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Single crystals of (NH
4)
3VOF
5 and (NH
4)
3VO
2F
4 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 (NH
4)
3VOF
5 and (NH
4)
3VO
2F
4, respectively] with similar unit-cell parameters and two independent vanadium atoms. Above RT [at 350 and 440 K for (NH
4)
3VOF
5 and (NH
4)
3VO
2F
4, 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 (NH
4)
3VOF
5 and (NH
4)
3VO
2F
4, respectively. The ligand atoms are distributed in a mixed (split) position of 24
e + 96
j, one of the ammonium groups is disordered on the tetrahedron 32
f site, but another one forms eight spatial orientations due to disorder of its hydrogen atoms in the 96
j 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.
Supporting information
CCDC references: 1571199; 1571200; 1571201
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)
top
Crystal data top
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) Å3 | 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 top
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 top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.025 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.099 | H-atom parameters not refined |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0869P)2] where P = (Fo2 + 2Fc2)/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 top
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 (Å2) top | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
V1—V1i | 0.3697 (8) | N1—F1xvii | 3.092 (4) |
V1—V1ii | 0.5228 (12) | N1—H11 | 0.8462 |
V1—F1iii | 1.586 (3) | N1—H12 | 0.8468 |
V1—F2 | 1.843 (3) | N1—H14 | 0.8468 |
V1—F2iv | 1.843 (3) | N1—H13 | 0.8468 |
V1—F2ii | 1.843 (3) | N2—F1xviii | 2.679 (3) |
V1—F2v | 1.843 (3) | N2—F1xvi | 2.679 (3) |
V1—F1vi | 2.108 (3) | N2—F2xix | 2.812 (3) |
N1—N1vii | 0.306 (10) | N2—F2x | 2.812 (3) |
N1—N1viii | 0.306 (10) | N2—H2 | 0.8508 |
N1—N1ix | 0.306 (10) | N2—H3 | 0.8467 |
N1—F2ix | 2.792 (5) | F1—F2xx | 2.596 (2) |
N1—F2x | 2.792 (5) | F1—F2i | 2.596 (2) |
N1—F2xi | 2.888 (3) | F1—F2xxi | 2.596 (2) |
N1—F2xii | 2.888 (3) | F1—F2xxii | 2.596 (2) |
N1—F2xiii | 2.925 (2) | F2—F1vi | 2.596 (2) |
N1—F2xiv | 2.925 (2) | F2—F2xxiii | 2.579 (4) |
N1—F2xv | 3.089 (6) | F2—F1iii | 2.596 (2) |
N1—F2v | 3.089 (6) | F2—F2xxiv | 2.579 (4) |
N1—F1xvi | 3.092 (4) | | |
| | | |
F1iii—V1—F2iv | 98.16 (2) | V1ii—V1—F2xxiii | 81.84 (2) |
F1iii—V1—F2v | 98.16 (2) | F2—V1—F2xxiv | 88.846 (6) |
F1iii—V1—F2xxiv | 98.16 (2) | F2ii—V1—F2xxiv | 88.847 (6) |
F1iii—V1—F2xxv | 98.16 (2) | F2iv—V1—F2xxv | 88.847 (6) |
V1ii—V1—F2v | 81.84 (2) | F2v—V1—F2xxv | 88.847 (6) |
V1ii—V1—F2xxiv | 81.84 (2) | F2—V1—F2ii | 163.69 (5) |
V1ii—V1—F2xxv | 81.84 (2) | F2iv—V1—F2v | 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)
top
Crystal data top
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) Å3 | Prizm, blue |
Z = 6 | 0.19 × 0.19 × 0.13 mm |
F(000) = 654 | |
Data collection top
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 top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.046 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.142 | w = 1/[σ2(Fo2) + (0.0874P)2 + 2.385P] where P = (Fo2 + 2Fc2)/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 top
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 (Å2) top | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
V1—V1i | 0.3434 (13) | F7—F8v | 2.647 (10) |
V1—F1 | 1.6317 (17) | F8—F8iii | 2.624 (9) |
V1—F2 | 1.8928 (16) | F8—F8iv | 2.656 (10) |
V1—F1i | 1.8923 (17) | N1—F3i | 2.970 (3) |
V1—F3 | 1.9153 (16) | N1—F7i | 2.970 (6) |
V1—F3i | 1.9153 (16) | N1—F2viii | 3.101 (2) |
V1—F2i | 2.1186 (16) | N1—F1viii | 3.104 (2) |
V2—F5ii | 1.778 (4) | N2—F7viii | 2.627 (11) |
V2—F6 | 1.776 (4) | N2—F7ix | 2.627 (11) |
F4—V2ii | 1.910 (4) | N2—F3i | 2.7691 (19) |
F4—V2iii | 1.910 (4) | N2—F3x | 2.7691 (19) |
F6—V2ii | 2.025 (4) | N2—F6viii | 2.881 (3) |
F5—V2iv | 2.011 (4) | N2—F6xi | 2.881 (3) |
V2—F8v | 1.704 (5) | N2—F1ix | 2.909 (3) |
V2—F7 | 1.796 (9) | N2—F1viii | 2.909 (3) |
V2—F8ii | 1.874 (5) | N3—N3xii | 1.269 (13) |
V2—F8vi | 1.875 (5) | N3—F5xiii | 2.057 (7) |
F7—V2iv | 1.887 (9) | N3—F2xii | 2.738 (2) |
F8—V2iv | 2.031 (5) | N3—F2xiv | 2.738 (2) |
F1—F1i | 2.674 (3) | N3—F2xv | 2.738 (2) |
F1—F3 | 2.6601 (19) | N3—F8xiii | 2.951 (7) |
F1—F2 | 2.647 (2) | N3—F8xvi | 2.951 (7) |
F1—F3i | 2.6601 (19) | N3—F8xvii | 2.951 (7) |
F2—F3i | 2.6814 (19) | N3—F8xviii | 2.951 (7) |
F2—F3 | 2.6814 (19) | N4—N4xix | 0.728 (7) |
F2—F2i | 2.638 (3) | N4—F8xvii | 2.170 (6) |
F4—F5 | 2.682 (4) | N4—F8xviii | 2.170 (6) |
F4—F6 | 2.687 (4) | N4—F8ix | 2.743 (6) |
F5—F6 | 2.678 (4) | N4—F8xi | 2.743 (6) |
F7—F8vii | 2.586 (10) | N4—F2xv | 2.854 (3) |
F7—F8i | 2.586 (10) | N4—F6viii | 2.857 (4) |
F7—F8vi | 2.647 (10) | N4—F5xiii | 2.905 (4) |
| | | |
F1—V1—F1i | 98.46 (12) | F5ii—V2—F5 | 172.43 (8) |
F1—V1—F3 | 96.85 (5) | F6—V2—F6ii | 172.93 (10) |
F1—V1—F3i | 96.85 (5) | F5ii—V2—F6ii | 89.29 (6) |
F1—V1—F2 | 97.10 (9) | F5—V2—F6ii | 83.15 (5) |
F1i—V1—F2i | 82.40 (8) | F4—V2—F6ii | 86.07 (4) |
F3—V1—F2i | 83.16 (5) | F8v—V2—F7 | 98.3 (4) |
F2—V1—F2i | 82.04 (10) | F7—V2—F8vi | 92.3 (3) |
F1i—V1—F3 | 88.63 (4) | F7—V2—F8vii | 84.8 (3) |
F2—V1—F3 | 89.52 (5) | F7i—V2—F8iv | 84.9 (3) |
F1i—V1—F3i | 88.63 (4) | F7vi—V2—F8ii | 89.6 (4) |
F2—V1—F3i | 89.52 (5) | F8v—V2—F7ii | 92.0 (3) |
F1i—V1—F2 | 164.44 (8) | F8vi—V2—F7ii | 86.8 (3) |
F3—V1—F3i | 166.28 (9) | F8i—V2—F7ii | 89.5 (4) |
F1—V1—F2i | 179.14 (9) | F8v—V2—F8vi | 94.2 (3) |
F6—V2—F5ii | 97.78 (7) | F8v—V2—F8ii | 85.6 (3) |
F6—V2—F5ii | 97.78 (7) | F8ii—V2—F8iv | 84.3 (3) |
F6—V2—F4ii | 93.50 (4) | F8iii—V2—F8ii | 95.7 (3) |
F5ii—V2—F4ii | 93.23 (5) | F7—V2—F7ii | 169.76 (10) |
F4ii—V2—F4 | 169.75 (9) | F8iii—V2—F8iv | 176.92 (5) |
F6—V2—F5 | 89.78 (6) | F8ii—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)
top
Crystal data top
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) Å3 | Plate, orange |
Z = 6 | 0.20 × 0.20 × 0.12 mm |
F(000) = 648 | |
Data collection top
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 top
Refinement on F2 | w = 1/[σ2(Fo2) + (0.0872P)2 + 1.6871P] where P = (Fo2 + 2Fc2)/3 |
Least-squares matrix: full | (Δ/σ)max = 0.005 |
R[F2 > 2σ(F2)] = 0.044 | Δρmax = 0.61 e Å−3 |
wR(F2) = 0.139 | Δρmin = −0.44 e Å−3 |
S = 0.98 | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/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 top
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 (Å2) top | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
V1—V1i | 0.3573 (15) | F6—V2xii | 1.692 (3) |
V1—F2 | 1.6708 (19) | F6—N3xx | 2.038 (6) |
V1—F1ii | 1.7027 (15) | F6—V2i | 2.077 (3) |
V1—F2i | 1.756 (2) | F6—V2xiii | 2.077 (3) |
V1—F3iii | 2.0067 (18) | F6—F9xii | 2.471 (16) |
V1—F1iii | 2.0407 (14) | F7—F8xiv | 0.965 (14) |
V1—F3ii | 2.0759 (17) | F7—F5xv | 1.582 (9) |
F1—F2ii | 2.610 (6) | F7—V2xii | 1.810 (8) |
F1—F2iv | 2.624 (6) | F7—V2xiii | 1.862 (8) |
F1—F3 | 2.641 (5) | F7—F9xiii | 1.91 (2) |
F1—F3v | 2.653 (5) | F7—V2i | 2.124 (8) |
F1—N2 | 2.8085 (16) | F7—F4xii | 2.153 (12) |
F1—N1ii | 2.992 (3) | F7—N4xx | 2.228 (11) |
F1—N1vi | 3.141 (9) | F8—F7xiv | 0.965 (14) |
F1—N1vii | 3.154 (9) | F8—F6xvii | 1.434 (7) |
F2—V1i | 1.756 (2) | F8—V2xiv | 1.561 (7) |
F2—F1ii | 2.610 (6) | F8—F9xiv | 1.844 (18) |
F2—F2i | 2.623 (3) | F8—V2xvii | 1.855 (7) |
F2—F1iii | 2.624 (6) | F8—V2xv | 1.889 (7) |
F2—F3iii | 2.635 (2) | F8—V2xviii | 2.073 (6) |
F2—N2viii | 2.933 (3) | F8—N4ix | 2.114 (7) |
F2—N1ix | 3.103 (6) | F8—F4xiv | 2.349 (8) |
F2—N1viii | 3.104 (6) | F9—F9i | 1.30 (3) |
F2—N1 | 3.229 (6) | F9—V2i | 1.823 (10) |
F3—V1iv | 2.0067 (18) | F9—F8xiv | 1.844 (18) |
F3—V1ii | 2.0759 (17) | F9—V2xiii | 1.884 (10) |
F3—F2iv | 2.635 (2) | F9—F7xiii | 1.91 (2) |
F3—F3v | 2.643 (3) | F9—V2xii | 1.958 (10) |
F3—F1v | 2.653 (5) | F9—F5xv | 2.103 (11) |
F3—N3x | 2.737 (2) | F9—F7xii | 2.374 (17) |
F3—N3iv | 2.742 (2) | N1—F1ii | 2.992 (3) |
F3—N4xi | 2.824 (8) | N1—F3viii | 3.038 (5) |
F3—N4iv | 2.847 (9) | N1—F3xxi | 3.063 (5) |
V2—V2xii | 0.394 (2) | N1—F7xii | 3.089 (13) |
V2—V2xiii | 0.432 (2) | N1—F2xxii | 3.103 (6) |
V2—V2i | 0.5174 (18) | N1—F2vi | 3.104 (6) |
V2—F8xiv | 1.561 (7) | N1—F9i | 3.119 (19) |
V2—F7 | 1.644 (9) | N1—F1viii | 3.141 (9) |
V2—F9 | 1.659 (10) | N2—F9vi | 2.661 (12) |
V2—F6 | 1.692 (3) | N2—F9xxii | 2.661 (12) |
V2—F5xv | 1.700 (3) | N2—F1ii | 2.8085 (16) |
V2—F4 | 1.789 (4) | N2—F5xxiii | 2.850 (3) |
V2—F7xii | 1.810 (8) | N2—F5xxiv | 2.850 (3) |
F4—F9i | 0.673 (14) | N2—F2xxii | 2.933 (3) |
F4—F9 | 0.673 (14) | N2—F2vi | 2.933 (3) |
F4—V2i | 1.789 (4) | N2—F7xxiv | 3.048 (11) |
F4—V2xiii | 1.980 (4) | N2—F7xxiii | 3.048 (11) |
F4—V2xii | 1.980 (4) | N3—N3xv | 1.316 (10) |
F4—F7xiii | 2.153 (12) | N3—F6xxiv | 2.037 (6) |
F4—F7xii | 2.153 (12) | N3—F3x | 2.737 (2) |
F4—F8xvi | 2.349 (8) | N3—F3xi | 2.737 (2) |
F4—F8xiv | 2.349 (8) | N3—F3iii | 2.742 (2) |
F5—F8 | 1.461 (7) | N3—F3xxv | 2.742 (2) |
F5—F8xiii | 1.461 (7) | N3—F8xxvi | 2.934 (8) |
F5—F7xiv | 1.582 (9) | N3—F8xxii | 2.934 (8) |
F5—F7xv | 1.582 (9) | N3—F7ix | 2.935 (11) |
F5—V2xiv | 1.700 (3) | N3—F7xxiv | 2.935 (11) |
F5—V2xv | 1.700 (3) | N4—N4xxvii | 0.756 (6) |
F5—V2xvii | 2.042 (3) | N4—F8xxii | 2.114 (7) |
F5—V2xviii | 2.042 (3) | N4—F7xxiv | 2.228 (11) |
F5—F9xv | 2.103 (11) | N4—F8xxiv | 2.706 (7) |
F5—F9xiv | 2.103 (11) | N4—F7xxii | 2.814 (10) |
F6—F8xix | 1.434 (7) | N4—F3xi | 2.824 (8) |
F6—F8xiv | 1.434 (7) | N4—F3iii | 2.846 (9) |
F6—F7 | 1.444 (10) | N4—F5xxiii | 2.877 (3) |
F6—F7xii | 1.444 (10) | N4—F6xxiv | 2.889 (3) |
| | | |
V1i—V1—F2 | 98.0 (4) | F1ii—V1—F3iii | 90.94 (19) |
V1i—V1—F1ii | 159.3 (5) | F2i—V1—F3iii | 163.66 (18) |
F2—V1—F1ii | 101.4 (3) | V1i—V1—F1iii | 17.2 (5) |
V1i—V1—F2i | 70.4 (4) | F2—V1—F1iii | 89.4 (3) |
F2—V1—F2i | 99.85 (11) | F1ii—V1—F1iii | 166.97 (12) |
F1ii—V1—F2i | 98.7 (3) | F2i—V1—F1iii | 86.5 (3) |
V1i—V1—F3iii | 96.2 (3) | F3iii—V1—F1iii | 81.47 (18) |
F2—V1—F3iii | 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. |
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