Superlattice formation in the lithiated vanadium oxide phases Li_0.67V₆O₁₃ and LiV₆O₁₃

Two new lithiated phases of V₆O₁₃ were formed by carefully tuning the temperature of electrochemical lithiation in a `coffee-bag' type Li-ion battery at 2.78 V versus Li/Li⁺. These were studied by single-crystal X-ray diffraction. A phase with the composition Li_2/3V₆O₁₃ was obtained at 308 K with a unit cell three times the volume of the original V₆O₁₃ cell. A single crystal discharged at ambient temperature was shown to be LiV₆O₁₃ and twice the unit-cell volume of the original V₆O₁₃ cell. On lithiation, the structures retain their basic V₆O₁₃ structure of alternating single and double layers of VO₆ octahedra. The lithium ions occupy chemically equivalent sites, where they coordinate fivefold to O atoms, and associate with the single layers of VO₆ octahedra. The insertion of lithium causes a significant elongation of one of the V-O bonds in each structure, which expands from 1.65 to 1.89 Å; this is due to the charge reduction of a specific V atom.

Computing details

Data reduction: STOEDATR for LiV6O13. Program(s) used to solve structure: MULTAN80 for LiV6O13. Program(s) used to refine structure: DUPALS for LiV6O13. Molecular graphics: ORTEP-II for LiV6O13. Software used to prepare material for publication: DISTAN for LiV6O13.

Figures

(Li067V6O13)

Crystal data

Li0.67V6O13	F(000) = 1464
Mr = 518.29	Dx = 3.861 Mg m^−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
a = 21.848 (2) Å	Cell parameters from 3403 reflections
b = 3.6904 (3) Å	θ = 2.5–28°
c = 17.245 (2) Å	µ = 6.09 mm^−1
β = 105.01 (1)°	T = 293 K
V = 1343.0 (2) Å^3	Needle, black
Z = 6	0.2 × 0.1 × 0.1 mm

Data collection

STOE IPDS diffractometer	1150 reflections with Inet > −15.0σ(Inet)
ω scan	Rint = 0.056
Absorption correction: numerical Jana'98 (Petricek & Dusek, 1997)	θmax = 28°, θmin = 2.5°
Tmin = 0.270, Tmax = 0.444	h = −28→28
3403 measured reflections	k = −4→4
1197 independent reflections	l = −21→22

Refinement

Refinement on F^2	179 parameters
R[F^2 > 2σ(F^2)] = 0.036	Weighting scheme based on measured s.u.'s w = 1/(σ^2(I) + (0.01I)^2)
wR(F^2) = 0.084	(Δ/σ)max = 0.001
S = 3.78	Δρmax = 0.78 e Å^−3
1197 reflections	Δρmin = −0.98 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
V11	0.12135 (3)	0	0.23855 (4)	0.0063 (2)
V12	0.44842 (3)	0	−0.09924 (4)	0.0084 (2)
V13	0.79923 (3)	0	0.54822 (3)	0.0061 (2)
V21	0.25918 (3)	0	0.15174 (4)	0.0050 (2)
V22	0.58889 (3)	0	−0.17546 (4)	0.0049 (2)
V23	0.94004 (3)	0	0.47324 (4)	0.0108 (2)
V31	0.36205 (3)	0	0.34553 (4)	0.0065 (2)
V32	0.69178 (3)	0	0.02124 (4)	0.0053 (2)
V33	0.02271 (3)	0	0.69348 (4)	0.0051 (2)
O11	0.38940 (14)	0	−0.2145 (2)	0.0072 (16)
O12	0.0625 (2)	0	0.1202 (3)	0.0121 (15)
O13	0.7298 (2)	0	0.4499 (2)	0.0069 (13)
O21	0.4251 (2)	0	0.4574 (3)	0.0051 (13)
O22	1.0865 (2)	0	0.7966 (2)	0.0051 (11)
O23	0.7577 (2)	0	0.1254 (2)	0.0054 (12)
O31	0.5485 (2)	0	−0.2998 (2)	0.0059 (12)
O32	0.2182 (2)	0	0.0309 (3)	0.0063 (14)
O33	0.8861 (2)	0	0.3553 (3)	0.0071 (12)
O41	0.5	0	0	0.015 (2)
O42	0.82961 (19)	0	0.6653 (2)	0.0081 (16)
O51	0.52580 (15)	0	−0.13944 (18)	0.0103 (10)
O52	0.20042 (15)	0	0.19700 (18)	0.0109 (10)
O53	0.86374 (16)	0	0.5180 (2)	0.0140 (11)
O61	0.62703 (16)	0	0.05310 (18)	0.0106 (10)
O62	0.29444 (16)	0	0.3696 (2)	0.0132 (10)
O63	0.95526 (15)	0	0.71941 (18)	0.0111 (10)
O71	0.6539 (2)	0	−0.0908 (3)	0.0065 (13)
O72	0.3280 (2)	0	0.2331 (2)	0.0080 (12)
O73	1.0085 (2)	0	0.4234 (3)	0.0065 (12)
Li1	0.7379 (6)	0	0.3396 (6)	0.036 (4)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V11	0.0096 (3)	0.0042 (4)	0.0049 (3)	0	0.0002 (2)	0
V12	0.0115 (3)	0.0055 (4)	0.0080 (3)	0	0.0030 (2)	0
V13	0.0095 (3)	0.0034 (3)	0.0052 (3)	0	0.0008 (2)	0
V21	0.0084 (3)	0.0038 (3)	0.0036 (3)	0	0.0014 (2)	0
V22	0.0085 (3)	0.0035 (3)	0.0037 (3)	0	0.0015 (2)	0
V23	0.0095 (3)	0.0205 (4)	0.0033 (3)	0	0.0000 (2)	0
V31	0.0088 (3)	0.0036 (3)	0.0062 (3)	0	0.0010 (2)	0
V32	0.0081 (3)	0.0037 (3)	0.0045 (3)	0	0.0017 (2)	0
V33	0.0073 (3)	0.0038 (3)	0.0041 (3)	0	0.0009 (2)	0
O11	0.006 (2)	0.007 (2)	0.006 (2)	0	−0.0004 (17)	0
O12	0.022 (2)	0.006 (2)	0.012 (2)	0	0.0071 (15)	0
O13	0.0127 (17)	0.004 (2)	0.0046 (18)	0	0.0000 (13)	0
O21	0.0056 (18)	0.0049 (18)	0.0031 (19)	0	−0.0025 (13)	0
O22	0.011 (2)	0.0030 (16)	0.0027 (15)	0	−0.0009 (13)	0
O23	0.010 (2)	0.0036 (17)	0.0030 (17)	0	−0.0012 (13)	0
O31	0.0122 (18)	0.0030 (16)	0.0040 (18)	0	0.0009 (14)	0
O32	0.015 (2)	0.0024 (19)	0.004 (2)	0	0.0021 (16)	0
O33	0.022 (2)	0.0028 (17)	0.0026 (16)	0	0.0013 (16)	0
O41	0.017 (3)	0.025 (4)	0.007 (2)	0	0.004 (2)	0
O42	0.008 (2)	0.013 (3)	0.003 (2)	0	−0.0006 (16)	0
O51	0.0126 (15)	0.0083 (16)	0.0101 (14)	0	0.0057 (11)	0
O52	0.0103 (14)	0.0116 (17)	0.0096 (13)	0	0.0040 (11)	0
O53	0.0118 (14)	0.0150 (18)	0.0122 (14)	0	0.0034 (11)	0
O61	0.0097 (15)	0.0128 (17)	0.0085 (13)	0	0.0040 (11)	0
O62	0.0158 (15)	0.0126 (16)	0.0109 (14)	0	0.0042 (12)	0
O63	0.0097 (14)	0.0097 (16)	0.0112 (14)	0	0.0042 (11)	0
O71	0.0119 (18)	0.004 (2)	0.0041 (18)	0	−0.0004 (13)	0
O72	0.0145 (19)	0.0063 (17)	0.0044 (17)	0	−0.0007 (14)	0
O73	0.0078 (17)	0.007 (2)	0.0039 (16)	0	−0.0008 (12)	0
Li1	0.066 (8)	0.036 (6)	0.025 (5)	0	0.026 (4)	0

Geometric parameters (Å, º)

V11—O11^i	1.8923 (8)	O13—O13^vi	2.525 (3)
V11—O11^ii	1.8923 (8)	O13—O42^v	2.775 (3)
V11—O12	2.112 (4)	O13—O42^vi	2.775 (3)
V11—O42^iii	1.726 (3)	O13—O53	2.857 (6)
V11—O52	2.034 (3)	O13—O53^v	2.910 (5)
V11—O63^iii	1.989 (3)	O13—O53^vi	2.910 (5)
V12—O11	2.071 (3)	O13—O62^xiv	2.887 (5)
V12—O12^i	1.8835 (10)	O13—O62^xv	2.887 (5)
V12—O12^ii	1.8835 (10)	O13—Li1	1.956 (12)
V12—O41	1.7888 (6)	O21—O31^iv	2.922 (7)
V12—O51	1.986 (3)	O21—O33^vii	2.540 (4)
V12—O61^iv	2.008 (3)	O21—O33^viii	2.540 (4)
V13—V13^v	2.9910 (7)	O21—O53^vii	2.649 (5)
V13—V13^vi	2.9910 (7)	O21—O53^viii	2.649 (5)
V13—O13	1.960 (4)	O21—O62	2.863 (5)
V13—O13^v	1.9540 (18)	O21—O73^vii	2.762 (6)
V13—O13^vi	1.9540 (18)	O21—O73^viii	2.762 (6)
V13—O42	1.955 (3)	O21—O73^v	2.862 (5)
V13—O53	1.624 (4)	O21—O73^vi	2.862 (5)
V13—O62^iii	2.775 (4)	O22—O31^xix	2.478 (3)
V13—Li1^v	2.935 (9)	O22—O31^xx	2.478 (3)
V13—Li1^vi	2.935 (9)	O22—O33^xiii	2.834 (7)
V21—V32^vii	2.9869 (7)	O22—O51^xix	2.672 (4)
V21—V32^viii	2.9869 (7)	O22—O51^xx	2.672 (4)
V21—O23^vii	1.8985 (12)	O22—O63	2.832 (5)
V21—O23^viii	1.8985 (12)	O22—O71^xix	2.804 (4)
V21—O32	2.044 (4)	O22—O71^xx	2.804 (4)
V21—O52	1.666 (3)	O22—O72^v	2.766 (5)
V21—O71^iv	2.396 (6)	O22—O72^vi	2.766 (5)
V21—O72	1.770 (4)	O23—O32^xiv	2.465 (4)
V22—V33^ix	2.9851 (7)	O23—O32^xv	2.465 (4)
V22—V33^x	2.9851 (7)	O23—O32^iv	2.877 (7)
V22—O22^xi	1.9044 (11)	O23—O52^xiv	2.701 (4)
V22—O22^xii	1.9044 (11)	O23—O52^xv	2.701 (4)
V22—O31	2.096 (4)	O23—O61	2.803 (5)
V22—O51	1.652 (3)	O23—O71^xxi	2.844 (6)
V22—O71	1.754 (5)	O23—O71^xxii	2.844 (6)
V22—O72^iv	2.284 (5)	O23—O72^xiv	2.781 (4)
V23—V23^xiii	2.5425 (11)	O23—O72^xv	2.781 (4)
V23—O21^xiv	1.8815 (9)	O31—O33^xxi	2.659 (6)
V23—O21^xv	1.8815 (9)	O31—O33^xxii	2.659 (6)
V23—O33	2.069 (4)	O31—O51	2.932 (6)
V23—O53	2.011 (4)	O31—O63^xi	2.830 (4)
V23—O73	1.909 (6)	O31—O63^xii	2.830 (4)
V23—O73^xiii	1.845 (5)	O31—O72^iv	2.645 (6)
V31—O21	2.060 (4)	O31—O73^xxi	2.851 (5)
V31—O31^iv	2.290 (5)	O31—O73^xxii	2.851 (5)
V31—O33^vii	1.9142 (15)	O32—O32^i	2.690 (6)
V31—O33^viii	1.9142 (15)	O32—O32^ii	2.690 (6)
V31—O62	1.635 (3)	O32—O52	2.989 (6)
V31—O72	1.889 (4)	O32—O61^vii	2.813 (5)
V32—O23	1.990 (4)	O32—O61^viii	2.813 (5)
V32—O32^xiv	1.9278 (17)	O32—O71^vii	2.873 (5)
V32—O32^xv	1.9278 (17)	O32—O71^viii	2.873 (5)
V32—O32^iv	2.364 (6)	O32—O71^iv	2.716 (7)
V32—O61	1.645 (3)	O33—O53	2.970 (6)
V32—O71	1.895 (5)	O33—O62^xiv	2.781 (5)
V33—O22^xvi	1.955 (3)	O33—O62^xv	2.781 (5)
V33—O31^xvii	1.9240 (15)	O33—O72^xiv	2.842 (4)
V33—O31^xviii	1.9240 (15)	O33—O72^xv	2.842 (4)
V33—O33^iii	2.355 (6)	O33—O73	2.627 (7)
V33—O63^xvi	1.647 (3)	O41—O51	2.608 (3)
V33—O73^iii	1.953 (5)	O41—O51^iv	2.608 (3)
O11—O12^i	2.504 (4)	O41—O61	2.688 (3)
O11—O12^ii	2.504 (4)	O41—O61^iv	2.688 (3)
O11—O42^xi	2.829 (3)	O42—O52^iii	2.623 (5)
O11—O42^xii	2.829 (3)	O42—O53	2.825 (5)
O11—O51	2.925 (4)	O42—O62^iii	2.620 (5)
O11—O52^i	2.767 (3)	O42—O63	2.661 (5)
O11—O52^ii	2.767 (3)	O42—Li1^v	2.350 (9)
O11—O61^iv	2.898 (5)	O42—Li1^vi	2.350 (9)
O11—O63^xi	2.761 (4)	O51—O71	2.706 (6)
O11—O63^xii	2.761 (4)	O52—O72	2.694 (5)
O12—O41^vii	2.846 (3)	O53—O73^xiii	2.711 (6)
O12—O41^viii	2.846 (3)	O61—O71	2.694 (7)
O12—O51^i	2.751 (5)	O62—O72	2.642 (6)
O12—O51^ii	2.751 (5)	O62—Li1^vii	2.206 (7)
O12—O52	2.961 (6)	O62—Li1^viii	2.206 (7)
O12—O61^vii	2.753 (5)	O63—O73^xiii	2.775 (7)
O12—O61^viii	2.753 (5)	O71—O72^iv	2.583 (8)
O12—O63^iii	2.891 (6)	O73—O73^xiii	2.762 (8)
O13—O13^v	2.525 (3)
O11^i—V11—O11^ii	154.37 (16)	O13^vi—O13—O13^v	93.90 (16)
O11^i—V11—O12	77.21 (11)	O13^vi—O13—O42^v	172.5 (2)
O11^i—V11—O42^iii	102.78 (11)	O13^vi—O13—O42^vi	91.12 (8)
O11^i—V11—O52	89.52 (12)	O13^vi—O13—O53	65.12 (15)
O11^i—V11—O63^iii	90.65 (12)	O13^vi—O13—O53^v	118.2 (2)
O11^ii—V11—O11^i	154.37 (16)	O13^vi—O13—O53^vi	62.96 (14)
O11^ii—V11—O12	77.21 (11)	O13^vi—O13—O62^xiv	131.9 (2)
O11^ii—V11—O42^iii	102.78 (11)	O13^vi—O13—O62^xv	74.52 (14)
O11^ii—V11—O52	89.52 (12)	O13^vi—O13—Li1	124.1 (2)
O11^ii—V11—O63^iii	90.65 (12)	O42^v—O13—O42^vi	83.35 (13)
O12—V11—O42^iii	179.2 (2)	O42^v—O13—O53	122.25 (17)
O12—V11—O52	91.14 (19)	O42^v—O13—O53^v	59.54 (12)
O12—V11—O63^iii	89.6 (2)	O42^v—O13—O53^vi	109.65 (19)
O42^iii—V11—O52	88.05 (17)	O42^v—O13—O62^xiv	55.08 (12)
O42^iii—V11—O63^iii	91.21 (17)	O42^v—O13—O62^xv	106.12 (18)
O52—V11—O63^iii	179.27 (12)	O42^v—O13—Li1	56.4 (2)
O11—V12—O12^i	78.42 (14)	O42^vi—O13—O42^v	83.35 (13)
O11—V12—O12^ii	78.42 (14)	O42^vi—O13—O53	122.25 (17)
O11—V12—O41	179.50 (12)	O42^vi—O13—O53^v	109.65 (19)
O11—V12—O51	92.27 (14)	O42^vi—O13—O53^vi	59.54 (12)
O11—V12—O61^iv	90.54 (14)	O42^vi—O13—O62^xiv	106.12 (18)
O12^i—V12—O12^ii	156.8 (2)	O42^vi—O13—O62^xv	55.08 (12)
O12^i—V12—O41	101.58 (14)	O42^vi—O13—Li1	56.4 (2)
O12^i—V12—O51	90.6 (2)	O53—O13—O53^v	128.08 (12)
O12^i—V12—O61^iv	90.0 (2)	O53—O13—O53^vi	128.08 (12)
O12^ii—V12—O12^i	156.8 (2)	O53—O13—O62^xiv	67.72 (14)
O12^ii—V12—O41	101.58 (14)	O53—O13—O62^xv	67.72 (14)
O12^ii—V12—O51	90.6 (2)	O53—O13—Li1	93.4 (4)
O12^ii—V12—O61^iv	90.0 (2)	O53^v—O13—O53	128.08 (12)
O41—V12—O51	87.23 (9)	O53^v—O13—O53^vi	78.70 (16)
O41—V12—O61^iv	89.96 (9)	O53^v—O13—O62^xiv	98.09 (8)
O51—V12—O61^iv	177.19 (12)	O53^v—O13—O62^xv	162.03 (18)
V13^v—V13—V13^vi	76.18 (2)	O53^v—O13—Li1	115.4 (3)
V13^v—V13—O13	40.09 (5)	O53^vi—O13—O53	128.08 (12)
V13^v—V13—O13^v	40.25 (12)	O53^vi—O13—O53^v	78.70 (16)
V13^v—V13—O13^vi	113.70 (13)	O53^vi—O13—O62^xiv	162.03 (18)
V13^v—V13—O42	125.25 (9)	O53^vi—O13—O62^xv	98.09 (8)
V13^v—V13—O53	112.38 (9)	O53^vi—O13—Li1	115.4 (3)
V13^v—V13—O62^iii	76.38 (5)	O62^xiv—O13—O62^xv	79.47 (15)
V13^v—V13—Li1^v	72.36 (18)	O62^xiv—O13—Li1	49.8 (2)
V13^v—V13—Li1^vi	118.2 (2)	O62^xv—O13—O62^xiv	79.47 (15)
V13^vi—V13—V13^v	76.18 (2)	O62^xv—O13—Li1	49.8 (2)
V13^vi—V13—O13	40.09 (5)	O31^iv—O21—O33^vii	57.76 (17)
V13^vi—V13—O13^v	113.70 (13)	O31^iv—O21—O33^viii	57.76 (17)
V13^vi—V13—O13^vi	40.25 (12)	O31^iv—O21—O53^vii	127.53 (14)
V13^vi—V13—O42	125.25 (9)	O31^iv—O21—O53^viii	127.53 (14)
V13^vi—V13—O53	112.38 (9)	O31^iv—O21—O62	85.30 (18)
V13^vi—V13—O62^iii	76.38 (5)	O31^iv—O21—O73^vii	60.12 (17)
V13^vi—V13—Li1^v	118.2 (2)	O31^iv—O21—O73^viii	60.12 (17)
V13^vi—V13—Li1^vi	72.36 (18)	O31^iv—O21—O73^v	118.9 (2)
O13—V13—O13^v	80.34 (13)	O31^iv—O21—O73^vi	118.9 (2)
O13—V13—O13^vi	80.34 (13)	O33^vii—O21—O33^viii	93.17 (19)
O13—V13—O42	150.8 (2)	O33^vii—O21—O53^vii	69.80 (15)
O13—V13—O53	105.3 (2)	O33^vii—O21—O53^viii	131.8 (2)
O13—V13—O62^iii	86.18 (17)	O33^vii—O21—O62	61.60 (16)
O13—V13—Li1^v	106.6 (2)	O33^vii—O21—O73^vii	59.23 (17)
O13—V13—Li1^vi	106.6 (2)	O33^vii—O21—O73^viii	117.3 (2)
O13^v—V13—O13	80.34 (13)	O33^vii—O21—O73^v	92.63 (10)
O13^v—V13—O13^vi	141.6 (2)	O33^vii—O21—O73^vi	169.3 (2)
O13^v—V13—O42	90.46 (13)	O33^viii—O21—O33^vii	93.17 (19)
O13^v—V13—O53	108.50 (16)	O33^viii—O21—O53^vii	131.8 (2)
O13^v—V13—O62^iii	72.92 (16)	O33^viii—O21—O53^viii	69.80 (15)
O13^v—V13—Li1^v	41.37 (19)	O33^viii—O21—O62	61.60 (16)
O13^v—V13—Li1^vi	115.9 (2)	O33^viii—O21—O73^vii	117.3 (2)
O13^vi—V13—O13	80.34 (13)	O33^viii—O21—O73^viii	59.23 (17)
O13^vi—V13—O13^v	141.6 (2)	O33^viii—O21—O73^v	169.3 (2)
O13^vi—V13—O42	90.46 (13)	O33^viii—O21—O73^vi	92.63 (10)
O13^vi—V13—O53	108.50 (16)	O53^vii—O21—O53^viii	88.3 (2)
O13^vi—V13—O62^iii	72.92 (16)	O53^vii—O21—O62	70.86 (14)
O13^vi—V13—Li1^v	115.9 (2)	O53^vii—O21—O73^vii	92.73 (11)
O13^vi—V13—Li1^vi	41.37 (19)	O53^vii—O21—O73^viii	168.1 (2)
O42—V13—O53	103.90 (17)	O53^vii—O21—O73^v	58.78 (15)
O42—V13—O62^iii	64.58 (14)	O53^vii—O21—O73^vi	112.3 (2)
O42—V13—Li1^v	52.95 (19)	O53^viii—O21—O53^vii	88.3 (2)
O42—V13—Li1^vi	52.95 (19)	O53^viii—O21—O62	70.86 (14)
O53—V13—O62^iii	168.48 (13)	O53^viii—O21—O73^vii	168.1 (2)
O53—V13—Li1^v	128.5 (2)	O53^viii—O21—O73^viii	92.73 (11)
O53—V13—Li1^vi	128.5 (2)	O53^viii—O21—O73^v	112.3 (2)
O62^iii—V13—Li1^v	45.4 (2)	O53^viii—O21—O73^vi	58.78 (15)
O62^iii—V13—Li1^vi	45.4 (2)	O62—O21—O73^vii	120.66 (17)
Li1^v—V13—Li1^vi	77.9 (2)	O62—O21—O73^viii	120.66 (17)
Li1^vi—V13—Li1^v	77.9 (2)	O62—O21—O73^v	129.08 (18)
V32^vii—V21—V32^viii	76.31 (2)	O62—O21—O73^vi	129.08 (18)
V32^vii—V21—O23^vii	40.96 (13)	O73^vii—O21—O73^viii	83.8 (2)
V32^vii—V21—O23^viii	116.47 (13)	O73^vii—O21—O73^v	58.80 (17)
V32^vii—V21—O32	39.79 (5)	O73^vii—O21—O73^vi	110.1 (2)
V32^vii—V21—O52	93.64 (8)	O73^viii—O21—O73^vii	83.8 (2)
V32^vii—V21—O71^iv	87.80 (10)	O73^viii—O21—O73^v	110.1 (2)
V32^vii—V21—O72	138.47 (6)	O73^viii—O21—O73^vi	58.80 (17)
V32^viii—V21—V32^vii	76.31 (2)	O73^v—O21—O73^vii	58.80 (17)
V32^viii—V21—O23^vii	116.47 (13)	O73^v—O21—O73^viii	110.1 (2)
V32^viii—V21—O23^viii	40.96 (13)	O73^v—O21—O73^vi	80.29 (15)
V32^viii—V21—O32	39.79 (5)	O73^vi—O21—O73^vii	110.1 (2)
V32^viii—V21—O52	93.64 (8)	O73^vi—O21—O73^viii	58.80 (17)
V32^viii—V21—O71^iv	87.80 (10)	O73^vi—O21—O73^v	80.29 (15)
V32^viii—V21—O72	138.47 (6)	O31^xix—O22—O31^xx	96.25 (17)
O23^vii—V21—O23^viii	152.8 (2)	O31^xix—O22—O33^xiii	59.64 (16)
O23^vii—V21—O32	77.31 (13)	O31^xix—O22—O51^xix	69.30 (14)
O23^vii—V21—O52	98.30 (17)	O31^xix—O22—O51^xx	132.5 (2)
O23^vii—V21—O71^iv	82.05 (17)	O31^xix—O22—O63	64.02 (14)
O23^vii—V21—O72	98.50 (13)	O31^xix—O22—O71^xix	89.95 (11)
O23^viii—V21—O23^vii	152.8 (2)	O31^xix—O22—O71^xx	168.3 (2)
O23^viii—V21—O32	77.31 (13)	O31^xix—O22—O72^v	60.29 (15)
O23^viii—V21—O52	98.30 (17)	O31^xix—O22—O72^vi	119.9 (2)
O23^viii—V21—O71^iv	82.05 (17)	O31^xx—O22—O31^xix	96.25 (17)
O23^viii—V21—O72	98.50 (13)	O31^xx—O22—O33^xiii	59.64 (16)
O32—V21—O52	106.9 (2)	O31^xx—O22—O51^xix	132.5 (2)
O32—V21—O71^iv	74.9 (2)	O31^xx—O22—O51^xx	69.30 (14)
O32—V21—O72	149.9 (2)	O31^xx—O22—O63	64.02 (14)
O52—V21—O71^iv	178.16 (16)	O31^xx—O22—O71^xix	168.3 (2)
O52—V21—O72	103.2 (2)	O31^xx—O22—O71^xx	89.95 (11)
O71^iv—V21—O72	75.0 (2)	O31^xx—O22—O72^v	119.9 (2)
V33^ix—V22—V33^x	76.36 (2)	O31^xx—O22—O72^vi	60.29 (15)
V33^ix—V22—O22^xi	39.95 (11)	O33^xiii—O22—O51^xix	128.89 (12)
V33^ix—V22—O22^xii	115.54 (12)	O33^xiii—O22—O51^xx	128.89 (12)
V33^ix—V22—O31	39.88 (4)	O33^xiii—O22—O63	89.76 (17)
V33^ix—V22—O51	89.83 (8)	O33^xiii—O22—O71^xix	116.2 (2)
V33^ix—V22—O71	139.41 (7)	O33^xiii—O22—O71^xx	116.2 (2)
V33^ix—V22—O72^iv	87.39 (8)	O33^xiii—O22—O72^v	60.99 (15)
V33^x—V22—V33^ix	76.36 (2)	O33^xiii—O22—O72^vi	60.99 (15)
V33^x—V22—O22^xi	115.54 (12)	O51^xix—O22—O51^xx	87.35 (17)
V33^x—V22—O22^xii	39.95 (11)	O51^xix—O22—O63	69.11 (12)
V33^x—V22—O31	39.88 (4)	O51^xix—O22—O71^xix	59.17 (14)
V33^x—V22—O51	89.83 (8)	O51^xix—O22—O71^xx	113.3 (2)
V33^x—V22—O71	139.41 (7)	O51^xix—O22—O72^v	92.68 (10)
V33^x—V22—O72^iv	87.39 (8)	O51^xix—O22—O72^vi	165.53 (19)
O22^xi—V22—O22^xii	151.34 (19)	O51^xx—O22—O51^xix	87.35 (17)
O22^xi—V22—O31	76.38 (12)	O51^xx—O22—O63	69.11 (12)
O22^xi—V22—O51	97.15 (15)	O51^xx—O22—O71^xix	113.3 (2)
O22^xi—V22—O71	100.01 (12)	O51^xx—O22—O71^xx	59.17 (14)
O22^xi—V22—O72^iv	82.10 (15)	O51^xx—O22—O72^v	165.53 (19)
O22^xii—V22—O22^xi	151.34 (19)	O51^xx—O22—O72^vi	92.68 (10)
O22^xii—V22—O31	76.38 (12)	O63—O22—O71^xix	127.72 (16)
O22^xii—V22—O51	97.15 (15)	O63—O22—O71^xx	127.72 (16)
O22^xii—V22—O71	100.01 (12)	O63—O22—O72^v	124.29 (13)
O22^xii—V22—O72^iv	82.10 (15)	O63—O22—O72^vi	124.29 (13)
O31—V22—O51	102.31 (18)	O71^xix—O22—O71^xx	82.30 (14)
O31—V22—O71	152.5 (2)	O71^xix—O22—O72^v	55.27 (16)
O31—V22—O72^iv	74.16 (18)	O71^xix—O22—O72^vi	107.96 (19)
O51—V22—O71	105.2 (2)	O71^xx—O22—O71^xix	82.30 (14)
O51—V22—O72^iv	176.46 (15)	O71^xx—O22—O72^v	107.96 (19)
O71—V22—O72^iv	78.3 (2)	O71^xx—O22—O72^vi	55.27 (16)
V23^xiii—V23—O21^xiv	100.18 (15)	O72^v—O22—O72^vi	83.71 (17)
V23^xiii—V23—O21^xv	100.18 (15)	O72^vi—O22—O72^v	83.71 (17)
V23^xiii—V23—O33	128.87 (18)	O32^xiv—O23—O32^xv	96.91 (19)
V23^xiii—V23—O53	137.68 (10)	O32^xiv—O23—O32^iv	59.87 (17)
V23^xiii—V23—O73	46.31 (15)	O32^xiv—O23—O52^xiv	70.54 (15)
V23^xiii—V23—O73^xiii	48.4 (2)	O32^xiv—O23—O52^xv	133.6 (2)
O21^xiv—V23—O21^xv	157.5 (2)	O32^xiv—O23—O61	64.17 (16)
O21^xiv—V23—O33	79.87 (15)	O32^xiv—O23—O71^xxi	61.04 (18)
O21^xiv—V23—O53	85.72 (18)	O32^xiv—O23—O71^xxii	119.1 (2)
O21^xiv—V23—O73	93.55 (18)	O32^xiv—O23—O72^xiv	89.02 (11)
O21^xiv—V23—O73^xiii	100.35 (14)	O32^xiv—O23—O72^xv	167.5 (2)
O21^xv—V23—O21^xiv	157.5 (2)	O32^xv—O23—O32^xiv	96.91 (19)
O21^xv—V23—O33	79.87 (15)	O32^xv—O23—O32^iv	59.87 (17)
O21^xv—V23—O53	85.72 (18)	O32^xv—O23—O52^xiv	133.6 (2)
O21^xv—V23—O73	93.55 (18)	O32^xv—O23—O52^xv	70.54 (15)
O21^xv—V23—O73^xiii	100.35 (14)	O32^xv—O23—O61	64.17 (16)
O33—V23—O53	93.4 (2)	O32^xv—O23—O71^xxi	119.1 (2)
O33—V23—O73	82.6 (2)	O32^xv—O23—O71^xxii	61.04 (18)
O33—V23—O73^xiii	177.3 (2)	O32^xv—O23—O72^xiv	167.5 (2)
O53—V23—O73	176.01 (18)	O32^xv—O23—O72^xv	89.02 (11)
O53—V23—O73^xiii	89.3 (2)	O32^iv—O23—O32^xiv	59.87 (17)
O73—V23—O73^xiii	94.7 (2)	O32^iv—O23—O32^xv	59.87 (17)
O73^xiii—V23—O73	94.7 (2)	O32^iv—O23—O52^xiv	130.32 (12)
O21—V31—O31^iv	84.2 (2)	O32^iv—O23—O52^xv	130.32 (12)
O21—V31—O33^vii	79.37 (14)	O32^iv—O23—O61	89.74 (18)
O21—V31—O33^viii	79.37 (14)	O32^iv—O23—O71^xxi	60.29 (17)
O21—V31—O62	101.0 (2)	O32^iv—O23—O71^xxii	60.29 (17)
O21—V31—O72	162.1 (2)	O32^iv—O23—O72^xiv	114.95 (19)
O31^iv—V31—O33^vii	77.92 (19)	O32^iv—O23—O72^xv	114.95 (19)
O31^iv—V31—O33^viii	77.92 (19)	O52^xiv—O23—O52^xv	86.19 (18)
O31^iv—V31—O62	174.75 (15)	O52^xiv—O23—O61	70.40 (14)
O31^iv—V31—O72	77.89 (19)	O52^xiv—O23—O71^xxi	94.17 (11)
O33^vii—V31—O33^viii	149.1 (2)	O52^xiv—O23—O71^xxii	163.6 (2)
O33^vii—V31—O62	102.91 (18)	O52^xiv—O23—O72^xiv	58.86 (13)
O33^vii—V31—O72	96.70 (15)	O52^xiv—O23—O72^xv	112.9 (2)
O33^viii—V31—O33^vii	149.1 (2)	O52^xv—O23—O52^xiv	86.19 (18)
O33^viii—V31—O62	102.91 (18)	O52^xv—O23—O61	70.40 (14)
O33^viii—V31—O72	96.70 (15)	O52^xv—O23—O71^xxi	163.6 (2)
O62—V31—O72	96.86 (19)	O52^xv—O23—O71^xxii	94.17 (11)
O23—V32—O32^xiv	77.97 (14)	O52^xv—O23—O72^xiv	112.9 (2)
O23—V32—O32^xv	77.97 (14)	O52^xv—O23—O72^xv	58.86 (13)
O23—V32—O32^iv	82.2 (2)	O61—O23—O71^xxi	125.11 (15)
O23—V32—O61	100.50 (19)	O61—O23—O71^xxii	125.11 (15)
O23—V32—O71	160.6 (2)	O61—O23—O72^xiv	128.30 (16)
O32^xiv—V32—O32^xv	146.3 (2)	O61—O23—O72^xv	128.30 (16)
O32^xiv—V32—O32^iv	76.86 (19)	O71^xxi—O23—O71^xxii	80.91 (18)
O32^xiv—V32—O61	103.63 (19)	O71^xxi—O23—O72^xiv	54.67 (16)
O32^xiv—V32—O71	97.46 (15)	O71^xxi—O23—O72^xv	106.4 (2)
O32^xv—V32—O32^xiv	146.3 (2)	O71^xxii—O23—O71^xxi	80.91 (18)
O32^xv—V32—O32^iv	76.86 (19)	O71^xxii—O23—O72^xiv	106.4 (2)
O32^xv—V32—O61	103.63 (19)	O71^xxii—O23—O72^xv	54.67 (16)
O32^xv—V32—O71	97.46 (15)	O72^xiv—O23—O72^xv	83.14 (14)
O32^iv—V32—O32^xiv	76.86 (19)	O72^xv—O23—O72^xiv	83.14 (14)
O32^iv—V32—O32^xv	76.86 (19)	O33^xxi—O31—O33^xxii	87.9 (2)
O32^iv—V32—O61	177.27 (16)	O33^xxi—O31—O51	125.27 (14)
O32^iv—V32—O71	78.4 (2)	O33^xxi—O31—O63^xi	93.42 (11)
O61—V32—O71	98.9 (2)	O33^xxi—O31—O63^xii	164.7 (2)
O22^xvi—V33—O31^xvii	79.41 (13)	O33^xxi—O31—O72^iv	64.79 (17)
O22^xvi—V33—O31^xviii	79.41 (13)	O33^xxi—O31—O73^xxi	56.82 (16)
O22^xvi—V33—O33^iii	81.67 (19)	O33^xxi—O31—O73^xxii	110.6 (2)
O22^xvi—V33—O63^xvi	103.32 (18)	O33^xxii—O31—O33^xxi	87.9 (2)
O22^xvi—V33—O73^iii	156.2 (2)	O33^xxii—O31—O51	125.27 (14)
O31^xvii—V33—O31^xviii	147.1 (2)	O33^xxii—O31—O63^xi	164.7 (2)
O31^xvii—V33—O33^iii	76.12 (16)	O33^xxii—O31—O63^xii	93.42 (11)
O31^xvii—V33—O63^xvi	104.60 (16)	O33^xxii—O31—O72^iv	64.79 (17)
O31^xvii—V33—O73^iii	94.65 (14)	O33^xxii—O31—O73^xxi	110.6 (2)
O31^xviii—V33—O31^xvii	147.1 (2)	O33^xxii—O31—O73^xxii	56.82 (16)
O31^xviii—V33—O33^iii	76.12 (16)	O51—O31—O63^xi	65.63 (13)
O31^xviii—V33—O63^xvi	104.60 (16)	O51—O31—O63^xii	65.63 (13)
O31^xviii—V33—O73^iii	94.65 (14)	O51—O31—O72^iv	89.57 (17)
O33^iii—V33—O63^xvi	175.01 (16)	O51—O31—O73^xxi	123.87 (19)
O33^iii—V33—O73^iii	74.5 (2)	O51—O31—O73^xxii	123.87 (19)
O63^xvi—V33—O73^iii	100.5 (2)	O63^xi—O31—O63^xii	81.37 (16)
O12^i—O11—O12^ii	94.93 (17)	O63^xi—O31—O72^iv	129.28 (13)
O12^i—O11—O42^xi	91.82 (9)	O63^xi—O31—O73^xxi	58.48 (15)
O12^i—O11—O42^xii	173.21 (15)	O63^xi—O31—O73^xxii	108.73 (19)
O12^i—O11—O51	60.28 (14)	O63^xii—O31—O63^xi	81.37 (16)
O12^i—O11—O52^i	68.15 (15)	O63^xii—O31—O72^iv	129.28 (13)
O12^i—O11—O52^ii	127.6 (2)	O63^xii—O31—O73^xxi	108.73 (19)
O12^i—O11—O61^iv	60.76 (16)	O63^xii—O31—O73^xxii	58.48 (15)
O12^i—O11—O63^xi	66.39 (15)	O72^iv—O31—O73^xxi	121.6 (2)
O12^i—O11—O63^xii	125.77 (19)	O72^iv—O31—O73^xxii	121.6 (2)
O12^ii—O11—O12^i	94.93 (17)	O73^xxi—O31—O73^xxii	80.68 (14)
O12^ii—O11—O42^xi	173.21 (15)	O73^xxii—O31—O73^xxi	80.68 (14)
O12^ii—O11—O42^xii	91.82 (9)	O32^i—O32—O32^ii	86.6 (2)
O12^ii—O11—O51	60.28 (14)	O32^i—O32—O52	126.04 (15)
O12^ii—O11—O52^i	127.6 (2)	O32^i—O32—O61^vii	93.46 (11)
O12^ii—O11—O52^ii	68.15 (15)	O32^i—O32—O61^viii	163.8 (2)
O12^ii—O11—O61^iv	60.76 (16)	O32^i—O32—O71^vii	58.33 (17)
O12^ii—O11—O63^xi	125.77 (19)	O32^i—O32—O71^viii	110.9 (2)
O12^ii—O11—O63^xii	66.39 (15)	O32^i—O32—O71^iv	64.22 (19)
O42^xi—O11—O42^xii	81.41 (11)	O32^ii—O32—O32^i	86.6 (2)
O42^xi—O11—O51	123.26 (13)	O32^ii—O32—O52	126.04 (15)
O42^xi—O11—O52^i	55.88 (11)	O32^ii—O32—O61^vii	163.8 (2)
O42^xi—O11—O52^ii	108.00 (13)	O32^ii—O32—O61^viii	93.46 (11)
O42^xi—O11—O61^iv	123.73 (13)	O32^ii—O32—O71^vii	110.9 (2)
O42^xi—O11—O63^xi	56.83 (11)	O32^ii—O32—O71^viii	58.33 (17)
O42^xi—O11—O63^xii	108.95 (17)	O32^ii—O32—O71^iv	64.22 (19)
O42^xii—O11—O42^xi	81.41 (11)	O52—O32—O61^vii	66.24 (15)
O42^xii—O11—O51	123.26 (13)	O52—O32—O61^viii	66.24 (15)
O42^xii—O11—O52^i	108.00 (13)	O52—O32—O71^vii	122.7 (2)
O42^xii—O11—O52^ii	55.88 (11)	O52—O32—O71^viii	122.7 (2)
O42^xii—O11—O61^iv	123.73 (13)	O52—O32—O71^iv	90.7 (2)
O42^xii—O11—O63^xi	108.95 (17)	O61^vii—O32—O61^viii	81.97 (18)
O42^xii—O11—O63^xii	56.83 (11)	O61^vii—O32—O71^vii	56.55 (15)
O51—O11—O52^i	128.43 (11)	O61^vii—O32—O71^viii	106.9 (2)
O51—O11—O52^ii	128.43 (11)	O61^vii—O32—O71^iv	130.02 (14)
O51—O11—O61^iv	86.57 (13)	O61^viii—O32—O61^vii	81.97 (18)
O51—O11—O63^xi	66.59 (10)	O61^viii—O32—O71^vii	106.9 (2)
O51—O11—O63^xii	66.59 (10)	O61^viii—O32—O71^viii	56.55 (15)
O52^i—O11—O52^ii	83.66 (12)	O61^viii—O32—O71^iv	130.02 (14)
O52^i—O11—O61^iv	68.11 (12)	O71^vii—O32—O71^viii	79.91 (15)
O52^i—O11—O63^xi	93.41 (8)	O71^vii—O32—O71^iv	122.6 (2)
O52^i—O11—O63^xii	162.01 (17)	O71^viii—O32—O71^vii	79.91 (15)
O52^ii—O11—O52^i	83.66 (12)	O71^viii—O32—O71^iv	122.6 (2)
O52^ii—O11—O61^iv	68.11 (12)	O71^iv—O32—O71^vii	122.6 (2)
O52^ii—O11—O63^xi	162.01 (17)	O71^iv—O32—O71^viii	122.6 (2)
O52^ii—O11—O63^xii	93.41 (8)	O53—O33—O62^xiv	67.53 (15)
O61^iv—O11—O63^xi	127.15 (11)	O53—O33—O62^xv	67.53 (15)
O61^iv—O11—O63^xii	127.15 (11)	O53—O33—O72^xiv	123.34 (19)
O63^xi—O11—O63^xii	83.88 (13)	O53—O33—O72^xv	123.34 (19)
O63^xii—O11—O63^xi	83.88 (13)	O53—O33—O73	88.6 (2)
O41^vii—O12—O41^viii	80.84 (13)	O62^xiv—O33—O62^xv	83.14 (18)
O41^vii—O12—O51^i	55.52 (9)	O62^xiv—O33—O72^xiv	56.03 (14)
O41^vii—O12—O51^ii	107.69 (19)	O62^xiv—O33—O72^xv	107.6 (2)
O41^vii—O12—O52	124.49 (17)	O62^xiv—O33—O73	129.31 (14)
O41^vii—O12—O61^vii	57.35 (9)	O62^xv—O33—O62^xiv	83.14 (18)
O41^vii—O12—O61^viii	109.25 (19)	O62^xv—O33—O72^xiv	107.6 (2)
O41^vii—O12—O63^iii	122.62 (17)	O62^xv—O33—O72^xv	56.03 (14)
O41^viii—O12—O41^vii	80.84 (13)	O62^xv—O33—O73	129.31 (14)
O41^viii—O12—O51^i	107.69 (19)	O72^xiv—O33—O72^xv	80.97 (14)
O41^viii—O12—O51^ii	55.52 (9)	O72^xiv—O33—O73	122.6 (2)
O41^viii—O12—O52	124.49 (17)	O72^xv—O33—O72^xiv	80.97 (14)
O41^viii—O12—O61^vii	109.25 (19)	O72^xv—O33—O73	122.6 (2)
O41^viii—O12—O61^viii	57.35 (9)	O51—O41—O51^iv	180
O41^viii—O12—O63^iii	122.62 (17)	O51—O41—O61	82.15 (10)
O51^i—O12—O51^ii	84.26 (19)	O51—O41—O61^iv	97.85 (10)
O51^i—O12—O52	127.61 (13)	O51^iv—O41—O51	180
O51^i—O12—O61^vii	93.02 (8)	O51^iv—O41—O61	97.85 (10)
O51^i—O12—O61^viii	162.2 (2)	O51^iv—O41—O61^iv	82.15 (10)
O51^i—O12—O63^iii	67.21 (15)	O61—O41—O61^iv	180
O51^ii—O12—O51^i	84.26 (19)	O61^iv—O41—O61	180
O51^ii—O12—O52	127.61 (13)	O52^iii—O42—O53	179.21 (18)
O51^ii—O12—O61^vii	162.2 (2)	O52^iii—O42—O62^iii	73.82 (16)
O51^ii—O12—O61^viii	93.02 (8)	O52^iii—O42—O63	99.18 (15)
O51^ii—O12—O63^iii	67.21 (15)	O52^iii—O42—Li1^v	74.4 (2)
O52—O12—O61^vii	67.36 (15)	O52^iii—O42—Li1^vi	74.4 (2)
O52—O12—O61^viii	67.36 (15)	O53—O42—O62^iii	106.96 (15)
O52—O12—O63^iii	86.86 (16)	O53—O42—O63	80.03 (16)
O61^vii—O12—O61^viii	84.17 (19)	O53—O42—Li1^v	106.1 (2)
O61^vii—O12—O63^iii	127.77 (13)	O53—O42—Li1^vi	106.1 (2)
O61^viii—O12—O61^vii	84.17 (19)	O62^iii—O42—O63	173.0 (2)
O61^viii—O12—O63^iii	127.77 (13)	O62^iii—O42—Li1^v	52.4 (2)
O13^v—O13—O13^vi	93.90 (16)	O62^iii—O42—Li1^vi	52.4 (2)
O13^v—O13—O42^v	91.12 (8)	O63—O42—Li1^v	126.4 (2)
O13^v—O13—O42^vi	172.5 (2)	O63—O42—Li1^vi	126.4 (2)
O13^v—O13—O53	65.12 (15)	Li1^v—O42—Li1^vi	103.5 (4)
O13^v—O13—O53^v	62.96 (14)	Li1^vi—O42—Li1^v	103.5 (4)
O13^v—O13—O53^vi	118.2 (2)	O72—O62—Li1^vii	93.4 (3)
O13^v—O13—O62^xiv	74.52 (14)	O72—O62—Li1^viii	93.4 (3)
O13^v—O13—O62^xv	131.9 (2)	Li1^vii—O62—Li1^viii	113.5 (4)
O13^v—O13—Li1	124.1 (2)	Li1^viii—O62—Li1^vii	113.5 (4)

Symmetry codes: (i) −x+1/2, −y−1/2, −z; (ii) −x+1/2, −y+1/2, −z; (iii) −x+1, −y, −z+1; (iv) −x+1, −y, −z; (v) −x+3/2, −y−1/2, −z+1; (vi) −x+3/2, −y+1/2, −z+1; (vii) x−1/2, y−1/2, z; (viii) x−1/2, y+1/2, z; (ix) x+1/2, y−1/2, z−1; (x) x+1/2, y+1/2, z−1; (xi) x−1/2, y−1/2, z−1; (xii) x−1/2, y+1/2, z−1; (xiii) −x+2, −y, −z+1; (xiv) x+1/2, y−1/2, z; (xv) x+1/2, y+1/2, z; (xvi) x−1, y, z; (xvii) x−1/2, y−1/2, z+1; (xviii) x−1/2, y+1/2, z+1; (xix) x+1/2, y−1/2, z+1; (xx) x+1/2, y+1/2, z+1; (xxi) −x+3/2, −y−1/2, −z; (xxii) −x+3/2, −y+1/2, −z.

(LiV6O13) ? #Insert the chemical name here.

Crystal data

LiV6O13	? #Insert any comments here.
Mr = 520.59	Dx = 3.852 Mg m^−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
a = 21.955 (10) Å	Cell parameters from 50 reflections
b = 3.686 (2) Å	θ = 17.5–39.0°
c = 11.850 (6) Å	µ = 6.07 mm^−1
β = 110.656 (10)°	T = 293 K
V = 897.3 (8) Å^3	Needle, black
Z = 4	0.28 × 0.11 × 0.11 mm
F(000) = 977.00

Data collection

STOE 4-circle diffractometer	10855 reflections with Inet > −15.0σ(Inet)
Radiation source: X-ray tube	Rint = 0.033
Graphite monochromator	θmax = 52.0°, θmin = 0.0°
θ/2θ scan b/P/b	h = −24→48
Absorption correction: integration Absstoe, Lundgren (1983)	k = 0→8
Tmin = 0.378, Tmax = 0.586	l = −25→26
10855 measured reflections	5 standard reflections every 180 min
5464 independent reflections	intensity decay: 11.3%

Refinement

Refinement on F^2	Weighting scheme based on measured s.u.'s w = 1/(σ^2(F) + .0150F^2)
Least-squares matrix: full	(Δ/σ)max = 0.002
R[F^2 > 2σ(F^2)] = 0.027	Δρmax = 1.50 e Å^−3
wR(F^2) = 0.057	Δρmin = −1.68 e Å^−3
S = 2.34	Extinction correction: Becker & Coppens (1974), anisotropic type II
5464 reflections	Extinction coefficient: (anisotropic), 0.7502E-07, 0.6778E-07, 0.1111E-07 .6345E-07, −0.2642E-07, −0.2650E-07
122 parameters

Special details

Experimental. ? #Insert any special details here.

Refinement. ? #Insert any special details here.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
V11	−0.224403 (7)	0.0000	−0.0728	0.0057
V12	0.249784 (8)	0.0000	0.393911 (13)	0.00609 (5)
V21	−0.046855 (8)	0.0000	0.039720 (13)	0.00820 (5)
V22	0.429189 (7)	0.0000	0.517668 (12)	0.00497 (4)
V31	−0.073104 (7)	0.0000	−0.288796 (12)	0.00478 (4)
V32	0.436179 (8)	0.0000	0.228260 (14)	0.00613 (5)
O11	0.75350 (4)	0.0000	1.07500 (6)	0.0072 (2)
O12	0.24874 (4)	0.0000	0.56894 (7)	0.0095 (3)
O21	−0.06013 (4)	0.0000	−0.44368 (6)	0.0071 (2)
O22	0.44623 (4)	0.0000	0.06385 (6)	0.0073 (2)
O31	−0.04309 (4)	0.0000	0.21544 (6)	0.0080 (2)
O32	0.44950 (4)	0.0000	0.69911 (6)	0.0068 (2)
O41	0.74967 (4)	0.0000	0.75183 (6)	0.0109 (3)
O51	−0.14567 (4)	0.0000	−0.02786 (7)	0.0111 (3)
O52	0.34862 (4)	0.0000	0.45210 (7)	0.0103 (3)
O61	−0.15270 (4)	0.0000	−0.32901 (7)	0.0098 (3)
O62	0.35732 (4)	0.0000	0.19222 (8)	0.0132 (3)
O71	−0.04508 (4)	0.0000	−0.11457 (6)	0.0071 (2)
O72	0.45801 (4)	0.0000	0.39539 (6)	0.0085 (2)
Li1	−0.1849 (2)	0.0000	0.2422 (3)	0.041 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V11	0.0060	0.0049	0.0064	0.0000	0.0024	0.0000
V12	0.00742 (4)	0.00518 (5)	0.00583 (4)	0.0000	0.00254 (3)	0.0000
V21	0.00650 (4)	0.01355 (6)	0.00484 (4)	0.0000	0.00234 (3)	0.0000
V22	0.00511 (4)	0.00418 (4)	0.00529 (4)	0.0000	0.00144 (3)	0.0000
V31	0.00526 (4)	0.00421 (4)	0.00498 (4)	0.0000	0.00194 (3)	0.0000
V32	0.00761 (4)	0.00410 (4)	0.00757 (4)	0.0000	0.00379 (3)	0.0000
O11	0.0096 (2)	0.0053 (2)	0.0077 (2)	0.0000	0.00422 (17)	0.0000
O12	0.0109 (3)	0.0066 (2)	0.0108 (2)	0.0000	0.0034 (2)	0.0000
O21	0.0106 (2)	0.0047 (2)	0.00696 (19)	0.0000	0.00421 (17)	0.0000
O22	0.0103 (2)	0.0052 (2)	0.0073 (2)	0.0000	0.00402 (17)	0.0000
O31	0.0133 (3)	0.0049 (2)	0.0070 (2)	0.0000	0.00484 (18)	0.0000
O32	0.0092 (2)	0.0046 (2)	0.00666 (19)	0.0000	0.00295 (17)	0.0000
O41	0.0110 (3)	0.0145 (3)	0.0069 (2)	0.0000	0.00300 (18)	0.0000
O51	0.0068 (2)	0.0133 (3)	0.0127 (3)	0.0000	0.0027 (2)	0.0000
O52	0.0057 (2)	0.0112 (3)	0.0129 (3)	0.0000	0.00183 (18)	0.0000
O61	0.0058 (2)	0.0121 (3)	0.0110 (2)	0.0000	0.00224 (17)	0.0000
O62	0.0088 (3)	0.0167 (3)	0.0143 (3)	0.0000	0.0043 (2)	0.0000
O71	0.00659 (19)	0.0095 (2)	0.00513 (18)	0.0000	0.00210 (15)	0.0000
O72	0.0111 (3)	0.0087 (2)	0.0069 (2)	0.0000	0.00445 (18)	0.0000
Li1	0.036 (2)	0.045 (2)	0.0261 (15)	0.0000	−0.0074 (14)	0.0000

Geometric parameters (Å, º)

V11—O11^i	1.9758 (12)	O31—O72	2.812 (3)
V11—O11^ii	1.9478 (10)	O31—O72	2.812 (3)
V11—O11^iii	1.9478 (10)	O32—V22	2.0360 (13)
V11—O41^i	1.9510 (13)	O32—V31	1.9271 (10)
V11—O51	1.6193 (11)	O32—V31	1.9271 (10)
V11—O62^iv	2.7576 (14)	O32—V32	2.3488 (15)
V11—Li1	2.9277 (9)	O32—O21	2.4601 (11)
V11—Li1	2.9277 (9)	O32—O21	2.4601 (11)
V12—O12	2.0823 (13)	O32—O22	2.9315 (15)
V12—O12^ii	1.8925 (10)	O32—O31	2.6788 (12)
V12—O12^iii	1.8925 (10)	O32—O31	2.6788 (12)
V12—O41^v	1.7313 (12)	O32—O52	2.9832 (16)
V12—O52	2.0320 (12)	O32—O61	2.8310 (13)
V12—O61^iv	1.9946 (13)	O32—O61	2.8310 (13)
V21—V21	2.5467 (10)	O32—O71	2.8461 (13)
V21—O22^vi	1.8794 (10)	O32—O71	2.8461 (13)
V21—O22^vii	1.8794 (10)	O32—O72	2.642 (4)
V21—O31	2.0546 (13)	O41—V11	1.9510 (13)
V21—O51	2.0303 (12)	O41—V12	1.7313 (12)
V21—O71	1.8424 (12)	O41—O11	2.7773 (13)
V21—O71^iv	1.8968 (12)	O41—O11	2.7773 (13)
V22—V31	2.9564 (11)	O41—O12	2.8395 (13)
V22—V31	2.9564 (11)	O41—O12	2.8395 (13)
V22—O21^viii	1.8936 (10)	O41—O51	2.8041 (15)
V22—O21^ix	1.8936 (10)	O41—O52	2.6111 (15)
V22—O32	2.0360 (13)	O41—O61	2.6384 (15)
V22—O52	1.6622 (11)	O41—O62	2.6563 (15)
V22—O72	1.774 (4)	O41—Li1	2.3447 (10)
V22—O72^v	2.323 (4)	O41—Li1	2.3447 (10)
V31—V22	2.9564 (11)	O51—V11	1.6193 (11)
V31—V22	2.9564 (11)	O51—V21	2.0303 (12)
V31—O21	1.9542 (12)	O51—O11	2.8792 (15)
V31—O31	2.3872 (13)	O51—O11	2.8950 (13)
V31—O32	1.9271 (10)	O51—O11	2.8950 (13)
V31—O32	1.9271 (10)	O51—O22	2.6649 (12)
V31—O61	1.6411 (12)	O51—O22	2.6649 (12)
V31—O71	1.9352 (12)	O51—O31	2.9671 (16)
V32—O22	2.0365 (14)	O51—O41	2.8041 (15)
V32—O31	1.9172 (10)	O51—O71	2.7448 (15)
V32—O31	1.9172 (10)	O52—V12	2.0320 (12)
V32—O32	2.3488 (15)	O52—V22	1.6622 (11)
V32—O62	1.6305 (13)	O52—O12	2.9780 (15)
V32—O72	1.866 (4)	O52—O12	2.7662 (13)
O11—V11	1.9758 (12)	O52—O12	2.7662 (13)
O11—V11	1.9478 (10)	O52—O21	2.6814 (12)
O11—V11	1.9478 (10)	O52—O21	2.6814 (12)
O11—O11	2.5272 (14)	O52—O32	2.9832 (16)
O11—O11	2.5272 (14)	O52—O41	2.6111 (15)
O11—O41	2.7773 (13)	O52—O72	2.713 (4)
O11—O41	2.7773 (13)	O52—Li1	2.9724 (13)
O11—O51	2.8792 (15)	O52—Li1	2.9724 (13)
O11—O51	2.8950 (13)	O61—V12	1.9946 (13)
O11—O51	2.8950 (13)	O61—V31	1.6411 (12)
O11—O62	2.8788 (12)	O61—O12	2.8810 (16)
O11—O62	2.8788 (12)	O61—O12	2.7742 (13)
O11—Li1	1.9658 (11)	O61—O12	2.7742 (13)
O12—V12	2.0823 (13)	O61—O21	2.8153 (15)
O12—V12	1.8925 (10)	O61—O32	2.8310 (13)
O12—V12	1.8925 (10)	O61—O32	2.8310 (13)
O12—O12	2.4765 (13)	O61—O41	2.6384 (15)
O12—O12	2.4765 (13)	O61—O71	2.7935 (15)
O12—O41	2.8395 (13)	O62—V11	2.7576 (14)
O12—O41	2.8395 (13)	O62—V32	1.6305 (13)
O12—O52	2.9780 (15)	O62—O11	2.8788 (12)
O12—O52	2.7662 (13)	O62—O11	2.8788 (12)
O12—O52	2.7662 (13)	O62—O22	2.8670 (14)
O12—O61	2.8810 (16)	O62—O31	2.7981 (13)
O12—O61	2.7742 (13)	O62—O31	2.7981 (13)
O12—O61	2.7742 (13)	O62—O41	2.6563 (15)
O21—V22	1.8936 (10)	O62—O72	2.632 (4)
O21—V22	1.8936 (10)	O62—Li1	2.2341 (9)
O21—V31	1.9542 (12)	O62—Li1	2.2341 (9)
O21—O31	2.8506 (15)	O71—V21	1.8424 (12)
O21—O32	2.4601 (11)	O71—V21	1.8968 (12)
O21—O32	2.4601 (11)	O71—V31	1.9352 (12)
O21—O52	2.6814 (12)	O71—O22	2.8615 (13)
O21—O52	2.6814 (12)	O71—O22	2.8615 (13)
O21—O61	2.8153 (15)	O71—O22	2.7473 (13)
O21—O72	2.780 (3)	O71—O22	2.7473 (13)
O21—O72	2.780 (3)	O71—O31	2.6093 (14)
O21—O72	2.801 (3)	O71—O32	2.8461 (13)
O21—O72	2.801 (3)	O71—O32	2.8461 (13)
O22—V21	1.8794 (10)	O71—O51	2.7448 (15)
O22—V21	1.8794 (10)	O71—O61	2.7935 (15)
O22—V32	2.0365 (14)	O71—O71	2.7385 (18)
O22—O31	2.5261 (12)	O72—V22	1.774 (4)
O22—O31	2.5261 (12)	O72—V22	2.323 (4)
O22—O32	2.9315 (15)	O72—V32	1.866 (4)
O22—O51	2.6649 (12)	O72—O21	2.780 (3)
O22—O51	2.6649 (12)	O72—O21	2.780 (3)
O22—O62	2.8670 (14)	O72—O21	2.801 (3)
O22—O71	2.8615 (13)	O72—O21	2.801 (3)
O22—O71	2.8615 (13)	O72—O31	2.812 (3)
O22—O71	2.7473 (13)	O72—O31	2.812 (3)
O22—O71	2.7473 (13)	O72—O32	2.642 (4)
O31—V21	2.0546 (13)	O72—O52	2.713 (4)
O31—V31	2.3872 (13)	O72—O62	2.632 (4)
O31—V32	1.9172 (10)	O72—O72	2.514 (8)
O31—V32	1.9172 (10)	Li1—V11	2.9277 (9)
O31—O21	2.8506 (15)	Li1—V11	2.9277 (9)
O31—O22	2.5261 (12)	Li1—O11^x	1.9658 (11)
O31—O22	2.5261 (12)	Li1—O41^ii	2.3447 (10)
O31—O32	2.6788 (12)	Li1—O41^iii	2.3447 (10)
O31—O32	2.6788 (12)	Li1—O52	2.9724 (13)
O31—O51	2.9671 (16)	Li1—O52	2.9724 (13)
O31—O62	2.7981 (13)	Li1—O62^xi	2.2341 (9)
O31—O62	2.7981 (13)	Li1—O62^xii	2.2341 (9)
O31—O71	2.6093 (14)
O11^i—V11—O11^ii	80.19 (3)	O32—V32—O62	174.13 (5)
O11—V11—O11	80.19 (3)	O32—V32—O72	76.70 (14)
O11—V11—O41	150.88 (4)	O62—V32—O72	97.44 (14)
O11^i—V11—O51	106.00 (4)	V11—O11—V11	99.81 (3)
O11—V11—O11	142.24 (5)	V11—O11—V11	99.81 (3)
O11^ii—V11—O41^i	90.85 (2)	V11—O11—Li1	126.62 (5)
O11^ii—V11—O51	108.15 (3)	V11—O11—V11	142.24 (5)
O11—V11—O41	90.85 (2)	V11—O11—Li1	96.85 (3)
O11—V11—O51	108.15 (3)	V11—O11—Li1	96.85 (3)
O41^i—V11—O51	103.12 (4)	V12—O12—V12	103.09 (2)
O12—V12—O12^ii	76.91 (2)	V12—O12—V12	103.09 (2)
O12—V12—O12	76.91 (2)	V12—O12—O12	48.10 (3)
O12—V12—O41	179.78 (4)	V12—O12—O12	48.10 (3)
O12—V12—O52	92.74 (4)	V12—O12—V12	153.74 (4)
O12—V12—O61^xii	89.90 (4)	V12—O12—O12	54.98 (3)
O12—V12—O12	153.74 (4)	V12—O12—O12	151.13 (5)
O12^ii—V12—O41^xiii	103.09 (2)	V12—O12—O12	151.13 (5)
O12^ii—V12—O52	89.57 (2)	V12—O12—O12	54.98 (3)
O12^ii—V12—O61^xii	91.03 (2)	O12—O12—O12	96.18 (6)
O12—V12—O41	103.09 (2)	V22—O21—V22	153.45 (4)
O12—V12—O52	89.57 (2)	V22—O21—V31	100.40 (2)
O12—V12—O61	91.03 (2)	V22—O21—O32	53.88 (3)
O41^xiii—V12—O52	87.49 (4)	V22—O21—O32	150.31 (4)
O41^xiii—V12—O61^xii	89.88 (4)	V22—O21—V31	100.40 (2)
O52—V12—O61	177.36 (3)	V22—O21—O32	150.31 (4)
O22—V21—O22	157.41 (5)	V22—O21—O32	53.88 (3)
O22^vi—V21—O31	79.76 (2)	V31—O21—O32	50.18 (3)
O22^vi—V21—O51	85.85 (3)	V31—O21—O32	50.18 (3)
O22^vi—V21—O71	100.49 (2)	O32—O21—O32	97.03 (5)
O22^vi—V21—O71^iv	93.36 (3)	V21—O22—V21	157.41 (5)
O22—V21—O31	79.76 (2)	V21—O22—V32	100.80 (2)
O22—V21—O51	85.85 (3)	V21—O22—V32	100.80 (2)
O22—V21—O71	100.49 (2)	V21—O31—V31	91.42 (3)
O22—V21—O71	93.36 (3)	V21—O31—V32	98.89 (3)
O31—V21—O51	93.16 (3)	V21—O31—V32	98.89 (3)
O31—V21—O71	176.71 (3)	V31—O31—V32	102.96 (3)
O31—V21—O71^iv	82.55 (4)	V31—O31—V32	102.96 (3)
O51—V21—O71	90.13 (4)	V32—O31—V32	148.01 (6)
O51—V21—O71	175.71 (3)	V22—O32—V31	96.45 (2)
O71^iv—V21—O71	94.16 (4)	V22—O32—V31	96.45 (2)
O21—V22—O21	153.45 (4)	V22—O32—V32	101.22 (4)
O21^viii—V22—O32	77.42 (2)	V22—O32—O21	48.70 (3)
O21^viii—V22—O52	97.68 (2)	V22—O32—O21	48.70 (3)
O21^viii—V22—O72	98.52 (3)	V31—O32—V31	146.03 (5)
O21^viii—V22—O72^v	82.59 (3)	V31—O32—V32	104.04 (3)
O21—V22—O32	77.42 (2)	V31—O32—O21	51.16 (3)
O21—V22—O52	97.68 (2)	V31—O32—O21	143.68 (4)
O21—V22—O72	98.52 (3)	V31—O32—V32	104.04 (3)
O21—V22—O72	82.59 (3)	V31—O32—O21	143.68 (4)
O32—V22—O52	107.11 (4)	V31—O32—O21	51.16 (3)
O32—V22—O72	148.68 (14)	V32—O32—O21	94.21 (3)
O32—V22—O72^v	74.31 (9)	V32—O32—O21	94.21 (3)
O52—V22—O72	104.21 (14)	O21—O32—O21	97.03 (5)
O52—V22—O72	178.59 (9)	V11—O41—V12	163.79 (5)
O72^v—V22—O72	74.37 (17)	V11—O41—Li1	85.41 (3)
O21—V31—O31	81.42 (4)	V11—O41—Li1	85.41 (3)
O21—V31—O32	78.67 (2)	V12—O41—Li1	104.36 (3)
O21—V31—O32	78.67 (2)	V12—O41—Li1	104.36 (3)
O21—V31—O61	102.73 (4)	Li1—O41—Li1	103.63 (5)
O21—V31—O71	154.85 (4)	V11—O51—V21	176.28 (5)
O31—V31—O32	75.93 (3)	V12—O52—V22	172.57 (5)
O31—V31—O32	75.93 (3)	V12—O61—V31	174.62 (6)
O31—V31—O61	175.84 (4)	V32—O62—Li1	115.58 (3)
O31—V31—O71	73.43 (3)	V32—O62—Li1	115.58 (3)
O32—V31—O32	146.03 (5)	Li1—O62—Li1	111.16 (5)
O32—V31—O61	104.72 (3)	V21—O71—V21	85.84 (4)
O32—V31—O71	94.93 (2)	V21—O71—V31	161.56 (5)
O32—V31—O61	104.72 (3)	V21—O71—V31	112.60 (4)
O32—V31—O71	94.93 (2)	V22—O72—V22	105.63 (17)
O61—V31—O71	102.42 (4)	V22—O72—V32	146.6 (3)
O22—V32—O31	79.36 (3)	V22—O72—V32	107.77 (18)
O22—V32—O31	79.36 (3)	O11—Li1—O41	79.70 (3)
O22—V32—O32	83.58 (4)	O11—Li1—O41	79.70 (3)
O22—V32—O62	102.29 (5)	O11—Li1—O62	86.29 (3)
O22—V32—O72	160.28 (14)	O11—Li1—O62	86.29 (3)
O31—V32—O31	148.01 (6)	O41—Li1—O41	103.63 (5)
O31—V32—O32	77.06 (3)	O41—Li1—O62	70.87 (4)
O31—V32—O62	103.83 (3)	O41—Li1—O62	165.73 (3)
O31—V32—O72	96.02 (4)	O41—Li1—O62	165.73 (3)
O31—V32—O32	77.06 (3)	O41—Li1—O62	70.87 (4)
O31—V32—O62	103.83 (3)	O62—Li1—O62	111.16 (5)
O31—V32—O72	96.02 (4)

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