—V1^iv	68.35 (6)	O3^xiv—V2—Ca1^xiv	45.50 (7)
O2^ii—Ca1—V1^iv	68.35 (6)	O3^x—V2—Ca1^xiv	112.53 (7)
O4—Ca1—V1^iv	101.08 (6)	V2^xiv—V2—Ca1^xiv	76.58 (3)
O4^iii—Ca1—V1^iv	101.08 (6)	V2^v—V2—Ca1^xiv	79.25 (3)
O3^iii—Ca1—V1^iv	144.92 (5)	V1—V2—Ca1^xiv	114.38 (3)
O3—Ca1—V1^iv	144.92 (5)	O2—V2—Ca1^ii	23.36 (10)
O1^iv—Ca1—V1^iv	19.64 (8)	O4^xiv—V2—Ca1^ii	95.36 (7)
V1—Ca1—V1^iv	94.27 (3)	O4—V2—Ca1^ii	124.02 (6)
V2^v—Ca1—V1^iv	126.38 (2)	O3^xiv—V2—Ca1^ii	87.30 (7)
V2^vi—Ca1—V1^iv	126.38 (2)	O3^x—V2—Ca1^ii	133.01 (7)
V1^vii—Ca1—V1^iv	163.32 (4)	V2^xiv—V2—Ca1^ii	121.89 (3)
O1^viii—Ca1—V1^iv	100.37 (6)	V2^v—V2—Ca1^ii	108.56 (3)
V2^i—Ca1—V1^iv	56.24 (2)	V1—V2—Ca1^ii	150.16 (3)
V2^ii—Ca1—V1^iv	56.24 (2)	Ca1^xiv—V2—Ca1^ii	95.05 (2)
O2^i—Ca1—V2	146.04 (6)	O2—V2—Ca1	84.84 (9)
O2^ii—Ca1—V2	70.50 (6)	O4^xiv—V2—Ca1	164.65 (7)
O4—Ca1—V2	22.55 (5)	O4—V2—Ca1	27.90 (6)
O4^iii—Ca1—V2	82.81 (6)	O3^xiv—V2—Ca1	93.27 (7)
O3^iii—Ca1—V2	128.51 (6)	O3^x—V2—Ca1	86.78 (7)
O3—Ca1—V2	80.57 (6)	V2^xiv—V2—Ca1	126.49 (3)
O1^iv—Ca1—V2	68.16 (5)	V2^v—V2—Ca1	56.11 (3)
V1—Ca1—V2	47.609 (16)	V1—V2—Ca1	55.98 (2)
V2^v—Ca1—V2	47.316 (15)	Ca1^xiv—V2—Ca1	135.34 (3)
V2^vi—Ca1—V2	109.18 (3)	Ca1^ii—V2—Ca1	99.83 (2)
V1^vii—Ca1—V2	109.91 (3)	O2—V2—Ca1^x	89.16 (9)
O1^viii—Ca1—V2	134.666 (15)	O4^xiv—V2—Ca1^x	90.28 (7)
V2^i—Ca1—V2	137.45 (3)	O4—V2—Ca1^x	88.19 (7)
V2^ii—Ca1—V2	80.17 (2)	O3^xiv—V2—Ca1^x	163.96 (7)
V1^iv—Ca1—V2	81.39 (2)	O3^x—V2—Ca1^x	25.54 (7)
O2^i—Ca1—V2^iii	70.50 (6)	V2^xiv—V2—Ca1^x	54.57 (3)
O2^ii—Ca1—V2^iii	146.04 (6)	V2^v—V2—Ca1^x	128.01 (3)
O4—Ca1—V2^iii	82.81 (6)	V1—V2—Ca1^x	55.71 (2)
O4^iii—Ca1—V2^iii	22.55 (5)	Ca1^xiv—V2—Ca1^x	131.13 (3)
O3^iii—Ca1—V2^iii	80.57 (6)	Ca1^ii—V2—Ca1^x	108.67 (2)
O3—Ca1—V2^iii	128.51 (6)	Ca1—V2—Ca1^x	82.79 (2)
O1^iv—Ca1—V2^iii	68.16 (5)	V1—O1—Ca1^xii	128.46 (16)
V1—Ca1—V2^iii	47.609 (16)	V1—O1—Ca1^xiii	111.52 (14)
V2^v—Ca1—V2^iii	109.18 (3)	Ca1^xii—O1—Ca1^xiii	120.02 (12)
V2^vi—Ca1—V2^iii	47.316 (15)	V1—O1—Ca1^x	37.86 (9)
V1^vii—Ca1—V2^iii	109.91 (3)	Ca1^xii—O1—Ca1^x	90.60 (8)
O1^viii—Ca1—V2^iii	134.666 (15)	Ca1^xiii—O1—Ca1^x	149.38 (10)
V2^i—Ca1—V2^iii	80.17 (2)	V1—O1—Ca1	32.66 (8)
V2^ii—Ca1—V2^iii	137.45 (3)	Ca1^xii—O1—Ca1	161.12 (11)
V1^iv—Ca1—V2^iii	81.39 (2)	Ca1^xiii—O1—Ca1	78.86 (6)
V2—Ca1—V2^iii	90.61 (3)	Ca1^x—O1—Ca1	70.52 (6)
O2^i—Ca1—V2^ix	58.67 (6)	V2—O2—Ca1^ii	140.83 (15)
O2^ii—Ca1—V2^ix	127.62 (6)	V2—O2—Ca1	72.27 (9)
O4—Ca1—V2^ix	126.51 (6)	Ca1^ii—O2—Ca1	128.46 (8)
O4^iii—Ca1—V2^ix	79.58 (5)	V2—O2—Ca1^x	69.08 (8)
O3^iii—Ca1—V2^ix	20.44 (5)	Ca1^ii—O2—Ca1^x	140.64 (8)
O3—Ca1—V2^ix	80.06 (6)	Ca1—O2—Ca1^x	77.31 (5)
O1^iv—Ca1—V2^ix	134.55 (3)	V2—O2—Ca1^xiv	42.88 (8)
V1—Ca1—V2^ix	110.79 (3)	Ca1^ii—O2—Ca1^xiv	98.30 (8)
V2^v—Ca1—V2^ix	106.61 (3)	Ca1—O2—Ca1^xiv	105.69 (5)
V2^vi—Ca1—V2^ix	46.184 (15)	Ca1^x—O2—Ca1^xiv	101.98 (5)
V1^vii—Ca1—V2^ix	46.254 (16)	V1^vii—O3—V2^v	128.49 (11)
O1^viii—Ca1—V2^ix	59.82 (4)	V1^vii—O3—V2^vii	99.28 (9)
V2^i—Ca1—V2^ix	71.33 (2)	V2^v—O3—V2^vii	98.45 (10)
V2^ii—Ca1—V2^ix	124.18 (3)	V1^vii—O3—Ca1	101.97 (10)
V1^iv—Ca1—V2^ix	127.00 (2)	V2^v—O3—Ca1	99.33 (9)
V2—Ca1—V2^ix	148.94 (4)	V2^vii—O3—Ca1	134.02 (11)
V2^iii—Ca1—V2^ix	82.79 (2)	V1^vii—O3—Ca1^xiii	65.39 (6)
O2^i—Ca1—V2^vii	127.62 (6)	V2^v—O3—Ca1^xiii	64.37 (6)
O2^ii—Ca1—V2^vii	58.67 (6)	V2^vii—O3—Ca1^xiii	123.14 (8)
O4—Ca1—V2^vii	79.58 (5)	Ca1—O3—Ca1^xiii	102.78 (7)
O4^iii—Ca1—V2^vii	126.51 (6)	V1^vii—O3—Ca1^vii	48.93 (5)
O3^iii—Ca1—V2^vii	80.06 (6)	V2^v—O3—Ca1^vii	160.82 (9)
O3—Ca1—V2^vii	20.44 (5)	V2^vii—O3—Ca1^vii	66.04 (6)
O1^iv—Ca1—V2^vii	134.55 (3)	Ca1—O3—Ca1^vii	99.67 (7)
V1—Ca1—V2^vii	110.79 (3)	Ca1^xiii—O3—Ca1^vii	113.51 (5)
V2^v—Ca1—V2^vii	46.184 (15)	V1^vii—O3—Ca1^v	104.72 (8)
V2^vi—Ca1—V2^vii	106.61 (3)	V2^v—O3—Ca1^v	60.92 (6)
V1^vii—Ca1—V2^vii	46.254 (16)	V2^vii—O3—Ca1^v	43.64 (5)
O1^viii—Ca1—V2^vii	59.82 (4)	Ca1—O3—Ca1^v	153.11 (8)
V2^i—Ca1—V2^vii	124.18 (3)	Ca1^xiii—O3—Ca1^v	85.56 (4)
V2^ii—Ca1—V2^vii	71.33 (2)	Ca1^vii—O3—Ca1^v	100.24 (5)
V1^iv—Ca1—V2^vii	127.00 (2)	V2^v—O4—V2	98.91 (10)
V2—Ca1—V2^vii	82.79 (2)	V2^v—O4—V1	132.78 (11)
V2^iii—Ca1—V2^vii	148.94 (4)	V2—O4—V1	99.27 (9)
V2^ix—Ca1—V2^vii	87.39 (3)	V2^v—O4—Ca1	100.78 (9)
O2^i—Ca1—O2	132.47 (4)	V2—O4—Ca1	129.54 (10)
O2^ii—Ca1—O2	51.54 (8)	V1—O4—Ca1	100.34 (9)
O4—Ca1—O2	45.27 (6)	V2^v—O4—Ca1^xiii	58.15 (6)
O4^iii—Ca1—O2	100.75 (7)	V2—O4—Ca1^xiii	132.43 (9)
O3^iii—Ca1—O2	149.54 (7)	V1—O4—Ca1^xiii	77.66 (6)
O3—Ca1—O2	89.13 (6)	Ca1—O4—Ca1^xiii	97.12 (6)
O1^iv—Ca1—O2	56.35 (4)	V2^v—O4—Ca1^x	161.89 (9)
V1—Ca1—O2	66.93 (4)	V2—O4—Ca1^x	65.68 (6)
V2^v—Ca1—O2	62.26 (4)	V1—O4—Ca1^x	47.07 (5)
V2^vi—Ca1—O2	131.07 (4)	Ca1—O4—Ca1^x	96.64 (7)
V1^vii—Ca1—O2	122.70 (4)	Ca1^xiii—O4—Ca1^x	124.57 (5)
O1^viii—Ca1—O2	119.82 (4)	V2^v—O4—Ca1^xiv	63.98 (6)
V2^i—Ca1—O2	119.35 (5)	V2—O4—Ca1^xiv	43.21 (5)
V2^ii—Ca1—O2	58.55 (4)	V1—O4—Ca1^xiv	104.16 (8)
V1^iv—Ca1—O2	64.12 (4)	Ca1—O4—Ca1^xiv	155.34 (8)
V2—Ca1—O2	22.89 (3)	Ca1^xiii—O4—Ca1^xiv	90.82 (4)
V2^iii—Ca1—O2	101.87 (4)	Ca1^x—O4—Ca1^xiv	97.95 (5)
V2^ix—Ca1—O2	168.77 (4)	V2^v—O4—Ca1^ii	90.24 (7)
V2^vii—Ca1—O2	83.44 (4)	V2—O4—Ca1^ii	37.38 (5)
O1—V1—O3^x	109.21 (10)	V1—O4—Ca1^ii	128.32 (8)
O1—V1—O3^xi	109.21 (10)	Ca1—O4—Ca1^ii	96.62 (6)
O3^x—V1—O3^xi	86.67 (13)	Ca1^xiii—O4—Ca1^ii	147.38 (5)
O1—V1—O4^iii	111.24 (10)	Ca1^x—O4—Ca1^ii	82.80 (3)
O3^x—V1—O4^iii	139.55 (10)	Ca1^xiv—O4—Ca1^ii	65.77 (3)
O3^xi—V1—O4^iii	79.94 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_200K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.542 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2728 reflections
a = 10.426 (3) Å	θ = 1.3–23.4°
b = 10.367 (2) Å	µ = 5.68 mm^−1
c = 5.2909 (15) Å	T = 200 K
V = 571.8 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	401 independent reflections
Radiation source: fine-focus sealed tube	363 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.471	l = −5→5
2460 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0493P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.057	(Δ/σ)max < 0.001
S = 0.93	Δρmax = 0.27 e Å^−3
401 reflections	Δρmin = −0.32 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.020 (2)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08481 (10)	0.2500	0.29974 (15)	0.0063 (3)
V1	0.28883 (7)	0.2500	0.79219 (13)	0.0051 (3)
V2	0.18737 (6)	0.52020 (6)	0.78357 (10)	0.0051 (3)
O1	0.4436 (3)	0.2500	0.8083 (5)	0.0103 (8)*
O2	0.0397 (2)	0.5656 (2)	0.7663 (4)	0.0113 (6)*
O3	0.22039 (19)	0.3797 (2)	0.0260 (4)	0.0060 (5)*
O4	0.22680 (19)	0.3795 (2)	0.5480 (4)	0.0058 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0047 (5)	0.0065 (6)	0.0076 (6)	0.000	−0.0003 (3)	0.000
V1	0.0047 (5)	0.0050 (6)	0.0055 (5)	0.000	−0.0004 (3)	0.000
V2	0.0049 (4)	0.0048 (5)	0.0055 (4)	0.0008 (2)	0.0001 (2)	0.0001 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.337 (3)	V1—Ca1^xiii	4.3966 (15)
Ca1—O2^ii	2.337 (3)	V1—Ca1^xiv	5.3483 (12)
Ca1—O4	2.392 (2)	V2—O2	1.613 (2)
Ca1—O4^iii	2.392 (2)	V2—O4^xiv	1.959 (2)
Ca1—O3^iii	2.430 (2)	V2—O4	1.962 (2)
Ca1—O3	2.430 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.543 (3)	V2—O3^x	1.971 (2)
Ca1—V1	3.3635 (13)	V2—V2^xiv	2.9798 (9)
Ca1—V2^v	3.3652 (11)	V2—V2^v	2.9798 (9)
Ca1—V2^vi	3.3652 (11)	V2—Ca1^xiv	3.3652 (11)
Ca1—V1^vii	3.4258 (13)	V2—Ca1^ii	3.7311 (11)
Ca1—O1^viii	3.538 (3)	V2—Ca1^x	4.0556 (10)
Ca1—V2^i	3.7311 (11)	O1—Ca1^xii	2.543 (3)
Ca1—V2^ii	3.7311 (11)	O1—Ca1^xiii	3.538 (3)
Ca1—V1^iv	3.7661 (14)	O1—Ca1^x	4.556 (3)
Ca1—V2	3.9424 (10)	O2—Ca1^ii	2.337 (3)
Ca1—V2^iii	3.9424 (10)	O2—Ca1^x	4.346 (2)
Ca1—V2^ix	4.0556 (10)	O2—Ca1^xiv	4.360 (3)
Ca1—V2^vii	4.0556 (10)	O3—V1^vii	1.962 (2)
Ca1—O2	4.125 (2)	O3—V2^v	1.964 (2)
V1—O1	1.616 (3)	O3—V2^vii	1.971 (2)
V1—O3^x	1.962 (2)	O3—Ca1^xiii	4.134 (2)
V1—O3^xi	1.962 (2)	O3—Ca1^vii	4.310 (2)
V1—O4^iii	1.972 (2)	O3—Ca1^v	4.505 (2)
V1—O4	1.972 (2)	O4—V2^v	1.959 (2)
V1—V2^iii	2.9946 (9)	O4—Ca1^xiii	4.373 (2)
V1—V2	2.9946 (9)	O4—Ca1^x	4.451 (2)
V1—Ca1^x	3.4258 (13)	O4—Ca1^xiv	4.515 (2)
V1—Ca1^xii	3.7661 (14)	O4—Ca1^ii	5.094 (2)
O2^i—Ca1—O2^ii	109.78 (12)	O1—V1—O4	111.23 (10)
O2^i—Ca1—O4	152.27 (8)	O3^x—V1—O4	80.04 (9)
O2^ii—Ca1—O4	88.09 (7)	O3^xi—V1—O4	139.51 (10)
O2^i—Ca1—O4^iii	88.09 (7)	O4^iii—V1—O4	85.81 (12)
O2^ii—Ca1—O4^iii	152.27 (8)	O1—V1—V2^iii	110.705 (19)
O4—Ca1—O4^iii	68.30 (10)	O3^x—V1—V2^iii	121.50 (7)
O2^i—Ca1—O3^iii	77.36 (7)	O3^xi—V1—V2^iii	40.52 (6)
O2^ii—Ca1—O3^iii	133.37 (8)	O4^iii—V1—V2^iii	40.30 (6)
O4—Ca1—O3^iii	106.14 (8)	O4—V1—V2^iii	120.73 (7)
O4^iii—Ca1—O3^iii	69.91 (7)	O1—V1—V2	110.705 (19)
O2^i—Ca1—O3	133.37 (8)	O3^x—V1—V2	40.52 (6)
O2^ii—Ca1—O3	77.36 (7)	O3^xi—V1—V2	121.50 (7)
O4—Ca1—O3	69.91 (7)	O4^iii—V1—V2	120.73 (7)
O4^iii—Ca1—O3	106.14 (8)	O4—V1—V2	40.30 (6)
O3^iii—Ca1—O3	67.22 (10)	V2^iii—V1—V2	138.59 (4)
O2^i—Ca1—O1^iv	78.49 (7)	O1—V1—Ca1	132.26 (11)
O2^ii—Ca1—O1^iv	78.49 (7)	O3^x—V1—Ca1	104.98 (7)
O4—Ca1—O1^iv	84.85 (8)	O3^xi—V1—Ca1	104.98 (7)
O4^iii—Ca1—O1^iv	84.85 (8)	O4^iii—V1—Ca1	44.38 (6)
O3^iii—Ca1—O1^iv	145.36 (5)	O4—V1—Ca1	44.38 (6)
O3—Ca1—O1^iv	145.36 (5)	V2^iii—V1—Ca1	76.397 (18)
O2^i—Ca1—V1	117.84 (6)	V2—V1—Ca1	76.397 (18)
O2^ii—Ca1—V1	117.84 (6)	O1—V1—Ca1^x	125.35 (11)
O4—Ca1—V1	35.22 (5)	O3^x—V1—Ca1^x	43.93 (6)
O4^iii—Ca1—V1	35.22 (5)	O3^xi—V1—Ca1^x	43.93 (6)
O3^iii—Ca1—V1	95.38 (6)	O4^iii—V1—Ca1^x	108.05 (7)
O3—Ca1—V1	95.38 (6)	O4—V1—Ca1^x	108.05 (7)
O1^iv—Ca1—V1	74.59 (8)	V2^iii—V1—Ca1^x	78.030 (18)
O2^i—Ca1—V2^v	165.31 (6)	V2—V1—Ca1^x	78.030 (18)
O2^ii—Ca1—V2^v	78.99 (6)	Ca1—V1—Ca1^x	102.39 (4)
O4—Ca1—V2^v	34.88 (5)	O1—V1—Ca1^xii	31.95 (10)
O4^iii—Ca1—V2^v	88.54 (6)	O3^x—V1—Ca1^xii	86.36 (6)
O3^iii—Ca1—V2^v	88.06 (6)	O3^xi—V1—Ca1^xii	86.36 (6)
O3—Ca1—V2^v	35.16 (5)	O4^iii—V1—Ca1^xii	130.10 (6)
O1^iv—Ca1—V2^v	115.42 (5)	O4—V1—Ca1^xii	130.10 (6)
V1—Ca1—V2^v	64.74 (2)	V2^iii—V1—Ca1^xii	107.347 (17)
O2^i—Ca1—V2^vi	78.99 (6)	V2—V1—Ca1^xii	107.347 (17)
O2^ii—Ca1—V2^vi	165.31 (6)	Ca1—V1—Ca1^xii	164.21 (3)
O4—Ca1—V2^vi	88.54 (6)	Ca1^x—V1—Ca1^xii	93.40 (3)
O4^iii—Ca1—V2^vi	34.88 (5)	O1—V1—Ca1^xiii	48.45 (10)
O3^iii—Ca1—V2^vi	35.16 (5)	O3^x—V1—Ca1^xiii	134.79 (7)
O3—Ca1—V2^vi	88.06 (6)	O3^xi—V1—Ca1^xiii	134.79 (7)
O1^iv—Ca1—V2^vi	115.42 (5)	O4^iii—V1—Ca1^xiii	76.32 (6)
V1—Ca1—V2^vi	64.74 (2)	O4—V1—Ca1^xiii	76.32 (6)
V2^v—Ca1—V2^vi	90.13 (4)	V2^iii—V1—Ca1^xiii	103.714 (17)
O2^i—Ca1—V1^vii	103.16 (6)	V2—V1—Ca1^xiii	103.714 (17)
O2^ii—Ca1—V1^vii	103.16 (6)	Ca1—V1—Ca1^xiii	83.80 (3)
O4—Ca1—V1^vii	92.65 (6)	Ca1^x—V1—Ca1^xiii	173.81 (3)
O4^iii—Ca1—V1^vii	92.65 (6)	Ca1^xii—V1—Ca1^xiii	80.41 (3)
O3^iii—Ca1—V1^vii	34.07 (5)	O1—V1—Ca1^xiv	75.737 (14)
O3—Ca1—V1^vii	34.07 (5)	O3^x—V1—Ca1^xiv	54.58 (6)
O1^iv—Ca1—V1^vii	176.98 (8)	O3^xi—V1—Ca1^xiv	138.53 (6)
V1—Ca1—V1^vii	102.39 (4)	O4^iii—V1—Ca1^xiv	138.20 (6)
V2^v—Ca1—V1^vii	62.73 (2)	O4—V1—Ca1^xiv	54.96 (6)
V2^vi—Ca1—V1^vii	62.73 (2)	V2^iii—V1—Ca1^xiv	173.56 (3)
O2^i—Ca1—O1^viii	68.47 (6)	V2—V1—Ca1^xiv	34.97 (2)
O2^ii—Ca1—O1^viii	68.47 (6)	Ca1—V1—Ca1^xiv	99.297 (15)
O4—Ca1—O1^viii	139.20 (6)	Ca1^x—V1—Ca1^xiv	98.458 (15)
O4^iii—Ca1—O1^viii	139.20 (6)	Ca1^xii—V1—Ca1^xiv	78.106 (13)
O3^iii—Ca1—O1^viii	72.54 (7)	Ca1^xiii—V1—Ca1^xiv	80.354 (13)
O3—Ca1—O1^viii	72.54 (7)	O2—V2—O4^xiv	108.76 (10)
O1^iv—Ca1—O1^viii	120.06 (12)	O2—V2—O4	112.40 (10)
V1—Ca1—O1^viii	165.35 (6)	O4^xiv—V2—O4	138.79 (5)
V2^v—Ca1—O1^viii	105.69 (4)	O2—V2—O3^xiv	105.91 (10)
V2^vi—Ca1—O1^viii	105.69 (4)	O4^xiv—V2—O3^xiv	89.52 (9)
V1^vii—Ca1—O1^viii	62.96 (6)	O4—V2—O3^xiv	81.33 (9)
O2^i—Ca1—V2^i	15.77 (6)	O2—V2—O3^x	114.79 (11)
O2^ii—Ca1—V2^i	94.72 (7)	O4^xiv—V2—O3^x	81.22 (9)
O4—Ca1—V2^i	153.39 (6)	O4—V2—O3^x	80.07 (9)
O4^iii—Ca1—V2^i	100.21 (5)	O3^xiv—V2—O3^x	139.13 (5)
O3^iii—Ca1—V2^i	91.07 (5)	O2—V2—V2^xiv	120.65 (7)
O3—Ca1—V2^i	136.50 (6)	O4^xiv—V2—V2^xiv	40.58 (6)
O1^iv—Ca1—V2^i	69.89 (6)	O4—V2—V2^xiv	111.57 (7)
V1—Ca1—V2^i	124.92 (2)	O3^xiv—V2—V2^xiv	118.40 (7)
V2^v—Ca1—V2^i	170.33 (3)	O3^x—V2—V2^xiv	40.69 (6)
V2^vi—Ca1—V2^i	94.69 (2)	O2—V2—V2^v	114.16 (7)
V1^vii—Ca1—V2^i	112.31 (2)	O4^xiv—V2—V2^v	120.56 (7)
O1^viii—Ca1—V2^i	64.93 (4)	O4—V2—V2^v	40.51 (6)
O2^i—Ca1—V2^ii	94.72 (7)	O3^xiv—V2—V2^v	40.86 (6)
O2^ii—Ca1—V2^ii	15.77 (6)	O3^x—V2—V2^v	113.41 (7)
O4—Ca1—V2^ii	100.21 (5)	V2^xiv—V2—V2^v	125.19 (4)
O4^iii—Ca1—V2^ii	153.39 (6)	O2—V2—V1	127.67 (10)
O3^iii—Ca1—V2^ii	136.50 (6)	O4^xiv—V2—V1	108.91 (7)
O3—Ca1—V2^ii	91.07 (5)	O4—V2—V1	40.56 (6)
O1^iv—Ca1—V2^ii	69.89 (6)	O3^xiv—V2—V1	109.37 (7)
V1—Ca1—V2^ii	124.92 (2)	O3^x—V2—V1	40.29 (6)
V2^v—Ca1—V2^ii	94.69 (2)	V2^xiv—V2—V1	72.55 (3)
V2^vi—Ca1—V2^ii	170.33 (3)	V2^v—V2—V1	74.17 (3)
V1^vii—Ca1—V2^ii	112.31 (2)	O2—V2—Ca1^xiv	117.96 (10)
O1^viii—Ca1—V2^ii	64.93 (4)	O4^xiv—V2—Ca1^xiv	44.27 (6)
V2^i—Ca1—V2^ii	79.36 (3)	O4—V2—Ca1^xiv	113.24 (7)
O2^i—Ca1—V1^iv	68.33 (6)	O3^xiv—V2—Ca1^xiv	45.43 (6)
O2^ii—Ca1—V1^iv	68.33 (6)	O3^x—V2—Ca1^xiv	112.53 (7)
O4—Ca1—V1^iv	101.08 (6)	V2^xiv—V2—Ca1^xiv	76.56 (3)
O4^iii—Ca1—V1^iv	101.08 (6)	V2^v—V2—Ca1^xiv	79.21 (3)
O3^iii—Ca1—V1^iv	144.92 (5)	V1—V2—Ca1^xiv	114.36 (3)
O3—Ca1—V1^iv	144.92 (5)	O2—V2—Ca1^ii	23.20 (9)
O1^iv—Ca1—V1^iv	19.66 (7)	O4^xiv—V2—Ca1^ii	95.33 (6)
V1—Ca1—V1^iv	94.25 (3)	O4—V2—Ca1^ii	123.99 (6)
V2^v—Ca1—V1^iv	126.36 (2)	O3^xiv—V2—Ca1^ii	87.32 (6)
V2^vi—Ca1—V1^iv	126.36 (2)	O3^x—V2—Ca1^ii	132.96 (6)
V1^vii—Ca1—V1^iv	163.36 (3)	V2^xiv—V2—Ca1^ii	121.87 (3)
O1^viii—Ca1—V1^iv	100.40 (6)	V2^v—V2—Ca1^ii	108.55 (3)
V2^i—Ca1—V1^iv	56.26 (2)	V1—V2—Ca1^ii	150.19 (3)
V2^ii—Ca1—V1^iv	56.26 (2)	Ca1^xiv—V2—Ca1^ii	95.04 (2)
O2^i—Ca1—V2	145.99 (6)	O2—V2—Ca1	84.93 (9)
O2^ii—Ca1—V2	70.52 (6)	O4^xiv—V2—Ca1	164.69 (7)
O4—Ca1—V2	22.57 (5)	O4—V2—Ca1	27.90 (6)
O4^iii—Ca1—V2	82.78 (6)	O3^xiv—V2—Ca1	93.30 (6)
O3^iii—Ca1—V2	128.50 (6)	O3^x—V2—Ca1	86.85 (7)
O3—Ca1—V2	80.56 (5)	V2^xiv—V2—Ca1	126.54 (3)
O1^iv—Ca1—V2	68.13 (5)	V2^v—V2—Ca1	56.12 (2)
V1—Ca1—V2	47.584 (16)	V1—V2—Ca1	56.02 (2)
V2^v—Ca1—V2	47.319 (15)	Ca1^xiv—V2—Ca1	135.31 (3)
V2^vi—Ca1—V2	109.15 (3)	Ca1^ii—V2—Ca1	99.83 (2)
V1^vii—Ca1—V2	109.91 (3)	O2—V2—Ca1^x	89.31 (8)
O1^viii—Ca1—V2	134.692 (15)	O4^xiv—V2—Ca1^x	90.34 (6)
V2^i—Ca1—V2	137.44 (3)	O4—V2—Ca1^x	88.25 (7)
V2^ii—Ca1—V2	80.17 (2)	O3^xiv—V2—Ca1^x	163.96 (7)
V1^iv—Ca1—V2	81.37 (2)	O3^x—V2—Ca1^x	25.51 (6)
O2^i—Ca1—V2^iii	70.52 (6)	V2^xiv—V2—Ca1^x	54.59 (2)
O2^ii—Ca1—V2^iii	145.99 (6)	V2^v—V2—Ca1^x	128.04 (3)
O4—Ca1—V2^iii	82.78 (5)	V1—V2—Ca1^x	55.72 (2)
O4^iii—Ca1—V2^iii	22.57 (5)	Ca1^xiv—V2—Ca1^x	131.14 (2)
O3^iii—Ca1—V2^iii	80.56 (5)	Ca1^ii—V2—Ca1^x	108.66 (2)
O3—Ca1—V2^iii	128.50 (6)	Ca1—V2—Ca1^x	82.82 (2)
O1^iv—Ca1—V2^iii	68.13 (5)	V1—O1—Ca1^xii	128.39 (15)
V1—Ca1—V2^iii	47.584 (16)	V1—O1—Ca1^xiii	111.55 (13)
V2^v—Ca1—V2^iii	109.15 (3)	Ca1^xii—O1—Ca1^xiii	120.06 (11)
V2^vi—Ca1—V2^iii	47.319 (15)	V1—O1—Ca1^x	37.83 (8)
V1^vii—Ca1—V2^iii	109.91 (3)	Ca1^xii—O1—Ca1^x	90.57 (8)
O1^viii—Ca1—V2^iii	134.692 (15)	Ca1^xiii—O1—Ca1^x	149.38 (9)
V2^i—Ca1—V2^iii	80.17 (2)	V1—O1—Ca1	32.70 (8)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.09 (11)
V1^iv—Ca1—V2^iii	81.37 (2)	Ca1^xiii—O1—Ca1	78.85 (6)
V2—Ca1—V2^iii	90.55 (3)	Ca1^x—O1—Ca1	70.52 (5)
O2^i—Ca1—V2^ix	58.72 (5)	V2—O2—Ca1^ii	141.03 (14)
O2^ii—Ca1—V2^ix	127.64 (6)	V2—O2—Ca1	72.16 (8)
O4—Ca1—V2^ix	126.47 (6)	Ca1^ii—O2—Ca1	128.51 (7)
O4^iii—Ca1—V2^ix	79.57 (5)	V2—O2—Ca1^x	68.91 (8)
O3^iii—Ca1—V2^ix	20.44 (5)	Ca1^ii—O2—Ca1^x	140.62 (7)
O3—Ca1—V2^ix	80.07 (6)	Ca1—O2—Ca1^x	77.25 (5)
O1^iv—Ca1—V2^ix	134.57 (3)	V2—O2—Ca1^xiv	42.98 (7)
V1—Ca1—V2^ix	110.79 (3)	Ca1^ii—O2—Ca1^xiv	98.40 (8)
V2^v—Ca1—V2^ix	106.60 (3)	Ca1—O2—Ca1^xiv	105.64 (5)
V2^vi—Ca1—V2^ix	46.199 (15)	Ca1^x—O2—Ca1^xiv	101.92 (5)
V1^vii—Ca1—V2^ix	46.246 (15)	V1^vii—O3—V2^v	128.43 (11)
O1^viii—Ca1—V2^ix	59.82 (4)	V1^vii—O3—V2^vii	99.19 (9)
V2^i—Ca1—V2^ix	71.34 (2)	V2^v—O3—V2^vii	98.45 (10)
V2^ii—Ca1—V2^ix	124.19 (3)	V1^vii—O3—Ca1	102.00 (9)
V1^iv—Ca1—V2^ix	127.02 (2)	V2^v—O3—Ca1	99.42 (8)
V2—Ca1—V2^ix	148.92 (3)	V2^vii—O3—Ca1	134.05 (10)
V2^iii—Ca1—V2^ix	82.82 (2)	V1^vii—O3—Ca1^xiii	65.38 (6)
O2^i—Ca1—V2^vii	127.64 (6)	V2^v—O3—Ca1^xiii	64.35 (6)
O2^ii—Ca1—V2^vii	58.72 (5)	V2^vii—O3—Ca1^xiii	123.10 (8)
O4—Ca1—V2^vii	79.57 (5)	Ca1—O3—Ca1^xiii	102.80 (6)
O4^iii—Ca1—V2^vii	126.47 (6)	V1^vii—O3—Ca1^vii	48.93 (5)
O3^iii—Ca1—V2^vii	80.07 (6)	V2^v—O3—Ca1^vii	160.74 (9)
O3—Ca1—V2^vii	20.44 (5)	V2^vii—O3—Ca1^vii	65.98 (6)
O1^iv—Ca1—V2^vii	134.57 (3)	Ca1—O3—Ca1^vii	99.66 (7)
V1—Ca1—V2^vii	110.79 (3)	Ca1^xiii—O3—Ca1^vii	113.50 (5)
V2^v—Ca1—V2^vii	46.199 (15)	V1^vii—O3—Ca1^v	104.63 (8)
V2^vi—Ca1—V2^vii	106.60 (3)	V2^v—O3—Ca1^v	60.90 (6)
V1^vii—Ca1—V2^vii	46.246 (15)	V2^vii—O3—Ca1^v	43.63 (5)
O1^viii—Ca1—V2^vii	59.82 (4)	Ca1—O3—Ca1^v	153.17 (7)
V2^i—Ca1—V2^vii	124.19 (3)	Ca1^xiii—O3—Ca1^v	85.54 (4)
V2^ii—Ca1—V2^vii	71.34 (2)	Ca1^vii—O3—Ca1^v	100.19 (5)
V1^iv—Ca1—V2^vii	127.02 (2)	V2^v—O4—V2	98.91 (10)
V2—Ca1—V2^vii	82.82 (2)	V2^v—O4—V1	132.78 (11)
V2^iii—Ca1—V2^vii	148.92 (3)	V2—O4—V1	99.14 (9)
V2^ix—Ca1—V2^vii	87.37 (3)	V2^v—O4—Ca1	100.85 (8)
O2^i—Ca1—O2	132.45 (4)	V2—O4—Ca1	129.53 (10)
O2^ii—Ca1—O2	51.49 (7)	V1—O4—Ca1	100.40 (9)
O4—Ca1—O2	45.31 (6)	V2^v—O4—Ca1^xiii	58.17 (5)
O4^iii—Ca1—O2	100.78 (6)	V2—O4—Ca1^xiii	132.41 (8)
O3^iii—Ca1—O2	149.53 (7)	V1—O4—Ca1^xiii	77.68 (6)
O3—Ca1—O2	89.08 (6)	Ca1—O4—Ca1^xiii	97.17 (6)
O1^iv—Ca1—O2	56.36 (4)	V2^v—O4—Ca1^x	161.81 (9)
V1—Ca1—O2	66.96 (3)	V2—O4—Ca1^x	65.61 (6)
V2^v—Ca1—O2	62.24 (3)	V1—O4—Ca1^x	47.03 (5)
V2^vi—Ca1—O2	131.08 (4)	Ca1—O4—Ca1^x	96.64 (6)
V1^vii—Ca1—O2	122.67 (4)	Ca1^xiii—O4—Ca1^x	124.56 (5)
O1^viii—Ca1—O2	119.78 (4)	V2^v—O4—Ca1^xiv	63.94 (6)
V2^i—Ca1—O2	119.36 (4)	V2—O4—Ca1^xiv	43.23 (5)
V2^ii—Ca1—O2	58.51 (3)	V1—O4—Ca1^xiv	104.08 (7)
V1^iv—Ca1—O2	64.12 (4)	Ca1—O4—Ca1^xiv	155.35 (7)
V2—Ca1—O2	22.91 (3)	Ca1^xiii—O4—Ca1^xiv	90.80 (4)
V2^iii—Ca1—O2	101.88 (4)	Ca1^x—O4—Ca1^xiv	97.92 (4)
V2^ix—Ca1—O2	168.74 (4)	V2^v—O4—Ca1^ii	90.24 (7)
V2^vii—Ca1—O2	83.41 (4)	V2—O4—Ca1^ii	37.39 (5)
O1—V1—O3^x	109.26 (10)	V1—O4—Ca1^ii	128.23 (8)
O1—V1—O3^xi	109.26 (10)	Ca1—O4—Ca1^ii	96.62 (6)
O3^x—V1—O3^xi	86.57 (13)	Ca1^xiii—O4—Ca1^ii	147.39 (5)
O1—V1—O4^iii	111.23 (10)	Ca1^x—O4—Ca1^ii	82.76 (3)
O3^x—V1—O4^iii	139.51 (10)	Ca1^xiv—O4—Ca1^ii	65.76 (3)
O3^xi—V1—O4^iii	80.04 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_187K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.543 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2725 reflections
a = 10.423 (3) Å	θ = 1.3–23.4°
b = 10.367 (2) Å	µ = 5.68 mm^−1
c = 5.2902 (15) Å	T = 187 K
V = 571.7 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	401 independent reflections
Radiation source: fine-focus sealed tube	368 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.035
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.471	l = −5→5
2458 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0482P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.056	(Δ/σ)max < 0.001
S = 0.94	Δρmax = 0.26 e Å^−3
401 reflections	Δρmin = −0.29 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0192 (18)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08491 (9)	0.2500	0.29974 (15)	0.0060 (3)
V1	0.28887 (7)	0.2500	0.79229 (13)	0.0047 (3)
V2	0.18737 (6)	0.52023 (6)	0.78361 (10)	0.0048 (3)
O1	0.4440 (3)	0.2500	0.8091 (5)	0.0091 (8)*
O2	0.0395 (2)	0.5657 (2)	0.7663 (4)	0.0106 (6)*
O3	0.22040 (19)	0.3797 (2)	0.0261 (4)	0.0058 (5)*
O4	0.22675 (19)	0.3795 (2)	0.5482 (4)	0.0060 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0041 (5)	0.0060 (6)	0.0078 (6)	0.000	−0.0005 (3)	0.000
V1	0.0041 (5)	0.0047 (6)	0.0053 (5)	0.000	−0.0004 (3)	0.000
V2	0.0045 (4)	0.0046 (4)	0.0052 (4)	0.0008 (2)	0.0000 (2)	0.0001 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.336 (3)	V1—Ca1^xiii	4.3966 (15)
Ca1—O2^ii	2.336 (3)	V1—Ca1^xiv	5.3482 (12)
Ca1—O4	2.391 (2)	V2—O2	1.614 (2)
Ca1—O4^iii	2.391 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3^iii	2.429 (2)	V2—O4	1.962 (2)
Ca1—O3	2.429 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.538 (3)	V2—O3^x	1.971 (2)
Ca1—V1	3.3629 (13)	V2—V2^xiv	2.9795 (9)
Ca1—V2^v	3.3639 (11)	V2—V2^v	2.9795 (9)
Ca1—V2^vi	3.3639 (11)	V2—Ca1^xiv	3.3639 (11)
Ca1—V1^vii	3.4243 (13)	V2—Ca1^ii	3.7314 (11)
Ca1—O1^viii	3.540 (3)	V2—Ca1^x	4.0552 (10)
Ca1—V2^i	3.7314 (11)	O1—Ca1^xii	2.538 (3)
Ca1—V2^ii	3.7314 (11)	O1—Ca1^xiii	3.540 (3)
Ca1—V1^iv	3.7656 (14)	O1—Ca1^x	4.554 (3)
Ca1—V2	3.9423 (10)	O2—Ca1^ii	2.336 (3)
Ca1—V2^iii	3.9423 (10)	O2—Ca1^x	4.347 (2)
Ca1—V2^ix	4.0552 (10)	O2—Ca1^xiv	4.360 (3)
Ca1—V2^vii	4.0552 (10)	O3—V1^vii	1.961 (2)
Ca1—O2	4.126 (2)	O3—V2^v	1.964 (2)
V1—O1	1.619 (3)	O3—V2^vii	1.971 (2)
V1—O3^x	1.961 (2)	O3—Ca1^xiii	4.134 (2)
V1—O3^xi	1.961 (2)	O3—Ca1^vii	4.309 (2)
V1—O4^iii	1.972 (2)	O3—Ca1^v	4.504 (2)
V1—O4	1.972 (2)	O4—V2^v	1.960 (2)
V1—V2^iii	2.9950 (9)	O4—Ca1^xiii	4.373 (2)
V1—V2	2.9950 (9)	O4—Ca1^x	4.449 (2)
V1—Ca1^x	3.4243 (13)	O4—Ca1^xiv	4.514 (2)
V1—Ca1^xii	3.7656 (14)	O4—Ca1^ii	5.095 (2)
O2^i—Ca1—O2^ii	109.79 (12)	O1—V1—O4	111.33 (9)
O2^i—Ca1—O4	152.25 (8)	O3^x—V1—O4	80.02 (9)
O2^ii—Ca1—O4	88.06 (7)	O3^xi—V1—O4	139.47 (10)
O2^i—Ca1—O4^iii	88.06 (7)	O4^iii—V1—O4	85.80 (12)
O2^ii—Ca1—O4^iii	152.25 (8)	O1—V1—V2^iii	110.705 (18)
O4—Ca1—O4^iii	68.33 (10)	O3^x—V1—V2^iii	121.49 (7)
O2^i—Ca1—O3^iii	77.34 (7)	O3^xi—V1—V2^iii	40.52 (6)
O2^ii—Ca1—O3^iii	133.37 (8)	O4^iii—V1—V2^iii	40.29 (6)
O4—Ca1—O3^iii	106.20 (8)	O4—V1—V2^iii	120.71 (7)
O4^iii—Ca1—O3^iii	69.95 (7)	O1—V1—V2	110.705 (18)
O2^i—Ca1—O3	133.37 (8)	O3^x—V1—V2	40.52 (6)
O2^ii—Ca1—O3	77.34 (7)	O3^xi—V1—V2	121.49 (7)
O4—Ca1—O3	69.95 (7)	O4^iii—V1—V2	120.71 (7)
O4^iii—Ca1—O3	106.20 (8)	O4—V1—V2	40.29 (6)
O3^iii—Ca1—O3	67.24 (10)	V2^iii—V1—V2	138.59 (4)
O2^i—Ca1—O1^iv	78.49 (7)	O1—V1—Ca1	132.36 (10)
O2^ii—Ca1—O1^iv	78.49 (7)	O3^x—V1—Ca1	104.98 (6)
O4—Ca1—O1^iv	84.82 (8)	O3^xi—V1—Ca1	104.98 (6)
O4^iii—Ca1—O1^iv	84.82 (8)	O4^iii—V1—Ca1	44.36 (6)
O3^iii—Ca1—O1^iv	145.35 (5)	O4—V1—Ca1	44.36 (6)
O3—Ca1—O1^iv	145.35 (5)	V2^iii—V1—Ca1	76.397 (17)
O2^i—Ca1—V1	117.83 (6)	V2—V1—Ca1	76.397 (17)
O2^ii—Ca1—V1	117.83 (6)	O1—V1—Ca1^x	125.23 (10)
O4—Ca1—V1	35.22 (5)	O3^x—V1—Ca1^x	43.93 (6)
O4^iii—Ca1—V1	35.22 (5)	O3^xi—V1—Ca1^x	43.93 (6)
O3^iii—Ca1—V1	95.41 (6)	O4^iii—V1—Ca1^x	108.03 (7)
O3—Ca1—V1	95.41 (6)	O4—V1—Ca1^x	108.03 (7)
O1^iv—Ca1—V1	74.59 (7)	V2^iii—V1—Ca1^x	78.036 (18)
O2^i—Ca1—V2^v	165.32 (6)	V2—V1—Ca1^x	78.036 (18)
O2^ii—Ca1—V2^v	78.97 (6)	Ca1—V1—Ca1^x	102.41 (4)
O4—Ca1—V2^v	34.91 (5)	O1—V1—Ca1^xii	31.82 (10)
O4^iii—Ca1—V2^v	88.58 (6)	O3^x—V1—Ca1^xii	86.38 (6)
O3^iii—Ca1—V2^v	88.09 (6)	O3^xi—V1—Ca1^xii	86.38 (6)
O3—Ca1—V2^v	35.17 (5)	O4^iii—V1—Ca1^xii	130.12 (6)
O1^iv—Ca1—V2^v	115.42 (5)	O4—V1—Ca1^xii	130.12 (6)
V1—Ca1—V2^v	64.76 (2)	V2^iii—V1—Ca1^xii	107.353 (17)
O2^i—Ca1—V2^vi	78.97 (6)	V2—V1—Ca1^xii	107.353 (17)
O2^ii—Ca1—V2^vi	165.32 (6)	Ca1—V1—Ca1^xii	164.18 (3)
O4—Ca1—V2^vi	88.58 (6)	Ca1^x—V1—Ca1^xii	93.41 (3)
O4^iii—Ca1—V2^vi	34.91 (5)	O1—V1—Ca1^xiii	48.58 (10)
O3^iii—Ca1—V2^vi	35.17 (5)	O3^x—V1—Ca1^xiii	134.79 (6)
O3—Ca1—V2^vi	88.09 (6)	O3^xi—V1—Ca1^xiii	134.79 (6)
O1^iv—Ca1—V2^vi	115.42 (5)	O4^iii—V1—Ca1^xiii	76.35 (6)
V1—Ca1—V2^vi	64.76 (2)	O4—V1—Ca1^xiii	76.35 (6)
V2^v—Ca1—V2^vi	90.17 (4)	V2^iii—V1—Ca1^xiii	103.710 (17)
O2^i—Ca1—V1^vii	103.15 (5)	V2—V1—Ca1^xiii	103.710 (17)
O2^ii—Ca1—V1^vii	103.15 (5)	Ca1—V1—Ca1^xiii	83.78 (3)
O4—Ca1—V1^vii	92.70 (6)	Ca1^x—V1—Ca1^xiii	173.80 (3)
O4^iii—Ca1—V1^vii	92.70 (6)	Ca1^xii—V1—Ca1^xiii	80.40 (3)
O3^iii—Ca1—V1^vii	34.07 (5)	O1—V1—Ca1^xiv	75.758 (14)
O3—Ca1—V1^vii	34.07 (5)	O3^x—V1—Ca1^xiv	54.58 (6)
O1^iv—Ca1—V1^vii	177.00 (8)	O3^xi—V1—Ca1^xiv	138.53 (6)
V1—Ca1—V1^vii	102.41 (4)	O4^iii—V1—Ca1^xiv	138.19 (6)
V2^v—Ca1—V1^vii	62.75 (2)	O4—V1—Ca1^xiv	54.96 (6)
V2^vi—Ca1—V1^vii	62.75 (2)	V2^iii—V1—Ca1^xiv	173.54 (3)
O2^i—Ca1—O1^viii	68.50 (6)	V2—V1—Ca1^xiv	34.95 (2)
O2^ii—Ca1—O1^viii	68.50 (6)	Ca1—V1—Ca1^xiv	99.277 (15)
O4—Ca1—O1^viii	139.18 (6)	Ca1^x—V1—Ca1^xiv	98.450 (15)
O4^iii—Ca1—O1^viii	139.18 (6)	Ca1^xii—V1—Ca1^xiv	78.124 (13)
O3^iii—Ca1—O1^viii	72.48 (7)	Ca1^xiii—V1—Ca1^xiv	80.364 (13)
O3—Ca1—O1^viii	72.48 (7)	O2—V2—O4^xiv	108.77 (10)
O1^iv—Ca1—O1^viii	120.11 (11)	O2—V2—O4	112.38 (10)
V1—Ca1—O1^viii	165.31 (6)	O4^xiv—V2—O4	138.79 (5)
V2^v—Ca1—O1^viii	105.65 (4)	O2—V2—O3^xiv	105.89 (10)
V2^vi—Ca1—O1^viii	105.65 (4)	O4^xiv—V2—O3^xiv	89.52 (9)
V1^vii—Ca1—O1^viii	62.90 (6)	O4—V2—O3^xiv	81.37 (9)
O2^i—Ca1—V2^i	15.78 (6)	O2—V2—O3^x	114.79 (10)
O2^ii—Ca1—V2^i	94.72 (7)	O4^xiv—V2—O3^x	81.24 (9)
O4—Ca1—V2^i	153.36 (6)	O4—V2—O3^x	80.03 (8)
O4^iii—Ca1—V2^i	100.18 (5)	O3^xiv—V2—O3^x	139.14 (4)
O3^iii—Ca1—V2^i	91.05 (5)	O2—V2—V2^xiv	120.66 (7)
O3—Ca1—V2^i	136.49 (6)	O4^xiv—V2—V2^xiv	40.58 (6)
O1^iv—Ca1—V2^i	69.88 (5)	O4—V2—V2^xiv	111.55 (7)
V1—Ca1—V2^i	124.92 (2)	O3^xiv—V2—V2^xiv	118.41 (7)
V2^v—Ca1—V2^i	170.32 (3)	O3^x—V2—V2^xiv	40.70 (6)
V2^vi—Ca1—V2^i	94.68 (2)	O2—V2—V2^v	114.15 (7)
V1^vii—Ca1—V2^i	112.31 (2)	O4^xiv—V2—V2^v	120.56 (7)
O1^viii—Ca1—V2^i	64.97 (4)	O4—V2—V2^v	40.53 (6)
O2^i—Ca1—V2^ii	94.72 (7)	O3^xiv—V2—V2^v	40.88 (6)
O2^ii—Ca1—V2^ii	15.78 (6)	O3^x—V2—V2^v	113.39 (7)
O4—Ca1—V2^ii	100.18 (5)	V2^xiv—V2—V2^v	125.19 (4)
O4^iii—Ca1—V2^ii	153.36 (6)	O2—V2—V1	127.67 (9)
O3^iii—Ca1—V2^ii	136.49 (6)	O4^xiv—V2—V1	108.90 (6)
O3—Ca1—V2^ii	91.05 (5)	O4—V2—V1	40.55 (6)
O1^iv—Ca1—V2^ii	69.88 (5)	O3^xiv—V2—V1	109.38 (6)
V1—Ca1—V2^ii	124.92 (2)	O3^x—V2—V1	40.27 (6)
V2^v—Ca1—V2^ii	94.68 (2)	V2^xiv—V2—V1	72.54 (3)
V2^vi—Ca1—V2^ii	170.32 (3)	V2^v—V2—V1	74.17 (3)
V1^vii—Ca1—V2^ii	112.31 (2)	O2—V2—Ca1^xiv	117.94 (9)
O1^viii—Ca1—V2^ii	64.97 (4)	O4^xiv—V2—Ca1^xiv	44.27 (6)
V2^i—Ca1—V2^ii	79.35 (3)	O4—V2—Ca1^xiv	113.27 (7)
O2^i—Ca1—V1^iv	68.32 (6)	O3^xiv—V2—Ca1^xiv	45.42 (6)
O2^ii—Ca1—V1^iv	68.32 (6)	O3^x—V2—Ca1^xiv	112.56 (7)
O4—Ca1—V1^iv	101.05 (6)	V2^xiv—V2—Ca1^xiv	76.58 (3)
O4^iii—Ca1—V1^iv	101.05 (6)	V2^v—V2—Ca1^xiv	79.22 (3)
O3^iii—Ca1—V1^iv	144.90 (5)	V1—V2—Ca1^xiv	114.38 (3)
O3—Ca1—V1^iv	144.90 (5)	O2—V2—Ca1^ii	23.19 (9)
O1^iv—Ca1—V1^iv	19.65 (7)	O4^xiv—V2—Ca1^ii	95.34 (6)
V1—Ca1—V1^iv	94.24 (3)	O4—V2—Ca1^ii	123.98 (6)
V2^v—Ca1—V1^iv	126.35 (2)	O3^xiv—V2—Ca1^ii	87.31 (6)
V2^vi—Ca1—V1^iv	126.35 (2)	O3^x—V2—Ca1^ii	132.96 (6)
V1^vii—Ca1—V1^iv	163.35 (3)	V2^xiv—V2—Ca1^ii	121.88 (3)
O1^viii—Ca1—V1^iv	100.45 (6)	V2^v—V2—Ca1^ii	108.56 (3)
V2^i—Ca1—V1^iv	56.25 (2)	V1—V2—Ca1^ii	150.19 (3)
V2^ii—Ca1—V1^iv	56.25 (2)	Ca1^xiv—V2—Ca1^ii	95.02 (2)
O2^i—Ca1—V2	145.98 (6)	O2—V2—Ca1	84.94 (8)
O2^ii—Ca1—V2	70.50 (6)	O4^xiv—V2—Ca1	164.67 (6)
O4—Ca1—V2	22.55 (5)	O4—V2—Ca1	27.86 (6)
O4^iii—Ca1—V2	82.79 (5)	O3^xiv—V2—Ca1	93.30 (6)
O3^iii—Ca1—V2	128.54 (6)	O3^x—V2—Ca1	86.82 (7)
O3—Ca1—V2	80.57 (5)	V2^xiv—V2—Ca1	126.52 (3)
O1^iv—Ca1—V2	68.12 (5)	V2^v—V2—Ca1	56.10 (2)
V1—Ca1—V2	47.596 (16)	V1—V2—Ca1	56.01 (2)
V2^v—Ca1—V2	47.319 (15)	Ca1^xiv—V2—Ca1	135.30 (3)
V2^vi—Ca1—V2	109.18 (3)	Ca1^ii—V2—Ca1	99.84 (2)
V1^vii—Ca1—V2	109.93 (3)	O2—V2—Ca1^x	89.34 (8)
O1^viii—Ca1—V2	134.683 (15)	O4^xiv—V2—Ca1^x	90.34 (6)
V2^i—Ca1—V2	137.43 (3)	O4—V2—Ca1^x	88.21 (6)
V2^ii—Ca1—V2	80.16 (2)	O3^xiv—V2—Ca1^x	163.95 (7)
V1^iv—Ca1—V2	81.36 (2)	O3^x—V2—Ca1^x	25.49 (6)
O2^i—Ca1—V2^iii	70.50 (6)	V2^xiv—V2—Ca1^x	54.58 (2)
O2^ii—Ca1—V2^iii	145.98 (6)	V2^v—V2—Ca1^x	128.02 (3)
O4—Ca1—V2^iii	82.79 (5)	V1—V2—Ca1^x	55.70 (2)
O4^iii—Ca1—V2^iii	22.55 (5)	Ca1^xiv—V2—Ca1^x	131.15 (2)
O3^iii—Ca1—V2^iii	80.57 (5)	Ca1^ii—V2—Ca1^x	108.68 (2)
O3—Ca1—V2^iii	128.54 (6)	Ca1—V2—Ca1^x	82.81 (2)
O1^iv—Ca1—V2^iii	68.12 (5)	V1—O1—Ca1^xii	128.53 (15)
V1—Ca1—V2^iii	47.596 (16)	V1—O1—Ca1^xiii	111.37 (13)
V2^v—Ca1—V2^iii	109.18 (3)	Ca1^xii—O1—Ca1^xiii	120.11 (11)
V2^vi—Ca1—V2^iii	47.319 (15)	V1—O1—Ca1^x	37.89 (8)
V1^vii—Ca1—V2^iii	109.93 (3)	Ca1^xii—O1—Ca1^x	90.63 (8)
O1^viii—Ca1—V2^iii	134.683 (15)	Ca1^xiii—O1—Ca1^x	149.26 (9)
V2^i—Ca1—V2^iii	80.16 (2)	V1—O1—Ca1	32.60 (8)
V2^ii—Ca1—V2^iii	137.43 (3)	Ca1^xii—O1—Ca1	161.13 (11)
V1^iv—Ca1—V2^iii	81.36 (2)	Ca1^xiii—O1—Ca1	78.76 (6)
V2—Ca1—V2^iii	90.57 (3)	Ca1^x—O1—Ca1	70.50 (5)
O2^i—Ca1—V2^ix	58.69 (5)	V2—O2—Ca1^ii	141.03 (14)
O2^ii—Ca1—V2^ix	127.65 (6)	V2—O2—Ca1	72.13 (8)
O4—Ca1—V2^ix	126.53 (6)	Ca1^ii—O2—Ca1	128.54 (7)
O4^iii—Ca1—V2^ix	79.59 (5)	V2—O2—Ca1^x	68.87 (8)
O3^iii—Ca1—V2^ix	20.45 (5)	Ca1^ii—O2—Ca1^x	140.65 (7)
O3—Ca1—V2^ix	80.10 (6)	Ca1—O2—Ca1^x	77.22 (5)
O1^iv—Ca1—V2^ix	134.55 (3)	V2—O2—Ca1^xiv	42.98 (7)
V1—Ca1—V2^ix	110.81 (3)	Ca1^ii—O2—Ca1^xiv	98.40 (7)
V2^v—Ca1—V2^ix	106.64 (3)	Ca1—O2—Ca1^xiv	105.61 (5)
V2^vi—Ca1—V2^ix	46.201 (15)	Ca1^x—O2—Ca1^xiv	101.89 (5)
V1^vii—Ca1—V2^ix	46.264 (15)	V1^vii—O3—V2^v	128.42 (11)
O1^viii—Ca1—V2^ix	59.78 (4)	V1^vii—O3—V2^vii	99.20 (9)
V2^i—Ca1—V2^ix	71.32 (2)	V2^v—O3—V2^vii	98.42 (9)
V2^ii—Ca1—V2^ix	124.18 (3)	V1^vii—O3—Ca1	102.00 (9)
V1^iv—Ca1—V2^ix	126.99 (2)	V2^v—O3—Ca1	99.42 (8)
V2—Ca1—V2^ix	148.96 (3)	V2^vii—O3—Ca1	134.07 (10)
V2^iii—Ca1—V2^ix	82.81 (2)	V1^vii—O3—Ca1^xiii	65.36 (6)
O2^i—Ca1—V2^vii	127.65 (6)	V2^v—O3—Ca1^xiii	64.36 (6)
O2^ii—Ca1—V2^vii	58.69 (5)	V2^vii—O3—Ca1^xiii	123.08 (8)
O4—Ca1—V2^vii	79.59 (5)	Ca1—O3—Ca1^xiii	102.79 (6)
O4^iii—Ca1—V2^vii	126.53 (6)	V1^vii—O3—Ca1^vii	48.93 (5)
O3^iii—Ca1—V2^vii	80.10 (6)	V2^v—O3—Ca1^vii	160.72 (9)
O3—Ca1—V2^vii	20.45 (5)	V2^vii—O3—Ca1^vii	65.99 (6)
O1^iv—Ca1—V2^vii	134.55 (3)	Ca1—O3—Ca1^vii	99.68 (7)
V1—Ca1—V2^vii	110.81 (3)	Ca1^xiii—O3—Ca1^vii	113.48 (5)
V2^v—Ca1—V2^vii	46.201 (15)	V1^vii—O3—Ca1^v	104.64 (7)
V2^vi—Ca1—V2^vii	106.64 (3)	V2^v—O3—Ca1^v	60.90 (6)
V1^vii—Ca1—V2^vii	46.264 (15)	V2^vii—O3—Ca1^v	43.60 (5)
O1^viii—Ca1—V2^vii	59.78 (4)	Ca1—O3—Ca1^v	153.16 (7)
V2^i—Ca1—V2^vii	124.18 (3)	Ca1^xiii—O3—Ca1^v	85.55 (4)
V2^ii—Ca1—V2^vii	71.32 (2)	Ca1^vii—O3—Ca1^v	100.17 (4)
V1^iv—Ca1—V2^vii	126.99 (2)	V2^v—O4—V2	98.88 (10)
V2—Ca1—V2^vii	82.81 (2)	V2^v—O4—V1	132.75 (11)
V2^iii—Ca1—V2^vii	148.96 (3)	V2—O4—V1	99.16 (9)
V2^ix—Ca1—V2^vii	87.40 (3)	V2^v—O4—Ca1	100.82 (8)
O2^i—Ca1—O2	132.43 (4)	V2—O4—Ca1	129.59 (10)
O2^ii—Ca1—O2	51.46 (7)	V1—O4—Ca1	100.42 (9)
O4—Ca1—O2	45.30 (6)	V2^v—O4—Ca1^xiii	58.16 (5)
O4^iii—Ca1—O2	100.80 (6)	V2—O4—Ca1^xiii	132.39 (8)
O3^iii—Ca1—O2	149.58 (7)	V1—O4—Ca1^xiii	77.66 (6)
O3—Ca1—O2	89.09 (6)	Ca1—O4—Ca1^xiii	97.13 (6)
O1^iv—Ca1—O2	56.35 (4)	V2^v—O4—Ca1^x	161.80 (9)
V1—Ca1—O2	66.98 (3)	V2—O4—Ca1^x	65.64 (6)
V2^v—Ca1—O2	62.25 (3)	V1—O4—Ca1^x	47.04 (5)
V2^vi—Ca1—O2	131.12 (4)	Ca1—O4—Ca1^x	96.68 (6)
V1^vii—Ca1—O2	122.69 (4)	Ca1^xiii—O4—Ca1^x	124.55 (5)
O1^viii—Ca1—O2	119.78 (4)	V2^v—O4—Ca1^xiv	63.93 (6)
V2^i—Ca1—O2	119.33 (4)	V2—O4—Ca1^xiv	43.20 (5)
V2^ii—Ca1—O2	58.48 (3)	V1—O4—Ca1^xiv	104.09 (7)
V1^iv—Ca1—O2	64.10 (3)	Ca1—O4—Ca1^xiv	155.34 (7)
V2—Ca1—O2	22.93 (3)	Ca1^xiii—O4—Ca1^xiv	90.81 (4)
V2^iii—Ca1—O2	101.90 (4)	Ca1^x—O4—Ca1^xiv	97.92 (4)
V2^ix—Ca1—O2	168.78 (4)	V2^v—O4—Ca1^ii	90.23 (7)
V2^vii—Ca1—O2	83.40 (4)	V2—O4—Ca1^ii	37.40 (5)
O1—V1—O3^x	109.19 (9)	V1—O4—Ca1^ii	128.26 (8)
O1—V1—O3^xi	109.19 (9)	Ca1—O4—Ca1^ii	96.65 (6)
O3^x—V1—O3^xi	86.56 (12)	Ca1^xiii—O4—Ca1^ii	147.37 (5)
O1—V1—O4^iii	111.33 (9)	Ca1^x—O4—Ca1^ii	82.79 (3)
O3^x—V1—O4^iii	139.47 (10)	Ca1^xiv—O4—Ca1^ii	65.74 (3)
O3^xi—V1—O4^iii	80.02 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_175K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.542 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2723 reflections
a = 10.421 (3) Å	θ = 1.3–23.4°
b = 10.369 (2) Å	µ = 5.68 mm^−1
c = 5.2905 (15) Å	T = 175 K
V = 571.7 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	400 independent reflections
Radiation source: fine-focus sealed tube	365 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.318, Tmax = 0.471	l = −5→5
2455 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0457P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.055	(Δ/σ)max < 0.001
S = 0.97	Δρmax = 0.26 e Å^−3
400 reflections	Δρmin = −0.33 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.020 (2)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08486 (9)	0.2500	0.29993 (15)	0.0058 (3)
V1	0.28889 (7)	0.2500	0.79225 (13)	0.0047 (3)
V2	0.18738 (6)	0.52022 (6)	0.78365 (10)	0.0048 (3)
O1	0.4439 (3)	0.2500	0.8091 (5)	0.0093 (8)*
O2	0.0396 (2)	0.5653 (2)	0.7663 (4)	0.0103 (6)*
O3	0.22031 (19)	0.3796 (2)	0.0262 (4)	0.0061 (5)*
O4	0.22685 (19)	0.3794 (2)	0.5482 (4)	0.0055 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0041 (5)	0.0061 (6)	0.0073 (6)	0.000	−0.0004 (3)	0.000
V1	0.0041 (5)	0.0047 (6)	0.0053 (5)	0.000	−0.0005 (3)	0.000
V2	0.0045 (4)	0.0046 (4)	0.0053 (4)	0.0008 (2)	0.0001 (2)	0.0002 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.339 (3)	V1—Ca1^xiii	4.3964 (15)
Ca1—O2^ii	2.339 (3)	V1—Ca1^xiv	5.3492 (12)
Ca1—O4	2.390 (2)	V2—O2	1.612 (2)
Ca1—O4^iii	2.390 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3	2.428 (2)	V2—O3^xiv	1.965 (2)
Ca1—O3^iii	2.428 (2)	V2—O4	1.963 (2)
Ca1—O1^iv	2.537 (3)	V2—O3^x	1.972 (2)
Ca1—V1	3.3623 (13)	V2—V2^xiv	2.9794 (9)
Ca1—V2^v	3.3643 (11)	V2—V2^v	2.9794 (9)
Ca1—V2^vi	3.3643 (11)	V2—Ca1^xiv	3.3643 (11)
Ca1—V1^vii	3.4256 (13)	V2—Ca1^ii	3.7311 (11)
Ca1—O1^viii	3.541 (3)	V2—Ca1^x	4.0562 (10)
Ca1—V2^i	3.7311 (11)	O1—Ca1^xii	2.537 (3)
Ca1—V2^ii	3.7311 (11)	O1—Ca1^xiii	3.541 (3)
Ca1—V1^iv	3.7641 (14)	O1—Ca1^x	4.554 (3)
Ca1—V2	3.9423 (10)	O2—Ca1^ii	2.339 (3)
Ca1—V2^iii	3.9423 (10)	O2—Ca1^x	4.346 (2)
Ca1—V2^ix	4.0562 (10)	O2—Ca1^xiv	4.360 (3)
Ca1—V2^vii	4.0562 (10)	O3—V1^vii	1.962 (2)
Ca1—O2	4.123 (2)	O3—V2^v	1.965 (2)
V1—O1	1.618 (3)	O3—V2^vii	1.972 (2)
V1—O3^x	1.962 (2)	O3—Ca1^xiii	4.133 (2)
V1—O3^xi	1.962 (2)	O3—Ca1^vii	4.308 (2)
V1—O4^iii	1.971 (2)	O3—Ca1^v	4.506 (2)
V1—O4	1.971 (2)	O4—V2^v	1.960 (2)
V1—V2^iii	2.9953 (9)	O4—Ca1^xiii	4.372 (2)
V1—V2	2.9953 (9)	O4—Ca1^x	4.450 (2)
V1—Ca1^x	3.4256 (13)	O4—Ca1^xiv	4.516 (2)
V1—Ca1^xii	3.7641 (14)	O4—Ca1^ii	5.096 (2)
O2^i—Ca1—O2^ii	109.89 (12)	O1—V1—O4	111.32 (9)
O2^i—Ca1—O4	152.24 (8)	O3^x—V1—O4	80.07 (9)
O2^ii—Ca1—O4	88.06 (7)	O3^xi—V1—O4	139.47 (10)
O2^i—Ca1—O4^iii	88.06 (7)	O4^iii—V1—O4	85.79 (12)
O2^ii—Ca1—O4^iii	152.24 (8)	O1—V1—V2^iii	110.699 (18)
O4—Ca1—O4^iii	68.27 (10)	O3^x—V1—V2^iii	121.45 (7)
O2^i—Ca1—O3	133.32 (8)	O3^xi—V1—V2^iii	40.55 (6)
O2^ii—Ca1—O3	77.29 (7)	O4^iii—V1—V2^iii	40.31 (6)
O4—Ca1—O3	69.96 (7)	O4—V1—V2^iii	120.72 (7)
O4^iii—Ca1—O3	106.17 (8)	O1—V1—V2	110.699 (18)
O2^i—Ca1—O3^iii	77.29 (7)	O3^x—V1—V2	40.55 (6)
O2^ii—Ca1—O3^iii	133.32 (8)	O3^xi—V1—V2	121.45 (7)
O4—Ca1—O3^iii	106.17 (8)	O4^iii—V1—V2	120.72 (7)
O4^iii—Ca1—O3^iii	69.96 (7)	O4—V1—V2	40.31 (6)
O3—Ca1—O3^iii	67.21 (10)	V2^iii—V1—V2	138.60 (4)
O2^i—Ca1—O1^iv	78.52 (7)	O1—V1—Ca1	132.38 (10)
O2^ii—Ca1—O1^iv	78.52 (7)	O3^x—V1—Ca1	104.97 (6)
O4—Ca1—O1^iv	84.86 (8)	O3^xi—V1—Ca1	104.97 (6)
O4^iii—Ca1—O1^iv	84.86 (8)	O4^iii—V1—Ca1	44.36 (6)
O3—Ca1—O1^iv	145.37 (5)	O4—V1—Ca1	44.36 (6)
O3^iii—Ca1—O1^iv	145.37 (5)	V2^iii—V1—Ca1	76.403 (17)
O2^i—Ca1—V1	117.82 (6)	V2—V1—Ca1	76.403 (17)
O2^ii—Ca1—V1	117.82 (6)	O1—V1—Ca1^x	125.21 (10)
O4—Ca1—V1	35.20 (5)	O3^x—V1—Ca1^x	43.88 (6)
O4^iii—Ca1—V1	35.20 (5)	O3^xi—V1—Ca1^x	43.88 (6)
O3—Ca1—V1	95.42 (6)	O4^iii—V1—Ca1^x	108.06 (6)
O3^iii—Ca1—V1	95.42 (6)	O4—V1—Ca1^x	108.06 (6)
O1^iv—Ca1—V1	74.61 (7)	V2^iii—V1—Ca1^x	78.036 (18)
O2^i—Ca1—V2^v	165.27 (6)	V2—V1—Ca1^x	78.036 (18)
O2^ii—Ca1—V2^v	78.91 (6)	Ca1—V1—Ca1^x	102.41 (4)
O4—Ca1—V2^v	34.91 (5)	O1—V1—Ca1^xii	31.82 (10)
O4^iii—Ca1—V2^v	88.55 (6)	O3^x—V1—Ca1^xii	86.38 (6)
O3—Ca1—V2^v	35.17 (5)	O3^xi—V1—Ca1^xii	86.38 (6)
O3^iii—Ca1—V2^v	88.09 (6)	O4^iii—V1—Ca1^xii	130.11 (6)
O1^iv—Ca1—V2^v	115.43 (5)	O4—V1—Ca1^xii	130.11 (6)
V1—Ca1—V2^v	64.77 (2)	V2^iii—V1—Ca1^xii	107.343 (17)
O2^i—Ca1—V2^vi	78.91 (6)	V2—V1—Ca1^xii	107.343 (17)
O2^ii—Ca1—V2^vi	165.27 (6)	Ca1—V1—Ca1^xii	164.20 (3)
O4—Ca1—V2^vi	88.55 (6)	Ca1^x—V1—Ca1^xii	93.39 (3)
O4^iii—Ca1—V2^vi	34.91 (5)	O1—V1—Ca1^xiii	48.60 (10)
O3—Ca1—V2^vi	88.09 (6)	O3^x—V1—Ca1^xiii	134.84 (7)
O3^iii—Ca1—V2^vi	35.17 (5)	O3^xi—V1—Ca1^xiii	134.84 (6)
O1^iv—Ca1—V2^vi	115.43 (5)	O4^iii—V1—Ca1^xiii	76.31 (6)
V1—Ca1—V2^vi	64.77 (2)	O4—V1—Ca1^xiii	76.31 (6)
V2^v—Ca1—V2^vi	90.18 (4)	V2^iii—V1—Ca1^xiii	103.706 (17)
O2^i—Ca1—V1^vii	103.10 (5)	V2—V1—Ca1^xiii	103.706 (17)
O2^ii—Ca1—V1^vii	103.10 (5)	Ca1—V1—Ca1^xiii	83.78 (3)
O4—Ca1—V1^vii	92.68 (6)	Ca1^x—V1—Ca1^xiii	173.81 (3)
O4^iii—Ca1—V1^vii	92.68 (6)	Ca1^xii—V1—Ca1^xiii	80.42 (3)
O3—Ca1—V1^vii	34.06 (5)	O1—V1—Ca1^xiv	75.758 (14)
O3^iii—Ca1—V1^vii	34.06 (5)	O3^x—V1—Ca1^xiv	54.61 (6)
O1^iv—Ca1—V1^vii	177.02 (8)	O3^xi—V1—Ca1^xiv	138.49 (6)
V1—Ca1—V1^vii	102.41 (4)	O4^iii—V1—Ca1^xiv	138.19 (6)
V2^v—Ca1—V1^vii	62.74 (2)	O4—V1—Ca1^xiv	54.97 (6)
V2^vi—Ca1—V1^vii	62.74 (2)	V2^iii—V1—Ca1^xiv	173.54 (3)
O2^i—Ca1—O1^viii	68.51 (6)	V2—V1—Ca1^xiv	34.95 (2)
O2^ii—Ca1—O1^viii	68.51 (6)	Ca1—V1—Ca1^xiv	99.290 (15)
O4—Ca1—O1^viii	139.18 (6)	Ca1^x—V1—Ca1^xiv	98.436 (15)
O4^iii—Ca1—O1^viii	139.18 (6)	Ca1^xii—V1—Ca1^xiv	78.118 (13)
O3—Ca1—O1^viii	72.45 (7)	Ca1^xiii—V1—Ca1^xiv	80.378 (13)
O3^iii—Ca1—O1^viii	72.45 (7)	O2—V2—O4^xiv	108.79 (10)
O1^iv—Ca1—O1^viii	120.11 (11)	O2—V2—O3^xiv	105.95 (10)
V1—Ca1—O1^viii	165.28 (6)	O4^xiv—V2—O3^xiv	89.48 (9)
V2^v—Ca1—O1^viii	105.63 (4)	O2—V2—O4	112.33 (10)
V2^vi—Ca1—O1^viii	105.63 (4)	O4^xiv—V2—O4	138.83 (5)
V1^vii—Ca1—O1^viii	62.88 (6)	O3^xiv—V2—O4	81.43 (9)
O2^i—Ca1—V2^i	15.82 (6)	O2—V2—O3^x	114.70 (10)
O2^ii—Ca1—V2^i	94.78 (7)	O4^xiv—V2—O3^x	81.30 (9)
O4—Ca1—V2^i	153.40 (6)	O3^xiv—V2—O3^x	139.17 (5)
O4^iii—Ca1—V2^i	100.22 (5)	O4—V2—O3^x	80.00 (8)
O3—Ca1—V2^i	136.45 (6)	O2—V2—V2^xiv	120.66 (7)
O3^iii—Ca1—V2^i	91.02 (5)	O4^xiv—V2—V2^xiv	40.62 (6)
O1^iv—Ca1—V2^i	69.90 (5)	O3^xiv—V2—V2^xiv	118.39 (7)
V1—Ca1—V2^i	124.93 (2)	O4—V2—V2^xiv	111.52 (7)
V2^v—Ca1—V2^i	170.29 (3)	O3^x—V2—V2^xiv	40.72 (6)
V2^vi—Ca1—V2^i	94.65 (2)	O2—V2—V2^v	114.13 (7)
V1^vii—Ca1—V2^i	112.27 (2)	O4^xiv—V2—V2^v	120.59 (7)
O1^viii—Ca1—V2^i	64.96 (4)	O3^xiv—V2—V2^v	40.92 (6)
O2^i—Ca1—V2^ii	94.78 (7)	O4—V2—V2^v	40.56 (6)
O2^ii—Ca1—V2^ii	15.82 (6)	O3^x—V2—V2^v	113.41 (7)
O4—Ca1—V2^ii	100.22 (5)	V2^xiv—V2—V2^v	125.21 (4)
O4^iii—Ca1—V2^ii	153.40 (6)	O2—V2—V1	127.57 (9)
O3—Ca1—V2^ii	91.02 (5)	O4^xiv—V2—V1	108.97 (6)
O3^iii—Ca1—V2^ii	136.45 (6)	O3^xiv—V2—V1	109.40 (7)
O1^iv—Ca1—V2^ii	69.90 (5)	O4—V2—V1	40.50 (6)
V1—Ca1—V2^ii	124.93 (2)	O3^x—V2—V1	40.29 (6)
V2^v—Ca1—V2^ii	94.65 (2)	V2^xiv—V2—V1	72.55 (3)
V2^vi—Ca1—V2^ii	170.29 (3)	V2^v—V2—V1	74.17 (3)
V1^vii—Ca1—V2^ii	112.27 (2)	O2—V2—Ca1^xiv	118.02 (9)
O1^viii—Ca1—V2^ii	64.96 (4)	O4^xiv—V2—Ca1^xiv	44.26 (6)
V2^i—Ca1—V2^ii	79.38 (3)	O3^xiv—V2—Ca1^xiv	45.40 (6)
O2^i—Ca1—V1^iv	68.38 (6)	O4—V2—Ca1^xiv	113.29 (7)
O2^ii—Ca1—V1^iv	68.38 (6)	O3^x—V2—Ca1^xiv	112.59 (7)
O4—Ca1—V1^iv	101.08 (6)	V2^xiv—V2—Ca1^xiv	76.58 (3)
O4^iii—Ca1—V1^iv	101.08 (5)	V2^v—V2—Ca1^xiv	79.24 (3)
O3—Ca1—V1^iv	144.91 (5)	V1—V2—Ca1^xiv	114.39 (3)
O3^iii—Ca1—V1^iv	144.91 (5)	O2—V2—Ca1^ii	23.30 (9)
O1^iv—Ca1—V1^iv	19.64 (7)	O4^xiv—V2—Ca1^ii	95.28 (6)
V1—Ca1—V1^iv	94.25 (3)	O3^xiv—V2—Ca1^ii	87.28 (6)
V2^v—Ca1—V1^iv	126.35 (2)	O4—V2—Ca1^ii	124.00 (6)
V2^vi—Ca1—V1^iv	126.35 (2)	O3^x—V2—Ca1^ii	132.96 (6)
V1^vii—Ca1—V1^iv	163.34 (3)	V2^xiv—V2—Ca1^ii	121.88 (3)
O1^viii—Ca1—V1^iv	100.46 (6)	V2^v—V2—Ca1^ii	108.53 (3)
V2^i—Ca1—V1^iv	56.28 (2)	V1—V2—Ca1^ii	150.19 (3)
V2^ii—Ca1—V1^iv	56.28 (2)	Ca1^xiv—V2—Ca1^ii	95.00 (2)
O2^i—Ca1—V2	146.03 (6)	O2—V2—Ca1	84.86 (8)
O2^ii—Ca1—V2	70.47 (6)	O4^xiv—V2—Ca1	164.72 (6)
O4—Ca1—V2	22.59 (5)	O3^xiv—V2—Ca1	93.35 (6)
O4^iii—Ca1—V2	82.78 (5)	O4—V2—Ca1	27.89 (6)
O3—Ca1—V2	80.57 (5)	O3^x—V2—Ca1	86.80 (7)
O3^iii—Ca1—V2	128.54 (6)	V2^xiv—V2—Ca1	126.52 (3)
O1^iv—Ca1—V2	68.14 (5)	V2^v—V2—Ca1	56.11 (2)
V1—Ca1—V2	47.604 (15)	V1—V2—Ca1	55.99 (2)
V2^v—Ca1—V2	47.316 (15)	Ca1^xiv—V2—Ca1	135.33 (3)
V2^vi—Ca1—V2	109.20 (3)	Ca1^ii—V2—Ca1	99.84 (2)
V1^vii—Ca1—V2	109.92 (3)	O2—V2—Ca1^x	89.27 (8)
O1^viii—Ca1—V2	134.675 (15)	O4^xiv—V2—Ca1^x	90.36 (6)
V2^i—Ca1—V2	137.47 (3)	O3^xiv—V2—Ca1^x	163.96 (7)
V2^ii—Ca1—V2	80.16 (2)	O4—V2—Ca1^x	88.19 (6)
V1^iv—Ca1—V2	81.37 (2)	O3^x—V2—Ca1^x	25.46 (6)
O2^i—Ca1—V2^iii	70.47 (6)	V2^xiv—V2—Ca1^x	54.57 (2)
O2^ii—Ca1—V2^iii	146.03 (6)	V2^v—V2—Ca1^x	128.03 (3)
O4—Ca1—V2^iii	82.78 (5)	V1—V2—Ca1^x	55.71 (2)
O4^iii—Ca1—V2^iii	22.59 (5)	Ca1^xiv—V2—Ca1^x	131.13 (2)
O3—Ca1—V2^iii	128.54 (6)	Ca1^ii—V2—Ca1^x	108.70 (2)
O3^iii—Ca1—V2^iii	80.57 (5)	Ca1—V2—Ca1^x	82.81 (2)
O1^iv—Ca1—V2^iii	68.14 (5)	V1—O1—Ca1^xii	128.54 (15)
V1—Ca1—V2^iii	47.604 (15)	V1—O1—Ca1^xiii	111.35 (13)
V2^v—Ca1—V2^iii	109.20 (3)	Ca1^xii—O1—Ca1^xiii	120.11 (11)
V2^vi—Ca1—V2^iii	47.316 (15)	V1—O1—Ca1^x	37.92 (8)
V1^vii—Ca1—V2^iii	109.92 (3)	Ca1^xii—O1—Ca1^x	90.62 (8)
O1^viii—Ca1—V2^iii	134.675 (15)	Ca1^xiii—O1—Ca1^x	149.27 (9)
V2^i—Ca1—V2^iii	80.16 (2)	V1—O1—Ca1	32.60 (8)
V2^ii—Ca1—V2^iii	137.47 (3)	Ca1^xii—O1—Ca1	161.13 (11)
V1^iv—Ca1—V2^iii	81.37 (2)	Ca1^xiii—O1—Ca1	78.76 (6)
V2—Ca1—V2^iii	90.59 (3)	Ca1^x—O1—Ca1	70.51 (5)
O2^i—Ca1—V2^ix	58.65 (5)	V2—O2—Ca1^ii	140.88 (14)
O2^ii—Ca1—V2^ix	127.64 (6)	V2—O2—Ca1	72.22 (8)
O4—Ca1—V2^ix	126.49 (6)	Ca1^ii—O2—Ca1	128.53 (7)
O4^iii—Ca1—V2^ix	79.59 (5)	V2—O2—Ca1^x	68.96 (8)
O3—Ca1—V2^ix	80.07 (6)	Ca1^ii—O2—Ca1^x	140.66 (7)
O3^iii—Ca1—V2^ix	20.43 (5)	Ca1—O2—Ca1^x	77.27 (5)
O1^iv—Ca1—V2^ix	134.55 (3)	V2—O2—Ca1^xiv	42.93 (7)
V1—Ca1—V2^ix	110.80 (3)	Ca1^ii—O2—Ca1^xiv	98.30 (7)
V2^v—Ca1—V2^ix	106.63 (3)	Ca1—O2—Ca1^xiv	105.66 (5)
V2^vi—Ca1—V2^ix	46.188 (15)	Ca1^x—O2—Ca1^xiv	101.92 (5)
V1^vii—Ca1—V2^ix	46.255 (15)	V1^vii—O3—V2^v	128.41 (11)
O1^viii—Ca1—V2^ix	59.77 (4)	V1^vii—O3—V2^vii	99.17 (9)
V2^i—Ca1—V2^ix	71.30 (2)	V2^v—O3—V2^vii	98.36 (10)
V2^ii—Ca1—V2^ix	124.17 (3)	V1^vii—O3—Ca1	102.05 (9)
V1^iv—Ca1—V2^ix	127.00 (2)	V2^v—O3—Ca1	99.43 (8)
V2—Ca1—V2^ix	148.95 (3)	V2^vii—O3—Ca1	134.11 (10)
V2^iii—Ca1—V2^ix	82.81 (2)	V1^vii—O3—Ca1^xiii	65.35 (6)
O2^i—Ca1—V2^vii	127.64 (6)	V2^v—O3—Ca1^xiii	64.38 (6)
O2^ii—Ca1—V2^vii	58.65 (5)	V2^vii—O3—Ca1^xiii	123.03 (8)
O4—Ca1—V2^vii	79.59 (5)	Ca1—O3—Ca1^xiii	102.80 (6)
O4^iii—Ca1—V2^vii	126.49 (6)	V1^vii—O3—Ca1^vii	48.93 (5)
O3—Ca1—V2^vii	20.43 (5)	V2^v—O3—Ca1^vii	160.68 (9)
O3^iii—Ca1—V2^vii	80.07 (6)	V2^vii—O3—Ca1^vii	66.01 (6)
O1^iv—Ca1—V2^vii	134.55 (3)	Ca1—O3—Ca1^vii	99.72 (7)
V1—Ca1—V2^vii	110.80 (3)	Ca1^xiii—O3—Ca1^vii	113.46 (5)
V2^v—Ca1—V2^vii	46.188 (15)	V1^vii—O3—Ca1^v	104.61 (7)
V2^vi—Ca1—V2^vii	106.63 (3)	V2^v—O3—Ca1^v	60.85 (6)
V1^vii—Ca1—V2^vii	46.255 (15)	V2^vii—O3—Ca1^v	43.58 (5)
O1^viii—Ca1—V2^vii	59.77 (4)	Ca1—O3—Ca1^v	153.14 (7)
V2^i—Ca1—V2^vii	124.17 (3)	Ca1^xiii—O3—Ca1^v	85.53 (4)
V2^ii—Ca1—V2^vii	71.30 (2)	Ca1^vii—O3—Ca1^v	100.17 (4)
V1^iv—Ca1—V2^vii	127.00 (2)	V2^v—O4—V2	98.82 (10)
V2—Ca1—V2^vii	82.81 (2)	V2^v—O4—V1	132.82 (11)
V2^iii—Ca1—V2^vii	148.95 (3)	V2—O4—V1	99.18 (9)
V2^ix—Ca1—V2^vii	87.38 (3)	V2^v—O4—Ca1	100.83 (8)
O2^i—Ca1—O2	132.48 (4)	V2—O4—Ca1	129.53 (10)
O2^ii—Ca1—O2	51.47 (7)	V1—O4—Ca1	100.43 (9)
O4—Ca1—O2	45.33 (6)	V2^v—O4—Ca1^xiii	58.20 (5)
O4^iii—Ca1—O2	100.78 (6)	V2—O4—Ca1^xiii	132.41 (8)
O3—Ca1—O2	89.11 (6)	V1—O4—Ca1^xiii	77.71 (6)
O3^iii—Ca1—O2	149.57 (7)	Ca1—O4—Ca1^xiii	97.15 (6)
O1^iv—Ca1—O2	56.35 (4)	V2^v—O4—Ca1^x	161.78 (9)
V1—Ca1—O2	66.97 (3)	V2—O4—Ca1^x	65.65 (5)
V2^v—Ca1—O2	62.25 (3)	V1—O4—Ca1^x	47.04 (5)
V2^vi—Ca1—O2	131.12 (4)	Ca1—O4—Ca1^x	96.67 (6)
V1^vii—Ca1—O2	122.69 (4)	Ca1^xiii—O4—Ca1^x	124.60 (5)
O1^viii—Ca1—O2	119.80 (4)	V2^v—O4—Ca1^xiv	63.92 (6)
V2^i—Ca1—O2	119.37 (4)	V2—O4—Ca1^xiv	43.18 (5)
V2^ii—Ca1—O2	58.50 (3)	V1—O4—Ca1^xiv	104.10 (7)
V1^iv—Ca1—O2	64.11 (3)	Ca1—O4—Ca1^xiv	155.30 (7)
V2—Ca1—O2	22.92 (3)	Ca1^xiii—O4—Ca1^xiv	90.83 (4)
V2^iii—Ca1—O2	101.90 (4)	Ca1^x—O4—Ca1^xiv	97.90 (4)
V2^ix—Ca1—O2	168.77 (4)	V2^v—O4—Ca1^ii	90.15 (7)
V2^vii—Ca1—O2	83.41 (4)	V2—O4—Ca1^ii	37.37 (5)
O1—V1—O3^x	109.21 (10)	V1—O4—Ca1^ii	128.26 (7)
O1—V1—O3^xi	109.21 (10)	Ca1—O4—Ca1^ii	96.62 (6)
O3^x—V1—O3^xi	86.48 (13)	Ca1^xiii—O4—Ca1^ii	147.33 (5)
O1—V1—O4^iii	111.32 (9)	Ca1^x—O4—Ca1^ii	82.79 (3)
O3^x—V1—O4^iii	139.47 (10)	Ca1^xiv—O4—Ca1^ii	65.71 (3)
O3^xi—V1—O4^iii	80.07 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_162K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.545 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2663 reflections
a = 10.418 (3) Å	θ = 1.3–23.4°
b = 10.368 (2) Å	µ = 5.68 mm^−1
c = 5.2892 (15) Å	T = 162 K
V = 571.3 (2) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	400 independent reflections
Radiation source: fine-focus sealed tube	362 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.034
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.318, Tmax = 0.470	l = −5→5
2398 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0438P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.053	(Δ/σ)max < 0.001
S = 0.96	Δρmax = 0.27 e Å^−3
400 reflections	Δρmin = −0.31 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0184 (19)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08493 (9)	0.2500	0.29986 (14)	0.0057 (3)
V1	0.28894 (7)	0.2500	0.79214 (13)	0.0045 (3)
V2	0.18736 (5)	0.52023 (5)	0.78355 (9)	0.0045 (3)
O1	0.4440 (3)	0.2500	0.8082 (5)	0.0087 (7)*
O2	0.0396 (2)	0.5654 (2)	0.7665 (3)	0.0100 (6)*
O3	0.22032 (19)	0.3797 (2)	0.0259 (4)	0.0055 (5)*
O4	0.22684 (19)	0.3794 (2)	0.5483 (4)	0.0053 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0045 (5)	0.0056 (6)	0.0069 (5)	0.000	−0.0004 (3)	0.000
V1	0.0037 (5)	0.0047 (5)	0.0050 (5)	0.000	−0.0002 (3)	0.000
V2	0.0041 (4)	0.0045 (4)	0.0050 (4)	0.0008 (2)	−0.0001 (2)	0.00011 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.338 (3)	V1—Ca1^xiii	4.3947 (14)
Ca1—O2^ii	2.338 (3)	V1—Ca1^xiv	5.3483 (11)
Ca1—O4	2.390 (2)	V2—O2	1.612 (2)
Ca1—O4^iii	2.390 (2)	V2—O4^xiv	1.960 (2)
Ca1—O3^iii	2.428 (2)	V2—O4	1.962 (2)
Ca1—O3	2.428 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.540 (3)	V2—O3^x	1.971 (2)
Ca1—V1	3.3611 (12)	V2—V2^xiv	2.9788 (9)
Ca1—V2^v	3.3632 (11)	V2—V2^v	2.9788 (9)
Ca1—V2^vi	3.3632 (11)	V2—Ca1^xiv	3.3632 (11)
Ca1—V1^vii	3.4247 (13)	V2—Ca1^ii	3.7306 (11)
Ca1—O1^viii	3.536 (3)	V2—Ca1^x	4.0554 (10)
Ca1—V2^i	3.7306 (11)	O1—Ca1^xii	2.540 (3)
Ca1—V2^ii	3.7306 (11)	O1—Ca1^xiii	3.536 (3)
Ca1—V1^iv	3.7638 (14)	O1—Ca1^x	4.556 (3)
Ca1—V2	3.9413 (10)	O2—Ca1^ii	2.338 (3)
Ca1—V2^iii	3.9413 (10)	O2—Ca1^x	4.345 (2)
Ca1—V2^ix	4.0554 (10)	O2—Ca1^xiv	4.358 (3)
Ca1—V2^vii	4.0554 (10)	O3—V1^vii	1.961 (2)
Ca1—O2	4.125 (2)	O3—V2^v	1.964 (2)
V1—O1	1.617 (3)	O3—V2^vii	1.971 (2)
V1—O3^x	1.961 (2)	O3—Ca1^xiii	4.133 (2)
V1—O3^xi	1.961 (2)	O3—Ca1^vii	4.306 (2)
V1—O4^iii	1.9704 (19)	O3—Ca1^v	4.505 (2)
V1—O4	1.9704 (19)	O4—V2^v	1.960 (2)
V1—V2^iii	2.9953 (8)	O4—Ca1^xiii	4.371 (2)
V1—V2	2.9953 (8)	O4—Ca1^x	4.448 (2)
V1—Ca1^x	3.4247 (13)	O4—Ca1^xiv	4.514 (2)
V1—Ca1^xii	3.7638 (14)	O4—Ca1^ii	5.095 (2)
O2^i—Ca1—O2^ii	109.83 (12)	O1—V1—O4	111.24 (9)
O2^i—Ca1—O4	152.27 (7)	O3^x—V1—O4	80.00 (8)
O2^ii—Ca1—O4	88.07 (7)	O3^xi—V1—O4	139.44 (10)
O2^i—Ca1—O4^iii	88.07 (7)	O4^iii—V1—O4	85.85 (12)
O2^ii—Ca1—O4^iii	152.27 (7)	O1—V1—V2^iii	110.708 (18)
O4—Ca1—O4^iii	68.30 (10)	O3^x—V1—V2^iii	121.46 (7)
O2^i—Ca1—O3^iii	77.27 (7)	O3^xi—V1—V2^iii	40.51 (6)
O2^ii—Ca1—O3^iii	133.29 (7)	O4^iii—V1—V2^iii	40.28 (6)
O4—Ca1—O3^iii	106.23 (8)	O4—V1—V2^iii	120.74 (7)
O4^iii—Ca1—O3^iii	70.00 (7)	O1—V1—V2	110.708 (18)
O2^i—Ca1—O3	133.29 (7)	O3^x—V1—V2	40.51 (6)
O2^ii—Ca1—O3	77.27 (7)	O3^xi—V1—V2	121.46 (7)
O4—Ca1—O3	70.00 (7)	O4^iii—V1—V2	120.74 (7)
O4^iii—Ca1—O3	106.23 (8)	O4—V1—V2	40.28 (6)
O3^iii—Ca1—O3	67.24 (10)	V2^iii—V1—V2	138.58 (4)
O2^i—Ca1—O1^iv	78.57 (6)	O1—V1—Ca1	132.24 (10)
O2^ii—Ca1—O1^iv	78.57 (6)	O3^x—V1—Ca1	104.95 (6)
O4—Ca1—O1^iv	84.77 (8)	O3^xi—V1—Ca1	104.95 (6)
O4^iii—Ca1—O1^iv	84.77 (8)	O4^iii—V1—Ca1	44.38 (6)
O3^iii—Ca1—O1^iv	145.35 (5)	O4—V1—Ca1	44.38 (6)
O3—Ca1—O1^iv	145.35 (5)	V2^iii—V1—Ca1	76.399 (17)
O2^i—Ca1—V1	117.85 (5)	V2—V1—Ca1	76.399 (17)
O2^ii—Ca1—V1	117.85 (5)	O1—V1—Ca1^x	125.35 (10)
O4—Ca1—V1	35.21 (5)	O3^x—V1—Ca1^x	43.90 (6)
O4^iii—Ca1—V1	35.21 (5)	O3^xi—V1—Ca1^x	43.90 (6)
O3^iii—Ca1—V1	95.45 (6)	O4^iii—V1—Ca1^x	108.03 (6)
O3—Ca1—V1	95.45 (6)	O4—V1—Ca1^x	108.03 (6)
O1^iv—Ca1—V1	74.54 (7)	V2^iii—V1—Ca1^x	78.033 (17)
O2^i—Ca1—V2^v	165.28 (6)	V2—V1—Ca1^x	78.033 (17)
O2^ii—Ca1—V2^v	78.92 (6)	Ca1—V1—Ca1^x	102.42 (4)
O4—Ca1—V2^v	34.93 (5)	O1—V1—Ca1^xii	31.97 (10)
O4^iii—Ca1—V2^v	88.59 (6)	O3^x—V1—Ca1^xii	86.40 (6)
O3^iii—Ca1—V2^v	88.12 (6)	O3^xi—V1—Ca1^xii	86.40 (6)
O3—Ca1—V2^v	35.19 (5)	O4^iii—V1—Ca1^xii	130.11 (6)
O1^iv—Ca1—V2^v	115.38 (5)	O4—V1—Ca1^xii	130.11 (6)
V1—Ca1—V2^v	64.78 (2)	V2^iii—V1—Ca1^xii	107.347 (17)
O2^i—Ca1—V2^vi	78.92 (6)	V2—V1—Ca1^xii	107.347 (17)
O2^ii—Ca1—V2^vi	165.28 (6)	Ca1—V1—Ca1^xii	164.21 (3)
O4—Ca1—V2^vi	88.59 (6)	Ca1^x—V1—Ca1^xii	93.37 (3)
O4^iii—Ca1—V2^vi	34.93 (5)	O1—V1—Ca1^xiii	48.45 (10)
O3^iii—Ca1—V2^vi	35.19 (5)	O3^x—V1—Ca1^xiii	134.82 (6)
O3—Ca1—V2^vi	88.12 (6)	O3^xi—V1—Ca1^xiii	134.82 (6)
O1^iv—Ca1—V2^vi	115.38 (5)	O4^iii—V1—Ca1^xiii	76.35 (6)
V1—Ca1—V2^vi	64.78 (2)	O4—V1—Ca1^xiii	76.35 (6)
V2^v—Ca1—V2^vi	90.20 (3)	V2^iii—V1—Ca1^xiii	103.714 (17)
O2^i—Ca1—V1^vii	103.09 (5)	V2—V1—Ca1^xiii	103.714 (17)
O2^ii—Ca1—V1^vii	103.09 (5)	Ca1—V1—Ca1^xiii	83.78 (3)
O4—Ca1—V1^vii	92.71 (6)	Ca1^x—V1—Ca1^xiii	173.80 (3)
O4^iii—Ca1—V1^vii	92.71 (6)	Ca1^xii—V1—Ca1^xiii	80.42 (3)
O3^iii—Ca1—V1^vii	34.07 (5)	O1—V1—Ca1^xiv	75.773 (13)
O3—Ca1—V1^vii	34.07 (5)	O3^x—V1—Ca1^xiv	54.58 (6)
O1^iv—Ca1—V1^vii	176.95 (7)	O3^xi—V1—Ca1^xiv	138.51 (6)
V1—Ca1—V1^vii	102.42 (4)	O4^iii—V1—Ca1^xiv	138.23 (6)
V2^v—Ca1—V1^vii	62.75 (2)	O4—V1—Ca1^xiv	54.94 (6)
V2^vi—Ca1—V1^vii	62.75 (2)	V2^iii—V1—Ca1^xiv	173.52 (3)
O2^i—Ca1—O1^viii	68.47 (5)	V2—V1—Ca1^xiv	34.939 (19)
O2^ii—Ca1—O1^viii	68.47 (5)	Ca1—V1—Ca1^xiv	99.281 (14)
O4—Ca1—O1^viii	139.20 (6)	Ca1^x—V1—Ca1^xiv	98.424 (14)
O4^iii—Ca1—O1^viii	139.20 (6)	Ca1^xii—V1—Ca1^xiv	78.131 (13)
O3^iii—Ca1—O1^viii	72.45 (6)	Ca1^xiii—V1—Ca1^xiv	80.388 (13)
O3—Ca1—O1^viii	72.45 (6)	O2—V2—O4^xiv	108.72 (10)
O1^iv—Ca1—O1^viii	120.15 (11)	O2—V2—O4	112.42 (10)
V1—Ca1—O1^viii	165.32 (6)	O4^xiv—V2—O4	138.80 (5)
V2^v—Ca1—O1^viii	105.64 (4)	O2—V2—O3^xiv	105.98 (10)
V2^vi—Ca1—O1^viii	105.64 (4)	O4^xiv—V2—O3^xiv	89.52 (9)
V1^vii—Ca1—O1^viii	62.90 (6)	O4—V2—O3^xiv	81.41 (9)
O2^i—Ca1—V2^i	15.80 (6)	O2—V2—O3^x	114.69 (10)
O2^ii—Ca1—V2^i	94.76 (6)	O4^xiv—V2—O3^x	81.28 (9)
O4—Ca1—V2^i	153.36 (5)	O4—V2—O3^x	79.97 (8)
O4^iii—Ca1—V2^i	100.18 (5)	O3^xiv—V2—O3^x	139.16 (4)
O3^iii—Ca1—V2^i	91.01 (5)	O2—V2—V2^xiv	120.60 (7)
O3—Ca1—V2^i	136.45 (6)	O4^xiv—V2—V2^xiv	40.60 (6)
O1^iv—Ca1—V2^i	69.94 (5)	O4—V2—V2^xiv	111.49 (6)
V1—Ca1—V2^i	124.92 (2)	O3^xiv—V2—V2^xiv	118.40 (7)
V2^v—Ca1—V2^i	170.30 (2)	O3^x—V2—V2^xiv	40.73 (6)
V2^vi—Ca1—V2^i	94.64 (2)	O2—V2—V2^v	114.20 (7)
V1^vii—Ca1—V2^i	112.28 (2)	O4^xiv—V2—V2^v	120.61 (7)
O1^viii—Ca1—V2^i	64.95 (4)	O4—V2—V2^v	40.56 (6)
O2^i—Ca1—V2^ii	94.76 (6)	O3^xiv—V2—V2^v	40.90 (6)
O2^ii—Ca1—V2^ii	15.80 (6)	O3^x—V2—V2^v	113.39 (7)
O4—Ca1—V2^ii	100.18 (5)	V2^xiv—V2—V2^v	125.20 (4)
O4^iii—Ca1—V2^ii	153.36 (5)	O2—V2—V1	127.62 (9)
O3^iii—Ca1—V2^ii	136.45 (6)	O4^xiv—V2—V1	108.94 (6)
O3—Ca1—V2^ii	91.01 (5)	O4—V2—V1	40.49 (6)
O1^iv—Ca1—V2^ii	69.94 (5)	O3^xiv—V2—V1	109.38 (6)
V1—Ca1—V2^ii	124.92 (2)	O3^x—V2—V1	40.27 (6)
V2^v—Ca1—V2^ii	94.64 (2)	V2^xiv—V2—V1	72.54 (2)
V2^vi—Ca1—V2^ii	170.30 (2)	V2^v—V2—V1	74.16 (3)
V1^vii—Ca1—V2^ii	112.28 (2)	O2—V2—Ca1^xiv	117.97 (9)
O1^viii—Ca1—V2^ii	64.95 (4)	O4^xiv—V2—Ca1^xiv	44.28 (6)
V2^i—Ca1—V2^ii	79.38 (3)	O4—V2—Ca1^xiv	113.30 (6)
O2^i—Ca1—V1^iv	68.38 (5)	O3^xiv—V2—Ca1^xiv	45.42 (6)
O2^ii—Ca1—V1^iv	68.38 (5)	O3^x—V2—Ca1^xiv	112.59 (6)
O4—Ca1—V1^iv	101.04 (5)	V2^xiv—V2—Ca1^xiv	76.58 (3)
O4^iii—Ca1—V1^iv	101.04 (5)	V2^v—V2—Ca1^xiv	79.25 (3)
O3^iii—Ca1—V1^iv	144.89 (5)	V1—V2—Ca1^xiv	114.39 (3)
O3—Ca1—V1^iv	144.89 (5)	O2—V2—Ca1^ii	23.27 (9)
O1^iv—Ca1—V1^iv	19.70 (7)	O4^xiv—V2—Ca1^ii	95.29 (6)
V1—Ca1—V1^iv	94.24 (3)	O4—V2—Ca1^ii	124.03 (6)
V2^v—Ca1—V1^iv	126.343 (19)	O3^xiv—V2—Ca1^ii	87.30 (6)
V2^vi—Ca1—V1^iv	126.343 (19)	O3^x—V2—Ca1^ii	132.96 (6)
V1^vii—Ca1—V1^iv	163.34 (3)	V2^xiv—V2—Ca1^ii	121.88 (3)
O1^viii—Ca1—V1^iv	100.45 (6)	V2^v—V2—Ca1^ii	108.55 (3)
V2^i—Ca1—V1^iv	56.28 (2)	V1—V2—Ca1^ii	150.20 (2)
V2^ii—Ca1—V1^iv	56.28 (2)	Ca1^xiv—V2—Ca1^ii	94.99 (2)
O2^i—Ca1—V2	146.04 (5)	O2—V2—Ca1	84.95 (8)
O2^ii—Ca1—V2	70.49 (5)	O4^xiv—V2—Ca1	164.69 (6)
O4—Ca1—V2	22.57 (5)	O4—V2—Ca1	27.88 (6)
O4^iii—Ca1—V2	82.81 (5)	O3^xiv—V2—Ca1	93.33 (6)
O3^iii—Ca1—V2	128.58 (6)	O3^x—V2—Ca1	86.77 (6)
O3—Ca1—V2	80.59 (5)	V2^xiv—V2—Ca1	126.50 (3)
O1^iv—Ca1—V2	68.09 (5)	V2^v—V2—Ca1	56.10 (2)
V1—Ca1—V2	47.619 (15)	V1—V2—Ca1	55.98 (2)
V2^v—Ca1—V2	47.320 (14)	Ca1^xiv—V2—Ca1	135.33 (2)
V2^vi—Ca1—V2	109.22 (3)	Ca1^ii—V2—Ca1	99.866 (19)
V1^vii—Ca1—V2	109.94 (3)	O2—V2—Ca1^x	89.27 (8)
O1^viii—Ca1—V2	134.662 (15)	O4^xiv—V2—Ca1^x	90.32 (6)
V2^i—Ca1—V2	137.44 (2)	O4—V2—Ca1^x	88.17 (6)
V2^ii—Ca1—V2	80.134 (19)	O3^xiv—V2—Ca1^x	163.94 (6)
V1^iv—Ca1—V2	81.35 (2)	O3^x—V2—Ca1^x	25.45 (6)
O2^i—Ca1—V2^iii	70.49 (5)	V2^xiv—V2—Ca1^x	54.56 (2)
O2^ii—Ca1—V2^iii	146.04 (5)	V2^v—V2—Ca1^x	128.01 (3)
O4—Ca1—V2^iii	82.81 (5)	V1—V2—Ca1^x	55.70 (2)
O4^iii—Ca1—V2^iii	22.57 (5)	Ca1^xiv—V2—Ca1^x	131.13 (2)
O3^iii—Ca1—V2^iii	80.59 (5)	Ca1^ii—V2—Ca1^x	108.71 (2)
O3—Ca1—V2^iii	128.58 (6)	Ca1—V2—Ca1^x	82.80 (2)
O1^iv—Ca1—V2^iii	68.09 (5)	V1—O1—Ca1^xii	128.33 (15)
V1—Ca1—V2^iii	47.619 (15)	V1—O1—Ca1^xiii	111.53 (12)
V2^v—Ca1—V2^iii	109.22 (3)	Ca1^xii—O1—Ca1^xiii	120.15 (11)
V2^vi—Ca1—V2^iii	47.320 (14)	V1—O1—Ca1^x	37.82 (8)
V1^vii—Ca1—V2^iii	109.94 (3)	Ca1^xii—O1—Ca1^x	90.51 (7)
O1^viii—Ca1—V2^iii	134.662 (15)	Ca1^xiii—O1—Ca1^x	149.35 (9)
V2^i—Ca1—V2^iii	80.134 (19)	V1—O1—Ca1	32.70 (7)
V2^ii—Ca1—V2^iii	137.44 (2)	Ca1^xii—O1—Ca1	161.02 (10)
V1^iv—Ca1—V2^iii	81.35 (2)	Ca1^xiii—O1—Ca1	78.83 (6)
V2—Ca1—V2^iii	90.61 (3)	Ca1^x—O1—Ca1	70.52 (5)
O2^i—Ca1—V2^ix	58.64 (5)	V2—O2—Ca1^ii	140.93 (14)
O2^ii—Ca1—V2^ix	127.60 (5)	V2—O2—Ca1	72.14 (8)
O4—Ca1—V2^ix	126.53 (6)	Ca1^ii—O2—Ca1	128.50 (7)
O4^iii—Ca1—V2^ix	79.61 (5)	V2—O2—Ca1^x	68.96 (8)
O3^iii—Ca1—V2^ix	20.42 (5)	Ca1^ii—O2—Ca1^x	140.70 (7)
O3—Ca1—V2^ix	80.09 (5)	Ca1—O2—Ca1^x	77.24 (5)
O1^iv—Ca1—V2^ix	134.55 (2)	V2—O2—Ca1^xiv	42.97 (7)
V1—Ca1—V2^ix	110.81 (3)	Ca1^ii—O2—Ca1^xiv	98.32 (7)
V2^v—Ca1—V2^ix	106.65 (3)	Ca1—O2—Ca1^xiv	105.64 (5)
V2^vi—Ca1—V2^ix	46.190 (14)	Ca1^x—O2—Ca1^xiv	101.93 (4)
V1^vii—Ca1—V2^ix	46.265 (15)	V1^vii—O3—V2^v	128.39 (11)
O1^viii—Ca1—V2^ix	59.78 (3)	V1^vii—O3—V2^vii	99.22 (9)
V2^i—Ca1—V2^ix	71.29 (2)	V2^v—O3—V2^vii	98.38 (9)
V2^ii—Ca1—V2^ix	124.17 (2)	V1^vii—O3—Ca1	102.03 (9)
V1^iv—Ca1—V2^ix	126.99 (2)	V2^v—O3—Ca1	99.39 (8)
V2—Ca1—V2^ix	148.98 (3)	V2^vii—O3—Ca1	134.13 (10)
V2^iii—Ca1—V2^ix	82.80 (2)	V1^vii—O3—Ca1^xiii	65.34 (6)
O2^i—Ca1—V2^vii	127.60 (5)	V2^v—O3—Ca1^xiii	64.36 (6)
O2^ii—Ca1—V2^vii	58.64 (5)	V2^vii—O3—Ca1^xiii	123.06 (8)
O4—Ca1—V2^vii	79.61 (5)	Ca1—O3—Ca1^xiii	102.75 (6)
O4^iii—Ca1—V2^vii	126.53 (6)	V1^vii—O3—Ca1^vii	48.94 (5)
O3^iii—Ca1—V2^vii	80.09 (5)	V2^v—O3—Ca1^vii	160.70 (9)
O3—Ca1—V2^vii	20.42 (5)	V2^vii—O3—Ca1^vii	66.03 (5)
O1^iv—Ca1—V2^vii	134.55 (2)	Ca1—O3—Ca1^vii	99.73 (7)
V1—Ca1—V2^vii	110.81 (3)	Ca1^xiii—O3—Ca1^vii	113.47 (5)
V2^v—Ca1—V2^vii	46.190 (14)	V1^vii—O3—Ca1^v	104.64 (7)
V2^vi—Ca1—V2^vii	106.65 (3)	V2^v—O3—Ca1^v	60.86 (6)
V1^vii—Ca1—V2^vii	46.265 (15)	V2^vii—O3—Ca1^v	43.58 (5)
O1^viii—Ca1—V2^vii	59.78 (3)	Ca1—O3—Ca1^v	153.13 (7)
V2^i—Ca1—V2^vii	124.17 (2)	Ca1^xiii—O3—Ca1^v	85.55 (4)
V2^ii—Ca1—V2^vii	71.29 (2)	Ca1^vii—O3—Ca1^v	100.19 (4)
V1^iv—Ca1—V2^vii	126.99 (2)	V2^v—O4—V2	98.84 (9)
V2—Ca1—V2^vii	82.80 (2)	V2^v—O4—V1	132.80 (11)
V2^iii—Ca1—V2^vii	148.98 (3)	V2—O4—V1	99.24 (9)
V2^ix—Ca1—V2^vii	87.40 (3)	V2^v—O4—Ca1	100.80 (8)
O2^i—Ca1—O2	132.47 (4)	V2—O4—Ca1	129.55 (10)
O2^ii—Ca1—O2	51.50 (7)	V1—O4—Ca1	100.40 (9)
O4—Ca1—O2	45.30 (6)	V2^v—O4—Ca1^xiii	58.19 (5)
O4^iii—Ca1—O2	100.77 (6)	V2—O4—Ca1^xiii	132.42 (8)
O3^iii—Ca1—O2	149.61 (6)	V1—O4—Ca1^xiii	77.67 (6)
O3—Ca1—O2	89.11 (6)	Ca1—O4—Ca1^xiii	97.12 (6)
O1^iv—Ca1—O2	56.32 (4)	V2^v—O4—Ca1^x	161.81 (8)
V1—Ca1—O2	66.97 (3)	V2—O4—Ca1^x	65.67 (5)
V2^v—Ca1—O2	62.25 (3)	V1—O4—Ca1^x	47.06 (5)
V2^vi—Ca1—O2	131.13 (4)	Ca1—O4—Ca1^x	96.68 (6)
V1^vii—Ca1—O2	122.70 (3)	Ca1^xiii—O4—Ca1^x	124.57 (5)
O1^viii—Ca1—O2	119.79 (4)	V2^v—O4—Ca1^xiv	63.94 (6)
V2^i—Ca1—O2	119.35 (4)	V2—O4—Ca1^xiv	43.18 (5)
V2^ii—Ca1—O2	58.49 (3)	V1—O4—Ca1^xiv	104.13 (7)
V1^iv—Ca1—O2	64.09 (3)	Ca1—O4—Ca1^xiv	155.31 (7)
V2—Ca1—O2	22.90 (3)	Ca1^xiii—O4—Ca1^xiv	90.84 (4)
V2^iii—Ca1—O2	101.90 (4)	Ca1^x—O4—Ca1^xiv	97.92 (4)
V2^ix—Ca1—O2	168.79 (4)	V2^v—O4—Ca1^ii	90.17 (7)
V2^vii—Ca1—O2	83.41 (4)	V2—O4—Ca1^ii	37.36 (4)
O1—V1—O3^x	109.32 (9)	V1—O4—Ca1^ii	128.29 (7)
O1—V1—O3^xi	109.32 (9)	Ca1—O4—Ca1^ii	96.64 (6)
O3^x—V1—O3^xi	86.53 (12)	Ca1^xiii—O4—Ca1^ii	147.35 (5)
O1—V1—O4^iii	111.24 (9)	Ca1^x—O4—Ca1^ii	82.80 (3)
O3^x—V1—O4^iii	139.44 (10)	Ca1^xiv—O4—Ca1^ii	65.71 (3)
O3^xi—V1—O4^iii	80.00 (8)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_150K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.545 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2729 reflections
a = 10.416 (3) Å	θ = 1.3–23.4°
b = 10.370 (2) Å	µ = 5.68 mm^−1
c = 5.2893 (15) Å	T = 150 K
V = 571.3 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	399 independent reflections
Radiation source: fine-focus sealed tube	366 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.033
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.470	l = −5→5
2461 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0477P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.055	(Δ/σ)max < 0.001
S = 0.93	Δρmax = 0.27 e Å^−3
399 reflections	Δρmin = −0.28 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0188 (19)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08498 (9)	0.2500	0.29988 (14)	0.0055 (3)
V1	0.28894 (7)	0.2500	0.79226 (13)	0.0044 (3)
V2	0.18733 (5)	0.52016 (5)	0.78354 (9)	0.0044 (3)
O1	0.4440 (3)	0.2500	0.8087 (5)	0.0083 (7)*
O2	0.0395 (2)	0.5651 (2)	0.7661 (3)	0.0095 (6)*
O3	0.22042 (19)	0.3796 (2)	0.0261 (4)	0.0055 (5)*
O4	0.22702 (19)	0.3794 (2)	0.5482 (3)	0.0051 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0038 (5)	0.0057 (6)	0.0071 (5)	0.000	−0.0005 (3)	0.000
V1	0.0036 (5)	0.0044 (5)	0.0054 (5)	0.000	−0.0003 (3)	0.000
V2	0.0038 (4)	0.0044 (4)	0.0051 (4)	0.0008 (2)	0.0001 (2)	−0.00002 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.341 (2)	V1—Ca1^xiii	4.3951 (14)
Ca1—O2^ii	2.341 (2)	V1—Ca1^xiv	5.3491 (12)
Ca1—O4	2.390 (2)	V2—O2	1.611 (2)
Ca1—O4^iii	2.390 (2)	V2—O4^xiv	1.959 (2)
Ca1—O3	2.428 (2)	V2—O3^xiv	1.964 (2)
Ca1—O3^iii	2.428 (2)	V2—O4	1.963 (2)
Ca1—O1^iv	2.538 (3)	V2—O3^x	1.972 (2)
Ca1—V1	3.3610 (12)	V2—V2^xiv	2.9788 (9)
Ca1—V2^v	3.3635 (11)	V2—V2^v	2.9788 (9)
Ca1—V2^vi	3.3635 (11)	V2—Ca1^xiv	3.3635 (11)
Ca1—V1^vii	3.4238 (13)	V2—Ca1^ii	3.7311 (11)
Ca1—O1^viii	3.538 (3)	V2—Ca1^x	4.0552 (10)
Ca1—V2^i	3.7311 (11)	O1—Ca1^xii	2.538 (3)
Ca1—V2^ii	3.7311 (11)	O1—Ca1^xiii	3.538 (3)
Ca1—V1^iv	3.7632 (14)	O1—Ca1^x	4.554 (3)
Ca1—V2	3.9409 (10)	O2—Ca1^ii	2.341 (2)
Ca1—V2^iii	3.9409 (10)	O2—Ca1^x	4.344 (2)
Ca1—V2^ix	4.0552 (10)	O2—Ca1^xiv	4.359 (2)
Ca1—V2^vii	4.0552 (10)	O3—V1^vii	1.961 (2)
Ca1—O2	4.122 (2)	O3—V2^v	1.964 (2)
V1—O1	1.618 (3)	O3—V2^vii	1.972 (2)
V1—O3^x	1.961 (2)	O3—Ca1^xiii	4.132 (2)
V1—O3^xi	1.961 (2)	O3—Ca1^vii	4.307 (2)
V1—O4^iii	1.9707 (19)	O3—Ca1^v	4.505 (2)
V1—O4	1.9707 (19)	O4—V2^v	1.959 (2)
V1—V2^iii	2.9953 (9)	O4—Ca1^xiii	4.369 (2)
V1—V2	2.9953 (9)	O4—Ca1^x	4.450 (2)
V1—Ca1^x	3.4238 (13)	O4—Ca1^xiv	4.514 (2)
V1—Ca1^xii	3.7632 (14)	O4—Ca1^ii	5.097 (2)
O2^i—Ca1—O2^ii	109.98 (12)	O1—V1—O4	111.23 (9)
O2^i—Ca1—O4	152.21 (7)	O3^x—V1—O4	80.05 (8)
O2^ii—Ca1—O4	88.00 (7)	O3^xi—V1—O4	139.54 (10)
O2^i—Ca1—O4^iii	88.00 (7)	O4^iii—V1—O4	85.83 (12)
O2^ii—Ca1—O4^iii	152.21 (7)	O1—V1—V2^iii	110.711 (18)
O4—Ca1—O4^iii	68.30 (10)	O3^x—V1—V2^iii	121.49 (7)
O2^i—Ca1—O3	133.35 (7)	O3^xi—V1—V2^iii	40.53 (6)
O2^ii—Ca1—O3	77.25 (7)	O4^iii—V1—V2^iii	40.30 (6)
O4—Ca1—O3	69.95 (7)	O4—V1—V2^iii	120.74 (7)
O4^iii—Ca1—O3	106.19 (8)	O1—V1—V2	110.711 (18)
O2^i—Ca1—O3^iii	77.25 (7)	O3^x—V1—V2	40.53 (6)
O2^ii—Ca1—O3^iii	133.35 (7)	O3^xi—V1—V2	121.49 (7)
O4—Ca1—O3^iii	106.19 (8)	O4^iii—V1—V2	120.74 (7)
O4^iii—Ca1—O3^iii	69.95 (7)	O4—V1—V2	40.30 (6)
O3—Ca1—O3^iii	67.25 (10)	V2^iii—V1—V2	138.58 (4)
O2^i—Ca1—O1^iv	78.53 (6)	O1—V1—Ca1	132.29 (10)
O2^ii—Ca1—O1^iv	78.53 (6)	O3^x—V1—Ca1	104.99 (6)
O4—Ca1—O1^iv	84.83 (8)	O3^xi—V1—Ca1	104.99 (6)
O4^iii—Ca1—O1^iv	84.83 (8)	O4^iii—V1—Ca1	44.39 (6)
O3—Ca1—O1^iv	145.35 (5)	O4—V1—Ca1	44.39 (6)
O3^iii—Ca1—O1^iv	145.35 (5)	V2^iii—V1—Ca1	76.392 (17)
O2^i—Ca1—V1	117.76 (5)	V2—V1—Ca1	76.392 (17)
O2^ii—Ca1—V1	117.76 (5)	O1—V1—Ca1^x	125.26 (10)
O4—Ca1—V1	35.22 (5)	O3^x—V1—Ca1^x	43.92 (6)
O4^iii—Ca1—V1	35.22 (5)	O3^xi—V1—Ca1^x	43.92 (6)
O3—Ca1—V1	95.45 (6)	O4^iii—V1—Ca1^x	108.10 (6)
O3^iii—Ca1—V1	95.45 (6)	O4—V1—Ca1^x	108.10 (6)
O1^iv—Ca1—V1	74.55 (7)	V2^iii—V1—Ca1^x	78.043 (17)
O2^i—Ca1—V2^v	165.28 (6)	V2—V1—Ca1^x	78.043 (17)
O2^ii—Ca1—V2^v	78.84 (6)	Ca1—V1—Ca1^x	102.44 (4)
O4—Ca1—V2^v	34.90 (5)	O1—V1—Ca1^xii	31.89 (10)
O4^iii—Ca1—V2^v	88.60 (6)	O3^x—V1—Ca1^xii	86.37 (6)
O3—Ca1—V2^v	35.17 (5)	O3^xi—V1—Ca1^xii	86.37 (6)
O3^iii—Ca1—V2^v	88.13 (6)	O4^iii—V1—Ca1^xii	130.07 (6)
O1^iv—Ca1—V2^v	115.39 (5)	O4—V1—Ca1^xii	130.07 (6)
V1—Ca1—V2^v	64.80 (2)	V2^iii—V1—Ca1^xii	107.358 (17)
O2^i—Ca1—V2^vi	78.84 (6)	V2—V1—Ca1^xii	107.358 (17)
O2^ii—Ca1—V2^vi	165.28 (6)	Ca1—V1—Ca1^xii	164.18 (3)
O4—Ca1—V2^vi	88.60 (6)	Ca1^x—V1—Ca1^xii	93.37 (3)
O4^iii—Ca1—V2^vi	34.90 (5)	O1—V1—Ca1^xiii	48.54 (10)
O3—Ca1—V2^vi	88.13 (6)	O3^x—V1—Ca1^xiii	134.80 (6)
O3^iii—Ca1—V2^vi	35.17 (5)	O3^xi—V1—Ca1^xiii	134.80 (6)
O1^iv—Ca1—V2^vi	115.39 (5)	O4^iii—V1—Ca1^xiii	76.27 (6)
V1—Ca1—V2^vi	64.80 (2)	O4—V1—Ca1^xiii	76.27 (6)
V2^v—Ca1—V2^vi	90.25 (4)	V2^iii—V1—Ca1^xiii	103.705 (17)
O2^i—Ca1—V1^vii	103.11 (5)	V2—V1—Ca1^xiii	103.705 (17)
O2^ii—Ca1—V1^vii	103.11 (5)	Ca1—V1—Ca1^xiii	83.76 (3)
O4—Ca1—V1^vii	92.68 (6)	Ca1^x—V1—Ca1^xiii	173.80 (3)
O4^iii—Ca1—V1^vii	92.68 (6)	Ca1^xii—V1—Ca1^xiii	80.43 (3)
O3—Ca1—V1^vii	34.08 (5)	O1—V1—Ca1^xiv	75.786 (13)
O3^iii—Ca1—V1^vii	34.08 (5)	O3^x—V1—Ca1^xiv	54.55 (6)
O1^iv—Ca1—V1^vii	176.99 (8)	O3^xi—V1—Ca1^xiv	138.51 (6)
V1—Ca1—V1^vii	102.44 (4)	O4^iii—V1—Ca1^xiv	138.19 (6)
V2^v—Ca1—V1^vii	62.76 (2)	O4—V1—Ca1^xiv	54.92 (6)
V2^vi—Ca1—V1^vii	62.76 (2)	V2^iii—V1—Ca1^xiv	173.50 (2)
O2^i—Ca1—O1^viii	68.55 (5)	V2—V1—Ca1^xiv	34.930 (19)
O2^ii—Ca1—O1^viii	68.55 (5)	Ca1—V1—Ca1^xiv	99.266 (14)
O4—Ca1—O1^viii	139.17 (6)	Ca1^x—V1—Ca1^xiv	98.420 (14)
O4^iii—Ca1—O1^viii	139.17 (6)	Ca1^xii—V1—Ca1^xiv	78.143 (13)
O3—Ca1—O1^viii	72.45 (6)	Ca1^xiii—V1—Ca1^xiv	80.394 (13)
O3^iii—Ca1—O1^viii	72.45 (6)	O2—V2—O4^xiv	108.78 (10)
O1^iv—Ca1—O1^viii	120.14 (11)	O2—V2—O3^xiv	105.95 (10)
V1—Ca1—O1^viii	165.31 (6)	O4^xiv—V2—O3^xiv	89.50 (9)
V2^v—Ca1—O1^viii	105.62 (4)	O2—V2—O4	112.35 (10)
V2^vi—Ca1—O1^viii	105.62 (4)	O4^xiv—V2—O4	138.82 (5)
V1^vii—Ca1—O1^viii	62.87 (6)	O3^xiv—V2—O4	81.41 (9)
O2^i—Ca1—V2^i	15.84 (6)	O2—V2—O3^x	114.71 (10)
O2^ii—Ca1—V2^i	94.84 (6)	O4^xiv—V2—O3^x	81.29 (9)
O4—Ca1—V2^i	153.39 (5)	O3^xiv—V2—O3^x	139.16 (4)
O4^iii—Ca1—V2^i	100.19 (5)	O4—V2—O3^x	79.99 (8)
O3—Ca1—V2^i	136.46 (6)	O2—V2—V2^xiv	120.67 (7)
O3^iii—Ca1—V2^i	91.00 (5)	O4^xiv—V2—V2^xiv	40.62 (6)
O1^iv—Ca1—V2^i	69.92 (5)	O3^xiv—V2—V2^xiv	118.39 (7)
V1—Ca1—V2^i	124.90 (2)	O4—V2—V2^xiv	111.50 (6)
V2^v—Ca1—V2^i	170.29 (2)	O3^x—V2—V2^xiv	40.71 (6)
V2^vi—Ca1—V2^i	94.60 (2)	O2—V2—V2^v	114.12 (7)
V1^vii—Ca1—V2^i	112.27 (2)	O4^xiv—V2—V2^v	120.62 (7)
O1^viii—Ca1—V2^i	64.97 (4)	O3^xiv—V2—V2^v	40.91 (6)
O2^i—Ca1—V2^ii	94.84 (6)	O4—V2—V2^v	40.54 (6)
O2^ii—Ca1—V2^ii	15.84 (6)	O3^x—V2—V2^v	113.41 (7)
O4—Ca1—V2^ii	100.19 (5)	V2^xiv—V2—V2^v	125.20 (4)
O4^iii—Ca1—V2^ii	153.39 (5)	O2—V2—V1	127.53 (9)
O3—Ca1—V2^ii	91.00 (5)	O4^xiv—V2—V1	108.99 (6)
O3^iii—Ca1—V2^ii	136.46 (6)	O3^xiv—V2—V1	109.43 (6)
O1^iv—Ca1—V2^ii	69.92 (5)	O4—V2—V1	40.50 (6)
V1—Ca1—V2^ii	124.90 (2)	O3^x—V2—V1	40.27 (6)
V2^v—Ca1—V2^ii	94.60 (2)	V2^xiv—V2—V1	72.55 (2)
V2^vi—Ca1—V2^ii	170.29 (2)	V2^v—V2—V1	74.19 (3)
V1^vii—Ca1—V2^ii	112.27 (2)	O2—V2—Ca1^xiv	118.04 (9)
O1^viii—Ca1—V2^ii	64.97 (4)	O4^xiv—V2—Ca1^xiv	44.27 (6)
V2^i—Ca1—V2^ii	79.41 (3)	O3^xiv—V2—Ca1^xiv	45.41 (6)
O2^i—Ca1—V1^iv	68.38 (5)	O4—V2—Ca1^xiv	113.26 (6)
O2^ii—Ca1—V1^iv	68.38 (5)	O3^x—V2—Ca1^xiv	112.57 (6)
O4—Ca1—V1^iv	101.08 (5)	V2^xiv—V2—Ca1^xiv	76.57 (3)
O4^iii—Ca1—V1^iv	101.08 (5)	V2^v—V2—Ca1^xiv	79.24 (3)
O3—Ca1—V1^iv	144.89 (5)	V1—V2—Ca1^xiv	114.41 (3)
O3^iii—Ca1—V1^iv	144.89 (5)	O2—V2—Ca1^ii	23.36 (9)
O1^iv—Ca1—V1^iv	19.68 (7)	O4^xiv—V2—Ca1^ii	95.22 (6)
V1—Ca1—V1^iv	94.23 (3)	O3^xiv—V2—Ca1^ii	87.24 (6)
V2^v—Ca1—V1^iv	126.331 (19)	O4—V2—Ca1^ii	124.07 (6)
V2^vi—Ca1—V1^iv	126.331 (19)	O3^x—V2—Ca1^ii	132.99 (6)
V1^vii—Ca1—V1^iv	163.33 (3)	V2^xiv—V2—Ca1^ii	121.86 (3)
O1^viii—Ca1—V1^iv	100.46 (6)	V2^v—V2—Ca1^ii	108.53 (3)
V2^i—Ca1—V1^iv	56.28 (2)	V1—V2—Ca1^ii	150.22 (2)
V2^ii—Ca1—V1^iv	56.28 (2)	Ca1^xiv—V2—Ca1^ii	94.95 (2)
O2^i—Ca1—V2	146.00 (6)	O2—V2—Ca1	84.85 (8)
O2^ii—Ca1—V2	70.39 (5)	O4^xiv—V2—Ca1	164.74 (6)
O4—Ca1—V2	22.61 (5)	O3^xiv—V2—Ca1	93.34 (6)
O4^iii—Ca1—V2	82.82 (5)	O4—V2—Ca1	27.92 (6)
O3—Ca1—V2	80.58 (5)	O3^x—V2—Ca1	86.80 (6)
O3^iii—Ca1—V2	128.59 (6)	V2^xiv—V2—Ca1	126.52 (3)
O1^iv—Ca1—V2	68.10 (5)	V2^v—V2—Ca1	56.11 (2)
V1—Ca1—V2	47.622 (15)	V1—V2—Ca1	55.99 (2)
V2^v—Ca1—V2	47.323 (14)	Ca1^xiv—V2—Ca1	135.33 (2)
V2^vi—Ca1—V2	109.25 (3)	Ca1^ii—V2—Ca1	99.89 (2)
V1^vii—Ca1—V2	109.95 (3)	O2—V2—Ca1^x	89.27 (8)
O1^viii—Ca1—V2	134.659 (15)	O4^xiv—V2—Ca1^x	90.34 (6)
V2^i—Ca1—V2	137.44 (3)	O3^xiv—V2—Ca1^x	163.97 (6)
V2^ii—Ca1—V2	80.11 (2)	O4—V2—Ca1^x	88.21 (6)
V1^iv—Ca1—V2	81.35 (2)	O3^x—V2—Ca1^x	25.47 (6)
O2^i—Ca1—V2^iii	70.39 (5)	V2^xiv—V2—Ca1^x	54.57 (2)
O2^ii—Ca1—V2^iii	146.00 (6)	V2^v—V2—Ca1^x	128.04 (3)
O4—Ca1—V2^iii	82.82 (5)	V1—V2—Ca1^x	55.69 (2)
O4^iii—Ca1—V2^iii	22.61 (5)	Ca1^xiv—V2—Ca1^x	131.12 (2)
O3—Ca1—V2^iii	128.59 (6)	Ca1^ii—V2—Ca1^x	108.73 (2)
O3^iii—Ca1—V2^iii	80.58 (5)	Ca1—V2—Ca1^x	82.81 (2)
O1^iv—Ca1—V2^iii	68.10 (5)	V1—O1—Ca1^xii	128.43 (15)
V1—Ca1—V2^iii	47.622 (15)	V1—O1—Ca1^xiii	111.43 (12)
V2^v—Ca1—V2^iii	109.25 (3)	Ca1^xii—O1—Ca1^xiii	120.14 (11)
V2^vi—Ca1—V2^iii	47.323 (14)	V1—O1—Ca1^x	37.87 (8)
V1^vii—Ca1—V2^iii	109.95 (3)	Ca1^xii—O1—Ca1^x	90.56 (8)
O1^viii—Ca1—V2^iii	134.659 (15)	Ca1^xiii—O1—Ca1^x	149.30 (9)
V2^i—Ca1—V2^iii	80.11 (2)	V1—O1—Ca1	32.65 (8)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.09 (10)
V1^iv—Ca1—V2^iii	81.35 (2)	Ca1^xiii—O1—Ca1	78.77 (6)
V2—Ca1—V2^iii	90.62 (3)	Ca1^x—O1—Ca1	70.53 (5)
O2^i—Ca1—V2^ix	58.62 (5)	V2—O2—Ca1^ii	140.80 (13)
O2^ii—Ca1—V2^ix	127.66 (6)	V2—O2—Ca1	72.24 (8)
O4—Ca1—V2^ix	126.52 (6)	Ca1^ii—O2—Ca1	128.59 (7)
O4^iii—Ca1—V2^ix	79.60 (5)	V2—O2—Ca1^x	68.96 (8)
O3—Ca1—V2^ix	80.10 (5)	Ca1^ii—O2—Ca1^x	140.66 (7)
O3^iii—Ca1—V2^ix	20.44 (5)	Ca1—O2—Ca1^x	77.28 (5)
O1^iv—Ca1—V2^ix	134.54 (2)	V2—O2—Ca1^xiv	42.92 (7)
V1—Ca1—V2^ix	110.84 (3)	Ca1^ii—O2—Ca1^xiv	98.22 (7)
V2^v—Ca1—V2^ix	106.67 (3)	Ca1—O2—Ca1^xiv	105.67 (5)
V2^vi—Ca1—V2^ix	46.190 (14)	Ca1^x—O2—Ca1^xiv	101.91 (4)
V1^vii—Ca1—V2^ix	46.269 (15)	V1^vii—O3—V2^v	128.45 (11)
O1^viii—Ca1—V2^ix	59.76 (3)	V1^vii—O3—V2^vii	99.20 (9)
V2^i—Ca1—V2^ix	71.27 (2)	V2^v—O3—V2^vii	98.38 (9)
V2^ii—Ca1—V2^ix	124.16 (2)	V1^vii—O3—Ca1	102.00 (9)
V1^iv—Ca1—V2^ix	126.98 (2)	V2^v—O3—Ca1	99.42 (8)
V2—Ca1—V2^ix	149.01 (3)	V2^vii—O3—Ca1	134.09 (10)
V2^iii—Ca1—V2^ix	82.81 (2)	V1^vii—O3—Ca1^xiii	65.36 (6)
O2^i—Ca1—V2^vii	127.66 (6)	V2^v—O3—Ca1^xiii	64.41 (6)
O2^ii—Ca1—V2^vii	58.62 (5)	V2^vii—O3—Ca1^xiii	123.10 (8)
O4—Ca1—V2^vii	79.60 (5)	Ca1—O3—Ca1^xiii	102.76 (6)
O4^iii—Ca1—V2^vii	126.52 (6)	V1^vii—O3—Ca1^vii	48.92 (5)
O3—Ca1—V2^vii	20.44 (5)	V2^v—O3—Ca1^vii	160.69 (9)
O3^iii—Ca1—V2^vii	80.10 (5)	V2^vii—O3—Ca1^vii	66.00 (5)
O1^iv—Ca1—V2^vii	134.54 (2)	Ca1—O3—Ca1^vii	99.71 (7)
V1—Ca1—V2^vii	110.84 (3)	Ca1^xiii—O3—Ca1^vii	113.46 (5)
V2^v—Ca1—V2^vii	46.190 (14)	V1^vii—O3—Ca1^v	104.67 (7)
V2^vi—Ca1—V2^vii	106.67 (3)	V2^v—O3—Ca1^v	60.85 (6)
V1^vii—Ca1—V2^vii	46.269 (15)	V2^vii—O3—Ca1^v	43.59 (5)
O1^viii—Ca1—V2^vii	59.76 (3)	Ca1—O3—Ca1^v	153.13 (7)
V2^i—Ca1—V2^vii	124.16 (2)	Ca1^xiii—O3—Ca1^v	85.59 (4)
V2^ii—Ca1—V2^vii	71.27 (2)	Ca1^vii—O3—Ca1^v	100.17 (4)
V1^iv—Ca1—V2^vii	126.98 (2)	V2^v—O4—V2	98.84 (9)
V2—Ca1—V2^vii	82.81 (2)	V2^v—O4—V1	132.92 (11)
V2^iii—Ca1—V2^vii	149.01 (3)	V2—O4—V1	99.19 (9)
V2^ix—Ca1—V2^vii	87.40 (3)	V2^v—O4—Ca1	100.82 (8)
O2^i—Ca1—O2	132.46 (4)	V2—O4—Ca1	129.47 (10)
O2^ii—Ca1—O2	51.41 (7)	V1—O4—Ca1	100.38 (9)
O4—Ca1—O2	45.35 (6)	V2^v—O4—Ca1^xiii	58.25 (5)
O4^iii—Ca1—O2	100.81 (6)	V2—O4—Ca1^xiii	132.49 (8)
O3—Ca1—O2	89.12 (6)	V1—O4—Ca1^xiii	77.74 (6)
O3^iii—Ca1—O2	149.63 (6)	Ca1—O4—Ca1^xiii	97.14 (6)
O1^iv—Ca1—O2	56.32 (4)	V2^v—O4—Ca1^x	161.79 (8)
V1—Ca1—O2	66.98 (3)	V2—O4—Ca1^x	65.63 (5)
V2^v—Ca1—O2	62.25 (3)	V1—O4—Ca1^x	47.00 (5)
V2^vi—Ca1—O2	131.17 (4)	Ca1—O4—Ca1^x	96.65 (6)
V1^vii—Ca1—O2	122.72 (4)	Ca1^xiii—O4—Ca1^x	124.58 (5)
O1^viii—Ca1—O2	119.79 (4)	V2^v—O4—Ca1^xiv	63.94 (6)
V2^i—Ca1—O2	119.34 (4)	V2—O4—Ca1^xiv	43.20 (5)
V2^ii—Ca1—O2	58.46 (3)	V1—O4—Ca1^xiv	104.15 (7)
V1^iv—Ca1—O2	64.08 (3)	Ca1—O4—Ca1^xiv	155.29 (7)
V2—Ca1—O2	22.92 (3)	Ca1^xiii—O4—Ca1^xiv	90.89 (4)
V2^iii—Ca1—O2	101.91 (4)	Ca1^x—O4—Ca1^xiv	97.90 (4)
V2^ix—Ca1—O2	168.82 (4)	V2^v—O4—Ca1^ii	90.12 (7)
V2^vii—Ca1—O2	83.42 (4)	V2—O4—Ca1^ii	37.33 (4)
O1—V1—O3^x	109.23 (9)	V1—O4—Ca1^ii	128.23 (7)
O1—V1—O3^xi	109.23 (9)	Ca1—O4—Ca1^ii	96.62 (6)
O3^x—V1—O3^xi	86.55 (12)	Ca1^xiii—O4—Ca1^ii	147.36 (5)
O1—V1—O4^iii	111.23 (9)	Ca1^x—O4—Ca1^ii	82.79 (3)
O3^x—V1—O4^iii	139.54 (10)	Ca1^xiv—O4—Ca1^ii	65.67 (3)
O3^xi—V1—O4^iii	80.05 (8)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_137K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.546 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2731 reflections
a = 10.413 (3) Å	θ = 1.3–23.4°
b = 10.370 (2) Å	µ = 5.69 mm^−1
c = 5.2886 (15) Å	T = 137 K
V = 571.1 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	400 independent reflections
Radiation source: fine-focus sealed tube	363 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.470	l = −5→5
2463 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.018	w = 1/[σ^2(Fo^2) + (0.0479P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.056	(Δ/σ)max < 0.001
S = 0.95	Δρmax = 0.23 e Å^−3
400 reflections	Δρmin = −0.29 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.019 (2)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08499 (10)	0.2500	0.29978 (15)	0.0052 (3)
V1	0.28896 (7)	0.2500	0.79221 (13)	0.0043 (3)
V2	0.18737 (6)	0.52013 (6)	0.78357 (10)	0.0043 (3)
O1	0.4443 (3)	0.2500	0.8088 (5)	0.0080 (8)*
O2	0.0393 (2)	0.5652 (2)	0.7661 (4)	0.0089 (6)*
O3	0.22027 (19)	0.3796 (2)	0.0261 (4)	0.0052 (5)*
O4	0.22704 (19)	0.3795 (2)	0.5478 (4)	0.0053 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0036 (5)	0.0054 (6)	0.0067 (6)	0.000	−0.0003 (3)	0.000
V1	0.0037 (5)	0.0045 (6)	0.0048 (5)	0.000	−0.0003 (3)	0.000
V2	0.0037 (4)	0.0043 (4)	0.0049 (4)	0.0008 (2)	0.0000 (2)	−0.0001 (2)

Geometric parameters (Å, º)

Ca1—O2^i	2.338 (3)	V1—Ca1^xiii	4.3936 (15)
Ca1—O2^ii	2.338 (3)	V1—Ca1^xiv	5.3486 (12)
Ca1—O4	2.390 (2)	V2—O2	1.614 (2)
Ca1—O4^iii	2.390 (2)	V2—O4^xiv	1.957 (2)
Ca1—O3^iii	2.426 (2)	V2—O3^xiv	1.965 (2)
Ca1—O3	2.426 (2)	V2—O4	1.963 (2)
Ca1—O1^iv	2.536 (3)	V2—O3^x	1.971 (2)
Ca1—V1	3.3606 (13)	V2—V2^v	2.9779 (9)
Ca1—V2^v	3.3628 (11)	V2—V2^xiv	2.9779 (9)
Ca1—V2^vi	3.3628 (11)	V2—Ca1^xiv	3.3628 (11)
Ca1—V1^vii	3.4230 (13)	V2—Ca1^ii	3.7308 (11)
Ca1—O1^viii	3.537 (3)	V2—Ca1^x	4.0542 (10)
Ca1—V2^i	3.7308 (11)	O1—Ca1^xii	2.536 (3)
Ca1—V2^ii	3.7308 (11)	O1—Ca1^xiii	3.537 (3)
Ca1—V1^iv	3.7627 (14)	O1—Ca1^x	4.554 (3)
Ca1—V2	3.9407 (10)	O2—Ca1^ii	2.338 (3)
Ca1—V2^iii	3.9407 (10)	O2—Ca1^x	4.344 (2)
Ca1—V2^ix	4.0542 (10)	O2—Ca1^xiv	4.361 (3)
Ca1—V2^vii	4.0542 (10)	O3—V1^vii	1.962 (2)
Ca1—O2	4.122 (2)	O3—V2^v	1.965 (2)
V1—O1	1.620 (3)	O3—V2^vii	1.971 (2)
V1—O3^x	1.962 (2)	O3—Ca1^xiii	4.133 (2)
V1—O3^xi	1.962 (2)	O3—Ca1^vii	4.307 (2)
V1—O4^iii	1.972 (2)	O3—Ca1^v	4.505 (2)
V1—O4	1.972 (2)	O4—V2^v	1.957 (2)
V1—V2^iii	2.9946 (9)	O4—Ca1^xiii	4.367 (2)
V1—V2	2.9946 (9)	O4—Ca1^x	4.451 (2)
V1—Ca1^x	3.4230 (13)	O4—Ca1^xiv	4.513 (2)
V1—Ca1^xii	3.7627 (14)	O4—Ca1^ii	5.096 (2)
O2^i—Ca1—O2^ii	110.09 (12)	O1—V1—O4	111.23 (9)
O2^i—Ca1—O4	152.21 (8)	O3^x—V1—O4	80.07 (9)
O2^ii—Ca1—O4	87.93 (7)	O3^xi—V1—O4	139.51 (10)
O2^i—Ca1—O4^iii	87.93 (7)	O4^iii—V1—O4	85.80 (12)
O2^ii—Ca1—O4^iii	152.21 (8)	O1—V1—V2^iii	110.706 (18)
O4—Ca1—O4^iii	68.36 (10)	O3^x—V1—V2^iii	121.45 (7)
O2^i—Ca1—O3^iii	77.18 (7)	O3^xi—V1—V2^iii	40.52 (6)
O2^ii—Ca1—O3^iii	133.35 (8)	O4^iii—V1—V2^iii	40.33 (6)
O4—Ca1—O3^iii	106.22 (8)	O4—V1—V2^iii	120.75 (7)
O4^iii—Ca1—O3^iii	69.93 (7)	O1—V1—V2	110.706 (18)
O2^i—Ca1—O3	133.35 (8)	O3^x—V1—V2	40.52 (6)
O2^ii—Ca1—O3	77.18 (7)	O3^xi—V1—V2	121.45 (7)
O4—Ca1—O3	69.93 (7)	O4^iii—V1—V2	120.75 (7)
O4^iii—Ca1—O3	106.22 (8)	O4—V1—V2	40.33 (6)
O3^iii—Ca1—O3	67.30 (10)	V2^iii—V1—V2	138.58 (4)
O2^i—Ca1—O1^iv	78.58 (7)	O1—V1—Ca1	132.31 (10)
O2^ii—Ca1—O1^iv	78.58 (7)	O3^x—V1—Ca1	104.96 (6)
O4—Ca1—O1^iv	84.82 (8)	O3^xi—V1—Ca1	104.96 (6)
O4^iii—Ca1—O1^iv	84.82 (8)	O4^iii—V1—Ca1	44.39 (6)
O3^iii—Ca1—O1^iv	145.32 (5)	O4—V1—Ca1	44.39 (6)
O3—Ca1—O1^iv	145.32 (5)	V2^iii—V1—Ca1	76.402 (18)
O2^i—Ca1—V1	117.72 (6)	V2—V1—Ca1	76.402 (18)
O2^ii—Ca1—V1	117.72 (6)	O1—V1—Ca1^x	125.24 (10)
O4—Ca1—V1	35.26 (5)	O3^x—V1—Ca1^x	43.89 (6)
O4^iii—Ca1—V1	35.26 (5)	O3^xi—V1—Ca1^x	43.89 (6)
O3^iii—Ca1—V1	95.47 (6)	O4^iii—V1—Ca1^x	108.13 (7)
O3—Ca1—V1	95.47 (6)	O4—V1—Ca1^x	108.13 (7)
O1^iv—Ca1—V1	74.50 (7)	V2^iii—V1—Ca1^x	78.040 (18)
O2^i—Ca1—V2^v	165.27 (6)	V2—V1—Ca1^x	78.040 (18)
O2^ii—Ca1—V2^v	78.77 (6)	Ca1—V1—Ca1^x	102.45 (4)
O4—Ca1—V2^v	34.86 (5)	O1—V1—Ca1^xii	31.88 (10)
O4^iii—Ca1—V2^v	88.62 (6)	O3^x—V1—Ca1^xii	86.40 (6)
O3^iii—Ca1—V2^v	88.18 (6)	O3^xi—V1—Ca1^xii	86.40 (6)
O3—Ca1—V2^v	35.19 (5)	O4^iii—V1—Ca1^xii	130.07 (6)
O1^iv—Ca1—V2^v	115.35 (5)	O4—V1—Ca1^xii	130.07 (6)
V1—Ca1—V2^v	64.80 (2)	V2^iii—V1—Ca1^xii	107.347 (17)
O2^i—Ca1—V2^vi	78.77 (6)	V2—V1—Ca1^xii	107.347 (17)
O2^ii—Ca1—V2^vi	165.27 (6)	Ca1—V1—Ca1^xii	164.19 (3)
O4—Ca1—V2^vi	88.62 (6)	Ca1^x—V1—Ca1^xii	93.36 (3)
O4^iii—Ca1—V2^vi	34.86 (5)	O1—V1—Ca1^xiii	48.56 (10)
O3^iii—Ca1—V2^vi	35.19 (5)	O3^x—V1—Ca1^xiii	134.84 (6)
O3—Ca1—V2^vi	88.18 (6)	O3^xi—V1—Ca1^xiii	134.84 (6)
O1^iv—Ca1—V2^vi	115.35 (5)	O4^iii—V1—Ca1^xiii	76.25 (6)
V1—Ca1—V2^vi	64.80 (2)	O4—V1—Ca1^xiii	76.25 (6)
V2^v—Ca1—V2^vi	90.28 (4)	V2^iii—V1—Ca1^xiii	103.708 (17)
O2^i—Ca1—V1^vii	103.09 (5)	V2—V1—Ca1^xiii	103.708 (17)
O2^ii—Ca1—V1^vii	103.09 (5)	Ca1—V1—Ca1^xiii	83.75 (3)
O4—Ca1—V1^vii	92.65 (6)	Ca1^x—V1—Ca1^xiii	173.80 (3)
O4^iii—Ca1—V1^vii	92.65 (6)	Ca1^xii—V1—Ca1^xiii	80.44 (3)
O3^iii—Ca1—V1^vii	34.10 (5)	O1—V1—Ca1^xiv	75.792 (14)
O3—Ca1—V1^vii	34.10 (5)	O3^x—V1—Ca1^xiv	54.58 (6)
O1^iv—Ca1—V1^vii	176.94 (8)	O3^xi—V1—Ca1^xiv	138.51 (6)
V1—Ca1—V1^vii	102.45 (4)	O4^iii—V1—Ca1^xiv	138.16 (6)
V2^v—Ca1—V1^vii	62.78 (2)	O4—V1—Ca1^xiv	54.92 (6)
V2^vi—Ca1—V1^vii	62.78 (2)	V2^iii—V1—Ca1^xiv	173.50 (3)
O2^i—Ca1—O1^viii	68.60 (6)	V2—V1—Ca1^xiv	34.92 (2)
O2^ii—Ca1—O1^viii	68.60 (6)	Ca1—V1—Ca1^xiv	99.259 (15)
O4—Ca1—O1^viii	139.11 (6)	Ca1^x—V1—Ca1^xiv	98.418 (15)
O4^iii—Ca1—O1^viii	139.11 (6)	Ca1^xii—V1—Ca1^xiv	78.151 (13)
O3^iii—Ca1—O1^viii	72.40 (7)	Ca1^xiii—V1—Ca1^xiv	80.396 (13)
O3—Ca1—O1^viii	72.40 (7)	O2—V2—O4^xiv	108.78 (10)
O1^iv—Ca1—O1^viii	120.23 (11)	O2—V2—O3^xiv	105.97 (10)
V1—Ca1—O1^viii	165.28 (6)	O4^xiv—V2—O3^xiv	89.45 (9)
V2^v—Ca1—O1^viii	105.60 (4)	O2—V2—O4	112.32 (10)
V2^vi—Ca1—O1^viii	105.60 (4)	O4^xiv—V2—O4	138.85 (5)
V1^vii—Ca1—O1^viii	62.83 (6)	O3^xiv—V2—O4	81.36 (9)
O2^i—Ca1—V2^i	15.89 (6)	O2—V2—O3^x	114.66 (10)
O2^ii—Ca1—V2^i	94.90 (7)	O4^xiv—V2—O3^x	81.34 (9)
O4—Ca1—V2^i	153.42 (6)	O3^xiv—V2—O3^x	139.20 (5)
O4^iii—Ca1—V2^i	100.16 (5)	O4—V2—O3^x	80.07 (8)
O3^iii—Ca1—V2^i	90.96 (5)	O2—V2—V2^v	114.10 (7)
O3—Ca1—V2^i	136.46 (6)	O4^xiv—V2—V2^v	120.60 (7)
O1^iv—Ca1—V2^i	69.95 (5)	O3^xiv—V2—V2^v	40.91 (6)
V1—Ca1—V2^i	124.89 (2)	O4—V2—V2^v	40.50 (6)
V2^v—Ca1—V2^i	170.30 (3)	O3^x—V2—V2^v	113.46 (7)
V2^vi—Ca1—V2^i	94.58 (2)	O2—V2—V2^xiv	120.66 (7)
V1^vii—Ca1—V2^i	112.27 (2)	O4^xiv—V2—V2^xiv	40.64 (6)
O1^viii—Ca1—V2^i	65.01 (4)	O3^xiv—V2—V2^xiv	118.37 (7)
O2^i—Ca1—V2^ii	94.90 (7)	O4—V2—V2^xiv	111.57 (7)
O2^ii—Ca1—V2^ii	15.89 (6)	O3^x—V2—V2^xiv	40.75 (6)
O4—Ca1—V2^ii	100.16 (5)	V2^v—V2—V2^xiv	125.24 (4)
O4^iii—Ca1—V2^ii	153.42 (6)	O2—V2—V1	127.52 (9)
O3^iii—Ca1—V2^ii	136.46 (6)	O4^xiv—V2—V1	109.02 (6)
O3—Ca1—V2^ii	90.96 (5)	O3^xiv—V2—V1	109.42 (6)
O1^iv—Ca1—V2^ii	69.95 (5)	O4—V2—V1	40.56 (6)
V1—Ca1—V2^ii	124.89 (2)	O3^x—V2—V1	40.30 (6)
V2^v—Ca1—V2^ii	94.58 (2)	V2^v—V2—V1	74.20 (3)
V2^vi—Ca1—V2^ii	170.30 (3)	V2^xiv—V2—V1	72.58 (3)
V1^vii—Ca1—V2^ii	112.27 (2)	O2—V2—Ca1^xiv	118.03 (9)
O1^viii—Ca1—V2^ii	65.01 (4)	O4^xiv—V2—Ca1^xiv	44.25 (6)
V2^i—Ca1—V2^ii	79.42 (3)	O3^xiv—V2—Ca1^xiv	45.38 (6)
O2^i—Ca1—V1^iv	68.42 (6)	O4—V2—Ca1^xiv	113.24 (7)
O2^ii—Ca1—V1^iv	68.42 (6)	O3^x—V2—Ca1^xiv	112.63 (7)
O4—Ca1—V1^iv	101.09 (6)	V2^v—V2—Ca1^xiv	79.24 (3)
O4^iii—Ca1—V1^iv	101.09 (6)	V2^xiv—V2—Ca1^xiv	76.58 (3)
O3^iii—Ca1—V1^iv	144.86 (5)	V1—V2—Ca1^xiv	114.43 (3)
O3—Ca1—V1^iv	144.86 (5)	O2—V2—Ca1^ii	23.37 (9)
O1^iv—Ca1—V1^iv	19.71 (7)	O4^xiv—V2—Ca1^ii	95.20 (6)
V1—Ca1—V1^iv	94.21 (3)	O3^xiv—V2—Ca1^ii	87.26 (6)
V2^v—Ca1—V1^iv	126.31 (2)	O4—V2—Ca1^ii	124.03 (6)
V2^vi—Ca1—V1^iv	126.31 (2)	O3^x—V2—Ca1^ii	132.94 (6)
V1^vii—Ca1—V1^iv	163.35 (3)	V2^v—V2—Ca1^ii	108.52 (3)
O1^viii—Ca1—V1^iv	100.52 (6)	V2^xiv—V2—Ca1^ii	121.83 (3)
V2^i—Ca1—V1^iv	56.29 (2)	V1—V2—Ca1^ii	150.22 (3)
V2^ii—Ca1—V1^iv	56.29 (2)	Ca1^xiv—V2—Ca1^ii	94.93 (2)
O2^i—Ca1—V2	146.00 (6)	O2—V2—Ca1	84.84 (8)
O2^ii—Ca1—V2	70.36 (6)	O4^xiv—V2—Ca1	164.76 (6)
O4—Ca1—V2	22.61 (5)	O3^xiv—V2—Ca1	93.35 (6)
O4^iii—Ca1—V2	82.85 (5)	O4—V2—Ca1	27.91 (6)
O3^iii—Ca1—V2	128.62 (6)	O3^x—V2—Ca1	86.80 (7)
O3—Ca1—V2	80.58 (5)	V2^v—V2—Ca1	56.10 (2)
O1^iv—Ca1—V2	68.06 (5)	V2^xiv—V2—Ca1	126.54 (3)
V1—Ca1—V2	47.614 (16)	V1—V2—Ca1	55.98 (2)
V2^v—Ca1—V2	47.312 (15)	Ca1^xiv—V2—Ca1	135.33 (3)
V2^vi—Ca1—V2	109.25 (3)	Ca1^ii—V2—Ca1	99.89 (2)
V1^vii—Ca1—V2	109.96 (3)	O2—V2—Ca1^x	89.27 (8)
O1^viii—Ca1—V2	134.668 (15)	O4^xiv—V2—Ca1^x	90.38 (6)
V2^i—Ca1—V2	137.44 (3)	O3^xiv—V2—Ca1^x	163.95 (7)
V2^ii—Ca1—V2	80.11 (2)	O4—V2—Ca1^x	88.26 (6)
V1^iv—Ca1—V2	81.33 (2)	O3^x—V2—Ca1^x	25.42 (6)
O2^i—Ca1—V2^iii	70.36 (6)	V2^v—V2—Ca1^x	128.04 (3)
O2^ii—Ca1—V2^iii	146.00 (6)	V2^xiv—V2—Ca1^x	54.57 (2)
O4—Ca1—V2^iii	82.85 (5)	V1—V2—Ca1^x	55.69 (2)
O4^iii—Ca1—V2^iii	22.61 (5)	Ca1^xiv—V2—Ca1^x	131.14 (2)
O3^iii—Ca1—V2^iii	80.58 (5)	Ca1^ii—V2—Ca1^x	108.73 (2)
O3—Ca1—V2^iii	128.62 (6)	Ca1—V2—Ca1^x	82.82 (2)
O1^iv—Ca1—V2^iii	68.06 (5)	V1—O1—Ca1^xii	128.41 (15)
V1—Ca1—V2^iii	47.614 (16)	V1—O1—Ca1^xiii	111.36 (13)
V2^v—Ca1—V2^iii	109.25 (3)	Ca1^xii—O1—Ca1^xiii	120.23 (11)
V2^vi—Ca1—V2^iii	47.312 (15)	V1—O1—Ca1^x	37.87 (8)
V1^vii—Ca1—V2^iii	109.96 (3)	Ca1^xii—O1—Ca1^x	90.54 (8)
O1^viii—Ca1—V2^iii	134.668 (15)	Ca1^xiii—O1—Ca1^x	149.24 (9)
V2^i—Ca1—V2^iii	80.11 (2)	V1—O1—Ca1	32.63 (8)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.04 (10)
V1^iv—Ca1—V2^iii	81.33 (2)	Ca1^xiii—O1—Ca1	78.74 (6)
V2—Ca1—V2^iii	90.60 (3)	Ca1^x—O1—Ca1	70.50 (5)
O2^i—Ca1—V2^ix	58.59 (5)	V2—O2—Ca1^ii	140.74 (14)
O2^ii—Ca1—V2^ix	127.69 (6)	V2—O2—Ca1	72.21 (8)
O4—Ca1—V2^ix	126.51 (6)	Ca1^ii—O2—Ca1	128.65 (7)
O4^iii—Ca1—V2^ix	79.55 (5)	V2—O2—Ca1^x	68.93 (8)
O3^iii—Ca1—V2^ix	20.41 (5)	Ca1^ii—O2—Ca1^x	140.72 (7)
O3—Ca1—V2^ix	80.12 (6)	Ca1—O2—Ca1^x	77.26 (5)
O1^iv—Ca1—V2^ix	134.55 (3)	V2—O2—Ca1^xiv	42.90 (7)
V1—Ca1—V2^ix	110.83 (3)	Ca1^ii—O2—Ca1^xiv	98.18 (7)
V2^v—Ca1—V2^ix	106.69 (3)	Ca1—O2—Ca1^xiv	105.62 (5)
V2^vi—Ca1—V2^ix	46.188 (15)	Ca1^x—O2—Ca1^xiv	101.87 (5)
V1^vii—Ca1—V2^ix	46.271 (15)	V1^vii—O3—V2^v	128.39 (11)
O1^viii—Ca1—V2^ix	59.74 (4)	V1^vii—O3—V2^vii	99.18 (9)
V2^i—Ca1—V2^ix	71.27 (2)	V2^v—O3—V2^vii	98.34 (9)
V2^ii—Ca1—V2^ix	124.18 (3)	V1^vii—O3—Ca1	102.01 (9)
V1^iv—Ca1—V2^ix	126.98 (2)	V2^v—O3—Ca1	99.43 (8)
V2—Ca1—V2^ix	149.00 (3)	V2^vii—O3—Ca1	134.17 (10)
V2^iii—Ca1—V2^ix	82.82 (2)	V1^vii—O3—Ca1^xiii	65.32 (6)
O2^i—Ca1—V2^vii	127.69 (6)	V2^v—O3—Ca1^xiii	64.39 (6)
O2^ii—Ca1—V2^vii	58.59 (5)	V2^vii—O3—Ca1^xiii	123.04 (8)
O4—Ca1—V2^vii	79.55 (5)	Ca1—O3—Ca1^xiii	102.73 (6)
O4^iii—Ca1—V2^vii	126.51 (6)	V1^vii—O3—Ca1^vii	48.93 (5)
O3^iii—Ca1—V2^vii	80.12 (6)	V2^v—O3—Ca1^vii	160.65 (9)
O3—Ca1—V2^vii	20.41 (5)	V2^vii—O3—Ca1^vii	66.01 (6)
O1^iv—Ca1—V2^vii	134.55 (2)	Ca1—O3—Ca1^vii	99.74 (7)
V1—Ca1—V2^vii	110.83 (3)	Ca1^xiii—O3—Ca1^vii	113.44 (5)
V2^v—Ca1—V2^vii	46.188 (15)	V1^vii—O3—Ca1^v	104.63 (7)
V2^vi—Ca1—V2^vii	106.69 (3)	V2^v—O3—Ca1^v	60.84 (6)
V1^vii—Ca1—V2^vii	46.271 (15)	V2^vii—O3—Ca1^v	43.55 (5)
O1^viii—Ca1—V2^vii	59.74 (4)	Ca1—O3—Ca1^v	153.15 (7)
V2^i—Ca1—V2^vii	124.18 (3)	Ca1^xiii—O3—Ca1^v	85.58 (4)
V2^ii—Ca1—V2^vii	71.27 (2)	Ca1^vii—O3—Ca1^v	100.16 (4)
V1^iv—Ca1—V2^vii	126.98 (2)	V2^v—O4—V2	98.86 (10)
V2—Ca1—V2^vii	82.82 (2)	V2^v—O4—V1	132.94 (11)
V2^iii—Ca1—V2^vii	149.00 (3)	V2—O4—V1	99.11 (9)
V2^ix—Ca1—V2^vii	87.41 (3)	V2^v—O4—Ca1	100.89 (8)
O2^i—Ca1—O2	132.46 (4)	V2—O4—Ca1	129.48 (10)
O2^ii—Ca1—O2	51.35 (7)	V1—O4—Ca1	100.35 (9)
O4—Ca1—O2	45.39 (6)	V2^v—O4—Ca1^xiii	58.29 (5)
O4^iii—Ca1—O2	100.87 (6)	V2—O4—Ca1^xiii	132.48 (8)
O3^iii—Ca1—O2	149.69 (6)	V1—O4—Ca1^xiii	77.74 (6)
O3—Ca1—O2	89.12 (6)	Ca1—O4—Ca1^xiii	97.16 (6)
O1^iv—Ca1—O2	56.28 (4)	V2^v—O4—Ca1^x	161.76 (9)
V1—Ca1—O2	67.01 (3)	V2—O4—Ca1^x	65.58 (6)
V2^v—Ca1—O2	62.27 (3)	V1—O4—Ca1^x	46.97 (5)
V2^vi—Ca1—O2	131.20 (4)	Ca1—O4—Ca1^x	96.62 (6)
V1^vii—Ca1—O2	122.74 (4)	Ca1^xiii—O4—Ca1^x	124.54 (5)
O1^viii—Ca1—O2	119.78 (4)	V2^v—O4—Ca1^xiv	63.93 (6)
V2^i—Ca1—O2	119.31 (4)	V2—O4—Ca1^xiv	43.20 (5)
V2^ii—Ca1—O2	58.42 (3)	V1—O4—Ca1^xiv	104.13 (7)
V1^iv—Ca1—O2	64.04 (3)	Ca1—O4—Ca1^xiv	155.34 (7)
V2—Ca1—O2	22.95 (3)	Ca1^xiii—O4—Ca1^xiv	90.91 (4)
V2^iii—Ca1—O2	101.91 (4)	Ca1^x—O4—Ca1^xiv	97.88 (4)
V2^ix—Ca1—O2	168.85 (4)	V2^v—O4—Ca1^ii	90.12 (7)
V2^vii—Ca1—O2	83.42 (4)	V2—O4—Ca1^ii	37.35 (5)
O1—V1—O3^x	109.26 (9)	V1—O4—Ca1^ii	128.17 (8)
O1—V1—O3^xi	109.26 (9)	Ca1—O4—Ca1^ii	96.65 (6)
O3^x—V1—O3^xi	86.51 (12)	Ca1^xiii—O4—Ca1^ii	147.40 (5)
O1—V1—O4^iii	111.23 (9)	Ca1^x—O4—Ca1^ii	82.77 (3)
O3^x—V1—O4^iii	139.51 (10)	Ca1^xiv—O4—Ca1^ii	65.66 (3)
O3^xi—V1—O4^iii	80.07 (9)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_125K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.548 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2713 reflections
a = 10.409 (3) Å	θ = 1.3–23.4°
b = 10.370 (2) Å	µ = 5.69 mm^−1
c = 5.2875 (15) Å	T = 125 K
V = 570.8 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	399 independent reflections
Radiation source: fine-focus sealed tube	366 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 0 pixels mm^-1	θmax = 23.0°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.470	l = −5→5
2445 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0451P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.054	(Δ/σ)max < 0.001
S = 0.97	Δρmax = 0.26 e Å^−3
399 reflections	Δρmin = −0.34 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0184 (19)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08500 (9)	0.2500	0.30004 (15)	0.0049 (3)
V1	0.28900 (7)	0.2500	0.79214 (13)	0.0040 (3)
V2	0.18734 (5)	0.52013 (5)	0.78351 (9)	0.0039 (3)
O1	0.4443 (3)	0.2500	0.8091 (5)	0.0076 (8)*
O2	0.0393 (2)	0.5652 (2)	0.7661 (4)	0.0086 (6)*
O3	0.22056 (19)	0.3795 (2)	0.0259 (4)	0.0049 (5)*
O4	0.22691 (19)	0.3793 (2)	0.5479 (4)	0.0047 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0033 (5)	0.0049 (6)	0.0063 (5)	0.000	−0.0003 (3)	0.000
V1	0.0033 (5)	0.0042 (6)	0.0044 (5)	0.000	0.0000 (3)	0.000
V2	0.0034 (4)	0.0038 (4)	0.0046 (4)	0.0008 (2)	0.0002 (2)	0.00017 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.338 (3)	V1—Ca1^xiii	4.3930 (14)
Ca1—O2^ii	2.338 (3)	V1—Ca1^xiv	5.3487 (12)
Ca1—O4	2.387 (2)	V2—O2	1.613 (2)
Ca1—O4^iii	2.387 (2)	V2—O4^xiv	1.959 (2)
Ca1—O3	2.428 (2)	V2—O4	1.963 (2)
Ca1—O3^iii	2.428 (2)	V2—O3^xiv	1.964 (2)
Ca1—O1^iv	2.533 (3)	V2—O3^x	1.972 (2)
Ca1—V1	3.3585 (13)	V2—V2^xiv	2.9775 (9)
Ca1—V2^v	3.3625 (11)	V2—V2^v	2.9775 (9)
Ca1—V2^vi	3.3625 (11)	V2—Ca1^xiv	3.3625 (11)
Ca1—V1^vii	3.4237 (13)	V2—Ca1^ii	3.7302 (11)
Ca1—O1^viii	3.538 (3)	V2—Ca1^x	4.0548 (10)
Ca1—V2^i	3.7302 (11)	O1—Ca1^xii	2.533 (3)
Ca1—V2^ii	3.7302 (11)	O1—Ca1^xiii	3.538 (3)
Ca1—V1^iv	3.7609 (14)	O1—Ca1^x	4.553 (3)
Ca1—V2	3.9392 (10)	O2—Ca1^ii	2.338 (3)
Ca1—V2^iii	3.9392 (10)	O2—Ca1^x	4.346 (2)
Ca1—V2^ix	4.0548 (10)	O2—Ca1^xiv	4.359 (3)
Ca1—V2^vii	4.0548 (10)	O3—V1^vii	1.959 (2)
Ca1—O2	4.121 (2)	O3—V2^v	1.964 (2)
V1—O1	1.619 (3)	O3—V2^vii	1.972 (2)
V1—O3^x	1.959 (2)	O3—Ca1^xiii	4.128 (2)
V1—O3^xi	1.959 (2)	O3—Ca1^vii	4.304 (2)
V1—O4^iii	1.971 (2)	O3—Ca1^v	4.504 (2)
V1—O4	1.971 (2)	O4—V2^v	1.959 (2)
V1—V2^iii	2.9949 (9)	O4—Ca1^xiii	4.368 (2)
V1—V2	2.9949 (9)	O4—Ca1^x	4.449 (2)
V1—Ca1^x	3.4237 (13)	O4—Ca1^xiv	4.515 (2)
V1—Ca1^xii	3.7609 (14)	O4—Ca1^ii	5.095 (2)
O2^i—Ca1—O2^ii	110.06 (12)	O1—V1—O4	111.33 (9)
O2^i—Ca1—O4	152.24 (7)	O3^x—V1—O4	80.07 (8)
O2^ii—Ca1—O4	87.94 (7)	O3^xi—V1—O4	139.52 (10)
O2^i—Ca1—O4^iii	87.94 (7)	O4^iii—V1—O4	85.78 (12)
O2^ii—Ca1—O4^iii	152.24 (7)	O1—V1—V2^iii	110.711 (18)
O4—Ca1—O4^iii	68.37 (10)	O3^x—V1—V2^iii	121.49 (7)
O2^i—Ca1—O3	133.28 (7)	O3^xi—V1—V2^iii	40.53 (6)
O2^ii—Ca1—O3	77.23 (7)	O4^iii—V1—V2^iii	40.32 (6)
O4—Ca1—O3	69.96 (7)	O4—V1—V2^iii	120.71 (7)
O4^iii—Ca1—O3	106.20 (8)	O1—V1—V2	110.711 (18)
O2^i—Ca1—O3^iii	77.23 (7)	O3^x—V1—V2	40.53 (6)
O2^ii—Ca1—O3^iii	133.28 (7)	O3^xi—V1—V2	121.49 (7)
O4—Ca1—O3^iii	106.20 (8)	O4^iii—V1—V2	120.71 (7)
O4^iii—Ca1—O3^iii	69.96 (7)	O4—V1—V2	40.32 (6)
O3—Ca1—O3^iii	67.17 (10)	V2^iii—V1—V2	138.58 (4)
O2^i—Ca1—O1^iv	78.59 (6)	O1—V1—Ca1	132.39 (10)
O2^ii—Ca1—O1^iv	78.59 (6)	O3^x—V1—Ca1	105.00 (6)
O4—Ca1—O1^iv	84.82 (8)	O3^xi—V1—Ca1	105.00 (6)
O4^iii—Ca1—O1^iv	84.82 (8)	O4^iii—V1—Ca1	44.36 (6)
O3—Ca1—O1^iv	145.39 (5)	O4—V1—Ca1	44.36 (6)
O3^iii—Ca1—O1^iv	145.39 (5)	V2^iii—V1—Ca1	76.396 (17)
O2^i—Ca1—V1	117.75 (5)	V2—V1—Ca1	76.396 (17)
O2^ii—Ca1—V1	117.75 (5)	O1—V1—Ca1^x	125.16 (10)
O4—Ca1—V1	35.26 (5)	O3^x—V1—Ca1^x	43.92 (6)
O4^iii—Ca1—V1	35.26 (5)	O3^xi—V1—Ca1^x	43.92 (6)
O3—Ca1—V1	95.45 (6)	O4^iii—V1—Ca1^x	108.09 (6)
O3^iii—Ca1—V1	95.45 (6)	O4—V1—Ca1^x	108.09 (6)
O1^iv—Ca1—V1	74.54 (7)	V2^iii—V1—Ca1^x	78.041 (18)
O2^i—Ca1—V2^v	165.24 (6)	V2—V1—Ca1^x	78.041 (18)
O2^ii—Ca1—V2^v	78.76 (6)	Ca1—V1—Ca1^x	102.45 (4)
O4—Ca1—V2^v	34.90 (5)	O1—V1—Ca1^xii	31.81 (10)
O4^iii—Ca1—V2^v	88.65 (6)	O3^x—V1—Ca1^xii	86.34 (6)
O3—Ca1—V2^v	35.19 (5)	O3^xi—V1—Ca1^xii	86.34 (6)
O3^iii—Ca1—V2^v	88.11 (6)	O4^iii—V1—Ca1^xii	130.12 (6)
O1^iv—Ca1—V2^v	115.38 (5)	O4—V1—Ca1^xii	130.12 (6)
V1—Ca1—V2^v	64.82 (2)	V2^iii—V1—Ca1^xii	107.351 (17)
O2^i—Ca1—V2^vi	78.76 (6)	V2—V1—Ca1^xii	107.351 (17)
O2^ii—Ca1—V2^vi	165.24 (6)	Ca1—V1—Ca1^xii	164.20 (3)
O4—Ca1—V2^vi	88.65 (6)	Ca1^x—V1—Ca1^xii	93.35 (3)
O4^iii—Ca1—V2^vi	34.90 (5)	O1—V1—Ca1^xiii	48.63 (10)
O3—Ca1—V2^vi	88.11 (6)	O3^x—V1—Ca1^xiii	134.80 (6)
O3^iii—Ca1—V2^vi	35.19 (5)	O3^xi—V1—Ca1^xiii	134.80 (6)
O1^iv—Ca1—V2^vi	115.38 (5)	O4^iii—V1—Ca1^xiii	76.29 (6)
V1—Ca1—V2^vi	64.82 (2)	O4—V1—Ca1^xiii	76.29 (6)
V2^v—Ca1—V2^vi	90.30 (4)	V2^iii—V1—Ca1^xiii	103.708 (17)
O2^i—Ca1—V1^vii	103.05 (5)	V2—V1—Ca1^xiii	103.708 (17)
O2^ii—Ca1—V1^vii	103.05 (5)	Ca1—V1—Ca1^xiii	83.76 (3)
O4—Ca1—V1^vii	92.69 (6)	Ca1^x—V1—Ca1^xiii	173.79 (3)
O4^iii—Ca1—V1^vii	92.69 (6)	Ca1^xii—V1—Ca1^xiii	80.45 (3)
O3—Ca1—V1^vii	34.04 (5)	O1—V1—Ca1^xiv	75.802 (14)
O3^iii—Ca1—V1^vii	34.04 (5)	O3^x—V1—Ca1^xiv	54.53 (6)
O1^iv—Ca1—V1^vii	176.99 (8)	O3^xi—V1—Ca1^xiv	138.48 (6)
V1—Ca1—V1^vii	102.45 (4)	O4^iii—V1—Ca1^xiv	138.19 (6)
V2^v—Ca1—V1^vii	62.77 (2)	O4—V1—Ca1^xiv	54.95 (6)
V2^vi—Ca1—V1^vii	62.77 (2)	V2^iii—V1—Ca1^xiv	173.49 (3)
O2^i—Ca1—O1^viii	68.59 (6)	V2—V1—Ca1^xiv	34.91 (2)
O2^ii—Ca1—O1^viii	68.59 (5)	Ca1—V1—Ca1^xiv	99.271 (14)
O4—Ca1—O1^viii	139.10 (6)	Ca1^x—V1—Ca1^xiv	98.393 (15)
O4^iii—Ca1—O1^viii	139.10 (6)	Ca1^xii—V1—Ca1^xiv	78.148 (13)
O3—Ca1—O1^viii	72.37 (7)	Ca1^xiii—V1—Ca1^xiv	80.420 (13)
O3^iii—Ca1—O1^viii	72.37 (7)	O2—V2—O4^xiv	108.77 (10)
O1^iv—Ca1—O1^viii	120.23 (11)	O2—V2—O4	112.32 (10)
V1—Ca1—O1^viii	165.23 (6)	O4^xiv—V2—O4	138.85 (5)
V2^v—Ca1—O1^viii	105.55 (4)	O2—V2—O3^xiv	105.85 (10)
V2^vi—Ca1—O1^viii	105.55 (4)	O4^xiv—V2—O3^xiv	89.46 (9)
V1^vii—Ca1—O1^viii	62.78 (6)	O4—V2—O3^xiv	81.46 (9)
O2^i—Ca1—V2^i	15.87 (6)	O2—V2—O3^x	114.77 (10)
O2^ii—Ca1—V2^i	94.91 (7)	O4^xiv—V2—O3^x	81.36 (9)
O4—Ca1—V2^i	153.42 (5)	O4—V2—O3^x	79.96 (8)
O4^iii—Ca1—V2^i	100.15 (5)	O3^xiv—V2—O3^x	139.19 (4)
O3—Ca1—V2^i	136.42 (6)	O2—V2—V2^xiv	120.66 (7)
O3^iii—Ca1—V2^i	91.00 (5)	O4^xiv—V2—V2^xiv	40.66 (6)
O1^iv—Ca1—V2^i	69.96 (5)	O4—V2—V2^xiv	111.54 (6)
V1—Ca1—V2^i	124.91 (2)	O3^xiv—V2—V2^xiv	118.44 (7)
V2^v—Ca1—V2^i	170.27 (2)	O3^x—V2—V2^xiv	40.74 (6)
V2^vi—Ca1—V2^i	94.56 (2)	O2—V2—V2^v	114.11 (7)
V1^vii—Ca1—V2^i	112.24 (2)	O4^xiv—V2—V2^v	120.57 (7)
O1^viii—Ca1—V2^i	65.02 (4)	O4—V2—V2^v	40.56 (6)
O2^i—Ca1—V2^ii	94.91 (7)	O3^xiv—V2—V2^v	40.94 (6)
O2^ii—Ca1—V2^ii	15.87 (6)	O3^x—V2—V2^v	113.36 (7)
O4—Ca1—V2^ii	100.15 (5)	V2^xiv—V2—V2^v	125.22 (4)
O4^iii—Ca1—V2^ii	153.42 (5)	O2—V2—V1	127.56 (9)
O3—Ca1—V2^ii	91.00 (5)	O4^xiv—V2—V1	109.02 (6)
O3^iii—Ca1—V2^ii	136.42 (6)	O4—V2—V1	40.52 (6)
O1^iv—Ca1—V2^ii	69.96 (5)	O3^xiv—V2—V1	109.49 (6)
V1—Ca1—V2^ii	124.91 (2)	O3^x—V2—V1	40.22 (6)
V2^v—Ca1—V2^ii	94.56 (2)	V2^xiv—V2—V1	72.57 (3)
V2^vi—Ca1—V2^ii	170.27 (2)	V2^v—V2—V1	74.19 (3)
V1^vii—Ca1—V2^ii	112.24 (2)	O2—V2—Ca1^xiv	117.99 (9)
O1^viii—Ca1—V2^ii	65.02 (4)	O4^xiv—V2—Ca1^xiv	44.20 (6)
V2^i—Ca1—V2^ii	79.44 (3)	O4—V2—Ca1^xiv	113.32 (7)
O2^i—Ca1—V1^iv	68.44 (5)	O3^xiv—V2—Ca1^xiv	45.44 (6)
O2^ii—Ca1—V1^iv	68.44 (5)	O3^x—V2—Ca1^xiv	112.56 (7)
O4—Ca1—V1^iv	101.08 (5)	V2^xiv—V2—Ca1^xiv	76.56 (3)
O4^iii—Ca1—V1^iv	101.08 (5)	V2^v—V2—Ca1^xiv	79.26 (3)
O3—Ca1—V1^iv	144.92 (5)	V1—V2—Ca1^xiv	114.44 (3)
O3^iii—Ca1—V1^iv	144.92 (5)	O2—V2—Ca1^ii	23.36 (9)
O1^iv—Ca1—V1^iv	19.69 (7)	O4^xiv—V2—Ca1^ii	95.21 (6)
V1—Ca1—V1^iv	94.23 (3)	O4—V2—Ca1^ii	124.03 (6)
V2^v—Ca1—V1^iv	126.32 (2)	O3^xiv—V2—Ca1^ii	87.15 (6)
V2^vi—Ca1—V1^iv	126.32 (2)	O3^x—V2—Ca1^ii	133.07 (6)
V1^vii—Ca1—V1^iv	163.32 (3)	V2^xiv—V2—Ca1^ii	121.85 (3)
O1^viii—Ca1—V1^iv	100.53 (6)	V2^v—V2—Ca1^ii	108.51 (3)
V2^i—Ca1—V1^iv	56.31 (2)	V1—V2—Ca1^ii	150.24 (3)
V2^ii—Ca1—V1^iv	56.31 (2)	Ca1^xiv—V2—Ca1^ii	94.91 (2)
O2^i—Ca1—V2	146.04 (6)	O2—V2—Ca1	84.88 (8)
O2^ii—Ca1—V2	70.36 (5)	O4^xiv—V2—Ca1	164.74 (6)
O4—Ca1—V2	22.60 (5)	O4—V2—Ca1	27.87 (6)
O4^iii—Ca1—V2	82.87 (5)	O3^xiv—V2—Ca1	93.37 (6)
O3—Ca1—V2	80.61 (5)	O3^x—V2—Ca1	86.75 (7)
O3^iii—Ca1—V2	128.58 (6)	V2^xiv—V2—Ca1	126.51 (3)
O1^iv—Ca1—V2	68.09 (5)	V2^v—V2—Ca1	56.12 (2)
V1—Ca1—V2	47.643 (15)	V1—V2—Ca1	55.96 (2)
V2^v—Ca1—V2	47.321 (14)	Ca1^xiv—V2—Ca1	135.37 (3)
V2^vi—Ca1—V2	109.30 (3)	Ca1^ii—V2—Ca1	99.91 (2)
V1^vii—Ca1—V2	109.96 (3)	O2—V2—Ca1^x	89.30 (8)
O1^viii—Ca1—V2	134.642 (15)	O4^xiv—V2—Ca1^x	90.38 (6)
V2^i—Ca1—V2	137.46 (3)	O4—V2—Ca1^x	88.21 (6)
V2^ii—Ca1—V2	80.09 (2)	O3^xiv—V2—Ca1^x	164.03 (6)
V1^iv—Ca1—V2	81.34 (2)	O3^x—V2—Ca1^x	25.50 (6)
O2^i—Ca1—V2^iii	70.36 (5)	V2^xiv—V2—Ca1^x	54.56 (2)
O2^ii—Ca1—V2^iii	146.04 (6)	V2^v—V2—Ca1^x	128.05 (3)
O4—Ca1—V2^iii	82.87 (5)	V1—V2—Ca1^x	55.69 (2)
O4^iii—Ca1—V2^iii	22.60 (5)	Ca1^xiv—V2—Ca1^x	131.10 (2)
O3—Ca1—V2^iii	128.58 (6)	Ca1^ii—V2—Ca1^x	108.76 (2)
O3^iii—Ca1—V2^iii	80.61 (5)	Ca1—V2—Ca1^x	82.80 (2)
O1^iv—Ca1—V2^iii	68.09 (5)	V1—O1—Ca1^xii	128.49 (15)
V1—Ca1—V2^iii	47.643 (15)	V1—O1—Ca1^xiii	111.28 (13)
V2^v—Ca1—V2^iii	109.30 (3)	Ca1^xii—O1—Ca1^xiii	120.23 (11)
V2^vi—Ca1—V2^iii	47.321 (14)	V1—O1—Ca1^x	37.94 (8)
V1^vii—Ca1—V2^iii	109.96 (3)	Ca1^xii—O1—Ca1^x	90.56 (8)
O1^viii—Ca1—V2^iii	134.642 (15)	Ca1^xiii—O1—Ca1^x	149.21 (9)
V2^i—Ca1—V2^iii	80.09 (2)	V1—O1—Ca1	32.57 (8)
V2^ii—Ca1—V2^iii	137.46 (3)	Ca1^xii—O1—Ca1	161.06 (10)
V1^iv—Ca1—V2^iii	81.34 (2)	Ca1^xiii—O1—Ca1	78.71 (6)
V2—Ca1—V2^iii	90.66 (3)	Ca1^x—O1—Ca1	70.50 (5)
O2^i—Ca1—V2^ix	58.57 (5)	V2—O2—Ca1^ii	140.77 (14)
O2^ii—Ca1—V2^ix	127.65 (6)	V2—O2—Ca1	72.18 (8)
O4—Ca1—V2^ix	126.54 (6)	Ca1^ii—O2—Ca1	128.64 (7)
O4^iii—Ca1—V2^ix	79.58 (5)	V2—O2—Ca1^x	68.91 (8)
O3—Ca1—V2^ix	80.06 (5)	Ca1^ii—O2—Ca1^x	140.73 (7)
O3^iii—Ca1—V2^ix	20.46 (5)	Ca1—O2—Ca1^x	77.24 (5)
O1^iv—Ca1—V2^ix	134.54 (2)	V2—O2—Ca1^xiv	42.94 (7)
V1—Ca1—V2^ix	110.84 (3)	Ca1^ii—O2—Ca1^xiv	98.18 (7)
V2^v—Ca1—V2^ix	106.69 (3)	Ca1—O2—Ca1^xiv	105.65 (5)
V2^vi—Ca1—V2^ix	46.175 (15)	Ca1^x—O2—Ca1^xiv	101.87 (4)
V1^vii—Ca1—V2^ix	46.268 (15)	V1^vii—O3—V2^v	128.55 (11)
O1^viii—Ca1—V2^ix	59.71 (3)	V1^vii—O3—V2^vii	99.25 (9)
V2^i—Ca1—V2^ix	71.24 (2)	V2^v—O3—V2^vii	98.32 (9)
V2^ii—Ca1—V2^ix	124.15 (2)	V1^vii—O3—Ca1	102.04 (9)
V1^iv—Ca1—V2^ix	126.97 (2)	V2^v—O3—Ca1	99.37 (8)
V2—Ca1—V2^ix	149.02 (3)	V2^vii—O3—Ca1	134.03 (10)
V2^iii—Ca1—V2^ix	82.80 (2)	V1^vii—O3—Ca1^xiii	65.39 (6)
O2^i—Ca1—V2^vii	127.65 (6)	V2^v—O3—Ca1^xiii	64.48 (6)
O2^ii—Ca1—V2^vii	58.57 (5)	V2^vii—O3—Ca1^xiii	123.14 (8)
O4—Ca1—V2^vii	79.58 (5)	Ca1—O3—Ca1^xiii	102.76 (6)
O4^iii—Ca1—V2^vii	126.54 (6)	V1^vii—O3—Ca1^vii	48.91 (5)
O3—Ca1—V2^vii	20.46 (5)	V2^v—O3—Ca1^vii	160.70 (9)
O3^iii—Ca1—V2^vii	80.06 (5)	V2^vii—O3—Ca1^vii	66.03 (6)
O1^iv—Ca1—V2^vii	134.54 (2)	Ca1—O3—Ca1^vii	99.74 (7)
V1—Ca1—V2^vii	110.84 (3)	Ca1^xiii—O3—Ca1^vii	113.49 (5)
V2^v—Ca1—V2^vii	46.175 (15)	V1^vii—O3—Ca1^v	104.72 (7)
V2^vi—Ca1—V2^vii	106.69 (3)	V2^v—O3—Ca1^v	60.83 (6)
V1^vii—Ca1—V2^vii	46.268 (15)	V2^vii—O3—Ca1^v	43.59 (5)
O1^viii—Ca1—V2^vii	59.71 (3)	Ca1—O3—Ca1^v	153.04 (7)
V2^i—Ca1—V2^vii	124.15 (2)	Ca1^xiii—O3—Ca1^v	85.62 (4)
V2^ii—Ca1—V2^vii	71.24 (2)	Ca1^vii—O3—Ca1^v	100.20 (4)
V1^iv—Ca1—V2^vii	126.97 (2)	V2^v—O4—V2	98.78 (9)
V2—Ca1—V2^vii	82.80 (2)	V2^v—O4—V1	132.86 (11)
V2^iii—Ca1—V2^vii	149.02 (3)	V2—O4—V1	99.16 (9)
V2^ix—Ca1—V2^vii	87.40 (3)	V2^v—O4—Ca1	100.90 (8)
O2^i—Ca1—O2	132.49 (4)	V2—O4—Ca1	129.53 (10)
O2^ii—Ca1—O2	51.36 (7)	V1—O4—Ca1	100.38 (9)
O4—Ca1—O2	45.37 (6)	V2^v—O4—Ca1^xiii	58.26 (5)
O4^iii—Ca1—O2	100.89 (6)	V2—O4—Ca1^xiii	132.44 (8)
O3—Ca1—O2	89.15 (6)	V1—O4—Ca1^xiii	77.71 (6)
O3^iii—Ca1—O2	149.63 (6)	Ca1—O4—Ca1^xiii	97.14 (6)
O1^iv—Ca1—O2	56.31 (4)	V2^v—O4—Ca1^x	161.72 (8)
V1—Ca1—O2	67.03 (3)	V2—O4—Ca1^x	65.63 (5)
V2^v—Ca1—O2	62.26 (3)	V1—O4—Ca1^x	47.01 (5)
V2^vi—Ca1—O2	131.24 (4)	Ca1—O4—Ca1^x	96.66 (6)
V1^vii—Ca1—O2	122.73 (4)	Ca1^xiii—O4—Ca1^x	124.56 (5)
O1^viii—Ca1—O2	119.77 (4)	V2^v—O4—Ca1^xiv	63.90 (6)
V2^i—Ca1—O2	119.34 (4)	V2—O4—Ca1^xiv	43.15 (5)
V2^ii—Ca1—O2	58.41 (3)	V1—O4—Ca1^xiv	104.11 (7)
V1^iv—Ca1—O2	64.06 (3)	Ca1—O4—Ca1^xiv	155.34 (7)
V2—Ca1—O2	22.95 (3)	Ca1^xiii—O4—Ca1^xiv	90.90 (4)
V2^iii—Ca1—O2	101.96 (4)	Ca1^x—O4—Ca1^xiv	97.86 (4)
V2^ix—Ca1—O2	168.83 (4)	V2^v—O4—Ca1^ii	90.09 (7)
V2^vii—Ca1—O2	83.40 (4)	V2—O4—Ca1^ii	37.35 (4)
O1—V1—O3^x	109.15 (9)	V1—O4—Ca1^ii	128.24 (7)
O1—V1—O3^xi	109.15 (9)	Ca1—O4—Ca1^ii	96.67 (6)
O3^x—V1—O3^xi	86.55 (12)	Ca1^xiii—O4—Ca1^ii	147.34 (5)
O1—V1—O4^iii	111.33 (9)	Ca1^x—O4—Ca1^ii	82.81 (3)
O3^x—V1—O4^iii	139.52 (10)	Ca1^xiv—O4—Ca1^ii	65.64 (3)
O3^xi—V1—O4^iii	80.07 (8)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_112K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.547 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.70930 Å
Hall symbol: -P 2ac 2n	Cell parameters from 2755 reflections
a = 10.409 (3) Å	θ = 1.3–23.4°
b = 10.372 (2) Å	µ = 5.69 mm^−1
c = 5.2884 (15) Å	T = 112 K
V = 571.0 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	400 independent reflections
Radiation source: fine-focus sealed tube	367 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.031
Detector resolution: 0 pixels mm^-1	θmax = 22.9°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.470	l = −5→5
2487 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0469P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.056	(Δ/σ)max = 0.001
S = 0.97	Δρmax = 0.28 e Å^−3
400 reflections	Δρmin = −0.34 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0184 (19)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08500 (9)	0.2500	0.29982 (14)	0.0048 (3)
V1	0.28912 (7)	0.2500	0.79222 (13)	0.0040 (3)
V2	0.18731 (6)	0.52011 (5)	0.78341 (10)	0.0040 (3)
O1	0.4444 (3)	0.2500	0.8089 (5)	0.0079 (8)*
O2	0.0390 (2)	0.5651 (2)	0.7660 (3)	0.0080 (6)*
O3	0.22043 (19)	0.3797 (2)	0.0260 (4)	0.0053 (5)*
O4	0.22708 (19)	0.3795 (2)	0.5480 (4)	0.0048 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0034 (5)	0.0049 (6)	0.0061 (5)	0.000	−0.0002 (3)	0.000
V1	0.0027 (5)	0.0046 (6)	0.0046 (5)	0.000	−0.0001 (3)	0.000
V2	0.0032 (4)	0.0040 (4)	0.0047 (4)	0.0005 (2)	0.0000 (2)	0.00000 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.338 (2)	V1—Ca1^xiii	4.3918 (15)
Ca1—O2^ii	2.338 (2)	V1—Ca1^xiv	5.3492 (11)
Ca1—O4	2.391 (2)	V2—O2	1.616 (2)
Ca1—O4^iii	2.391 (2)	V2—O4^xiv	1.959 (2)
Ca1—O3^iii	2.428 (2)	V2—O3^xiv	1.963 (2)
Ca1—O3	2.428 (2)	V2—O4	1.962 (2)
Ca1—O1^iv	2.535 (3)	V2—O3^x	1.971 (2)
Ca1—V1	3.3608 (13)	V2—V2^xiv	2.9782 (9)
Ca1—V2^v	3.3631 (11)	V2—V2^v	2.9781 (9)
Ca1—V2^vi	3.3631 (11)	V2—Ca1^xiv	3.3631 (11)
Ca1—V1^vii	3.4235 (13)	V2—Ca1^ii	3.7301 (11)
Ca1—O1^viii	3.536 (3)	V2—Ca1^x	4.0548 (10)
Ca1—V2^i	3.7301 (11)	O1—Ca1^xii	2.535 (3)
Ca1—V2^ii	3.7301 (11)	O1—Ca1^xiii	3.536 (3)
Ca1—V1^iv	3.7604 (14)	O1—Ca1^x	4.554 (3)
Ca1—V2	3.9400 (10)	O2—Ca1^ii	2.338 (2)
Ca1—V2^iii	3.9400 (10)	O2—Ca1^x	4.345 (2)
Ca1—V2^ix	4.0548 (10)	O2—Ca1^xiv	4.362 (2)
Ca1—V2^vii	4.0548 (10)	O3—V2^v	1.963 (2)
Ca1—O2	4.122 (2)	O3—V1^vii	1.962 (2)
V1—O1	1.619 (3)	O3—V2^vii	1.971 (2)
V1—O3^x	1.962 (2)	O3—Ca1^xiii	4.130 (2)
V1—O3^xi	1.962 (2)	O3—Ca1^vii	4.307 (2)
V1—O4^iii	1.972 (2)	O3—Ca1^v	4.504 (2)
V1—O4	1.972 (2)	O4—V2^v	1.959 (2)
V1—V2^iii	2.9958 (9)	O4—Ca1^xiii	4.367 (2)
V1—V2	2.9958 (9)	O4—Ca1^x	4.450 (2)
V1—Ca1^x	3.4235 (13)	O4—Ca1^xiv	4.513 (2)
V1—Ca1^xii	3.7604 (14)	O4—Ca1^ii	5.096 (2)
O2^i—Ca1—O2^ii	110.24 (12)	O1—V1—O4	111.26 (9)
O2^i—Ca1—O4	152.17 (7)	O3^x—V1—O4	79.99 (8)
O2^ii—Ca1—O4	87.84 (7)	O3^xi—V1—O4	139.50 (10)
O2^i—Ca1—O4^iii	87.84 (7)	O4^iii—V1—O4	85.87 (12)
O2^ii—Ca1—O4^iii	152.17 (7)	O1—V1—V2^iii	110.738 (18)
O4—Ca1—O4^iii	68.38 (10)	O3^x—V1—V2^iii	121.48 (7)
O2^i—Ca1—O3^iii	77.12 (7)	O3^xi—V1—V2^iii	40.50 (6)
O2^ii—Ca1—O3^iii	133.35 (7)	O4^iii—V1—V2^iii	40.27 (6)
O4—Ca1—O3^iii	106.24 (8)	O4—V1—V2^iii	120.73 (7)
O4^iii—Ca1—O3^iii	69.93 (7)	O1—V1—V2	110.738 (18)
O2^i—Ca1—O3	133.35 (7)	O3^x—V1—V2	40.50 (6)
O2^ii—Ca1—O3	77.12 (7)	O3^xi—V1—V2	121.48 (7)
O4—Ca1—O3	69.93 (7)	O4^iii—V1—V2	120.73 (7)
O4^iii—Ca1—O3	106.24 (8)	O4—V1—V2	40.27 (6)
O3^iii—Ca1—O3	67.32 (10)	V2^iii—V1—V2	138.52 (4)
O2^i—Ca1—O1^iv	78.62 (7)	O1—V1—Ca1	132.33 (10)
O2^ii—Ca1—O1^iv	78.62 (7)	O3^x—V1—Ca1	104.94 (6)
O4—Ca1—O1^iv	84.77 (8)	O3^xi—V1—Ca1	104.94 (6)
O4^iii—Ca1—O1^iv	84.77 (8)	O4^iii—V1—Ca1	44.41 (6)
O3^iii—Ca1—O1^iv	145.30 (5)	O4—V1—Ca1	44.41 (6)
O3—Ca1—O1^iv	145.30 (5)	V2^iii—V1—Ca1	76.368 (17)
O2^i—Ca1—V1	117.67 (5)	V2—V1—Ca1	76.368 (17)
O2^ii—Ca1—V1	117.67 (5)	O1—V1—Ca1^x	125.24 (10)
O4—Ca1—V1	35.26 (5)	O3^x—V1—Ca1^x	43.93 (6)
O4^iii—Ca1—V1	35.26 (5)	O3^xi—V1—Ca1^x	43.93 (6)
O3^iii—Ca1—V1	95.45 (6)	O4^iii—V1—Ca1^x	108.07 (6)
O3—Ca1—V1	95.45 (6)	O4—V1—Ca1^x	108.07 (6)
O1^iv—Ca1—V1	74.48 (7)	V2^iii—V1—Ca1^x	78.032 (18)
O2^i—Ca1—V2^v	165.22 (6)	V2—V1—Ca1^x	78.032 (18)
O2^ii—Ca1—V2^v	78.67 (6)	Ca1—V1—Ca1^x	102.43 (4)
O4—Ca1—V2^v	34.89 (5)	O1—V1—Ca1^xii	31.89 (10)
O4^iii—Ca1—V2^v	88.66 (6)	O3^x—V1—Ca1^xii	86.38 (6)
O3^iii—Ca1—V2^v	88.19 (6)	O3^xi—V1—Ca1^xii	86.38 (6)
O3—Ca1—V2^v	35.16 (5)	O4^iii—V1—Ca1^xii	130.08 (6)
O1^iv—Ca1—V2^v	115.34 (5)	O4—V1—Ca1^xii	130.08 (6)
V1—Ca1—V2^v	64.82 (2)	V2^iii—V1—Ca1^xii	107.377 (17)
O2^i—Ca1—V2^vi	78.67 (6)	V2—V1—Ca1^xii	107.377 (17)
O2^ii—Ca1—V2^vi	165.22 (6)	Ca1—V1—Ca1^xii	164.22 (3)
O4—Ca1—V2^vi	88.66 (6)	Ca1^x—V1—Ca1^xii	93.35 (3)
O4^iii—Ca1—V2^vi	34.89 (5)	O1—V1—Ca1^xiii	48.59 (10)
O3^iii—Ca1—V2^vi	35.16 (5)	O3^x—V1—Ca1^xiii	134.81 (6)
O3—Ca1—V2^vi	88.19 (6)	O3^xi—V1—Ca1^xiii	134.81 (6)
O1^iv—Ca1—V2^vi	115.34 (5)	O4^iii—V1—Ca1^xiii	76.28 (6)
V1—Ca1—V2^vi	64.82 (2)	O4—V1—Ca1^xiii	76.28 (6)
V2^v—Ca1—V2^vi	90.31 (4)	V2^iii—V1—Ca1^xiii	103.710 (17)
O2^i—Ca1—V1^vii	103.06 (5)	V2—V1—Ca1^xiii	103.710 (17)
O2^ii—Ca1—V1^vii	103.06 (5)	Ca1—V1—Ca1^xiii	83.74 (3)
O4—Ca1—V1^vii	92.67 (6)	Ca1^x—V1—Ca1^xiii	173.83 (3)
O4^iii—Ca1—V1^vii	92.67 (6)	Ca1^xii—V1—Ca1^xiii	80.48 (3)
O3^iii—Ca1—V1^vii	34.11 (5)	O1—V1—Ca1^xiv	75.819 (14)
O3—Ca1—V1^vii	34.11 (5)	O3^x—V1—Ca1^xiv	54.53 (6)
O1^iv—Ca1—V1^vii	176.91 (8)	O3^xi—V1—Ca1^xiv	138.53 (6)
V1—Ca1—V1^vii	102.43 (4)	O4^iii—V1—Ca1^xiv	138.20 (6)
V2^v—Ca1—V1^vii	62.77 (2)	O4—V1—Ca1^xiv	54.88 (6)
V2^vi—Ca1—V1^vii	62.77 (2)	V2^iii—V1—Ca1^xiv	173.44 (3)
O2^i—Ca1—O1^viii	68.65 (5)	V2—V1—Ca1^xiv	34.92 (2)
O2^ii—Ca1—O1^viii	68.65 (5)	Ca1—V1—Ca1^xiv	99.246 (14)
O4—Ca1—O1^viii	139.10 (6)	Ca1^x—V1—Ca1^xiv	98.402 (14)
O4^iii—Ca1—O1^viii	139.10 (6)	Ca1^xii—V1—Ca1^xiv	78.175 (13)
O3^iii—Ca1—O1^viii	72.38 (7)	Ca1^xiii—V1—Ca1^xiv	80.421 (13)
O3—Ca1—O1^viii	72.38 (7)	O2—V2—O4^xiv	108.79 (10)
O1^iv—Ca1—O1^viii	120.29 (11)	O2—V2—O3^xiv	105.96 (10)
V1—Ca1—O1^viii	165.23 (6)	O4^xiv—V2—O3^xiv	89.52 (9)
V2^v—Ca1—O1^viii	105.56 (4)	O2—V2—O4	112.35 (10)
V2^vi—Ca1—O1^viii	105.56 (4)	O4^xiv—V2—O4	138.81 (5)
V1^vii—Ca1—O1^viii	62.81 (6)	O3^xiv—V2—O4	81.38 (9)
O2^i—Ca1—V2^i	15.94 (6)	O2—V2—O3^x	114.69 (10)
O2^ii—Ca1—V2^i	95.01 (6)	O4^xiv—V2—O3^x	81.26 (9)
O4—Ca1—V2^i	153.40 (5)	O3^xiv—V2—O3^x	139.17 (4)
O4^iii—Ca1—V2^i	100.12 (5)	O4—V2—O3^x	80.04 (8)
O3^iii—Ca1—V2^i	90.95 (5)	O2—V2—V2^xiv	120.66 (7)
O3—Ca1—V2^i	136.48 (6)	O4^xiv—V2—V2^xiv	40.60 (6)
O1^iv—Ca1—V2^i	69.98 (5)	O3^xiv—V2—V2^xiv	118.38 (7)
V1—Ca1—V2^i	124.88 (2)	O4—V2—V2^xiv	111.52 (6)
V2^v—Ca1—V2^i	170.30 (2)	O3^x—V2—V2^xiv	40.70 (6)
V2^vi—Ca1—V2^i	94.55 (2)	O2—V2—V2^v	114.12 (7)
V1^vii—Ca1—V2^i	112.28 (2)	O4^xiv—V2—V2^v	120.62 (7)
O1^viii—Ca1—V2^i	65.05 (4)	O3^xiv—V2—V2^v	40.90 (6)
O2^i—Ca1—V2^ii	95.01 (6)	O4—V2—V2^v	40.52 (6)
O2^ii—Ca1—V2^ii	15.94 (6)	O3^x—V2—V2^v	113.44 (7)
O4—Ca1—V2^ii	100.12 (5)	V2^xiv—V2—V2^v	125.21 (4)
O4^iii—Ca1—V2^ii	153.40 (5)	O2—V2—V1	127.53 (9)
O3^iii—Ca1—V2^ii	136.48 (6)	O4^xiv—V2—V1	108.97 (6)
O3—Ca1—V2^ii	90.95 (5)	O3^xiv—V2—V1	109.42 (6)
O1^iv—Ca1—V2^ii	69.98 (5)	O4—V2—V1	40.53 (6)
V1—Ca1—V2^ii	124.88 (2)	O3^x—V2—V1	40.29 (6)
V2^v—Ca1—V2^ii	94.55 (2)	V2^xiv—V2—V1	72.55 (3)
V2^vi—Ca1—V2^ii	170.30 (2)	V2^v—V2—V1	74.20 (3)
V1^vii—Ca1—V2^ii	112.28 (2)	O2—V2—Ca1^xiv	118.04 (9)
O1^viii—Ca1—V2^ii	65.05 (4)	O4^xiv—V2—Ca1^xiv	44.28 (6)
V2^i—Ca1—V2^ii	79.47 (3)	O3^xiv—V2—Ca1^xiv	45.41 (6)
O2^i—Ca1—V1^iv	68.48 (5)	O4—V2—Ca1^xiv	113.25 (7)
O2^ii—Ca1—V1^iv	68.48 (5)	O3^x—V2—Ca1^xiv	112.56 (7)
O4—Ca1—V1^iv	101.05 (5)	V2^xiv—V2—Ca1^xiv	76.56 (3)
O4^iii—Ca1—V1^iv	101.05 (5)	V2^v—V2—Ca1^xiv	79.24 (3)
O3^iii—Ca1—V1^iv	144.86 (5)	V1—V2—Ca1^xiv	114.42 (3)
O3—Ca1—V1^iv	144.86 (5)	O2—V2—Ca1^ii	23.42 (9)
O1^iv—Ca1—V1^iv	19.72 (7)	O4^xiv—V2—Ca1^ii	95.18 (6)
V1—Ca1—V1^iv	94.20 (3)	O3^xiv—V2—Ca1^ii	87.23 (6)
V2^v—Ca1—V1^iv	126.299 (19)	O4—V2—Ca1^ii	124.11 (6)
V2^vi—Ca1—V1^iv	126.299 (19)	O3^x—V2—Ca1^ii	133.00 (6)
V1^vii—Ca1—V1^iv	163.37 (3)	V2^xiv—V2—Ca1^ii	121.83 (3)
O1^viii—Ca1—V1^iv	100.57 (6)	V2^v—V2—Ca1^ii	108.53 (3)
V2^i—Ca1—V1^iv	56.31 (2)	V1—V2—Ca1^ii	150.28 (3)
V2^ii—Ca1—V1^iv	56.31 (2)	Ca1^xiv—V2—Ca1^ii	94.90 (2)
O2^i—Ca1—V2	146.01 (6)	O2—V2—Ca1	84.84 (8)
O2^ii—Ca1—V2	70.27 (5)	O4^xiv—V2—Ca1	164.73 (6)
O4—Ca1—V2	22.60 (5)	O3^xiv—V2—Ca1	93.35 (6)
O4^iii—Ca1—V2	82.88 (5)	O4—V2—Ca1	27.93 (6)
O3^iii—Ca1—V2	128.63 (6)	O3^x—V2—Ca1	86.82 (7)
O3—Ca1—V2	80.56 (5)	V2^xiv—V2—Ca1	126.52 (3)
O1^iv—Ca1—V2	68.04 (5)	V2^v—V2—Ca1	56.12 (2)
V1—Ca1—V2	47.640 (15)	V1—V2—Ca1	55.99 (2)
V2^v—Ca1—V2	47.322 (14)	Ca1^xiv—V2—Ca1	135.35 (3)
V2^vi—Ca1—V2	109.30 (3)	Ca1^ii—V2—Ca1	99.94 (2)
V1^vii—Ca1—V2	109.95 (3)	O2—V2—Ca1^x	89.26 (8)
O1^viii—Ca1—V2	134.648 (15)	O4^xiv—V2—Ca1^x	90.32 (6)
V2^i—Ca1—V2	137.44 (3)	O3^xiv—V2—Ca1^x	163.95 (7)
V2^ii—Ca1—V2	80.06 (2)	O4—V2—Ca1^x	88.23 (6)
V1^iv—Ca1—V2	81.31 (2)	O3^x—V2—Ca1^x	25.46 (6)
O2^i—Ca1—V2^iii	70.27 (5)	V2^xiv—V2—Ca1^x	54.57 (2)
O2^ii—Ca1—V2^iii	146.01 (6)	V2^v—V2—Ca1^x	128.05 (3)
O4—Ca1—V2^iii	82.88 (5)	V1—V2—Ca1^x	55.69 (2)
O4^iii—Ca1—V2^iii	22.60 (5)	Ca1^xiv—V2—Ca1^x	131.12 (2)
O3^iii—Ca1—V2^iii	80.56 (5)	Ca1^ii—V2—Ca1^x	108.76 (2)
O3—Ca1—V2^iii	128.63 (6)	Ca1—V2—Ca1^x	82.81 (2)
O1^iv—Ca1—V2^iii	68.04 (5)	V1—O1—Ca1^xii	128.39 (15)
V1—Ca1—V2^iii	47.640 (16)	V1—O1—Ca1^xiii	111.33 (13)
V2^v—Ca1—V2^iii	109.30 (3)	Ca1^xii—O1—Ca1^xiii	120.29 (11)
V2^vi—Ca1—V2^iii	47.322 (14)	V1—O1—Ca1^x	37.88 (8)
V1^vii—Ca1—V2^iii	109.95 (3)	Ca1^xii—O1—Ca1^x	90.51 (8)
O1^viii—Ca1—V2^iii	134.648 (15)	Ca1^xiii—O1—Ca1^x	149.21 (9)
V2^i—Ca1—V2^iii	80.06 (2)	V1—O1—Ca1	32.62 (8)
V2^ii—Ca1—V2^iii	137.44 (3)	Ca1^xii—O1—Ca1	161.01 (10)
V1^iv—Ca1—V2^iii	81.31 (2)	Ca1^xiii—O1—Ca1	78.71 (6)
V2—Ca1—V2^iii	90.65 (3)	Ca1^x—O1—Ca1	70.50 (5)
O2^i—Ca1—V2^ix	58.53 (5)	V2—O2—Ca1^ii	140.64 (13)
O2^ii—Ca1—V2^ix	127.70 (6)	V2—O2—Ca1	72.18 (8)
O4—Ca1—V2^ix	126.56 (6)	Ca1^ii—O2—Ca1	128.73 (7)
O4^iii—Ca1—V2^ix	79.57 (5)	V2—O2—Ca1^x	68.91 (8)
O3^iii—Ca1—V2^ix	20.43 (5)	Ca1^ii—O2—Ca1^x	140.77 (7)
O3—Ca1—V2^ix	80.14 (5)	Ca1—O2—Ca1^x	77.25 (5)
O1^iv—Ca1—V2^ix	134.55 (2)	V2—O2—Ca1^xiv	42.88 (7)
V1—Ca1—V2^ix	110.84 (3)	Ca1^ii—O2—Ca1^xiv	98.10 (7)
V2^v—Ca1—V2^ix	106.70 (3)	Ca1—O2—Ca1^xiv	105.60 (5)
V2^vi—Ca1—V2^ix	46.184 (15)	Ca1^x—O2—Ca1^xiv	101.83 (4)
V1^vii—Ca1—V2^ix	46.283 (15)	V2^v—O3—V1^vii	128.42 (11)
O1^viii—Ca1—V2^ix	59.71 (3)	V2^v—O3—V2^vii	98.40 (9)
V2^i—Ca1—V2^ix	71.24 (2)	V1^vii—O3—V2^vii	99.21 (9)
V2^ii—Ca1—V2^ix	124.18 (2)	V2^v—O3—Ca1	99.43 (8)
V1^iv—Ca1—V2^ix	126.98 (2)	V1^vii—O3—Ca1	101.96 (9)
V2—Ca1—V2^ix	149.04 (3)	V2^vii—O3—Ca1	134.11 (10)
V2^iii—Ca1—V2^ix	82.81 (2)	V2^v—O3—Ca1^xiii	64.43 (6)
O2^i—Ca1—V2^vii	127.70 (6)	V1^vii—O3—Ca1^xiii	65.31 (6)
O2^ii—Ca1—V2^vii	58.53 (5)	V2^vii—O3—Ca1^xiii	123.13 (8)
O4—Ca1—V2^vii	79.57 (5)	Ca1—O3—Ca1^xiii	102.70 (6)
O4^iii—Ca1—V2^vii	126.56 (6)	V2^v—O3—Ca1^vii	160.69 (9)
O3^iii—Ca1—V2^vii	80.14 (5)	V1^vii—O3—Ca1^vii	48.94 (5)
O3—Ca1—V2^vii	20.43 (5)	V2^vii—O3—Ca1^vii	65.99 (6)
O1^iv—Ca1—V2^vii	134.55 (2)	Ca1—O3—Ca1^vii	99.71 (7)
V1—Ca1—V2^vii	110.84 (3)	Ca1^xiii—O3—Ca1^vii	113.44 (5)
V2^v—Ca1—V2^vii	46.184 (15)	V2^v—O3—Ca1^v	60.85 (6)
V2^vi—Ca1—V2^vii	106.70 (3)	V1^vii—O3—Ca1^v	104.69 (7)
V1^vii—Ca1—V2^vii	46.283 (15)	V2^vii—O3—Ca1^v	43.60 (5)
O1^viii—Ca1—V2^vii	59.71 (3)	Ca1—O3—Ca1^v	153.15 (7)
V2^i—Ca1—V2^vii	124.18 (2)	Ca1^xiii—O3—Ca1^v	85.63 (4)
V2^ii—Ca1—V2^vii	71.24 (2)	Ca1^vii—O3—Ca1^v	100.18 (4)
V1^iv—Ca1—V2^vii	126.98 (2)	V2^v—O4—V2	98.88 (9)
V2—Ca1—V2^vii	82.81 (2)	V2^v—O4—V1	132.92 (11)
V2^iii—Ca1—V2^vii	149.04 (3)	V2—O4—V1	99.20 (9)
V2^ix—Ca1—V2^vii	87.41 (3)	V2^v—O4—Ca1	100.83 (8)
O2^i—Ca1—O2	132.48 (4)	V2—O4—Ca1	129.47 (10)
O2^ii—Ca1—O2	51.27 (7)	V1—O4—Ca1	100.33 (9)
O4—Ca1—O2	45.40 (6)	V2^v—O4—Ca1^xiii	58.29 (5)
O4^iii—Ca1—O2	100.90 (6)	V2—O4—Ca1^xiii	132.54 (8)
O3^iii—Ca1—O2	149.73 (6)	V1—O4—Ca1^xiii	77.70 (6)
O3—Ca1—O2	89.12 (6)	Ca1—O4—Ca1^xiii	97.10 (6)
O1^iv—Ca1—O2	56.26 (4)	V2^v—O4—Ca1^x	161.82 (9)
V1—Ca1—O2	67.05 (3)	V2—O4—Ca1^x	65.62 (5)
V2^v—Ca1—O2	62.30 (3)	V1—O4—Ca1^x	47.01 (5)
V2^vi—Ca1—O2	131.26 (4)	Ca1—O4—Ca1^x	96.62 (6)
V1^vii—Ca1—O2	122.76 (4)	Ca1^xiii—O4—Ca1^x	124.55 (5)
O1^viii—Ca1—O2	119.76 (4)	V2^v—O4—Ca1^xiv	63.96 (6)
V2^i—Ca1—O2	119.29 (4)	V2—O4—Ca1^xiv	43.21 (5)
V2^ii—Ca1—O2	58.36 (3)	V1—O4—Ca1^xiv	104.17 (7)
V1^iv—Ca1—O2	64.00 (3)	Ca1—O4—Ca1^xiv	155.32 (7)
V2—Ca1—O2	22.98 (3)	Ca1^xiii—O4—Ca1^xiv	90.94 (4)
V2^iii—Ca1—O2	101.95 (4)	Ca1^x—O4—Ca1^xiv	97.90 (4)
V2^ix—Ca1—O2	168.88 (4)	V2^v—O4—Ca1^ii	90.12 (7)
V2^vii—Ca1—O2	83.42 (4)	V2—O4—Ca1^ii	37.31 (4)
O1—V1—O3^x	109.24 (9)	V1—O4—Ca1^ii	128.24 (7)
O1—V1—O3^xi	109.24 (9)	Ca1—O4—Ca1^ii	96.67 (6)
O3^x—V1—O3^xi	86.59 (12)	Ca1^xiii—O4—Ca1^ii	147.40 (5)
O1—V1—O4^iii	111.26 (9)	Ca1^x—O4—Ca1^ii	82.80 (3)
O3^x—V1—O4^iii	139.50 (10)	Ca1^xiv—O4—Ca1^ii	65.64 (3)
O3^xi—V1—O4^iii	79.99 (8)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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_100K)

Crystal data

O7V3·Ca	F(000) = 580
Mr = 304.90	Dx = 3.547 Mg m^−3
Orthorhombic, Pnma	? radiation, λ = 0.70930 Å
Hall symbol: -P 2ac 2n	Cell parameters from 3202 reflections
a = 10.409 (3) Å	θ = 2.0–23.2°
b = 10.374 (2) Å	µ = 5.69 mm^−1
c = 5.2876 (15) Å	T = 100 K
V = 571.0 (3) Å^3	, brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection

STOE IPDS 2 diffractometer	399 independent reflections
Radiation source: fine-focus sealed tube	366 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 0 pixels mm^-1	θmax = 22.9°, θmin = 3.9°
Rotation method scans	h = −11→11
Absorption correction: numerical X-SHAPE (Stoe & Cie, 1996)	k = −10→10
Tmin = 0.317, Tmax = 0.470	l = −5→5
2474 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.019	w = 1/[σ^2(Fo^2) + (0.0472P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.055	(Δ/σ)max = 0.001
S = 0.95	Δρmax = 0.24 e Å^−3
399 reflections	Δρmin = −0.28 e Å^−3
38 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0180 (18)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ca1	0.08497 (9)	0.2500	0.29980 (14)	0.0045 (3)
V1	0.28919 (7)	0.2500	0.79228 (13)	0.0036 (3)
V2	0.18733 (5)	0.52010 (5)	0.78334 (9)	0.0037 (3)
O1	0.4445 (3)	0.2500	0.8089 (5)	0.0073 (7)*
O2	0.0391 (2)	0.5650 (2)	0.7658 (3)	0.0076 (6)*
O3	0.22037 (19)	0.37948 (19)	0.0260 (4)	0.0048 (5)*
O4	0.22696 (19)	0.37927 (19)	0.5478 (3)	0.0043 (5)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ca1	0.0032 (5)	0.0049 (6)	0.0055 (5)	0.000	−0.0003 (3)	0.000
V1	0.0022 (5)	0.0041 (5)	0.0046 (5)	0.000	−0.0006 (3)	0.000
V2	0.0028 (4)	0.0039 (4)	0.0044 (4)	0.0007 (2)	−0.0001 (2)	0.00003 (19)

Geometric parameters (Å, º)

Ca1—O2^i	2.339 (2)	V2—O3^xiv	1.965 (2)
Ca1—O2^ii	2.339 (2)	V2—O4	1.964 (2)
Ca1—O4	2.388 (2)	V2—O3^x	1.973 (2)
Ca1—O4^iii	2.388 (2)	V2—V2^v	2.9775 (9)
Ca1—O3^iii	2.426 (2)	V2—V2^xiv	2.9775 (9)
Ca1—O3	2.426 (2)	V2—Ca1^xiv	3.3635 (11)
Ca1—O1^iv	2.533 (3)	V2—Ca1^ii	3.7303 (11)
Ca1—V1	3.3615 (12)	V2—Ca1^x	4.0551 (10)
Ca1—V2^v	3.3635 (11)	O1—Ca1^xii	2.533 (3)
Ca1—V2^vi	3.3635 (11)	O1—Ca1^xiii	3.535 (3)
Ca1—V1^vii	3.4235 (13)	O1—Ca1^x	4.554 (3)
Ca1—O1^viii	3.535 (3)	O2—Ca1^ii	2.339 (2)
Ca1—V2^i	3.7303 (11)	O2—O2^ii	3.223 (4)
Ca1—V2^ii	3.7303 (11)	O2—Ca1^x	4.345 (2)
Ca1—V1^iv	3.7591 (14)	O2—Ca1^xiv	4.362 (2)
Ca1—V2	3.9400 (10)	O2—O2^iv	5.2071 (13)
Ca1—V2^iii	3.9400 (10)	O2—O2^xii	5.2071 (13)
Ca1—V2^ix	4.0551 (10)	O2—O2^vii	5.2876 (15)
Ca1—V2^vii	4.0551 (10)	O2—O2^xiv	5.300 (4)
Ca1—O2	4.121 (2)	O2—O2^v	5.300 (4)
V1—O1	1.619 (3)	O2—O2^i	5.956 (2)
V1—O3^x	1.961 (2)	O3—V1^vii	1.961 (2)
V1—O3^xi	1.961 (2)	O3—V2^v	1.965 (2)
V1—O4^iii	1.9720 (19)	O3—V2^vii	1.973 (2)
V1—O4	1.9720 (19)	O3—Ca1^xiii	4.130 (2)
V1—V2^iii	2.9963 (9)	O3—Ca1^vii	4.305 (2)
V1—V2	2.9963 (9)	O3—Ca1^v	4.507 (2)
V1—Ca1^x	3.4235 (13)	O4—V2^v	1.960 (2)
V1—Ca1^xii	3.7591 (14)	O4—Ca1^xiii	4.366 (2)
V1—Ca1^xiii	4.3908 (14)	O4—Ca1^x	4.449 (2)
V1—Ca1^xiv	5.3501 (11)	O4—Ca1^xiv	4.517 (2)
V2—O2	1.614 (2)	O4—Ca1^ii	5.097 (2)
V2—O4^xiv	1.960 (2)
O2^i—Ca1—O2^ii	110.27 (11)	V2—V1—Ca1^x	78.034 (17)
O2^i—Ca1—O4	152.12 (7)	Ca1—V1—Ca1^x	102.39 (4)
O2^ii—Ca1—O4	87.84 (7)	O1—V1—Ca1^xii	31.90 (10)
O2^i—Ca1—O4^iii	87.84 (7)	O3^x—V1—Ca1^xii	86.42 (6)
O2^ii—Ca1—O4^iii	152.12 (7)	O3^xi—V1—Ca1^xii	86.42 (6)
O4—Ca1—O4^iii	68.33 (10)	O4^iii—V1—Ca1^xii	130.18 (6)
O2^i—Ca1—O3^iii	77.17 (7)	O4—V1—Ca1^xii	130.18 (6)
O2^ii—Ca1—O3^iii	133.34 (7)	V2^iii—V1—Ca1^xii	107.389 (17)
O4—Ca1—O3^iii	106.21 (8)	V2—V1—Ca1^xii	107.388 (17)
O4^iii—Ca1—O3^iii	69.96 (7)	Ca1—V1—Ca1^xii	164.24 (3)
O2^i—Ca1—O3	133.34 (7)	Ca1^x—V1—Ca1^xii	93.37 (3)
O2^ii—Ca1—O3	77.17 (7)	O1—V1—Ca1^xiii	48.60 (10)
O4—Ca1—O3	69.96 (7)	O3^x—V1—Ca1^xiii	134.87 (6)
O4^iii—Ca1—O3	106.21 (8)	O3^xi—V1—Ca1^xiii	134.87 (6)
O3^iii—Ca1—O3	67.23 (10)	O4^iii—V1—Ca1^xiii	76.29 (6)
O2^i—Ca1—O1^iv	78.61 (6)	O4—V1—Ca1^xiii	76.29 (6)
O2^ii—Ca1—O1^iv	78.61 (6)	V2^iii—V1—Ca1^xiii	103.701 (17)
O4—Ca1—O1^iv	84.76 (8)	V2—V1—Ca1^xiii	103.701 (17)
O4^iii—Ca1—O1^iv	84.76 (8)	Ca1—V1—Ca1^xiii	83.75 (3)
O3^iii—Ca1—O1^iv	145.35 (5)	Ca1^x—V1—Ca1^xiii	173.86 (3)
O3—Ca1—O1^iv	145.35 (5)	Ca1^xii—V1—Ca1^xiii	80.49 (3)
O2^i—Ca1—V1	117.65 (5)	O1—V1—Ca1^xiv	75.825 (13)
O2^ii—Ca1—V1	117.65 (5)	O3^x—V1—Ca1^xiv	54.59 (6)
O4—Ca1—V1	35.23 (5)	O3^xi—V1—Ca1^xiv	138.50 (6)
O4^iii—Ca1—V1	35.23 (5)	O4^iii—V1—Ca1^xiv	138.13 (6)
O3^iii—Ca1—V1	95.45 (6)	O4—V1—Ca1^xiv	54.97 (6)
O3—Ca1—V1	95.45 (6)	V2^iii—V1—Ca1^xiv	173.43 (3)
O1^iv—Ca1—V1	74.48 (7)	V2—V1—Ca1^xiv	34.922 (19)
O2^i—Ca1—V2^v	165.23 (6)	Ca1—V1—Ca1^xiv	99.241 (14)
O2^ii—Ca1—V2^v	78.66 (6)	Ca1^x—V1—Ca1^xiv	98.407 (14)
O4—Ca1—V2^v	34.90 (5)	Ca1^xii—V1—Ca1^xiv	78.183 (13)
O4^iii—Ca1—V2^v	88.64 (5)	Ca1^xiii—V1—Ca1^xiv	80.423 (13)
O3^iii—Ca1—V2^v	88.16 (6)	O2—V2—O4^xiv	108.80 (10)
O3—Ca1—V2^v	35.19 (5)	O2—V2—O3^xiv	105.94 (10)
O1^iv—Ca1—V2^v	115.33 (5)	O4^xiv—V2—O3^xiv	89.38 (9)
V1—Ca1—V2^v	64.81 (2)	O2—V2—O4	112.28 (10)
O2^i—Ca1—V2^vi	78.66 (6)	O4^xiv—V2—O4	138.87 (5)
O2^ii—Ca1—V2^vi	165.23 (6)	O3^xiv—V2—O4	81.52 (9)
O4—Ca1—V2^vi	88.64 (5)	O2—V2—O3^x	114.66 (10)
O4^iii—Ca1—V2^vi	34.90 (5)	O4^xiv—V2—O3^x	81.41 (9)
O3^iii—Ca1—V2^vi	35.19 (5)	O3^xiv—V2—O3^x	139.22 (4)
O3—Ca1—V2^vi	88.16 (6)	O4—V2—O3^x	79.96 (8)
O1^iv—Ca1—V2^vi	115.33 (5)	O2—V2—V2^v	114.10 (7)
V1—Ca1—V2^vi	64.82 (2)	O4^xiv—V2—V2^v	120.58 (7)
V2^v—Ca1—V2^vi	90.32 (3)	O3^xiv—V2—V2^v	40.97 (6)
O2^i—Ca1—V1^vii	103.09 (5)	O4—V2—V2^v	40.59 (6)
O2^ii—Ca1—V1^vii	103.09 (5)	O3^x—V2—V2^v	113.42 (7)
O4—Ca1—V1^vii	92.65 (6)	O2—V2—V2^xiv	120.67 (7)
O4^iii—Ca1—V1^vii	92.65 (6)	O4^xiv—V2—V2^xiv	40.68 (6)
O3^iii—Ca1—V1^vii	34.06 (5)	O3^xiv—V2—V2^xiv	118.36 (7)
O3—Ca1—V1^vii	34.06 (5)	O4—V2—V2^xiv	111.53 (6)
O1^iv—Ca1—V1^vii	176.87 (8)	O3^x—V2—V2^xiv	40.77 (6)
V1—Ca1—V1^vii	102.39 (4)	V2^v—V2—V2^xiv	125.23 (4)
V2^v—Ca1—V1^vii	62.75 (2)	O2—V2—V1	127.52 (9)
V2^vi—Ca1—V1^vii	62.75 (2)	O4^xiv—V2—V1	109.02 (6)
O2^i—Ca1—O1^viii	68.69 (5)	O3^xiv—V2—V1	109.50 (6)
O2^ii—Ca1—O1^viii	68.69 (5)	O4—V2—V1	40.52 (6)
O4—Ca1—O1^viii	139.11 (6)	O3^x—V2—V1	40.23 (6)
O4^iii—Ca1—O1^viii	139.11 (6)	V2^v—V2—V1	74.22 (3)
O3^iii—Ca1—O1^viii	72.36 (6)	V2^xiv—V2—V1	72.54 (2)
O3—Ca1—O1^viii	72.36 (6)	O2—V2—Ca1^xiv	118.05 (9)
O1^iv—Ca1—O1^viii	120.32 (11)	O4^xiv—V2—Ca1^xiv	44.20 (6)
V1—Ca1—O1^viii	165.21 (6)	O3^xiv—V2—Ca1^xiv	45.36 (6)
V2^v—Ca1—O1^viii	105.54 (4)	O4—V2—Ca1^xiv	113.33 (6)
V2^vi—Ca1—O1^viii	105.54 (4)	O3^x—V2—Ca1^xiv	112.62 (6)
V1^vii—Ca1—O1^viii	62.82 (6)	V2^v—V2—Ca1^xiv	79.25 (3)
O2^i—Ca1—V2^i	15.94 (6)	V2^xiv—V2—Ca1^xiv	76.56 (3)
O2^ii—Ca1—V2^i	95.03 (6)	V1—V2—Ca1^xiv	114.42 (3)
O4—Ca1—V2^i	153.38 (5)	O2—V2—Ca1^ii	23.44 (8)
O4^iii—Ca1—V2^i	100.13 (5)	O4^xiv—V2—Ca1^ii	95.13 (6)
O3^iii—Ca1—V2^i	90.98 (5)	O3^xiv—V2—Ca1^ii	87.18 (6)
O3—Ca1—V2^i	136.47 (6)	O4—V2—Ca1^ii	124.10 (6)
O1^iv—Ca1—V2^i	69.98 (5)	O3^x—V2—Ca1^ii	132.99 (6)
V1—Ca1—V2^i	124.87 (2)	V2^v—V2—Ca1^ii	108.53 (3)
V2^v—Ca1—V2^i	170.31 (2)	V2^xiv—V2—Ca1^ii	121.81 (3)
V2^vi—Ca1—V2^i	94.53 (2)	V1—V2—Ca1^ii	150.30 (3)
V1^vii—Ca1—V2^i	112.30 (2)	Ca1^xiv—V2—Ca1^ii	94.88 (2)
O1^viii—Ca1—V2^i	65.07 (4)	O2—V2—Ca1	84.81 (8)
O2^i—Ca1—V2^ii	95.03 (6)	O4^xiv—V2—Ca1	164.78 (6)
O2^ii—Ca1—V2^ii	15.94 (6)	O3^xiv—V2—Ca1	93.43 (6)
O4—Ca1—V2^ii	100.13 (5)	O4—V2—Ca1	27.88 (6)
O4^iii—Ca1—V2^ii	153.38 (5)	O3^x—V2—Ca1	86.75 (6)
O3^iii—Ca1—V2^ii	136.47 (6)	V2^v—V2—Ca1	56.13 (2)
O3—Ca1—V2^ii	90.98 (5)	V2^xiv—V2—Ca1	126.52 (3)
O1^iv—Ca1—V2^ii	69.98 (5)	V1—V2—Ca1	56.00 (2)
V1—Ca1—V2^ii	124.87 (2)	Ca1^xiv—V2—Ca1	135.37 (2)
V2^v—Ca1—V2^ii	94.53 (2)	Ca1^ii—V2—Ca1	99.95 (2)
V2^vi—Ca1—V2^ii	170.31 (2)	O2—V2—Ca1^x	89.25 (8)
V1^vii—Ca1—V2^ii	112.30 (2)	O4^xiv—V2—Ca1^x	90.41 (6)
O1^viii—Ca1—V2^ii	65.07 (4)	O3^xiv—V2—Ca1^x	164.01 (6)
V2^i—Ca1—V2^ii	79.49 (3)	O4—V2—Ca1^x	88.18 (6)
O2^i—Ca1—V1^iv	68.47 (5)	O3^x—V2—Ca1^x	25.44 (6)
O2^ii—Ca1—V1^iv	68.47 (5)	V2^v—V2—Ca1^x	128.05 (3)
O4—Ca1—V1^iv	101.06 (5)	V2^xiv—V2—Ca1^x	54.58 (2)
O4^iii—Ca1—V1^iv	101.06 (5)	V1—V2—Ca1^x	55.68 (2)
O3^iii—Ca1—V1^iv	144.90 (5)	Ca1^xiv—V2—Ca1^x	131.12 (2)
O3—Ca1—V1^iv	144.90 (5)	Ca1^ii—V2—Ca1^x	108.75 (2)
O1^iv—Ca1—V1^iv	19.73 (7)	Ca1—V2—Ca1^x	82.79 (2)
V1—Ca1—V1^iv	94.21 (3)	V1—O1—Ca1^xii	128.37 (14)
V2^v—Ca1—V1^iv	126.296 (19)	V1—O1—Ca1^xiii	111.32 (12)
V2^vi—Ca1—V1^iv	126.296 (19)	Ca1^xii—O1—Ca1^xiii	120.32 (11)
V1^vii—Ca1—V1^iv	163.40 (3)	V1—O1—Ca1^x	37.86 (8)
O1^viii—Ca1—V1^iv	100.58 (6)	Ca1^xii—O1—Ca1^x	90.51 (7)
V2^i—Ca1—V1^iv	56.31 (2)	Ca1^xiii—O1—Ca1^x	149.18 (9)
V2^ii—Ca1—V1^iv	56.31 (2)	V1—O1—Ca1	32.61 (7)
O2^i—Ca1—V2	146.01 (5)	Ca1^xii—O1—Ca1	160.98 (10)
O2^ii—Ca1—V2	70.25 (5)	Ca1^xiii—O1—Ca1	78.70 (5)
O4—Ca1—V2	22.61 (5)	Ca1^x—O1—Ca1	70.48 (5)
O4^iii—Ca1—V2	82.86 (5)	V2—O2—Ca1^ii	140.62 (13)
O3^iii—Ca1—V2	128.60 (6)	V2—O2—O2^ii	99.82 (12)
O3—Ca1—V2	80.59 (5)	Ca1^ii—O2—O2^ii	94.28 (10)
O1^iv—Ca1—V2	68.05 (5)	V2—O2—Ca1	72.22 (8)
V1—Ca1—V2	47.646 (15)	Ca1^ii—O2—Ca1	128.75 (7)
V2^v—Ca1—V2	47.308 (14)	O2^ii—O2—Ca1	34.47 (6)
V2^vi—Ca1—V2	109.30 (3)	V2—O2—Ca1^x	68.94 (7)
V1^vii—Ca1—V2	109.92 (3)	Ca1^ii—O2—Ca1^x	140.73 (7)
O1^viii—Ca1—V2	134.641 (15)	O2^ii—O2—Ca1^x	106.25 (10)
V2^i—Ca1—V2	137.45 (2)	Ca1—O2—Ca1^x	77.25 (5)
V2^ii—Ca1—V2	80.05 (2)	V2—O2—Ca1^xiv	42.88 (7)
V1^iv—Ca1—V2	81.32 (2)	Ca1^ii—O2—Ca1^xiv	98.07 (7)
O2^i—Ca1—V2^iii	70.25 (5)	O2^ii—O2—Ca1^xiv	116.53 (9)
O2^ii—Ca1—V2^iii	146.01 (5)	Ca1—O2—Ca1^xiv	105.64 (5)
O4—Ca1—V2^iii	82.86 (5)	Ca1^x—O2—Ca1^xiv	101.86 (4)
O4^iii—Ca1—V2^iii	22.61 (5)	V2—O2—O2^iv	163.15 (9)
O3^iii—Ca1—V2^iii	80.59 (5)	Ca1^ii—O2—O2^iv	56.18 (6)
O3—Ca1—V2^iii	128.60 (6)	O2^ii—O2—O2^iv	73.71 (8)
O1^iv—Ca1—V2^iii	68.05 (5)	Ca1—O2—O2^iv	95.54 (4)
V1—Ca1—V2^iii	47.646 (15)	Ca1^x—O2—O2^iv	97.51 (4)
V2^v—Ca1—V2^iii	109.30 (3)	Ca1^xiv—O2—O2^iv	153.89 (3)
V2^vi—Ca1—V2^iii	47.308 (14)	V2—O2—O2^xii	17.56 (8)
V1^vii—Ca1—V2^iii	109.92 (3)	Ca1^ii—O2—O2^xii	123.16 (6)
O1^viii—Ca1—V2^iii	134.641 (15)	O2^ii—O2—O2^xii	102.96 (9)
V2^i—Ca1—V2^iii	80.05 (2)	Ca1—O2—O2^xii	82.24 (4)
V2^ii—Ca1—V2^iii	137.45 (2)	Ca1^x—O2—O2^xii	84.90 (4)
V1^iv—Ca1—V2^iii	81.32 (2)	Ca1^xiv—O2—O2^xii	26.45 (3)
V2—Ca1—V2^iii	90.66 (3)	O2^iv—O2—O2^xii	176.31 (8)
O2^i—Ca1—V2^ix	58.55 (5)	V2—O2—O2^vii	93.29 (7)
O2^ii—Ca1—V2^ix	127.74 (5)	Ca1^ii—O2—O2^vii	81.47 (5)
O4—Ca1—V2^ix	126.53 (6)	O2^ii—O2—O2^vii	29.26 (8)
O4^iii—Ca1—V2^ix	79.58 (5)	Ca1—O2—O2^vii	53.27 (3)
O3^iii—Ca1—V2^ix	20.44 (5)	Ca1^x—O2—O2^vii	130.53 (3)
O3—Ca1—V2^ix	80.10 (5)	Ca1^xiv—O2—O2^vii	92.36 (3)
O1^iv—Ca1—V2^ix	134.55 (2)	O2^iv—O2—O2^vii	88.16 (4)
V1—Ca1—V2^ix	110.83 (3)	O2^xii—O2—O2^vii	88.16 (4)
V2^v—Ca1—V2^ix	106.70 (3)	V2—O2—O2^xiv	26.64 (7)
V2^vi—Ca1—V2^ix	46.168 (14)	Ca1^ii—O2—O2^xiv	137.75 (9)
V1^vii—Ca1—V2^ix	46.288 (15)	O2^ii—O2—O2^xiv	122.54 (11)
O1^viii—Ca1—V2^ix	59.71 (3)	Ca1—O2—O2^xiv	90.03 (6)
V2^i—Ca1—V2^ix	71.25 (2)	Ca1^x—O2—O2^xiv	52.65 (3)
V2^ii—Ca1—V2^ix	124.20 (2)	Ca1^xiv—O2—O2^xiv	49.33 (4)
V1^iv—Ca1—V2^ix	126.98 (2)	O2^iv—O2—O2^xiv	147.57 (5)
V2—Ca1—V2^ix	149.02 (3)	O2^xii—O2—O2^xiv	35.71 (5)
V2^iii—Ca1—V2^ix	82.79 (2)	O2^vii—O2—O2^xiv	119.92 (3)
O2^i—Ca1—V2^vii	127.74 (5)	V2—O2—O2^v	33.21 (7)
O2^ii—Ca1—V2^vii	58.55 (5)	Ca1^ii—O2—O2^v	126.31 (8)
O4—Ca1—V2^vii	79.58 (5)	O2^ii—O2—O2^v	70.58 (6)
O4^iii—Ca1—V2^vii	126.53 (6)	Ca1—O2—O2^v	53.40 (4)
O3^iii—Ca1—V2^vii	80.10 (5)	Ca1^x—O2—O2^v	92.39 (6)
O3—Ca1—V2^vii	20.44 (5)	Ca1^xiv—O2—O2^v	52.36 (4)
O1^iv—Ca1—V2^vii	134.55 (2)	O2^iv—O2—O2^v	144.29 (5)
V1—Ca1—V2^vii	110.83 (3)	O2^xii—O2—O2^v	32.43 (5)
V2^v—Ca1—V2^vii	46.168 (14)	O2^vii—O2—O2^v	60.08 (3)
V2^vi—Ca1—V2^vii	106.70 (3)	O2^xiv—O2—O2^v	59.85 (5)
V1^vii—Ca1—V2^vii	46.288 (15)	V2—O2—O2^i	84.62 (8)
O1^viii—Ca1—V2^vii	59.71 (3)	Ca1^ii—O2—O2^i	124.69 (9)
V2^i—Ca1—V2^vii	124.20 (2)	O2^ii—O2—O2^i	35.82 (8)
V2^ii—Ca1—V2^vii	71.25 (2)	Ca1—O2—O2^i	16.83 (2)
V1^iv—Ca1—V2^vii	126.98 (2)	Ca1^x—O2—O2^i	70.53 (3)
V2—Ca1—V2^vii	82.79 (2)	Ca1^xiv—O2—O2^i	121.68 (6)
V2^iii—Ca1—V2^vii	149.02 (3)	O2^iv—O2—O2^i	81.27 (4)
V2^ix—Ca1—V2^vii	87.42 (3)	O2^xii—O2—O2^i	96.97 (5)
O2^i—Ca1—O2	132.49 (4)	O2^vii—O2—O2^i	61.83 (3)
O2^ii—Ca1—O2	51.25 (7)	O2^xiv—O2—O2^i	97.30 (6)
O4—Ca1—O2	45.41 (6)	O2^v—O2—O2^i	69.88 (5)
O4^iii—Ca1—O2	100.88 (6)	V1^vii—O3—V2^v	128.40 (11)
O3^iii—Ca1—O2	149.68 (6)	V1^vii—O3—V2^vii	99.23 (9)
O3—Ca1—O2	89.15 (6)	V2^v—O3—V2^vii	98.25 (9)
O1^iv—Ca1—O2	56.27 (4)	V1^vii—O3—Ca1	102.07 (9)
V1—Ca1—O2	67.05 (3)	V2^v—O3—Ca1	99.45 (8)
V2^v—Ca1—O2	62.28 (3)	V2^vii—O3—Ca1	134.12 (10)
V2^vi—Ca1—O2	131.26 (4)	V1^vii—O3—Ca1^xiii	65.29 (6)
V1^vii—Ca1—O2	122.73 (3)	V2^v—O3—Ca1^xiii	64.44 (6)
O1^viii—Ca1—O2	119.77 (4)	V2^vii—O3—Ca1^xiii	123.08 (8)
V2^i—Ca1—O2	119.31 (4)	Ca1—O3—Ca1^xiii	102.74 (6)
V2^ii—Ca1—O2	58.36 (3)	V1^vii—O3—Ca1^vii	48.99 (5)
V1^iv—Ca1—O2	64.02 (3)	V2^v—O3—Ca1^vii	160.61 (9)
V2—Ca1—O2	22.97 (3)	V2^vii—O3—Ca1^vii	66.03 (5)
V2^iii—Ca1—O2	101.96 (4)	Ca1—O3—Ca1^vii	99.75 (7)
V2^ix—Ca1—O2	168.86 (4)	Ca1^xiii—O3—Ca1^vii	113.47 (5)
V2^vii—Ca1—O2	83.41 (4)	V1^vii—O3—Ca1^v	104.65 (7)
O1—V1—O3^x	109.30 (9)	V2^v—O3—Ca1^v	60.77 (6)
O1—V1—O3^xi	109.30 (9)	V2^vii—O3—Ca1^v	43.54 (5)
O3^x—V1—O3^xi	86.49 (12)	Ca1—O3—Ca1^v	153.08 (7)
O1—V1—O4^iii	111.32 (9)	Ca1^xiii—O3—Ca1^v	85.61 (4)
O3^x—V1—O4^iii	139.37 (10)	Ca1^vii—O3—Ca1^v	100.17 (4)
O3^xi—V1—O4^iii	80.05 (8)	V2^v—O4—V2	98.73 (9)
O1—V1—O4	111.32 (9)	V2^v—O4—V1	132.88 (11)
O3^x—V1—O4	80.05 (8)	V2—O4—V1	99.16 (8)
O3^xi—V1—O4	139.37 (10)	V2^v—O4—Ca1	100.90 (8)
O4^iii—V1—O4	85.69 (12)	V2—O4—Ca1	129.51 (10)
O1—V1—V2^iii	110.743 (18)	V1—O4—Ca1	100.45 (9)
O3^x—V1—V2^iii	121.42 (7)	V2^v—O4—Ca1^xiii	58.32 (5)
O3^xi—V1—V2^iii	40.53 (6)	V2—O4—Ca1^xiii	132.44 (8)
O4^iii—V1—V2^iii	40.31 (6)	V1—O4—Ca1^xiii	77.69 (6)
O4—V1—V2^iii	120.62 (7)	Ca1—O4—Ca1^xiii	97.16 (6)
O1—V1—V2	110.743 (18)	V2^v—O4—Ca1^x	161.71 (8)
O3^x—V1—V2	40.53 (6)	V2—O4—Ca1^x	65.65 (5)
O3^xi—V1—V2	121.42 (7)	V1—O4—Ca1^x	47.02 (5)
O4^iii—V1—V2	120.62 (7)	Ca1—O4—Ca1^x	96.66 (6)
O4—V1—V2	40.31 (6)	Ca1^xiii—O4—Ca1^x	124.55 (5)
V2^iii—V1—V2	138.51 (4)	V2^v—O4—Ca1^xiv	63.87 (6)
O1—V1—Ca1	132.34 (10)	V2—O4—Ca1^xiv	43.14 (5)
O3^x—V1—Ca1	104.90 (6)	V1—O4—Ca1^xiv	104.08 (7)
O3^xi—V1—Ca1	104.90 (6)	Ca1—O4—Ca1^xiv	155.29 (7)
O4^iii—V1—Ca1	44.32 (6)	Ca1^xiii—O4—Ca1^xiv	90.91 (4)
O4—V1—Ca1	44.32 (6)	Ca1^x—O4—Ca1^xiv	97.87 (4)
V2^iii—V1—Ca1	76.351 (17)	V2^v—O4—Ca1^ii	90.05 (7)
V2—V1—Ca1	76.351 (17)	V2—O4—Ca1^ii	37.30 (4)
O1—V1—Ca1^x	125.27 (10)	V1—O4—Ca1^ii	128.22 (7)
O3^x—V1—Ca1^x	43.87 (6)	Ca1—O4—Ca1^ii	96.68 (6)
O3^xi—V1—Ca1^x	43.87 (6)	Ca1^xiii—O4—Ca1^ii	147.34 (5)
O4^iii—V1—Ca1^x	108.05 (6)	Ca1^x—O4—Ca1^ii	82.79 (3)
O4—V1—Ca1^x	108.05 (6)	Ca1^xiv—O4—Ca1^ii	65.60 (3)
V2^iii—V1—Ca1^x	78.034 (17)

Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, −y+1, −z+1; (iii) x, −y+1/2, z; (iv) x−1/2, y, −z+3/2; (v) −x+1/2, −y+1, z−1/2; (vi) −x+1/2, y−1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, y, −z+1/2; (ix) x, −y+1/2, z−1; (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.