Orientational disorder and phase transitions in ammonium oxo­fluoro­vanadates, (NH₄)₃VOF₅ and (NH₄)₃VO₂F₄

Single crystals of (NH₄)₃VOF₅ and (NH₄)₃VO₂F₄ were obtained from aqueous fluoride solutions and phase transitions in these compounds were investigated using X-ray diffraction, differential scanning microcalorimetry (DSM) and vibrational spectroscopy. The room-temperature (RT) phases of these compounds belong to orthorhombic symmetry [Immm and I222, Z = 6, for (NH₄)₃VOF₅ and (NH₄)₃VO₂F₄, respectively] with similar unit-cell parameters and two independent vanadium atoms. Above RT [at 350 and 440 K for (NH₄)₃VOF₅ and (NH₄)₃VO₂F₄, respectively], the compounds undergo reversible phase transitions into high-symmetry dynamically disordered elpasolite-like (, Z = 4) structures with six and 12 spatial orientations of the vanadium octahedron for (NH₄)₃VOF₅ and (NH₄)₃VO₂F₄, respectively. The ligand atoms are distributed in a mixed (split) position of 24e + 96j, one of the ammonium groups is disordered on the tetrahedron 32f site, but another one forms eight spatial orientations due to disorder of its hydrogen atoms in the 96j position. DSM and spectroscopic data enable the phase transition from high temperature to room temperature to be connected with the transition from isotropic orientations of the octahedron to its two different dynamic states.

Computing details

For all structures, data collection: Bruker APEX2; cell refinement: Bruker SAINT; data reduction: Bruker SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2014); molecular graphics: Bruker SHELXTL; software used to prepare material for publication: Bruker SHELXTL.

pentafluorooxovanadium (I)

Crystal data

H12N3VOF5	Mo Kα radiation, λ = 0.71073 Å
Mr = 216.07	Cell parameters from 841 reflections
Cubic, Fm3m	θ = 3.9–27.3°
a = 9.0522 (4) Å	µ = 1.38 mm^−1
V = 741.76 (10) Å^3	T = 365 K
Z = 4	Prizm, blue
F(000) = 436	0.30 × 0.25 × 0.12 mm
Dx = 1.935 Mg m^−3

Data collection

Bruker APEX-II CCD diffractometer	96 reflections with I > 2σ(I)
Detector resolution: 8.33 pixels mm^-1	Rint = 0.019
ω scans	θmax = 34.5°, θmin = 3.9°
Absorption correction: multi-scan Bruker SADABS	h = −14→10
	k = −14→13
1457 measured reflections	l = −14→12
111 independent 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)] = 0.025	Hydrogen site location: difference Fourier map
wR(F^2) = 0.099	H-atom parameters not refined
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0869P)^2] where P = (Fo^2 + 2Fc^2)/3
111 reflections	(Δ/σ)max = 0.023
17 parameters	Δρmax = 0.16 e Å^−3
0 restraints	Δρmin = −0.45 e Å^−3

Special details

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

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
V1	0.02888 (7)	0.0000	0.0000	0.0251 (2)	0.1666
N1	0.2620 (4)	0.2620 (4)	0.2620 (4)	0.0550 (8)	0.25
N2	0.5000	0.5000	0.5000	0.0943 (18)
F1	0.0000	0.0000	0.2040 (3)	0.0993 (15)	0.3333
F2	0.0000	0.0541 (4)	0.1941 (4)	0.156 (2)	0.1667
H11	0.2080	0.2080	0.2080	0.098*	0.25
H12	0.2080	0.3160	0.3160	0.098*	0.0833
H14	0.3160	0.2080	0.3160	0.098*	0.0833
H13	0.3160	0.3160	0.2080	0.098*	0.0833
H2	0.5880	0.4670	0.5000	0.046*	0.125
H3	0.4460	0.4460	0.4460	0.098*	0.125

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0226 (5)	0.02636 (16)	0.02636 (16)	0.000	0.000	0.000
N1	0.0550 (8)	0.0550 (8)	0.0550 (8)	0.0069 (12)	0.0069 (12)	0.0069 (12)
N2	0.0943 (18)	0.0943 (18)	0.0943 (18)	0.000	0.000	0.000
F1	0.142 (2)	0.142 (2)	0.0145 (8)	0.000	0.000	0.000
F2	0.077 (2)	0.322 (6)	0.0688 (14)	0.000	0.000	−0.101 (2)

Geometric parameters (Å, º)

V1—V1^i	0.3697 (8)	N1—F1^xvii	3.092 (4)
V1—V1^ii	0.5228 (12)	N1—H11	0.8462
V1—F1^iii	1.586 (3)	N1—H12	0.8468
V1—F2	1.843 (3)	N1—H14	0.8468
V1—F2^iv	1.843 (3)	N1—H13	0.8468
V1—F2^ii	1.843 (3)	N2—F1^xviii	2.679 (3)
V1—F2^v	1.843 (3)	N2—F1^xvi	2.679 (3)
V1—F1^vi	2.108 (3)	N2—F2^xix	2.812 (3)
N1—N1^vii	0.306 (10)	N2—F2^x	2.812 (3)
N1—N1^viii	0.306 (10)	N2—H2	0.8508
N1—N1^ix	0.306 (10)	N2—H3	0.8467
N1—F2^ix	2.792 (5)	F1—F2^xx	2.596 (2)
N1—F2^x	2.792 (5)	F1—F2^i	2.596 (2)
N1—F2^xi	2.888 (3)	F1—F2^xxi	2.596 (2)
N1—F2^xii	2.888 (3)	F1—F2^xxii	2.596 (2)
N1—F2^xiii	2.925 (2)	F2—F1^vi	2.596 (2)
N1—F2^xiv	2.925 (2)	F2—F2^xxiii	2.579 (4)
N1—F2^xv	3.089 (6)	F2—F1^iii	2.596 (2)
N1—F2^v	3.089 (6)	F2—F2^xxiv	2.579 (4)
N1—F1^xvi	3.092 (4)
F1^iii—V1—F2^iv	98.16 (2)	V1^ii—V1—F2^xxiii	81.84 (2)
F1^iii—V1—F2^v	98.16 (2)	F2—V1—F2^xxiv	88.846 (6)
F1^iii—V1—F2^xxiv	98.16 (2)	F2^ii—V1—F2^xxiv	88.847 (6)
F1^iii—V1—F2^xxv	98.16 (2)	F2^iv—V1—F2^xxv	88.847 (6)
V1^ii—V1—F2^v	81.84 (2)	F2^v—V1—F2^xxv	88.847 (6)
V1^ii—V1—F2^xxiv	81.84 (2)	F2—V1—F2^ii	163.69 (5)
V1^ii—V1—F2^xxv	81.84 (2)	F2^iv—V1—F2^v	163.69 (5)

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

pentafluorooxovanadium (II)

Crystal data

H12N3VOF5	Dx = 1.973 Mg m^−3
Mr = 216.07	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Immm	Cell parameters from 2148 reflections
a = 6.2986 (3) Å	θ = 3.9–27.4°
b = 9.1638 (4) Å	µ = 1.41 mm^−1
c = 18.9044 (8) Å	T = 296 K
V = 1091.15 (8) Å^3	Prizm, blue
Z = 6	0.19 × 0.19 × 0.13 mm
F(000) = 654

Data collection

Bruker APEX-II CCD diffractometer	837 reflections with I > 2σ(I)
Detector resolution: 8.33 pixels mm^-1	Rint = 0.024
ω scans	θmax = 30.4°, θmin = 2.2°
Absorption correction: multi-scan Bruker SADABS	h = −8→8
	k = −13→13
6473 measured reflections	l = −26→25
967 independent 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)] = 0.046	Secondary atom site location: difference Fourier map
wR(F^2) = 0.142	w = 1/[σ^2(Fo^2) + (0.0874P)^2 + 2.385P] where P = (Fo^2 + 2Fc^2)/3
S = 1.00	(Δ/σ)max = 0.004
967 reflections	Δρmax = 0.77 e Å^−3
78 parameters	Δρmin = −0.39 e Å^−3

Special details

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

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
V1	0.02726 (11)	0.0000	0.31798 (3)	0.02161 (14)	0.5
F1	0.2123 (3)	0.0000	0.25757 (9)	0.0617 (5)
F2	0.2094 (3)	0.0000	0.39761 (8)	0.0593 (5)
F3	0.0000	−0.20751 (18)	0.32597 (11)	0.0701 (6)
V2	0.0198 (2)	0.01273 (17)	0.0000	0.0276 (2)	0.25
F4	0.0000	0.0000	0.1007 (2)	0.0631 (18)	0.5
F5	0.0000	−0.2063 (4)	0.0000	0.0426 (10)	0.5
F6	0.3011 (6)	0.0000	0.0000	0.0448 (11)	0.5
F7	0.1076 (19)	0.0000	0.0902 (5)	0.114 (4)	0.25
F8	0.1933 (7)	−0.1432 (5)	0.0281 (4)	0.088 (3)	0.25
N1	0.0000	0.2671 (2)	0.17157 (11)	0.0385 (5)
N2	0.0000	0.5000	0.36277 (18)	0.0414 (7)
N3	0.5000	0.0692 (7)	0.5000	0.0432 (14)	0.5
N4	0.0578 (6)	0.2037 (4)	0.5000	0.0365 (10)	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0200 (4)	0.0244 (2)	0.0204 (2)	0.000	−0.0005 (2)	0.000
F1	0.0442 (8)	0.0976 (13)	0.0434 (8)	0.000	0.0187 (7)	0.000
F2	0.0515 (8)	0.0908 (12)	0.0357 (7)	0.000	−0.0229 (6)	0.000
F3	0.1131 (17)	0.0214 (6)	0.0759 (12)	0.000	0.000	0.0060 (7)
V2	0.0200 (4)	0.0310 (5)	0.0318 (4)	−0.0080 (16)	0.000	0.000
F4	0.135 (5)	0.039 (2)	0.0151 (16)	0.000	0.000	0.000
F5	0.0341 (17)	0.0256 (15)	0.068 (3)	0.000	0.000	0.000
F6	0.0226 (15)	0.0354 (17)	0.076 (3)	0.000	0.000	0.000
F7	0.121 (8)	0.184 (11)	0.039 (4)	0.000	−0.035 (4)	0.000
F8	0.043 (2)	0.057 (2)	0.164 (8)	0.0191 (19)	−0.024 (3)	0.025 (3)
N1	0.0373 (9)	0.0371 (9)	0.0411 (9)	0.000	0.000	0.0029 (8)
N2	0.0489 (15)	0.0347 (13)	0.0407 (14)	0.000	0.000	0.000
N3	0.044 (3)	0.044 (3)	0.042 (3)	0.000	0.000	0.000
N4	0.047 (2)	0.0326 (15)	0.0298 (15)	−0.0069 (13)	0.000	0.000

Geometric parameters (Å, º)

V1—V1^i	0.3434 (13)	F7—F8^v	2.647 (10)
V1—F1	1.6317 (17)	F8—F8^iii	2.624 (9)
V1—F2	1.8928 (16)	F8—F8^iv	2.656 (10)
V1—F1^i	1.8923 (17)	N1—F3^i	2.970 (3)
V1—F3	1.9153 (16)	N1—F7^i	2.970 (6)
V1—F3^i	1.9153 (16)	N1—F2^viii	3.101 (2)
V1—F2^i	2.1186 (16)	N1—F1^viii	3.104 (2)
V2—F5^ii	1.778 (4)	N2—F7^viii	2.627 (11)
V2—F6	1.776 (4)	N2—F7^ix	2.627 (11)
F4—V2^ii	1.910 (4)	N2—F3^i	2.7691 (19)
F4—V2^iii	1.910 (4)	N2—F3^x	2.7691 (19)
F6—V2^ii	2.025 (4)	N2—F6^viii	2.881 (3)
F5—V2^iv	2.011 (4)	N2—F6^xi	2.881 (3)
V2—F8^v	1.704 (5)	N2—F1^ix	2.909 (3)
V2—F7	1.796 (9)	N2—F1^viii	2.909 (3)
V2—F8^ii	1.874 (5)	N3—N3^xii	1.269 (13)
V2—F8^vi	1.875 (5)	N3—F5^xiii	2.057 (7)
F7—V2^iv	1.887 (9)	N3—F2^xii	2.738 (2)
F8—V2^iv	2.031 (5)	N3—F2^xiv	2.738 (2)
F1—F1^i	2.674 (3)	N3—F2^xv	2.738 (2)
F1—F3	2.6601 (19)	N3—F8^xiii	2.951 (7)
F1—F2	2.647 (2)	N3—F8^xvi	2.951 (7)
F1—F3^i	2.6601 (19)	N3—F8^xvii	2.951 (7)
F2—F3^i	2.6814 (19)	N3—F8^xviii	2.951 (7)
F2—F3	2.6814 (19)	N4—N4^xix	0.728 (7)
F2—F2^i	2.638 (3)	N4—F8^xvii	2.170 (6)
F4—F5	2.682 (4)	N4—F8^xviii	2.170 (6)
F4—F6	2.687 (4)	N4—F8^ix	2.743 (6)
F5—F6	2.678 (4)	N4—F8^xi	2.743 (6)
F7—F8^vii	2.586 (10)	N4—F2^xv	2.854 (3)
F7—F8^i	2.586 (10)	N4—F6^viii	2.857 (4)
F7—F8^vi	2.647 (10)	N4—F5^xiii	2.905 (4)
F1—V1—F1^i	98.46 (12)	F5^ii—V2—F5	172.43 (8)
F1—V1—F3	96.85 (5)	F6—V2—F6^ii	172.93 (10)
F1—V1—F3^i	96.85 (5)	F5^ii—V2—F6^ii	89.29 (6)
F1—V1—F2	97.10 (9)	F5—V2—F6^ii	83.15 (5)
F1^i—V1—F2^i	82.40 (8)	F4—V2—F6^ii	86.07 (4)
F3—V1—F2^i	83.16 (5)	F8^v—V2—F7	98.3 (4)
F2—V1—F2^i	82.04 (10)	F7—V2—F8^vi	92.3 (3)
F1^i—V1—F3	88.63 (4)	F7—V2—F8^vii	84.8 (3)
F2—V1—F3	89.52 (5)	F7^i—V2—F8^iv	84.9 (3)
F1^i—V1—F3^i	88.63 (4)	F7^vi—V2—F8^ii	89.6 (4)
F2—V1—F3^i	89.52 (5)	F8^v—V2—F7^ii	92.0 (3)
F1^i—V1—F2	164.44 (8)	F8^vi—V2—F7^ii	86.8 (3)
F3—V1—F3^i	166.28 (9)	F8^i—V2—F7^ii	89.5 (4)
F1—V1—F2^i	179.14 (9)	F8^v—V2—F8^vi	94.2 (3)
F6—V2—F5^ii	97.78 (7)	F8^v—V2—F8^ii	85.6 (3)
F6—V2—F5^ii	97.78 (7)	F8^ii—V2—F8^iv	84.3 (3)
F6—V2—F4^ii	93.50 (4)	F8^iii—V2—F8^ii	95.7 (3)
F5^ii—V2—F4^ii	93.23 (5)	F7—V2—F7^ii	169.76 (10)
F4^ii—V2—F4	169.75 (9)	F8^iii—V2—F8^iv	176.92 (5)
F6—V2—F5	89.78 (6)	F8^ii—V2—F8	169.56 (9)
F4—V2—F5	86.27 (5)

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

tetrafluorodioxovanadium (III)

Crystal data

H12N3VO2F4	Dx = 1.965 Mg m^−3
Mr = 213.07	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, I222	Cell parameters from 3096 reflections
a = 6.2738 (3) Å	θ = 2.5–29.3°
b = 9.1388 (4) Å	µ = 1.41 mm^−1
c = 18.8424 (8) Å	T = 296 K
V = 1080.33 (8) Å^3	Plate, orange
Z = 6	0.20 × 0.20 × 0.12 mm
F(000) = 648

Data collection

Bruker APEX-II CCD diffractometer	1348 reflections with I > 2σ(I)
Detector resolution: 8.33 pixels mm^-1	Rint = 0.020
ω scans	θmax = 29.8°, θmin = 2.2°
Absorption correction: multi-scan Bruker SADABS	h = −8→7
	k = −12→12
6313 measured reflections	l = −26→26
1555 independent reflections

Refinement

Refinement on F^2	w = 1/[σ^2(Fo^2) + (0.0872P)^2 + 1.6871P] where P = (Fo^2 + 2Fc^2)/3
Least-squares matrix: full	(Δ/σ)max = 0.005
R[F^2 > 2σ(F^2)] = 0.044	Δρmax = 0.61 e Å^−3
wR(F^2) = 0.139	Δρmin = −0.44 e Å^−3
S = 0.98	Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
1555 reflections	Extinction coefficient: 0.0046 (12)
118 parameters	Absolute structure: Refined as an inversion twin.
0 restraints	Absolute structure parameter: 0.45(10)
H-atom parameters not defined

Special details

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

Refinement. Refined as a 2-component inversion twin.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
V1	0.0087 (2)	0.01860 (7)	0.31481 (3)	0.02969 (15)	0.5
F1	−0.0004 (9)	0.79650 (14)	0.32561 (10)	0.0597 (5)
F2	0.2090 (2)	0.0009 (7)	0.25701 (8)	0.0561 (4)
F3	0.2106 (2)	0.9989 (5)	0.39686 (7)	0.0500 (4)
V2	0.02741 (16)	0.02114 (9)	0.00513 (9)	0.0243 (3)	0.25
F4	0.0000	0.0000	0.09907 (19)	0.0490 (12)	0.5
F5	0.7038 (5)	0.0000	0.0000	0.0398 (8)	0.5
F6	0.0000	0.2051 (3)	0.0000	0.0377 (8)	0.5
F7	0.1872 (13)	0.1413 (10)	−0.0322 (7)	0.096 (4)	0.25
F8	0.7995 (11)	0.1405 (7)	−0.0188 (5)	0.054 (3)	0.25
F9	0.099 (2)	0.020 (2)	0.0898 (5)	0.124 (4)	0.25
N1	0.0015 (10)	0.2701 (2)	0.17012 (11)	0.0394 (4)
N2	0.0000	0.5000	0.36480 (16)	0.0436 (6)
N3	0.5000	0.0720 (5)	0.5000	0.0400 (12)	0.5
N4	0.0603 (5)	0.2010 (3)	0.5003 (6)	0.0357 (8)	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0392 (3)	0.0251 (3)	0.0248 (2)	−0.0083 (7)	0.0108 (4)	0.0052 (2)
F1	0.0860 (12)	0.0220 (5)	0.0710 (9)	−0.0001 (15)	0.013 (2)	0.0041 (6)
F2	0.0425 (7)	0.0836 (10)	0.0421 (7)	0.007 (2)	0.0165 (6)	0.005 (2)
F3	0.0419 (6)	0.0727 (9)	0.0355 (6)	−0.0043 (19)	−0.0196 (5)	0.0048 (19)
V2	0.0221 (6)	0.0208 (7)	0.0301 (5)	−0.0041 (4)	−0.0075 (8)	−0.0073 (7)
F4	0.097 (3)	0.0353 (16)	0.0144 (12)	−0.008 (5)	0.000	0.000
F5	0.0217 (12)	0.0381 (15)	0.060 (2)	0.000	0.000	0.010 (4)
F6	0.0330 (14)	0.0215 (12)	0.059 (2)	0.000	0.005 (5)	0.000
F7	0.039 (4)	0.072 (4)	0.177 (10)	−0.005 (3)	0.040 (4)	0.070 (5)
F8	0.044 (3)	0.032 (3)	0.084 (7)	0.022 (2)	−0.004 (4)	−0.015 (3)
F9	0.152 (10)	0.168 (10)	0.053 (4)	0.055 (11)	−0.046 (5)	−0.058 (6)
N1	0.0381 (8)	0.0354 (8)	0.0447 (8)	−0.0010 (17)	−0.003 (2)	−0.0007 (7)
N2	0.0502 (14)	0.0406 (12)	0.0399 (12)	0.000 (3)	0.000	0.000
N3	0.046 (3)	0.035 (2)	0.038 (2)	0.000	0.006 (7)	0.000
N4	0.046 (2)	0.0315 (13)	0.0297 (13)	−0.0071 (11)	−0.005 (6)	−0.003 (4)

Geometric parameters (Å, º)

V1—V1^i	0.3573 (15)	F6—V2^xii	1.692 (3)
V1—F2	1.6708 (19)	F6—N3^xx	2.038 (6)
V1—F1^ii	1.7027 (15)	F6—V2^i	2.077 (3)
V1—F2^i	1.756 (2)	F6—V2^xiii	2.077 (3)
V1—F3^iii	2.0067 (18)	F6—F9^xii	2.471 (16)
V1—F1^iii	2.0407 (14)	F7—F8^xiv	0.965 (14)
V1—F3^ii	2.0759 (17)	F7—F5^xv	1.582 (9)
F1—F2^ii	2.610 (6)	F7—V2^xii	1.810 (8)
F1—F2^iv	2.624 (6)	F7—V2^xiii	1.862 (8)
F1—F3	2.641 (5)	F7—F9^xiii	1.91 (2)
F1—F3^v	2.653 (5)	F7—V2^i	2.124 (8)
F1—N2	2.8085 (16)	F7—F4^xii	2.153 (12)
F1—N1^ii	2.992 (3)	F7—N4^xx	2.228 (11)
F1—N1^vi	3.141 (9)	F8—F7^xiv	0.965 (14)
F1—N1^vii	3.154 (9)	F8—F6^xvii	1.434 (7)
F2—V1^i	1.756 (2)	F8—V2^xiv	1.561 (7)
F2—F1^ii	2.610 (6)	F8—F9^xiv	1.844 (18)
F2—F2^i	2.623 (3)	F8—V2^xvii	1.855 (7)
F2—F1^iii	2.624 (6)	F8—V2^xv	1.889 (7)
F2—F3^iii	2.635 (2)	F8—V2^xviii	2.073 (6)
F2—N2^viii	2.933 (3)	F8—N4^ix	2.114 (7)
F2—N1^ix	3.103 (6)	F8—F4^xiv	2.349 (8)
F2—N1^viii	3.104 (6)	F9—F9^i	1.30 (3)
F2—N1	3.229 (6)	F9—V2^i	1.823 (10)
F3—V1^iv	2.0067 (18)	F9—F8^xiv	1.844 (18)
F3—V1^ii	2.0759 (17)	F9—V2^xiii	1.884 (10)
F3—F2^iv	2.635 (2)	F9—F7^xiii	1.91 (2)
F3—F3^v	2.643 (3)	F9—V2^xii	1.958 (10)
F3—F1^v	2.653 (5)	F9—F5^xv	2.103 (11)
F3—N3^x	2.737 (2)	F9—F7^xii	2.374 (17)
F3—N3^iv	2.742 (2)	N1—F1^ii	2.992 (3)
F3—N4^xi	2.824 (8)	N1—F3^viii	3.038 (5)
F3—N4^iv	2.847 (9)	N1—F3^xxi	3.063 (5)
V2—V2^xii	0.394 (2)	N1—F7^xii	3.089 (13)
V2—V2^xiii	0.432 (2)	N1—F2^xxii	3.103 (6)
V2—V2^i	0.5174 (18)	N1—F2^vi	3.104 (6)
V2—F8^xiv	1.561 (7)	N1—F9^i	3.119 (19)
V2—F7	1.644 (9)	N1—F1^viii	3.141 (9)
V2—F9	1.659 (10)	N2—F9^vi	2.661 (12)
V2—F6	1.692 (3)	N2—F9^xxii	2.661 (12)
V2—F5^xv	1.700 (3)	N2—F1^ii	2.8085 (16)
V2—F4	1.789 (4)	N2—F5^xxiii	2.850 (3)
V2—F7^xii	1.810 (8)	N2—F5^xxiv	2.850 (3)
F4—F9^i	0.673 (14)	N2—F2^xxii	2.933 (3)
F4—F9	0.673 (14)	N2—F2^vi	2.933 (3)
F4—V2^i	1.789 (4)	N2—F7^xxiv	3.048 (11)
F4—V2^xiii	1.980 (4)	N2—F7^xxiii	3.048 (11)
F4—V2^xii	1.980 (4)	N3—N3^xv	1.316 (10)
F4—F7^xiii	2.153 (12)	N3—F6^xxiv	2.037 (6)
F4—F7^xii	2.153 (12)	N3—F3^x	2.737 (2)
F4—F8^xvi	2.349 (8)	N3—F3^xi	2.737 (2)
F4—F8^xiv	2.349 (8)	N3—F3^iii	2.742 (2)
F5—F8	1.461 (7)	N3—F3^xxv	2.742 (2)
F5—F8^xiii	1.461 (7)	N3—F8^xxvi	2.934 (8)
F5—F7^xiv	1.582 (9)	N3—F8^xxii	2.934 (8)
F5—F7^xv	1.582 (9)	N3—F7^ix	2.935 (11)
F5—V2^xiv	1.700 (3)	N3—F7^xxiv	2.935 (11)
F5—V2^xv	1.700 (3)	N4—N4^xxvii	0.756 (6)
F5—V2^xvii	2.042 (3)	N4—F8^xxii	2.114 (7)
F5—V2^xviii	2.042 (3)	N4—F7^xxiv	2.228 (11)
F5—F9^xv	2.103 (11)	N4—F8^xxiv	2.706 (7)
F5—F9^xiv	2.103 (11)	N4—F7^xxii	2.814 (10)
F6—F8^xix	1.434 (7)	N4—F3^xi	2.824 (8)
F6—F8^xiv	1.434 (7)	N4—F3^iii	2.846 (9)
F6—F7	1.444 (10)	N4—F5^xxiii	2.877 (3)
F6—F7^xii	1.444 (10)	N4—F6^xxiv	2.889 (3)
V1^i—V1—F2	98.0 (4)	F1^ii—V1—F3^iii	90.94 (19)
V1^i—V1—F1^ii	159.3 (5)	F2^i—V1—F3^iii	163.66 (18)
F2—V1—F1^ii	101.4 (3)	V1^i—V1—F1^iii	17.2 (5)
V1^i—V1—F2^i	70.4 (4)	F2—V1—F1^iii	89.4 (3)
F2—V1—F2^i	99.85 (11)	F1^ii—V1—F1^iii	166.97 (12)
F1^ii—V1—F2^i	98.7 (3)	F2^i—V1—F1^iii	86.5 (3)
V1^i—V1—F3^iii	96.2 (3)	F3^iii—V1—F1^iii	81.47 (18)
F2—V1—F3^iii	91.08 (10)

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