Buy article online - an online subscription or single-article purchase is required to access this article.
Ammonium fluoride salts of seven- and eight-coordinated tantalum were grown in the form of well shaped single crystals at different pH of solutions, and their crystal structures were determined by X-ray diffraction. The first one, (NH
4)
3TaOF
6, belongs to elpasolite-type structure (
,
Z = 4) and is characterized by strong dynamic disorder. The ligand atoms (O and F) are each distributed in three positions (one 24
e and two 96
j). The tantalum atom is seven-coordinated in the form of a pentagonal bipyramid (PB) and occupies the 4
a position without leaving the symmetry center of the polyhedron during its fast reorientation. One of the ammonium groups is tetrahedrally disordered (the nitrogen atom is shifted from the 8
c into the 32
f site), while the other group in the 4
b site forms eight spatial orientations due to disordering of hydrogen atoms in the 96
k and 32
f positions. Strong dynamic disorder of [TaOF
6]
3– as a flexible unit is reflected in the IR spectrum at 736 cm
−1 and in the
19F MAS NMR spectrum at −51 ppm, indicating a state with synchronous stretching vibrations of Ta—O and Ta—F bonds. Two double ammonium fluoride salts of tantalum, which are formed concomitantly, differ slightly in composition but their crystal structures contain the same polyhedra in the form of a mono-capped trigonal prism (CTP or TPRS-7) and a distorted cube (CU or CU-8) with one vacant vertex. The latter tantalum polyhedron is detected for the first time. The CU polyhedron in one of the modifications of the tantalum double salt splits into two CTPs during a phase transition with decreasing temperature. The presence of oxygen in the compounds is confirmed by vibrational spectroscopy.
Supporting information
CCDC references: 1959354; 1959355; 1959356; 1959357
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.
Crystal data top
(NH4)3·TaOF6 | Mo Kα radiation, λ = 0.71073 Å |
Mr = 365.08 | Cell parameters from 4131 reflections |
Cubic, Fm3m | θ = 3.8–38.7° |
a = 9.3310 (1) Å | µ = 13.59 mm−1 |
V = 812.43 (3) Å3 | T = 296 K |
Z = 4 | Octahedron, colourless |
F(000) = 672 | 0.20 × 0.18 × 0.15 mm |
Dx = 2.985 Mg m−3 | |
Data collection top
Bruker APEX-II CCD diffractometer | 191 reflections with I > 2σ(I) |
Detector resolution: 8.33 pixels mm-1 | Rint = 0.018 |
φ and ω scans | θmax = 42.9°, θmin = 3.8° |
Absorption correction: multi-scan Bruker SADABS | h = −15→16 |
| k = −17→17 |
4884 measured reflections | l = −16→16 |
191 independent reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.006 | H-atom parameters not refined |
wR(F2) = 0.014 | w = 1/[σ2(Fo2) + (0.0081P)2 + 0.0421P] where P = (Fo2 + 2Fc2)/3 |
S = 1.17 | (Δ/σ)max < 0.001 |
191 reflections | Δρmax = 0.23 e Å−3 |
22 parameters | Δρmin = −0.25 e Å−3 |
0 restraints | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0082 (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) |
Ta1 | 0.0000 | 0.0000 | 0.0000 | 0.03118 (5) | |
N1 | 0.2618 (9) | 0.2618 (9) | 0.2618 (9) | 0.041 (3) | 0.25 |
N2 | 0.5000 | 0.5000 | 0.5000 | 0.0598 (11) | |
F1 | 0.0000 | 0.0000 | 0.2024 (11) | 0.089 (7) | 0.5 |
F2 | 0.0000 | 0.059 (3) | 0.2030 (17) | 0.054 (3) | 0.0833 |
F3 | 0.0000 | 0.1261 (9) | 0.1852 (10) | 0.054 (3) | 0.0833 |
H11 | 0.2070 | 0.2070 | 0.2070 | 0.098* | 0.25 |
H12 | 0.2070 | 0.3170 | 0.3170 | 0.098* | 0.0833 |
H13 | 0.3170 | 0.2070 | 0.3170 | 0.098* | 0.0833 |
H14 | 0.3170 | 0.3170 | 0.2070 | 0.098* | 0.0833 |
H2 | 0.5930 | 0.4814 | 0.4814 | 0.044* | 0.125 |
H3 | 0.4445 | 0.4445 | 0.4445 | 0.098* | 0.125 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ta1 | 0.03118 (5) | 0.03118 (5) | 0.03118 (5) | 0.000 | 0.000 | 0.000 |
N1 | 0.041 (3) | 0.041 (3) | 0.041 (3) | −0.0016 (13) | −0.0016 (13) | −0.0016 (13) |
N2 | 0.0598 (11) | 0.0598 (11) | 0.0598 (11) | 0.000 | 0.000 | 0.000 |
F1 | 0.122 (11) | 0.122 (11) | 0.0243 (19) | 0.000 | 0.000 | 0.000 |
F2 | 0.064 (6) | 0.066 (12) | 0.032 (4) | 0.000 | 0.000 | −0.008 (7) |
F3 | 0.049 (3) | 0.066 (6) | 0.048 (5) | 0.000 | 0.000 | −0.032 (5) |
Geometric parameters (Å, º) top
Ta1—F1 | 1.888 (11) | N2—F1xv | 2.777 (11) |
Ta1—F1i | 1.888 (11) | N2—F1xvi | 2.777 (11) |
Ta1—F1ii | 1.888 (11) | N2—F2xvii | 2.826 (18) |
Ta1—F2iii | 1.974 (13) | N2—F2x | 2.826 (18) |
Ta1—F2iv | 1.974 (13) | N2—H2 | 0.9018 |
Ta1—F3v | 2.091 (8) | N2—H3 | 0.8970 |
Ta1—F3vi | 2.091 (8) | F1—F2xviii | 2.32 (2) |
N1—N1vii | 0.31 (2) | F1—F2xix | 2.32 (2) |
N1—N1viii | 0.31 (2) | F1—F1i | 2.671 (15) |
N1—N1ix | 0.31 (2) | F1—F1xx | 2.671 (15) |
N1—F3x | 2.559 (9) | F1—F2i | 2.732 (7) |
N1—F3xi | 2.559 (9) | F1—F2v | 2.732 (7) |
N1—F3xii | 2.606 (6) | F1—F2xxi | 2.732 (7) |
N1—F3xiii | 2.606 (6) | F1—F2xxii | 2.732 (7) |
N1—F3xiv | 2.606 (6) | F1—F3v | 2.817 (7) |
N1—H11 | 0.8844 | F1—F3i | 2.817 (7) |
N1—H12 | 0.8904 | F1—F3xxi | 2.817 (7) |
N1—H13 | 0.8904 | F1—F3xxii | 2.817 (7) |
N1—H14 | 0.8904 | F1—F3xxiii | 2.817 (7) |
| | | |
F1—Ta1—F1i | 90.0 | F1xxv—Ta1—F2iii | 90.0 |
F1—Ta1—F1ii | 90.0 | F2xxvi—Ta1—F3xxvii | 72.1 (8) |
F1xxiv—Ta1—F2iii | 73.7 (8) | | |
Symmetry codes: (i) −y, −z, −x; (ii) y, z, x; (iii) x, −z, −y; (iv) −x, z, y; (v) −z, −y, x; (vi) z, y, −x; (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) x+1/2, z, −y+1/2; (xii) x+1/2, y, −z+1/2; (xiii) −z+1/2, y, −x+1/2; (xiv) y, x+1/2, −z+1/2; (xv) −y+1/2, −z+1, −x+1/2; (xvi) x+1/2, y+1/2, z; (xvii) −z+1, y+1/2, −x+1/2; (xviii) −x, −z, y; (xix) −z, x, y; (xx) −z, −x, −y; (xxi) −z, y, −x; (xxii) y, −z, x; (xxiii) z, −y, x; (xxiv) −x, −y, −z; (xxv) z, x, y; (xxvi) z, −x, −y; (xxvii) y, x, z. |
Crystal data top
(NH4)3·[TaF6.83O0.17]·F0.83 | Dx = 2.922 Mg m−3 |
Mr = 383.91 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3m:H | Cell parameters from 9478 reflections |
a = 8.5414 (1) Å | θ = 4.4–34.0° |
c = 41.4381 (4) Å | µ = 12.68 mm−1 |
V = 2618.11 (7) Å3 | T = 296 K |
Z = 6 | Prism, colourless |
F(000) = 2118 | 0.30 × 0.22 × 0.16 mm |
Data collection top
Bruker APEX-II CCD diffractometer | 1257 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.028 |
Absorption correction: multi-scan Bruker SADABS | θmax = 34.1°, θmin = 4.8° |
| h = −13→13 |
16286 measured reflections | k = −13→13 |
1353 independent reflections | l = −60→65 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.035 | H-atom parameters not refined |
wR(F2) = 0.101 | w = 1/[σ2(Fo2) + (0.052P)2 + 12.6611P] where P = (Fo2 + 2Fc2)/3 |
S = 1.19 | (Δ/σ)max = 0.007 |
1353 reflections | Δρmax = 1.41 e Å−3 |
74 parameters | Δρmin = −1.37 e Å−3 |
3 restraints | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00028 (8) |
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) |
Ta1 | 0.6667 | 0.3333 | 0.03301 (14) | 0.0351 (14) | 0.65 (4) |
Ta11 | 0.6317 (12) | 0.331 (3) | 0.0390 (4) | 0.0359 (19) | 0.058 (6) |
Ta2 | 0.0000 | 0.0000 | 0.13224 (19) | 0.0284 (6) | 0.52 (5) |
Ta22 | 0.0000 | 0.0000 | 0.1281 (4) | 0.0374 (12) | 0.48 (5) |
F1 | 0.6667 | 0.3333 | −0.0113 (3) | 0.097 (4) | |
F2 | 0.6667 | 0.3333 | 0.0861 (4) | 0.120 (7) | 0.7353 |
F3 | 0.4032 (9) | 0.2016 (5) | 0.02183 (19) | 0.116 (3) | |
F4 | 0.5381 (6) | 0.0762 (12) | 0.0532 (3) | 0.109 (3) | 0.7575 |
F5 | −0.1004 (4) | 0.1004 (4) | 0.09892 (12) | 0.0727 (14) | |
F6 | 0.1280 (4) | 0.2560 (8) | 0.14164 (15) | 0.0847 (18) | |
F7 | 0.0000 | 0.0000 | 0.1781 (2) | 0.090 (4) | |
F8 | 0.3333 | 0.6667 | 0.2454 (4) | 0.093 (4) | |
F9 | 0.3333 | 0.6667 | 0.1667 | 0.058 (5) | 0.4507 |
F10 | 0.0000 | 0.0000 | 0.0000 | 0.082 (5) | 0.8856 |
N1 | 0.1682 (5) | 0.8318 (5) | 0.21132 (18) | 0.0613 (16) | |
N2 | 0.6775 (14) | 0.8387 (7) | 0.04667 (19) | 0.091 (4) | |
H1 | 0.2231 | 0.7769 | 0.2230 | 0.068* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ta1 | 0.0378 (19) | 0.0378 (19) | 0.0298 (9) | 0.0189 (10) | 0.000 | 0.000 |
Ta11 | 0.020 (2) | 0.054 (6) | 0.039 (3) | 0.023 (3) | 0.0116 (17) | 0.002 (3) |
Ta2 | 0.0329 (7) | 0.0329 (7) | 0.0194 (11) | 0.0165 (3) | 0.000 | 0.000 |
Ta22 | 0.0400 (8) | 0.0400 (8) | 0.032 (3) | 0.0200 (4) | 0.000 | 0.000 |
F1 | 0.112 (6) | 0.112 (6) | 0.067 (5) | 0.056 (3) | 0.000 | 0.000 |
F2 | 0.121 (11) | 0.121 (11) | 0.119 (15) | 0.060 (6) | 0.000 | 0.000 |
F3 | 0.070 (4) | 0.144 (6) | 0.111 (5) | 0.035 (2) | −0.008 (4) | −0.004 (2) |
F4 | 0.080 (4) | 0.085 (6) | 0.163 (10) | 0.042 (3) | 0.016 (3) | 0.032 (7) |
F5 | 0.076 (2) | 0.076 (2) | 0.073 (3) | 0.043 (3) | −0.0170 (12) | 0.0170 (12) |
F6 | 0.101 (4) | 0.057 (3) | 0.081 (3) | 0.0287 (15) | −0.0054 (13) | −0.011 (3) |
F7 | 0.113 (6) | 0.113 (6) | 0.042 (4) | 0.057 (3) | 0.000 | 0.000 |
F8 | 0.057 (4) | 0.057 (4) | 0.166 (13) | 0.0286 (18) | 0.000 | 0.000 |
F9 | 0.052 (8) | 0.052 (8) | 0.071 (14) | 0.026 (4) | 0.000 | 0.000 |
F10 | 0.064 (6) | 0.064 (6) | 0.119 (15) | 0.032 (3) | 0.000 | 0.000 |
N1 | 0.059 (3) | 0.059 (3) | 0.066 (3) | 0.030 (3) | −0.0072 (15) | 0.0072 (15) |
N2 | 0.141 (10) | 0.068 (3) | 0.086 (5) | 0.071 (5) | −0.064 (7) | −0.032 (3) |
Geometric parameters (Å, º) top
Ta1—Ta11i | 0.381 (11) | Ta2—F5vii | 2.028 (7) |
Ta1—Ta11ii | 0.381 (11) | Ta22—F5 | 1.917 (11) |
Ta1—Ta11iii | 0.381 (11) | Ta22—F5vi | 1.917 (11) |
Ta1—Ta11iv | 0.381 (11) | Ta22—F5vii | 1.917 (11) |
Ta1—Ta11v | 0.381 (11) | Ta22—F6 | 1.975 (7) |
Ta1—F1 | 1.835 (12) | Ta22—F6vi | 1.975 (7) |
Ta1—F3ii | 2.003 (7) | Ta22—F6vii | 1.975 (7) |
Ta1—F3 | 2.003 (7) | Ta22—F7 | 2.070 (18) |
Ta1—F3iii | 2.003 (7) | F1—Ta11i | 2.10 (2) |
Ta1—F2 | 2.201 (19) | F1—Ta11iii | 2.10 (2) |
Ta1—F4ii | 2.079 (9) | F1—Ta11ii | 2.10 (2) |
Ta1—F4 | 2.079 (9) | F1—Ta11iv | 2.10 (2) |
Ta11—Ta11iv | 0.26 (4) | F1—Ta11v | 2.10 (2) |
Ta11—Ta11v | 0.32 (3) | F2—Ta11ii | 1.97 (2) |
Ta11—Ta11iii | 0.499 (16) | F2—Ta11i | 1.97 (2) |
Ta11—Ta11ii | 0.499 (16) | F2—Ta11iv | 1.97 (2) |
Ta11—Ta11i | 0.575 (19) | F2—Ta11iii | 1.97 (2) |
Ta11—F4iii | 1.77 (2) | F2—Ta11v | 1.97 (2) |
Ta11—F2 | 1.97 (2) | F3—Ta11iv | 1.839 (13) |
Ta11—F3 | 1.839 (13) | F3—Ta11v | 2.11 (2) |
Ta11—F4 | 1.99 (2) | F3—Ta11ii | 2.11 (2) |
Ta11—F3iii | 2.11 (2) | F3—Ta11iii | 2.307 (18) |
Ta11—F1 | 2.10 (2) | F3—Ta11i | 2.307 (18) |
Ta11—F4ii | 2.243 (12) | F4—Ta11iv | 1.77 (2) |
Ta2—F7 | 1.901 (12) | F4—Ta11ii | 1.77 (2) |
Ta2—F6 | 1.933 (6) | F4—Ta11i | 1.99 (2) |
Ta2—F6vi | 1.933 (6) | F4—Ta11v | 2.243 (12) |
Ta2—F6vii | 1.933 (6) | F4—Ta11iii | 2.243 (12) |
Ta2—F5 | 2.028 (7) | N1—H1 | 0.9462 |
Ta2—F5vi | 2.028 (7) | | |
| | | |
Ta11i—Ta1—Ta11ii | 39 (6) | Ta11iv—Ta11—F3 | 86.0 (6) |
Ta11i—Ta1—Ta11iii | 50 (5) | Ta11v—Ta11—F3 | 146.2 (6) |
Ta11ii—Ta1—Ta11iii | 82 (3) | Ta11iii—Ta11—F3 | 157.2 (6) |
Ta11i—Ta1—Ta11iv | 82 (3) | Ta11ii—Ta11—F3 | 117 (4) |
Ta11ii—Ta1—Ta11iv | 50 (5) | Ta11i—Ta11—F3 | 139.6 (6) |
Ta11iii—Ta1—Ta11iv | 98 (4) | F4iii—Ta11—F3 | 80.1 (4) |
Ta11i—Ta1—Ta11v | 82 (3) | F2—Ta11—F3 | 119.9 (8) |
Ta11ii—Ta1—Ta11v | 98 (4) | Ta11iv—Ta11—F4 | 27.1 (5) |
Ta11iii—Ta1—Ta11v | 39 (6) | Ta11v—Ta11—F4 | 138.2 (3) |
Ta11iv—Ta1—Ta11v | 82 (3) | Ta11iii—Ta11—F4 | 114 (4) |
Ta11i—Ta1—F1 | 130.8 (18) | Ta11ii—Ta11—F4 | 57 (4) |
Ta11ii—Ta1—F1 | 130.8 (18) | Ta11i—Ta11—F4 | 81.7 (3) |
Ta11iii—Ta1—F1 | 130.8 (18) | F4iii—Ta11—F4 | 122.0 (8) |
Ta11iv—Ta1—F1 | 130.8 (18) | F2—Ta11—F4 | 72.3 (7) |
Ta11v—Ta1—F1 | 130.8 (18) | F3—Ta11—F4 | 74.5 (6) |
Ta11i—Ta1—F3ii | 59 (2) | Ta11iv—Ta11—F3iii | 137.6 (4) |
Ta11ii—Ta1—F3ii | 59 (2) | Ta11v—Ta11—F3iii | 29.0 (3) |
Ta11iii—Ta1—F3ii | 101 (3) | Ta11iii—Ta11—F3iii | 51 (3) |
Ta11iv—Ta1—F3ii | 101 (3) | Ta11ii—Ta11—F3iii | 107 (4) |
Ta11v—Ta1—F3ii | 140 (3) | Ta11i—Ta11—F3iii | 82.2 (3) |
F1—Ta1—F3ii | 76.6 (3) | F4iii—Ta11—F3iii | 72.9 (8) |
Ta11i—Ta1—F3 | 140 (3) | F2—Ta11—F3iii | 107.8 (8) |
Ta11ii—Ta1—F3 | 101 (3) | F3—Ta11—F3iii | 117.2 (9) |
Ta11iii—Ta1—F3 | 140 (3) | F4—Ta11—F3iii | 163.7 (6) |
Ta11iv—Ta1—F3 | 59 (2) | Ta11iv—Ta11—F1 | 86.5 (5) |
Ta11v—Ta1—F3 | 101 (3) | Ta11v—Ta11—F1 | 85.6 (4) |
F1—Ta1—F3 | 76.6 (3) | Ta11iii—Ta11—F1 | 83.2 (2) |
F3ii—Ta1—F3 | 114.8 (2) | Ta11ii—Ta11—F1 | 83.2 (2) |
Ta11i—Ta1—F3iii | 101 (3) | Ta11i—Ta11—F1 | 82.1 (3) |
Ta11ii—Ta1—F3iii | 140 (3) | F4iii—Ta11—F1 | 115.4 (9) |
Ta11iii—Ta1—F3iii | 59 (2) | F2—Ta11—F1 | 163.7 (5) |
Ta11iv—Ta1—F3iii | 140 (3) | F3—Ta11—F1 | 74.0 (6) |
Ta11v—Ta1—F3iii | 59 (2) | F4—Ta11—F1 | 106.3 (9) |
F1—Ta1—F3iii | 76.6 (3) | F3iii—Ta11—F1 | 68.8 (6) |
F3ii—Ta1—F3iii | 114.8 (2) | Ta11iv—Ta11—F4ii | 86.7 (5) |
F3—Ta1—F3iii | 114.8 (2) | Ta11v—Ta11—F4ii | 36.3 (5) |
Ta11i—Ta1—F2 | 49.2 (18) | Ta11iii—Ta11—F4ii | 16.8 (15) |
Ta11ii—Ta1—F2 | 49.2 (18) | Ta11ii—Ta11—F4ii | 54 (3) |
Ta11iii—Ta1—F2 | 49.2 (18) | Ta11i—Ta11—F4ii | 30.4 (5) |
Ta11iv—Ta1—F2 | 49.2 (18) | F4iii—Ta11—F4ii | 109.8 (9) |
Ta11v—Ta1—F2 | 49.2 (18) | F2—Ta11—F4ii | 67.1 (5) |
F1—Ta1—F2 | 180.0 | F3—Ta11—F4ii | 169.5 (11) |
F3ii—Ta1—F2 | 103.4 (3) | F4—Ta11—F4ii | 101.9 (7) |
F3—Ta1—F2 | 103.4 (3) | F3iii—Ta11—F4ii | 64.4 (4) |
F3iii—Ta1—F2 | 103.4 (3) | F1—Ta11—F4ii | 98.0 (6) |
Ta11i—Ta1—F4ii | 33 (3) | F7—Ta2—F6 | 78.4 (3) |
Ta11ii—Ta1—F4ii | 72 (3) | F7—Ta2—F6vi | 78.4 (3) |
Ta11iii—Ta1—F4ii | 33 (3) | F6—Ta2—F6vi | 116.0 (2) |
Ta11iv—Ta1—F4ii | 110.9 (19) | F7—Ta2—F6vii | 78.4 (3) |
Ta11v—Ta1—F4ii | 72 (3) | F6—Ta2—F6vii | 116.0 (2) |
F1—Ta1—F4ii | 113.8 (3) | F6vi—Ta2—F6vii | 116.0 (2) |
F3ii—Ta1—F4ii | 69.40 (15) | F7—Ta2—F5 | 132.9 (2) |
F3—Ta1—F4ii | 169.6 (5) | F6—Ta2—F5 | 77.20 (19) |
F3iii—Ta1—F4ii | 69.40 (15) | F6vi—Ta2—F5 | 77.21 (19) |
F2—Ta1—F4ii | 66.2 (3) | F6vii—Ta2—F5 | 148.7 (5) |
Ta11i—Ta1—F4 | 72 (3) | F7—Ta2—F5vi | 132.9 (2) |
Ta11ii—Ta1—F4 | 33 (3) | F6—Ta2—F5vi | 148.7 (5) |
Ta11iii—Ta1—F4 | 110.9 (19) | F6vi—Ta2—F5vi | 77.21 (19) |
Ta11iv—Ta1—F4 | 33 (3) | F6vii—Ta2—F5vi | 77.21 (19) |
Ta11v—Ta1—F4 | 110.9 (19) | F5—Ta2—F5vi | 78.7 (4) |
F1—Ta1—F4 | 113.8 (3) | F7—Ta2—F5vii | 132.9 (2) |
F3ii—Ta1—F4 | 69.40 (15) | F6—Ta2—F5vii | 77.20 (19) |
F3—Ta1—F4 | 69.40 (15) | F6vi—Ta2—F5vii | 148.7 (5) |
F3iii—Ta1—F4 | 169.6 (5) | F6vii—Ta2—F5vii | 77.21 (19) |
F2—Ta1—F4 | 66.2 (3) | F5—Ta2—F5vii | 78.7 (4) |
F4ii—Ta1—F4 | 104.8 (4) | F5vi—Ta2—F5vii | 78.7 (4) |
Ta11iv—Ta11—Ta11v | 120.00 (14) | F5—Ta22—F5vi | 84.3 (6) |
Ta11iv—Ta11—Ta11iii | 94 (4) | F5—Ta22—F5vii | 84.3 (6) |
Ta11v—Ta11—Ta11iii | 26 (4) | F5vi—Ta22—F5vii | 84.3 (6) |
Ta11iv—Ta11—Ta11ii | 34 (4) | F5—Ta22—F6 | 78.9 (2) |
Ta11v—Ta11—Ta11ii | 86 (4) | F5vi—Ta22—F6 | 157.3 (8) |
Ta11iii—Ta11—Ta11ii | 60.000 (3) | F5vii—Ta22—F6 | 78.9 (2) |
Ta11iv—Ta11—Ta11i | 60.00 (6) | F5—Ta22—F6vi | 78.9 (2) |
Ta11v—Ta11—Ta11i | 60.00 (2) | F5vi—Ta22—F6vi | 78.9 (2) |
Ta11iii—Ta11—Ta11i | 34 (4) | F5vii—Ta22—F6vi | 157.3 (8) |
Ta11ii—Ta11—Ta11i | 26 (4) | F6—Ta22—F6vi | 112.3 (4) |
Ta11iv—Ta11—F4iii | 149.1 (6) | F5—Ta22—F6vii | 157.3 (8) |
Ta11v—Ta11—F4iii | 84.8 (5) | F5vi—Ta22—F6vii | 78.9 (2) |
Ta11iii—Ta11—F4iii | 110 (4) | F5vii—Ta22—F6vii | 78.9 (2) |
Ta11ii—Ta11—F4iii | 158.6 (18) | F6—Ta22—F6vii | 112.3 (4) |
Ta11i—Ta11—F4iii | 140.2 (4) | F6vi—Ta22—F6vii | 112.3 (4) |
Ta11iv—Ta11—F2 | 86.3 (6) | F5—Ta22—F7 | 129.2 (4) |
Ta11v—Ta11—F2 | 85.4 (5) | F5vi—Ta22—F7 | 129.2 (4) |
Ta11iii—Ta11—F2 | 82.7 (3) | F5vii—Ta22—F7 | 129.2 (4) |
Ta11ii—Ta11—F2 | 82.7 (3) | F6—Ta22—F7 | 73.5 (5) |
Ta11i—Ta11—F2 | 81.6 (3) | F6vi—Ta22—F7 | 73.5 (5) |
F4iii—Ta11—F2 | 77.2 (8) | F6vii—Ta22—F7 | 73.5 (5) |
Symmetry codes: (i) −x+y+1, y, z; (ii) −y+1, x−y, z; (iii) −x+y+1, −x+1, z; (iv) x, x−y, z; (v) −y+1, −x+1, z; (vi) −y, x−y, z; (vii) −x+y, −x, z. |
Crystal data top
(NH4)2.75·[TaF6.75O0.125]·F0.75 | Dx = 3.023 Mg m−3 |
Mr = 375.44 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pnma | Cell parameters from 9906 reflections |
a = 11.5018 (1) Å | θ = 2.4–29.9° |
b = 8.5736 (1) Å | µ = 13.41 mm−1 |
c = 33.4597 (4) Å | T = 296 K |
V = 3299.52 (6) Å3 | Plate, colourless |
Z = 4 | 0.25 × 0.22 × 0.05 mm |
F(000) = 2750 | |
Data collection top
Bruker APEX-II CCD diffractometer | 4364 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.029 |
Absorption correction: multi-scan Bruker SADABS | θmax = 30.0°, θmin = 1.9° |
| h = −16→15 |
33291 measured reflections | k = −11→12 |
5102 independent reflections | l = −46→46 |
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)] = 0.033 | w = 1/[σ2(Fo2) + (0.045P)2 + 8.7205P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.090 | (Δ/σ)max = 0.006 |
S = 1.10 | Δρmax = 1.79 e Å−3 |
5102 reflections | Δρmin = −1.31 e Å−3 |
312 parameters | Extinction correction: SHELXL-2014/7 (Sheldrick 2014, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
7 restraints | Extinction coefficient: 0.00053 (5) |
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) |
Ta1 | 0.0446 (6) | 0.2500 | 0.2959 (2) | 0.0321 (6) | 0.49 (3) |
Ta11 | 0.0328 (5) | 0.2500 | 0.29070 (19) | 0.0283 (5) | 0.51 (3) |
Ta2 | 0.6003 (4) | 0.2500 | 0.6918 (4) | 0.0425 (9) | 0.34 (2) |
Ta22 | 0.60325 (19) | 0.2500 | 0.68355 (12) | 0.0343 (4) | 0.66 (2) |
Ta3 | 0.1186 (11) | 0.2500 | 0.5961 (2) | 0.046 (2) | 0.107 (10) |
Ta33 | 0.1567 (3) | 0.22580 (10) | 0.60210 (4) | 0.0412 (5) | 0.447 (5) |
Ta4 | 0.6766 (4) | 0.2500 | 0.51307 (13) | 0.0426 (4) | 0.85 (3) |
Ta44 | 0.6656 (10) | 0.2500 | 0.5167 (4) | 0.025 (2) | 0.15 (3) |
F1 | 0.1167 (10) | 0.2500 | 0.3449 (2) | 0.142 (4) | |
F2 | −0.0400 (4) | 0.0812 (5) | 0.32044 (15) | 0.0864 (14) | |
F3 | 0.1511 (4) | 0.0821 (5) | 0.28705 (14) | 0.0779 (12) | |
F4 | −0.1144 (4) | 0.2500 | 0.26833 (15) | 0.0594 (13) | |
F5 | 0.0694 (4) | 0.2500 | 0.23612 (14) | 0.0560 (12) | |
F6 | 0.5269 (6) | 0.0975 (7) | 0.72036 (17) | 0.126 (2) | |
F7 | 0.4578 (6) | 0.2500 | 0.6558 (3) | 0.131 (4) | |
F8 | 0.6117 (4) | 0.0598 (5) | 0.65553 (13) | 0.0783 (12) | |
F9 | 0.7043 (6) | 0.2500 | 0.73143 (19) | 0.0841 (18) | |
F10 | 0.7576 (4) | 0.2500 | 0.66259 (17) | 0.0663 (14) | |
F11 | 0.1726 (4) | 0.2500 | 0.66047 (15) | 0.0584 (13) | 0.9594 |
F12 | −0.0069 (5) | 0.2500 | 0.6223 (2) | 0.089 (2) | 0.9412 |
F13 | 0.0573 (5) | 0.0478 (8) | 0.5804 (2) | 0.112 (2) | 0.7458 |
F14 | 0.2307 (4) | 0.0458 (5) | 0.61650 (14) | 0.0870 (14) | 0.9523 |
F15 | 0.3023 (5) | 0.2500 | 0.57342 (19) | 0.0816 (18) | 0.9604 |
F16 | 0.1162 (8) | 0.2500 | 0.5406 (3) | 0.125 (4) | 0.7549 |
F17 | 0.8271 (6) | 0.2500 | 0.5383 (3) | 0.098 (3) | 0.7706 |
F18 | 0.6624 (7) | 0.0603 (9) | 0.5456 (2) | 0.092 (2) | 0.659 |
F19 | 0.5581 (11) | 0.2500 | 0.4715 (4) | 0.091 (3) | 0.5903 |
F20 | 0.5157 (11) | 0.2500 | 0.5373 (6) | 0.079 (5) | 0.3689 |
F21 | 0.6442 (18) | 0.2500 | 0.5701 (4) | 0.124 (7) | 0.4403 |
F22 | 0.5533 (15) | 0.103 (3) | 0.5086 (7) | 0.155 (9) | 0.343 |
F23 | 0.681 (4) | 0.2500 | 0.4553 (7) | 0.131 (14) | 0.2542 |
F24 | 0.768 (2) | 0.066 (3) | 0.5250 (9) | 0.180 (12) | 0.3098 |
F25 | 0.7386 (7) | 0.0978 (9) | 0.4776 (2) | 0.106 (2) | 0.7273 |
F26 | 0.6417 (5) | 0.2500 | 0.35302 (17) | 0.0658 (14) | |
F27 | 0.3615 (4) | 0.2500 | 0.40245 (15) | 0.0655 (14) | |
F28 | 0.0812 (5) | 0.2500 | 0.44689 (16) | 0.0682 (15) | |
N1 | 0.2873 (4) | 0.9840 (6) | 0.69903 (16) | 0.0556 (12) | |
N2 | 0.9615 (7) | 0.2500 | 0.7061 (2) | 0.0554 (18) | |
N3 | 0.3048 (8) | 0.2500 | 0.4843 (2) | 0.064 (2) | |
N4 | 0.8662 (8) | 0.2500 | 0.4020 (3) | 0.072 (2) | |
N5 | 0.4563 (5) | 0.9730 (7) | 0.59219 (17) | 0.0638 (14) | |
N6 | 0.1745 (5) | 0.0101 (7) | 0.39329 (16) | 0.0612 (13) | |
N7 | 0.0000 | 0.0000 | 0.5000 | 0.086 (3) | |
N8 | 0.8858 (7) | 0.2500 | 0.1805 (2) | 0.0593 (18) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ta1 | 0.0419 (12) | 0.0300 (5) | 0.0242 (12) | 0.000 | −0.0088 (8) | 0.000 |
Ta11 | 0.0324 (7) | 0.0312 (4) | 0.0212 (10) | 0.000 | −0.0058 (7) | 0.000 |
Ta2 | 0.0533 (11) | 0.0272 (7) | 0.047 (2) | 0.000 | 0.0176 (11) | 0.000 |
Ta22 | 0.0351 (5) | 0.0351 (4) | 0.0327 (8) | 0.000 | 0.0021 (5) | 0.000 |
Ta3 | 0.022 (3) | 0.082 (4) | 0.0358 (19) | 0.000 | −0.0200 (17) | 0.000 |
Ta33 | 0.0487 (8) | 0.0340 (7) | 0.0408 (3) | 0.0051 (2) | −0.0082 (4) | 0.0080 (2) |
Ta4 | 0.0565 (9) | 0.0394 (5) | 0.0319 (6) | 0.000 | −0.0056 (6) | 0.000 |
Ta44 | 0.025 (4) | 0.027 (2) | 0.023 (2) | 0.000 | 0.0061 (17) | 0.000 |
F1 | 0.277 (12) | 0.071 (4) | 0.079 (5) | 0.000 | −0.109 (7) | 0.000 |
F2 | 0.071 (2) | 0.078 (3) | 0.110 (4) | −0.002 (2) | 0.024 (2) | 0.049 (3) |
F3 | 0.068 (2) | 0.067 (3) | 0.099 (3) | 0.029 (2) | 0.012 (2) | 0.018 (2) |
F4 | 0.043 (2) | 0.088 (4) | 0.047 (3) | 0.000 | −0.0039 (19) | 0.000 |
F5 | 0.053 (2) | 0.075 (3) | 0.040 (2) | 0.000 | 0.007 (2) | 0.000 |
F6 | 0.175 (5) | 0.108 (4) | 0.096 (4) | −0.080 (4) | 0.054 (4) | −0.004 (3) |
F7 | 0.075 (4) | 0.095 (5) | 0.222 (11) | 0.000 | −0.075 (6) | 0.000 |
F8 | 0.106 (3) | 0.053 (2) | 0.076 (3) | −0.008 (2) | −0.014 (2) | −0.011 (2) |
F9 | 0.098 (4) | 0.093 (5) | 0.062 (4) | 0.000 | −0.008 (3) | 0.000 |
F10 | 0.046 (2) | 0.085 (4) | 0.068 (3) | 0.000 | 0.006 (2) | 0.000 |
F11 | 0.065 (3) | 0.063 (3) | 0.047 (3) | 0.000 | −0.007 (2) | 0.000 |
F12 | 0.061 (3) | 0.131 (6) | 0.075 (4) | 0.000 | −0.015 (3) | 0.000 |
F13 | 0.104 (5) | 0.121 (6) | 0.112 (6) | 0.016 (5) | −0.028 (4) | −0.026 (5) |
F14 | 0.108 (4) | 0.063 (3) | 0.090 (3) | −0.001 (3) | 0.015 (3) | −0.010 (3) |
F15 | 0.083 (4) | 0.090 (5) | 0.072 (4) | 0.000 | 0.012 (3) | 0.000 |
F16 | 0.087 (6) | 0.175 (12) | 0.114 (9) | 0.000 | −0.027 (6) | 0.000 |
F17 | 0.053 (4) | 0.112 (8) | 0.129 (8) | 0.000 | −0.032 (4) | 0.000 |
F18 | 0.109 (6) | 0.074 (4) | 0.094 (5) | −0.009 (4) | −0.007 (4) | 0.039 (4) |
F19 | 0.082 (7) | 0.104 (9) | 0.086 (8) | 0.000 | −0.033 (6) | 0.000 |
F20 | 0.029 (6) | 0.084 (11) | 0.124 (15) | 0.000 | 0.006 (7) | 0.000 |
F21 | 0.137 (15) | 0.20 (2) | 0.039 (8) | 0.000 | 0.018 (9) | 0.000 |
F22 | 0.102 (11) | 0.19 (2) | 0.173 (19) | −0.091 (14) | 0.024 (12) | −0.053 (17) |
F23 | 0.20 (4) | 0.16 (3) | 0.031 (13) | 0.000 | 0.030 (17) | 0.000 |
F24 | 0.18 (2) | 0.15 (2) | 0.20 (3) | 0.12 (2) | −0.04 (2) | −0.03 (2) |
F25 | 0.126 (6) | 0.102 (5) | 0.091 (5) | 0.032 (4) | 0.022 (4) | −0.044 (4) |
F26 | 0.084 (4) | 0.056 (3) | 0.058 (3) | 0.000 | 0.007 (3) | 0.000 |
F27 | 0.067 (3) | 0.078 (4) | 0.051 (3) | 0.000 | 0.005 (3) | 0.000 |
F28 | 0.067 (3) | 0.083 (4) | 0.054 (3) | 0.000 | −0.001 (3) | 0.000 |
N1 | 0.052 (3) | 0.053 (3) | 0.062 (3) | −0.007 (2) | −0.016 (2) | 0.016 (2) |
N2 | 0.064 (4) | 0.052 (4) | 0.050 (4) | 0.000 | −0.006 (3) | 0.000 |
N3 | 0.084 (5) | 0.061 (5) | 0.047 (4) | 0.000 | 0.002 (4) | 0.000 |
N4 | 0.081 (6) | 0.054 (5) | 0.080 (6) | 0.000 | 0.013 (5) | 0.000 |
N5 | 0.068 (3) | 0.063 (3) | 0.060 (3) | 0.001 (3) | −0.011 (2) | −0.006 (3) |
N6 | 0.070 (3) | 0.055 (3) | 0.059 (3) | 0.003 (2) | −0.008 (2) | 0.004 (3) |
N7 | 0.074 (5) | 0.117 (8) | 0.066 (5) | 0.004 (5) | −0.018 (4) | −0.039 (6) |
N8 | 0.084 (5) | 0.045 (4) | 0.049 (4) | 0.000 | −0.007 (4) | 0.000 |
Geometric parameters (Å, º) top
Ta1—F1 | 1.837 (10) | Ta33—F14i | 2.189 (5) |
Ta1—F3 | 1.913 (6) | Ta33—F13i | 2.367 (7) |
Ta1—F3i | 1.913 (6) | Ta4—F23 | 1.93 (3) |
Ta1—F2i | 1.927 (5) | Ta4—F22i | 1.904 (15) |
Ta1—F2 | 1.927 (5) | Ta4—F22 | 1.904 (15) |
Ta1—F5 | 2.020 (8) | Ta4—F25i | 1.903 (7) |
Ta1—F4 | 2.049 (9) | Ta4—F25 | 1.903 (7) |
Ta11—F4 | 1.851 (8) | Ta4—F24i | 1.94 (2) |
Ta11—F5 | 1.874 (7) | Ta4—F24 | 1.94 (2) |
Ta11—F2i | 1.945 (5) | Ta4—F17 | 1.927 (8) |
Ta11—F2 | 1.945 (5) | Ta4—F19 | 1.946 (11) |
Ta11—F3 | 1.985 (5) | Ta4—F21 | 1.946 (15) |
Ta11—F3i | 1.985 (5) | Ta4—F18 | 1.963 (7) |
Ta11—F1 | 2.055 (9) | Ta4—F18i | 1.963 (7) |
Ta2—F9 | 1.786 (11) | Ta44—F21 | 1.81 (2) |
Ta2—F6 | 1.827 (8) | Ta44—F22 | 1.825 (17) |
Ta2—F6i | 1.827 (8) | Ta44—F22i | 1.825 (17) |
Ta2—F7 | 2.034 (10) | Ta44—F20 | 1.857 (18) |
Ta2—F8i | 2.037 (8) | Ta44—F18 | 1.893 (10) |
Ta2—F8 | 2.037 (8) | Ta44—F18i | 1.893 (10) |
Ta2—F10 | 2.055 (9) | Ta44—F24i | 1.99 (2) |
Ta22—F8i | 1.883 (5) | Ta44—F24 | 1.99 (2) |
Ta22—F8 | 1.883 (5) | Ta44—F19 | 1.952 (17) |
Ta22—F10 | 1.908 (6) | Ta44—F17 | 1.994 (14) |
Ta22—F7 | 1.913 (7) | Ta44—F23 | 2.06 (3) |
Ta22—F9 | 1.980 (7) | Ta44—F25i | 2.030 (11) |
Ta22—F6 | 2.000 (6) | F11—Ta33i | 1.973 (5) |
Ta22—F6i | 2.000 (6) | F12—Ta33i | 2.009 (7) |
Ta3—Ta33 | 0.524 (10) | F13—Ta33i | 2.367 (7) |
Ta3—Ta33i | 0.524 (10) | F14—Ta33i | 2.189 (5) |
Ta3—F12 | 1.687 (11) | F15—Ta33i | 1.941 (6) |
Ta3—F16 | 1.860 (14) | F16—Ta33i | 2.121 (10) |
Ta3—F13i | 1.944 (9) | F17—F24 | 1.77 (3) |
Ta3—F13 | 1.944 (9) | F17—F24i | 1.77 (3) |
Ta3—F11 | 2.240 (11) | F18—F24 | 1.40 (3) |
Ta3—F15 | 2.245 (12) | F18—F22 | 1.80 (2) |
Ta3—F14 | 2.278 (10) | F19—F23 | 1.51 (4) |
Ta3—F14i | 2.278 (10) | F19—F22i | 1.77 (3) |
Ta33—Ta33i | 0.4149 (17) | F19—F22 | 1.77 (3) |
Ta33—F14 | 1.827 (5) | F20—F22 | 1.64 (2) |
Ta33—F15 | 1.941 (6) | F20—F22i | 1.64 (2) |
Ta33—F11 | 1.973 (5) | F23—F25 | 1.64 (2) |
Ta33—F12 | 2.009 (7) | F23—F25i | 1.64 (2) |
Ta33—F13 | 2.040 (7) | F24—F25 | 1.65 (3) |
Ta33—F16 | 2.121 (10) | | |
| | | |
F1—Ta1—F3 | 81.3 (4) | F13i—Ta3—F14i | 66.5 (2) |
F1—Ta1—F3i | 81.3 (4) | F11—Ta3—F14i | 63.6 (3) |
F3—Ta1—F3i | 97.6 (4) | F15—Ta3—F14i | 64.4 (3) |
F1—Ta1—F2i | 81.2 (4) | F14—Ta33—F15 | 79.5 (2) |
F3i—Ta1—F2i | 79.9 (2) | F14—Ta33—F11 | 77.55 (18) |
F1—Ta1—F2 | 81.2 (4) | F11—Ta33—F12 | 75.1 (2) |
F3—Ta1—F2 | 79.9 (2) | Ta3—Ta33—F13 | 72.1 (5) |
F2i—Ta1—F2 | 97.3 (4) | F14—Ta33—F13 | 73.9 (2) |
F3—Ta1—F5 | 75.9 (2) | F15—Ta33—F13 | 112.8 (2) |
F3i—Ta1—F5 | 75.9 (2) | F11—Ta33—F13 | 118.9 (2) |
F2i—Ta1—F4 | 75.0 (3) | F12—Ta33—F13 | 70.9 (2) |
F2—Ta1—F4 | 75.0 (3) | F15—Ta33—F16 | 72.5 (3) |
F5—Ta1—F4 | 71.3 (3) | F12—Ta33—F16 | 96.3 (3) |
F4—Ta11—F5 | 79.1 (3) | F13—Ta33—F16 | 66.7 (2) |
F4—Ta11—F2i | 79.3 (2) | F15—Ta33—F14i | 71.19 (16) |
F4—Ta11—F2 | 79.3 (2) | F11—Ta33—F14i | 69.62 (14) |
F2i—Ta11—F2 | 96.1 (4) | F16—Ta33—F13i | 61.05 (19) |
F5—Ta11—F3 | 77.7 (2) | F14i—Ta33—F13i | 61.44 (19) |
F2i—Ta11—F3 | 150.0 (4) | F23—Ta4—F22i | 86.6 (12) |
F2—Ta11—F3 | 77.7 (2) | F23—Ta4—F22 | 86.6 (12) |
F4—Ta11—F3i | 127.0 (3) | F22i—Ta4—F22 | 83.1 (16) |
F5—Ta11—F3i | 77.6 (2) | F22i—Ta4—F25i | 77.1 (7) |
F2i—Ta11—F3i | 77.7 (2) | F25i—Ta4—F25 | 86.5 (6) |
F3—Ta11—F3i | 93.0 (4) | F22i—Ta4—F24i | 83.3 (13) |
F2i—Ta11—F1 | 75.5 (3) | F22—Ta4—F24 | 83.3 (13) |
F2—Ta11—F1 | 75.5 (3) | F25i—Ta4—F17 | 86.4 (4) |
F3—Ta11—F1 | 74.5 (3) | F25—Ta4—F17 | 86.4 (4) |
F3i—Ta11—F1 | 74.5 (3) | F25i—Ta4—F19 | 79.4 (4) |
F9—Ta2—F6 | 85.5 (5) | F25—Ta4—F19 | 79.4 (4) |
F9—Ta2—F6i | 85.5 (5) | F22i—Ta4—F21 | 86.2 (8) |
F6—Ta2—F6i | 91.4 (6) | F22—Ta4—F21 | 86.2 (8) |
F6—Ta2—F7 | 86.4 (4) | F24i—Ta4—F21 | 84.4 (10) |
F6i—Ta2—F7 | 86.4 (4) | F24—Ta4—F21 | 84.4 (10) |
F6i—Ta2—F8i | 76.6 (2) | F17—Ta4—F21 | 75.0 (7) |
F7—Ta2—F8i | 72.5 (4) | F25i—Ta4—F18 | 160.9 (5) |
F6—Ta2—F8 | 76.6 (2) | F25—Ta4—F18 | 79.0 (4) |
F7—Ta2—F8 | 72.5 (4) | F17—Ta4—F18 | 80.3 (3) |
F9—Ta2—F10 | 76.4 (3) | F25i—Ta4—F18i | 79.0 (4) |
F8i—Ta2—F10 | 70.1 (3) | F17—Ta4—F18i | 80.3 (3) |
F8—Ta2—F10 | 70.1 (3) | F21—Ta44—F22 | 92.8 (10) |
F8i—Ta22—F10 | 76.6 (2) | F21—Ta44—F22i | 92.8 (10) |
F8—Ta22—F10 | 76.6 (2) | F22—Ta44—F22i | 87.5 (17) |
F8i—Ta22—F7 | 78.7 (2) | F20—Ta44—F18 | 78.0 (6) |
F8—Ta22—F7 | 78.7 (2) | F20—Ta44—F18i | 78.0 (6) |
F10—Ta22—F7 | 129.4 (5) | F21—Ta44—F24i | 86.7 (11) |
F10—Ta22—F9 | 75.6 (3) | F22i—Ta44—F24i | 83.9 (13) |
F8—Ta22—F6 | 76.3 (2) | F21—Ta44—F24 | 86.7 (11) |
F7—Ta22—F6 | 85.1 (4) | F22—Ta44—F24 | 83.9 (13) |
F9—Ta22—F6 | 76.1 (3) | F18—Ta44—F24 | 42.2 (10) |
F8i—Ta22—F6i | 76.3 (2) | F20—Ta44—F19 | 72.6 (8) |
F7—Ta22—F6i | 85.1 (4) | F21—Ta44—F17 | 76.5 (9) |
F9—Ta22—F6i | 76.1 (3) | F18—Ta44—F17 | 80.4 (5) |
F6—Ta22—F6i | 81.6 (4) | F18i—Ta44—F17 | 80.4 (5) |
F12—Ta3—F13i | 80.2 (4) | F22—Ta44—F23 | 85.0 (12) |
F16—Ta3—F13i | 74.0 (4) | F22i—Ta44—F23 | 85.0 (12) |
F12—Ta3—F13 | 80.2 (4) | F24i—Ta44—F23 | 95.2 (13) |
F16—Ta3—F13 | 74.0 (4) | F24—Ta44—F23 | 95.2 (13) |
F12—Ta3—F11 | 74.9 (3) | F19—Ta44—F23 | 44.2 (13) |
F16—Ta3—F15 | 71.1 (3) | F17—Ta44—F23 | 106.5 (14) |
F11—Ta3—F15 | 93.7 (6) | F22i—Ta44—F25i | 75.7 (8) |
F13—Ta3—F14 | 66.5 (2) | F18i—Ta44—F25i | 77.6 (4) |
F11—Ta3—F14 | 63.6 (3) | F19—Ta44—F25i | 76.3 (6) |
F15—Ta3—F14 | 64.4 (3) | F17—Ta44—F25i | 81.3 (5) |
Symmetry code: (i) x, −y+1/2, z. |
Crystal data top
(NH4)2.75·[TaF6.75O0.125]·F0.75 | F(000) = 5500 |
Mr = 375.44 | Dx = 3.091 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 35.0618 (9) Å | Cell parameters from 9771 reflections |
b = 8.5377 (2) Å | θ = 2.5–30.0° |
c = 22.7987 (5) Å | µ = 13.71 mm−1 |
β = 108.991 (1)° | T = 123 K |
V = 6453.3 (3) Å3 | Plate, colourless |
Z = 4 | 0.31 × 0.27 × 0.08 mm |
Data collection top
Bruker APEX-II CCD diffractometer | 17166 reflections with I > 2σ(I) |
Detector resolution: 8.33 pixels mm-1 | Rint = 0.042 |
φ and ω scans | θmax = 30.1°, θmin = 1.8° |
Absorption correction: multi-scan Bruker SADABS | h = −49→49 |
| k = −12→10 |
72403 measured reflections | l = −32→31 |
18811 independent reflections | |
Refinement top
Refinement on F2 | 4 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.037 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.086 | w = 1/[σ2(Fo2) + (0.0332P)2 + 37.7647P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.004 |
18811 reflections | Δρmax = 2.50 e Å−3 |
848 parameters | Δρmin = −2.35 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. |
Refinement. Refined as a 2-component twin. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ta1 | 0.29661 (2) | 0.27696 (3) | 0.13454 (2) | 0.01651 (7) | |
Ta2 | 0.40343 (4) | 0.82702 (10) | 0.26916 (4) | 0.0125 (3) | 0.842 (10) |
Ta22 | 0.4013 (3) | 0.8085 (17) | 0.2776 (7) | 0.063 (3) | 0.158 (10) |
Ta3 | 0.20668 (2) | 0.24343 (4) | 0.82898 (2) | 0.01492 (7) | |
Ta4 | 0.1055 (2) | 0.7912 (3) | 0.8775 (3) | 0.0382 (10) | 0.57 (2) |
Ta44 | 0.09808 (8) | 0.7932 (3) | 0.88583 (12) | 0.0097 (6) | 0.43 (2) |
Ta5 | 0.18080 (2) | 0.75352 (4) | 0.13857 (2) | 0.01764 (7) | |
Ta6 | 0.31366 (18) | 0.7599 (5) | 0.46054 (16) | 0.0121 (5) | 0.40 (2) |
Ta66 | 0.3025 (3) | 0.7495 (3) | 0.46106 (11) | 0.0227 (7) | 0.60 (2) |
Ta7 | 0.48474 (2) | 0.72995 (4) | 0.58583 (2) | 0.01540 (7) | |
Ta8 | 0.98473 (11) | 0.2529 (5) | 0.9101 (3) | 0.0251 (7) | 0.51 (2) |
Ta88 | 0.98912 (10) | 0.2714 (4) | 0.8939 (3) | 0.0212 (6) | 0.49 (2) |
F1 | 0.35481 (18) | 0.2585 (6) | 0.1514 (3) | 0.0299 (13) | |
F2 | 0.31901 (19) | 0.4603 (6) | 0.1851 (3) | 0.0322 (13) | |
F3 | 0.29978 (18) | 0.4240 (5) | 0.0715 (2) | 0.0286 (12) | |
F4 | 0.29854 (18) | 0.1183 (5) | 0.0727 (2) | 0.0266 (12) | |
F5 | 0.3098 (3) | 0.0895 (7) | 0.1848 (3) | 0.050 (2) | |
F6 | 0.26590 (19) | 0.2993 (8) | 0.1916 (3) | 0.0383 (15) | |
F7 | 0.24217 (17) | 0.2705 (6) | 0.0805 (2) | 0.0260 (12) | |
F8 | 0.41357 (18) | 0.6079 (6) | 0.2524 (3) | 0.0359 (14) | |
F9 | 0.3481 (2) | 0.7629 (6) | 0.2646 (3) | 0.0305 (13) | |
F10 | 0.4175 (2) | 0.7451 (7) | 0.3547 (3) | 0.0368 (15) | |
F11 | 0.46116 (17) | 0.8183 (6) | 0.2937 (3) | 0.0354 (14) | |
F12 | 0.37702 (18) | 0.8003 (6) | 0.1807 (2) | 0.0268 (11) | |
F13 | 0.38670 (19) | 0.9948 (6) | 0.3127 (3) | 0.0304 (13) | |
F14 | 0.41666 (16) | 1.0140 (5) | 0.2326 (2) | 0.0235 (11) | |
F15 | 0.16136 (17) | 0.2592 (6) | 0.7495 (2) | 0.0281 (12) | |
F16 | 0.22222 (18) | 0.4247 (6) | 0.7898 (3) | 0.0296 (13) | |
F17 | 0.21303 (18) | 0.0567 (6) | 0.7845 (3) | 0.0307 (13) | |
F18 | 0.16899 (17) | 0.1029 (6) | 0.8484 (2) | 0.0291 (12) | |
F19 | 0.17453 (18) | 0.4106 (6) | 0.8492 (3) | 0.0287 (12) | |
F20 | 0.22721 (17) | 0.2470 (6) | 0.9189 (2) | 0.0246 (11) | |
F21 | 0.26480 (16) | 0.2225 (5) | 0.8488 (2) | 0.0193 (10) | |
F22 | 0.0484 (3) | 0.7097 (8) | 0.8304 (3) | 0.063 (2) | |
F23 | 0.0709 (2) | 0.7790 (7) | 0.9401 (4) | 0.0447 (17) | |
F24 | 0.1119 (2) | 0.5758 (6) | 0.9086 (3) | 0.0443 (16) | |
F25 | 0.1172 (3) | 0.7378 (8) | 0.8098 (3) | 0.061 (3) | |
F26 | 0.07884 (19) | 0.9633 (6) | 0.8259 (3) | 0.0377 (15) | |
F27 | 0.1186 (2) | 0.9776 (6) | 0.9326 (3) | 0.0417 (17) | |
F28 | 0.1609 (2) | 0.7793 (6) | 0.9158 (3) | 0.0388 (16) | |
F29 | 0.14859 (19) | 0.7617 (6) | 0.0511 (3) | 0.0325 (13) | |
F30 | 0.14994 (17) | 0.9457 (6) | 0.1354 (3) | 0.0305 (12) | |
F31 | 0.15510 (19) | 0.5517 (6) | 0.1291 (2) | 0.0336 (13) | |
F32 | 0.21748 (18) | 0.6286 (7) | 0.1071 (3) | 0.0362 (14) | |
F33 | 0.21419 (18) | 0.9172 (7) | 0.1159 (3) | 0.0308 (12) | |
F34 | 0.15790 (19) | 0.7394 (6) | 0.2061 (3) | 0.0255 (12) | |
F35 | 0.22816 (17) | 0.7492 (6) | 0.2115 (3) | 0.0262 (12) | |
F36 | 0.3213 (5) | 0.7764 (8) | 0.3846 (4) | 0.141 (7) | |
F37 | 0.2691 (3) | 0.6132 (9) | 0.4051 (4) | 0.102 (4) | |
F38 | 0.33975 (18) | 0.5725 (5) | 0.4648 (2) | 0.0298 (12) | |
F39 | 0.3454 (2) | 0.9232 (6) | 0.4806 (3) | 0.0430 (16) | |
F40 | 0.2728 (2) | 0.9276 (7) | 0.4235 (3) | 0.061 (2) | |
F41 | 0.2651 (2) | 0.7352 (7) | 0.4987 (3) | 0.050 (2) | |
F42 | 0.33528 (19) | 0.7313 (6) | 0.5493 (2) | 0.0264 (12) | |
F43 | 0.45853 (19) | 0.6941 (6) | 0.6492 (3) | 0.0261 (12)* | 0.9236 |
F44 | 0.5167 (2) | 0.5524 (8) | 0.6305 (3) | 0.0340 (16)* | 0.8043 |
F45 | 0.5229 (3) | 0.8326 (10) | 0.6573 (4) | 0.0267 (19)* | 0.5763 |
F46 | 0.4596 (3) | 0.9268 (11) | 0.5832 (5) | 0.029 (2)* | 0.5503 |
F47 | 0.5330 (3) | 0.7441 (9) | 0.5634 (4) | 0.031 (2)* | 0.632 |
F48 | 0.4516 (3) | 0.5438 (10) | 0.5538 (4) | 0.0332 (19)* | 0.6424 |
F49 | 0.4854 (4) | 0.8850 (12) | 0.5183 (5) | 0.028 (2)* | 0.4933 |
F50 | 0.4620 (4) | 0.7662 (13) | 0.4957 (6) | 0.032 (3)* | 0.4721 |
F51 | 0.4278 (5) | 0.7484 (14) | 0.5357 (7) | 0.037 (3)* | 0.4564 |
F52 | 0.4687 (5) | 0.9486 (15) | 0.6128 (7) | 0.029 (3)* | 0.4054 |
F53 | 0.5089 (7) | 0.633 (3) | 0.5313 (11) | 0.044 (5)* | 0.2781 |
F54 | 0.5346 (7) | 0.847 (2) | 0.6238 (10) | 0.030 (4)* | 0.2624 |
F55 | 1.0450 (3) | 0.2040 (10) | 0.9311 (4) | 0.034 (2)* | 0.6214 |
F56 | 0.9619 (3) | 0.2748 (11) | 0.8148 (5) | 0.040 (2)* | 0.6349 |
F57 | 0.9501 (3) | 0.4461 (11) | 0.8931 (4) | 0.042 (2)* | 0.6392 |
F58 | 1.0207 (4) | 0.4260 (12) | 0.8914 (5) | 0.046 (3)* | 0.6381 |
F59 | 0.9837 (4) | 0.0592 (13) | 0.8639 (5) | 0.046 (3)* | 0.5901 |
F60 | 0.9313 (5) | 0.2214 (15) | 0.8875 (6) | 0.050 (3)* | 0.5411 |
F61 | 1.0255 (5) | 0.1168 (18) | 0.8927 (7) | 0.042 (4)* | 0.4052 |
F62 | 0.9896 (5) | 0.1193 (17) | 0.9710 (7) | 0.038 (4)* | 0.3809 |
F63 | 1.0010 (6) | 0.3971 (19) | 0.9757 (8) | 0.037 (4)* | 0.3376 |
F64 | 0.9557 (5) | 0.0502 (17) | 0.8951 (7) | 0.039 (4)* | 0.3967 |
F65 | 1.0091 (6) | 0.2593 (19) | 0.8200 (9) | 0.037 (4)* | 0.343 |
F66 | 0.9603 (7) | 0.238 (2) | 0.9744 (10) | 0.042 (5)* | 0.316 |
F67 | 1.0252 (5) | 0.2423 (15) | 0.9903 (7) | 0.026 (3)* | 0.3803 |
F68 | 0.9699 (7) | 0.455 (2) | 0.8368 (10) | 0.042 (5)* | 0.2993 |
F80 | 0.05722 (17) | 0.2718 (6) | 0.7393 (3) | 0.0333 (14) | |
F81 | 0.35226 (17) | 0.2933 (6) | 0.3553 (2) | 0.0243 (11) | |
F82 | 0.39897 (18) | 0.2533 (6) | 0.0191 (3) | 0.0366 (15) | |
F83 | 0.1993 (3) | 0.4983 (10) | 0.9853 (4) | 0.085 (3) | |
F84 | 0.0929 (3) | 0.2668 (8) | 0.1148 (4) | 0.056 (2) | |
F85 | 0.1503 (2) | 0.2855 (7) | 0.0072 (4) | 0.064 (3) | |
N1 | 0.2016 (3) | 0.0297 (10) | 0.9943 (4) | 0.035 (2) | |
N2 | 0.3062 (2) | 0.4596 (8) | 0.8071 (3) | 0.0206 (15) | |
N3 | 0.2994 (2) | 0.9840 (8) | 0.7971 (3) | 0.0216 (15) | |
N4 | 0.1069 (3) | 0.0136 (10) | 0.7190 (4) | 0.037 (2) | |
N5 | 0.1046 (3) | 0.5029 (9) | 0.7200 (4) | 0.0265 (17) | |
N6 | 0.0144 (3) | 0.2493 (11) | 0.6016 (5) | 0.040 (2) | |
N7 | 0.4128 (3) | 0.0221 (9) | 0.4468 (4) | 0.0290 (18) | |
N8 | 0.4095 (3) | 0.5005 (9) | 0.4280 (4) | 0.0321 (19) | |
N9 | 0.0980 (3) | 0.2289 (9) | 0.3630 (4) | 0.0271 (18) | |
N10 | 0.0911 (3) | 0.4781 (12) | 0.0172 (4) | 0.045 (3) | |
N11 | 0.0843 (4) | 0.0276 (11) | 0.0299 (5) | 0.058 (3) | |
N12 | 0.2929 (3) | 0.7749 (7) | 0.1365 (4) | 0.0271 (17) | |
N13 | 0.3897 (2) | 0.5278 (10) | 0.1154 (4) | 0.0283 (18) | |
N14 | 0.3896 (2) | 0.0295 (9) | 0.0984 (3) | 0.0232 (15) | |
N15 | 0.9970 (3) | 0.9894 (11) | 0.7506 (5) | 0.048 (3) | |
N16 | 0.4855 (3) | 0.2409 (8) | 0.5775 (4) | 0.030 (2) | |
N17 | 0.4007 (2) | 0.3052 (9) | 0.2832 (3) | 0.0233 (16) | |
N18 | 0.4983 (3) | 0.5509 (14) | 0.2545 (5) | 0.057 (4) | |
N19 | 0.3174 (2) | 0.2533 (7) | 0.9696 (3) | 0.0175 (14) | |
N20 | 0.2027 (3) | 0.7658 (9) | 0.3278 (4) | 0.036 (2) | |
N21 | 0.4480 (3) | 0.3062 (11) | 0.1774 (5) | 0.051 (3) | |
N22 | 0.1805 (3) | 0.2466 (8) | 0.1340 (4) | 0.0295 (18) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ta1 | 0.01972 (18) | 0.01549 (13) | 0.01511 (14) | −0.00104 (12) | 0.00677 (13) | −0.00104 (10) |
Ta2 | 0.0109 (3) | 0.0109 (3) | 0.0161 (4) | −0.00029 (18) | 0.0047 (2) | 0.00307 (19) |
Ta22 | 0.029 (3) | 0.068 (5) | 0.091 (6) | 0.001 (3) | 0.020 (4) | −0.028 (4) |
Ta3 | 0.01119 (16) | 0.01797 (13) | 0.01549 (14) | −0.00128 (11) | 0.00421 (12) | 0.00102 (12) |
Ta4 | 0.0403 (16) | 0.0197 (5) | 0.0354 (11) | −0.0089 (7) | −0.0140 (11) | 0.0012 (5) |
Ta44 | 0.0067 (8) | 0.0135 (5) | 0.0113 (7) | −0.0005 (4) | 0.0064 (5) | −0.0048 (3) |
Ta5 | 0.01626 (17) | 0.01808 (13) | 0.01662 (15) | 0.00105 (12) | 0.00264 (13) | −0.00195 (11) |
Ta6 | 0.0102 (12) | 0.0128 (6) | 0.0126 (5) | 0.0017 (6) | 0.0027 (7) | −0.0017 (4) |
Ta66 | 0.0353 (19) | 0.0124 (4) | 0.0150 (4) | 0.0039 (7) | 0.0010 (7) | −0.0005 (2) |
Ta7 | 0.01007 (16) | 0.02050 (15) | 0.01569 (15) | 0.00051 (11) | 0.00429 (13) | −0.00119 (11) |
Ta8 | 0.0127 (6) | 0.0224 (6) | 0.0333 (14) | 0.0027 (4) | −0.0020 (7) | −0.0068 (8) |
Ta88 | 0.0125 (6) | 0.0195 (5) | 0.0267 (11) | 0.0002 (4) | −0.0003 (6) | −0.0055 (6) |
F1 | 0.013 (3) | 0.031 (3) | 0.048 (4) | 0.009 (2) | 0.012 (3) | −0.003 (2) |
F2 | 0.039 (4) | 0.026 (2) | 0.033 (3) | −0.013 (2) | 0.013 (3) | −0.012 (2) |
F3 | 0.040 (4) | 0.024 (2) | 0.021 (3) | −0.005 (2) | 0.010 (2) | 0.0081 (18) |
F4 | 0.037 (4) | 0.020 (2) | 0.023 (3) | −0.002 (2) | 0.011 (2) | −0.0065 (18) |
F5 | 0.099 (7) | 0.031 (3) | 0.035 (3) | 0.007 (3) | 0.041 (4) | 0.009 (2) |
F6 | 0.025 (3) | 0.067 (4) | 0.029 (3) | −0.013 (3) | 0.018 (3) | −0.022 (3) |
F7 | 0.019 (3) | 0.038 (3) | 0.018 (2) | 0.001 (2) | 0.001 (2) | −0.001 (2) |
F8 | 0.030 (4) | 0.022 (2) | 0.047 (3) | −0.001 (2) | 0.001 (3) | −0.002 (2) |
F9 | 0.035 (4) | 0.035 (3) | 0.024 (3) | −0.018 (3) | 0.013 (3) | −0.004 (2) |
F10 | 0.039 (4) | 0.047 (3) | 0.030 (3) | 0.020 (3) | 0.018 (3) | 0.021 (2) |
F11 | 0.015 (3) | 0.027 (2) | 0.060 (4) | 0.001 (2) | 0.006 (3) | 0.011 (3) |
F12 | 0.027 (3) | 0.035 (3) | 0.020 (2) | 0.000 (2) | 0.010 (2) | 0.000 (2) |
F13 | 0.040 (4) | 0.020 (2) | 0.041 (3) | 0.004 (2) | 0.028 (3) | 0.000 (2) |
F14 | 0.025 (3) | 0.020 (2) | 0.025 (3) | −0.001 (2) | 0.008 (2) | −0.0008 (18) |
F15 | 0.012 (3) | 0.040 (3) | 0.022 (3) | 0.006 (2) | −0.009 (2) | 0.003 (2) |
F16 | 0.023 (3) | 0.024 (2) | 0.045 (3) | 0.005 (2) | 0.016 (3) | 0.020 (2) |
F17 | 0.023 (3) | 0.031 (3) | 0.036 (3) | 0.000 (2) | 0.006 (2) | −0.017 (2) |
F18 | 0.027 (3) | 0.032 (3) | 0.032 (3) | −0.007 (2) | 0.015 (2) | 0.001 (2) |
F19 | 0.028 (3) | 0.025 (2) | 0.038 (3) | 0.008 (2) | 0.019 (3) | 0.000 (2) |
F20 | 0.027 (3) | 0.028 (2) | 0.019 (3) | −0.002 (2) | 0.008 (2) | −0.0003 (19) |
F21 | 0.012 (3) | 0.025 (2) | 0.020 (2) | 0.0064 (18) | 0.003 (2) | 0.0034 (18) |
F22 | 0.064 (6) | 0.056 (4) | 0.041 (4) | −0.029 (4) | −0.023 (4) | 0.004 (3) |
F23 | 0.026 (4) | 0.036 (3) | 0.066 (5) | 0.002 (3) | 0.006 (3) | −0.013 (3) |
F24 | 0.059 (5) | 0.022 (2) | 0.054 (4) | 0.000 (3) | 0.021 (4) | −0.003 (3) |
F25 | 0.075 (6) | 0.055 (4) | 0.031 (4) | 0.032 (4) | −0.010 (4) | −0.023 (3) |
F26 | 0.029 (3) | 0.028 (3) | 0.041 (3) | 0.001 (2) | −0.010 (3) | 0.007 (2) |
F27 | 0.049 (4) | 0.021 (2) | 0.038 (3) | −0.011 (3) | −0.011 (3) | −0.005 (2) |
F28 | 0.043 (4) | 0.026 (3) | 0.031 (3) | −0.005 (3) | −0.010 (3) | 0.004 (2) |
F29 | 0.030 (4) | 0.037 (3) | 0.023 (3) | −0.004 (2) | −0.003 (3) | 0.001 (2) |
F30 | 0.033 (3) | 0.023 (2) | 0.041 (3) | 0.003 (2) | 0.019 (3) | 0.005 (2) |
F31 | 0.045 (4) | 0.021 (2) | 0.032 (3) | −0.001 (2) | 0.009 (3) | −0.006 (2) |
F32 | 0.018 (3) | 0.051 (3) | 0.041 (3) | 0.004 (3) | 0.010 (3) | −0.021 (3) |
F33 | 0.024 (3) | 0.041 (3) | 0.029 (3) | −0.002 (2) | 0.011 (2) | 0.012 (2) |
F34 | 0.027 (3) | 0.030 (3) | 0.023 (3) | 0.000 (2) | 0.013 (2) | 0.0006 (19) |
F35 | 0.017 (3) | 0.030 (2) | 0.024 (3) | −0.003 (2) | −0.003 (2) | 0.0072 (19) |
F36 | 0.38 (2) | 0.029 (3) | 0.056 (5) | 0.037 (7) | 0.130 (9) | 0.013 (3) |
F37 | 0.074 (6) | 0.066 (5) | 0.105 (7) | 0.042 (4) | −0.058 (5) | −0.066 (5) |
F38 | 0.039 (4) | 0.020 (2) | 0.034 (3) | 0.003 (2) | 0.018 (3) | −0.004 (2) |
F39 | 0.052 (5) | 0.025 (3) | 0.061 (4) | 0.007 (3) | 0.031 (4) | 0.015 (3) |
F40 | 0.076 (6) | 0.026 (3) | 0.046 (4) | 0.014 (3) | −0.027 (4) | 0.004 (3) |
F41 | 0.030 (4) | 0.037 (3) | 0.060 (5) | 0.003 (3) | −0.018 (3) | 0.008 (3) |
F42 | 0.031 (3) | 0.028 (2) | 0.016 (2) | 0.003 (2) | 0.001 (2) | 0.0027 (19) |
F80 | 0.015 (3) | 0.034 (3) | 0.046 (4) | −0.009 (2) | 0.004 (3) | −0.005 (2) |
F81 | 0.021 (3) | 0.021 (2) | 0.031 (3) | −0.006 (2) | 0.010 (2) | 0.001 (2) |
F82 | 0.012 (3) | 0.037 (3) | 0.052 (4) | −0.007 (2) | −0.001 (3) | 0.016 (2) |
F83 | 0.113 (9) | 0.067 (5) | 0.058 (5) | 0.029 (5) | 0.006 (5) | −0.002 (4) |
F84 | 0.047 (5) | 0.071 (5) | 0.051 (5) | −0.001 (4) | 0.018 (4) | −0.004 (4) |
F85 | 0.047 (5) | 0.022 (3) | 0.081 (6) | 0.008 (3) | −0.036 (4) | −0.010 (3) |
N1 | 0.047 (6) | 0.040 (4) | 0.016 (4) | −0.015 (4) | 0.009 (4) | 0.000 (3) |
N2 | 0.015 (4) | 0.022 (3) | 0.026 (4) | −0.008 (3) | 0.008 (3) | −0.002 (3) |
N3 | 0.021 (4) | 0.019 (3) | 0.026 (4) | 0.000 (3) | 0.009 (3) | −0.001 (3) |
N4 | 0.038 (6) | 0.036 (4) | 0.025 (4) | 0.007 (4) | −0.007 (4) | −0.007 (3) |
N5 | 0.026 (5) | 0.029 (4) | 0.025 (4) | −0.002 (3) | 0.008 (4) | 0.004 (3) |
N6 | 0.044 (6) | 0.030 (4) | 0.041 (5) | 0.009 (4) | 0.005 (5) | −0.001 (3) |
N7 | 0.025 (5) | 0.026 (3) | 0.031 (4) | 0.000 (3) | 0.002 (4) | −0.002 (3) |
N8 | 0.022 (5) | 0.025 (3) | 0.049 (5) | −0.004 (3) | 0.012 (4) | 0.012 (3) |
N9 | 0.027 (5) | 0.020 (3) | 0.040 (5) | 0.008 (3) | 0.018 (4) | 0.004 (3) |
N10 | 0.043 (6) | 0.055 (5) | 0.031 (5) | −0.036 (5) | 0.003 (4) | 0.005 (4) |
N11 | 0.061 (8) | 0.032 (5) | 0.058 (7) | 0.013 (5) | −0.013 (6) | −0.007 (4) |
N12 | 0.034 (5) | 0.012 (3) | 0.042 (5) | 0.005 (3) | 0.022 (4) | 0.002 (3) |
N13 | 0.016 (4) | 0.038 (4) | 0.032 (4) | 0.006 (3) | 0.008 (3) | −0.005 (3) |
N14 | 0.017 (4) | 0.032 (3) | 0.022 (4) | 0.004 (3) | 0.010 (3) | 0.006 (3) |
N15 | 0.020 (5) | 0.046 (5) | 0.064 (7) | 0.010 (4) | −0.007 (5) | 0.027 (5) |
N16 | 0.043 (6) | 0.021 (3) | 0.036 (5) | 0.004 (3) | 0.028 (4) | 0.002 (3) |
N17 | 0.014 (4) | 0.026 (3) | 0.030 (4) | 0.000 (3) | 0.007 (3) | 0.009 (3) |
N18 | 0.055 (7) | 0.083 (8) | 0.047 (6) | 0.054 (6) | 0.035 (5) | 0.045 (5) |
N19 | 0.018 (4) | 0.016 (3) | 0.017 (3) | 0.003 (3) | 0.004 (3) | 0.000 (2) |
N20 | 0.034 (6) | 0.025 (4) | 0.032 (4) | 0.004 (3) | −0.011 (4) | −0.004 (3) |
N21 | 0.051 (7) | 0.037 (5) | 0.059 (7) | 0.020 (5) | 0.011 (6) | 0.005 (5) |
N22 | 0.031 (5) | 0.024 (3) | 0.036 (5) | 0.000 (3) | 0.014 (4) | 0.003 (3) |
Geometric parameters (Å, º) top
Ta1—F7 | 1.906 (6) | Ta6—F38 | 1.830 (6) |
Ta1—F5 | 1.934 (6) | Ta6—F36 | 1.842 (8) |
Ta1—F3 | 1.939 (4) | Ta6—F42 | 1.931 (6) |
Ta1—F6 | 1.949 (5) | Ta6—F40 | 2.007 (7) |
Ta1—F2 | 1.951 (5) | Ta6—F37 | 2.078 (9) |
Ta1—F1 | 1.956 (6) | Ta6—F41 | 2.160 (9) |
Ta1—F4 | 1.973 (4) | Ta66—F41 | 1.792 (11) |
Ta2—F11 | 1.918 (6) | Ta66—F37 | 1.839 (8) |
Ta2—F14 | 1.926 (5) | Ta66—F40 | 1.885 (7) |
Ta2—F12 | 1.939 (5) | Ta66—F42 | 1.971 (6) |
Ta2—F13 | 1.940 (5) | Ta66—F38 | 1.980 (7) |
Ta2—F8 | 1.965 (5) | Ta66—F39 | 2.053 (10) |
Ta2—F10 | 1.978 (5) | Ta66—F36 | 2.067 (10) |
Ta2—F9 | 1.986 (6) | Ta7—F46 | 1.890 (10) |
Ta22—F10 | 1.749 (16) | Ta7—F53 | 1.91 (2) |
Ta22—F9 | 1.832 (15) | Ta7—F47 | 1.924 (10) |
Ta22—F8 | 1.900 (11) | Ta7—F45 | 1.947 (9) |
Ta22—F13 | 1.924 (10) | Ta7—F54 | 1.95 (2) |
Ta22—F11 | 2.013 (14) | Ta7—F51 | 1.957 (15) |
Ta22—F12 | 2.093 (14) | Ta7—F44 | 1.962 (7) |
Ta22—F14 | 2.19 (2) | Ta7—F48 | 1.964 (9) |
Ta3—F20 | 1.938 (5) | Ta7—F50 | 1.971 (13) |
Ta3—F18 | 1.940 (5) | Ta7—F43 | 1.971 (6) |
Ta3—F17 | 1.941 (5) | Ta7—F49 | 2.035 (10) |
Ta3—F21 | 1.947 (5) | Ta7—F52 | 2.098 (14) |
Ta3—F16 | 1.951 (5) | Ta8—F62 | 1.760 (14) |
Ta3—F19 | 1.965 (5) | Ta8—F60 | 1.795 (16) |
Ta3—F15 | 1.988 (5) | Ta8—F63 | 1.877 (18) |
Ta4—F25 | 1.780 (12) | Ta8—F67 | 1.916 (16) |
Ta4—F28 | 1.856 (10) | Ta8—F66 | 1.93 (2) |
Ta4—F26 | 1.923 (6) | Ta8—F59 | 1.955 (11) |
Ta4—F24 | 1.958 (6) | Ta8—F61 | 1.979 (17) |
Ta4—F27 | 1.987 (7) | Ta8—F64 | 1.980 (16) |
Ta4—F22 | 2.059 (9) | Ta8—F57 | 2.010 (10) |
Ta4—F23 | 2.155 (14) | Ta8—F55 | 2.052 (12) |
Ta44—F23 | 1.796 (8) | Ta8—F56 | 2.066 (13) |
Ta44—F27 | 1.906 (6) | Ta8—F58 | 2.077 (13) |
Ta44—F22 | 1.925 (8) | Ta88—F58 | 1.736 (12) |
Ta44—F24 | 1.946 (6) | Ta88—F56 | 1.744 (12) |
Ta44—F26 | 1.957 (6) | Ta88—F61 | 1.841 (16) |
Ta44—F28 | 2.086 (8) | Ta88—F59 | 1.924 (11) |
Ta44—F25 | 2.104 (8) | Ta88—F55 | 1.951 (11) |
Ta5—F31 | 1.924 (5) | Ta88—F68 | 2.01 (2) |
Ta5—F35 | 1.931 (5) | Ta88—F57 | 2.020 (10) |
Ta5—F29 | 1.947 (5) | Ta88—F65 | 2.03 (2) |
Ta5—F30 | 1.954 (5) | Ta88—F60 | 2.031 (16) |
Ta5—F34 | 1.959 (5) | Ta88—F63 | 2.074 (18) |
Ta5—F32 | 1.977 (5) | Ta88—F67 | 2.165 (16) |
Ta5—F33 | 1.995 (5) | Ta88—F62 | 2.181 (13) |
Ta6—F39 | 1.749 (9) | | |
| | | |
F7—Ta1—F3 | 80.0 (2) | F60—Ta8—F63 | 110.2 (8) |
F7—Ta1—F6 | 77.3 (2) | F62—Ta8—F67 | 50.6 (7) |
F5—Ta1—F6 | 76.3 (3) | F60—Ta8—F67 | 130.3 (8) |
F3—Ta1—F2 | 79.0 (2) | F63—Ta8—F67 | 48.1 (7) |
F6—Ta1—F2 | 74.4 (2) | F62—Ta8—F66 | 46.5 (8) |
F5—Ta1—F1 | 77.5 (3) | F60—Ta8—F66 | 61.8 (9) |
F2—Ta1—F1 | 75.8 (2) | F63—Ta8—F66 | 62.1 (9) |
F7—Ta1—F4 | 77.2 (2) | F67—Ta8—F66 | 69.2 (9) |
F5—Ta1—F4 | 78.4 (2) | F62—Ta8—F59 | 81.7 (6) |
F3—Ta1—F4 | 83.7 (2) | F60—Ta8—F59 | 83.3 (6) |
F1—Ta1—F4 | 79.0 (2) | F63—Ta8—F59 | 158.8 (7) |
F11—Ta2—F14 | 77.2 (2) | F67—Ta8—F59 | 110.6 (5) |
F14—Ta2—F12 | 75.4 (2) | F66—Ta8—F59 | 114.7 (8) |
F13—Ta2—F10 | 77.0 (2) | F62—Ta8—F61 | 83.5 (7) |
F8—Ta2—F10 | 81.5 (2) | F60—Ta8—F61 | 127.5 (7) |
F12—Ta2—F9 | 77.6 (2) | F63—Ta8—F61 | 119.6 (8) |
F13—Ta2—F9 | 77.2 (2) | F67—Ta8—F61 | 78.8 (6) |
F8—Ta2—F9 | 87.9 (2) | F66—Ta8—F61 | 129.9 (9) |
F10—Ta2—F9 | 83.1 (3) | F59—Ta8—F61 | 44.2 (6) |
F10—Ta22—F9 | 94.5 (10) | F62—Ta8—F64 | 58.9 (7) |
F10—Ta22—F8 | 89.7 (7) | F60—Ta8—F64 | 52.4 (6) |
F9—Ta22—F8 | 94.5 (7) | F63—Ta8—F64 | 135.8 (9) |
F10—Ta22—F13 | 83.1 (6) | F67—Ta8—F64 | 107.6 (7) |
F9—Ta22—F13 | 81.3 (5) | F66—Ta8—F64 | 75.1 (8) |
F8—Ta22—F13 | 171.4 (12) | F59—Ta8—F64 | 41.3 (6) |
F10—Ta22—F11 | 81.4 (5) | F61—Ta8—F64 | 79.4 (7) |
F9—Ta22—F11 | 170.1 (9) | F62—Ta8—F57 | 125.6 (7) |
F8—Ta22—F11 | 76.5 (4) | F60—Ta8—F57 | 63.8 (5) |
F13—Ta22—F11 | 107.0 (6) | F63—Ta8—F57 | 67.9 (6) |
F10—Ta22—F12 | 159.7 (9) | F67—Ta8—F57 | 115.8 (5) |
F9—Ta22—F12 | 77.3 (4) | F66—Ta8—F57 | 79.2 (7) |
F8—Ta22—F12 | 72.8 (4) | F59—Ta8—F57 | 133.3 (5) |
F13—Ta22—F12 | 113.3 (7) | F61—Ta8—F57 | 150.8 (8) |
F11—Ta22—F12 | 103.6 (8) | F64—Ta8—F57 | 116.1 (6) |
F10—Ta22—F14 | 132.1 (6) | F62—Ta8—F55 | 81.7 (6) |
F9—Ta22—F14 | 119.2 (7) | F60—Ta8—F55 | 159.4 (5) |
F8—Ta22—F14 | 117.8 (8) | F63—Ta8—F55 | 85.7 (7) |
F13—Ta22—F14 | 70.8 (5) | F67—Ta8—F55 | 51.9 (5) |
F11—Ta22—F14 | 69.5 (6) | F66—Ta8—F55 | 119.2 (8) |
F12—Ta22—F14 | 67.0 (6) | F59—Ta8—F55 | 77.9 (5) |
F20—Ta3—F18 | 79.3 (2) | F61—Ta8—F55 | 34.1 (5) |
F20—Ta3—F17 | 119.9 (2) | F64—Ta8—F55 | 107.1 (6) |
F18—Ta3—F17 | 79.3 (2) | F57—Ta8—F55 | 136.3 (5) |
F20—Ta3—F21 | 75.8 (2) | F62—Ta8—F56 | 142.4 (6) |
F18—Ta3—F21 | 129.0 (2) | F60—Ta8—F56 | 72.5 (5) |
F17—Ta3—F21 | 75.9 (2) | F63—Ta8—F56 | 133.8 (7) |
F20—Ta3—F16 | 114.1 (2) | F67—Ta8—F56 | 157.1 (7) |
F18—Ta3—F16 | 155.2 (2) | F66—Ta8—F56 | 133.6 (8) |
F17—Ta3—F16 | 108.4 (3) | F59—Ta8—F56 | 65.0 (5) |
F21—Ta3—F16 | 75.7 (2) | F61—Ta8—F56 | 84.2 (6) |
F20—Ta3—F19 | 77.6 (2) | F64—Ta8—F56 | 84.0 (5) |
F18—Ta3—F19 | 84.8 (2) | F57—Ta8—F56 | 73.7 (4) |
F17—Ta3—F19 | 153.1 (2) | F55—Ta8—F56 | 106.3 (6) |
F21—Ta3—F19 | 130.5 (2) | F62—Ta8—F58 | 135.5 (6) |
F16—Ta3—F19 | 78.4 (2) | F60—Ta8—F58 | 134.0 (6) |
F20—Ta3—F15 | 150.9 (2) | F63—Ta8—F58 | 69.5 (6) |
F18—Ta3—F15 | 81.3 (2) | F67—Ta8—F58 | 85.4 (5) |
F17—Ta3—F15 | 76.9 (2) | F66—Ta8—F58 | 130.9 (7) |
F21—Ta3—F15 | 133.2 (2) | F59—Ta8—F58 | 113.4 (6) |
F16—Ta3—F15 | 77.8 (2) | F61—Ta8—F58 | 81.4 (6) |
F19—Ta3—F15 | 79.4 (2) | F64—Ta8—F58 | 154.0 (7) |
F25—Ta4—F28 | 83.8 (6) | F57—Ta8—F58 | 75.2 (5) |
F25—Ta4—F26 | 82.5 (4) | F55—Ta8—F58 | 62.8 (4) |
F28—Ta4—F26 | 123.7 (5) | F56—Ta8—F58 | 76.9 (5) |
F25—Ta4—F24 | 92.4 (4) | F58—Ta88—F56 | 95.5 (6) |
F28—Ta4—F24 | 78.4 (3) | F58—Ta88—F61 | 95.3 (7) |
F26—Ta4—F24 | 156.2 (4) | F56—Ta88—F61 | 98.4 (6) |
F25—Ta4—F27 | 133.0 (6) | F58—Ta88—F59 | 134.0 (6) |
F28—Ta4—F27 | 75.8 (3) | F56—Ta88—F59 | 72.0 (5) |
F26—Ta4—F27 | 75.0 (3) | F61—Ta88—F59 | 46.2 (6) |
F24—Ta4—F27 | 123.2 (4) | F58—Ta88—F55 | 71.2 (5) |
F25—Ta4—F22 | 85.4 (4) | F56—Ta88—F55 | 126.1 (6) |
F28—Ta4—F22 | 156.5 (4) | F61—Ta88—F55 | 36.2 (6) |
F26—Ta4—F22 | 75.1 (3) | F59—Ta88—F55 | 81.1 (5) |
F24—Ta4—F22 | 81.4 (3) | F58—Ta88—F68 | 57.9 (8) |
F27—Ta4—F22 | 125.9 (6) | F56—Ta88—F68 | 50.4 (7) |
F25—Ta4—F23 | 154.1 (4) | F61—Ta88—F68 | 129.7 (9) |
F28—Ta4—F23 | 114.5 (4) | F59—Ta88—F68 | 122.2 (7) |
F26—Ta4—F23 | 100.1 (5) | F55—Ta88—F68 | 126.2 (8) |
F24—Ta4—F23 | 74.8 (4) | F58—Ta88—F57 | 82.9 (5) |
F27—Ta4—F23 | 71.6 (4) | F56—Ta88—F57 | 80.6 (4) |
F22—Ta4—F23 | 70.7 (5) | F61—Ta88—F57 | 177.8 (8) |
F23—Ta44—F27 | 81.8 (3) | F59—Ta88—F57 | 134.8 (5) |
F23—Ta44—F22 | 81.8 (4) | F55—Ta88—F57 | 143.4 (4) |
F27—Ta44—F22 | 140.3 (4) | F68—Ta88—F57 | 48.2 (7) |
F23—Ta44—F24 | 83.9 (3) | F58—Ta88—F65 | 67.4 (7) |
F27—Ta44—F24 | 128.5 (3) | F56—Ta88—F65 | 50.4 (7) |
F22—Ta44—F24 | 85.2 (3) | F61—Ta88—F65 | 61.5 (7) |
F23—Ta44—F26 | 113.0 (3) | F59—Ta88—F65 | 71.2 (6) |
F27—Ta44—F26 | 76.1 (3) | F55—Ta88—F65 | 77.1 (7) |
F22—Ta44—F26 | 77.5 (3) | F68—Ta88—F65 | 68.7 (8) |
F24—Ta44—F26 | 153.3 (3) | F57—Ta88—F65 | 116.5 (6) |
F23—Ta44—F28 | 120.8 (3) | F58—Ta88—F60 | 142.3 (5) |
F27—Ta44—F28 | 72.4 (3) | F56—Ta88—F60 | 74.4 (5) |
F22—Ta44—F28 | 145.7 (4) | F61—Ta88—F60 | 121.9 (7) |
F24—Ta44—F28 | 73.3 (3) | F59—Ta88—F60 | 78.2 (5) |
F26—Ta44—F28 | 111.0 (3) | F55—Ta88—F60 | 143.8 (6) |
F23—Ta44—F25 | 159.2 (4) | F68—Ta88—F60 | 90.0 (8) |
F27—Ta44—F25 | 118.9 (3) | F57—Ta88—F60 | 59.8 (5) |
F22—Ta44—F25 | 80.6 (4) | F65—Ta88—F60 | 122.5 (7) |
F24—Ta44—F25 | 83.5 (3) | F58—Ta88—F63 | 72.1 (6) |
F26—Ta44—F25 | 73.9 (3) | F56—Ta88—F63 | 143.5 (6) |
F28—Ta44—F25 | 70.9 (3) | F61—Ta88—F63 | 116.6 (7) |
F31—Ta5—F35 | 108.7 (2) | F59—Ta88—F63 | 140.7 (7) |
F31—Ta5—F29 | 79.8 (2) | F55—Ta88—F63 | 83.3 (6) |
F35—Ta5—F29 | 158.9 (3) | F68—Ta88—F63 | 96.0 (8) |
F31—Ta5—F30 | 121.0 (3) | F57—Ta88—F63 | 64.1 (6) |
F35—Ta5—F30 | 111.0 (2) | F65—Ta88—F63 | 138.8 (8) |
F29—Ta5—F30 | 78.6 (2) | F60—Ta88—F63 | 94.4 (7) |
F31—Ta5—F34 | 74.7 (2) | F58—Ta88—F67 | 87.3 (5) |
F35—Ta5—F34 | 77.2 (3) | F56—Ta88—F67 | 173.8 (5) |
F29—Ta5—F34 | 123.9 (3) | F61—Ta88—F67 | 75.8 (6) |
F30—Ta5—F34 | 73.6 (2) | F59—Ta88—F67 | 102.1 (5) |
F31—Ta5—F32 | 79.2 (3) | F55—Ta88—F67 | 49.7 (5) |
F35—Ta5—F32 | 79.9 (2) | F68—Ta88—F67 | 135.2 (7) |
F29—Ta5—F32 | 82.9 (3) | F57—Ta88—F67 | 105.3 (5) |
F30—Ta5—F32 | 149.0 (3) | F65—Ta88—F67 | 126.4 (7) |
F34—Ta5—F32 | 137.2 (2) | F60—Ta88—F67 | 106.7 (7) |
F31—Ta5—F33 | 153.0 (2) | F63—Ta88—F67 | 42.7 (6) |
F35—Ta5—F33 | 79.8 (2) | F58—Ta88—F62 | 129.8 (6) |
F29—Ta5—F33 | 84.5 (2) | F56—Ta88—F62 | 134.5 (6) |
F30—Ta5—F33 | 76.5 (2) | F61—Ta88—F62 | 76.2 (7) |
F34—Ta5—F33 | 132.2 (2) | F59—Ta88—F62 | 72.5 (6) |
F32—Ta5—F33 | 77.2 (3) | F55—Ta88—F62 | 74.3 (6) |
F39—Ta6—F38 | 114.8 (4) | F68—Ta88—F62 | 154.1 (8) |
F39—Ta6—F36 | 84.8 (5) | F57—Ta88—F62 | 106.0 (6) |
F38—Ta6—F36 | 83.9 (4) | F65—Ta88—F62 | 136.5 (6) |
F39—Ta6—F42 | 80.1 (3) | F60—Ta88—F62 | 71.3 (6) |
F38—Ta6—F42 | 79.3 (3) | F63—Ta88—F62 | 68.7 (7) |
F36—Ta6—F42 | 150.1 (7) | F67—Ta88—F62 | 42.6 (6) |
F39—Ta6—F40 | 81.2 (3) | Ta22—F8—Ta2 | 8.0 (6) |
F38—Ta6—F40 | 157.3 (4) | Ta22—F9—Ta2 | 7.0 (6) |
F36—Ta6—F40 | 81.5 (5) | Ta22—F10—Ta2 | 4.9 (5) |
F42—Ta6—F40 | 120.9 (3) | Ta2—F11—Ta22 | 7.6 (5) |
F39—Ta6—F37 | 158.0 (4) | Ta2—F12—Ta22 | 6.6 (5) |
F38—Ta6—F37 | 76.6 (3) | Ta22—F13—Ta2 | 8.2 (6) |
F36—Ta6—F37 | 77.5 (6) | Ta2—F14—Ta22 | 2.7 (3) |
F42—Ta6—F37 | 121.5 (5) | Ta44—F22—Ta4 | 9.9 (3) |
F40—Ta6—F37 | 83.2 (3) | Ta44—F23—Ta4 | 2.25 (16) |
F39—Ta6—F41 | 119.3 (3) | Ta44—F24—Ta4 | 10.8 (3) |
F38—Ta6—F41 | 109.8 (3) | Ta4—F25—Ta44 | 5.1 (2) |
F36—Ta6—F41 | 139.6 (7) | Ta4—F26—Ta44 | 10.8 (3) |
F42—Ta6—F41 | 70.0 (3) | Ta44—F27—Ta4 | 10.6 (3) |
F40—Ta6—F41 | 72.0 (4) | Ta4—F28—Ta44 | 8.4 (3) |
F37—Ta6—F41 | 69.6 (4) | Ta6—F36—Ta66 | 9.86 (14) |
F41—Ta66—F37 | 83.6 (6) | Ta66—F37—Ta6 | 9.5 (2) |
F41—Ta66—F40 | 83.7 (5) | Ta6—F38—Ta66 | 11.29 (11) |
F37—Ta66—F40 | 93.6 (4) | Ta6—F39—Ta66 | 8.01 (15) |
F41—Ta66—F42 | 77.3 (3) | Ta66—F40—Ta6 | 11.35 (14) |
F37—Ta66—F42 | 133.3 (4) | Ta66—F41—Ta6 | 4.80 (16) |
F40—Ta66—F42 | 125.4 (3) | Ta6—F42—Ta66 | 11.82 (12) |
F41—Ta66—F38 | 120.2 (3) | F54—F45—Ta7 | 75.8 (14) |
F37—Ta66—F38 | 79.0 (3) | F52—F46—Ta7 | 98.6 (17) |
F40—Ta66—F38 | 153.5 (5) | F53—F47—F54 | 134.4 (15) |
F42—Ta66—F38 | 74.9 (3) | F53—F47—Ta7 | 69.1 (11) |
F41—Ta66—F39 | 122.9 (3) | F54—F47—Ta7 | 66.3 (9) |
F37—Ta66—F39 | 149.7 (6) | F50—F49—Ta7 | 68.4 (7) |
F40—Ta66—F39 | 76.9 (3) | F49—F50—F51 | 108.3 (11) |
F42—Ta66—F39 | 72.2 (3) | F49—F50—Ta7 | 73.7 (8) |
F38—Ta66—F39 | 96.7 (5) | F51—F50—Ta7 | 63.4 (7) |
F41—Ta66—F36 | 153.6 (6) | F50—F51—Ta7 | 64.3 (7) |
F37—Ta66—F36 | 77.9 (6) | F46—F52—Ta7 | 62.9 (15) |
F40—Ta66—F36 | 78.9 (4) | F47—F53—Ta7 | 70.5 (11) |
F42—Ta66—F36 | 129.1 (7) | F45—F54—F47 | 133.2 (19) |
F38—Ta66—F36 | 74.6 (4) | F45—F54—Ta7 | 75.0 (14) |
F39—Ta66—F36 | 72.0 (5) | F47—F54—Ta7 | 64.4 (8) |
F46—Ta7—F53 | 131.9 (8) | F61—F55—F67 | 114.3 (12) |
F46—Ta7—F47 | 112.2 (4) | F61—F55—Ta88 | 66.8 (10) |
F53—Ta7—F47 | 40.4 (8) | F67—F55—Ta88 | 71.6 (7) |
F46—Ta7—F45 | 79.2 (4) | F61—F55—Ta8 | 69.6 (10) |
F53—Ta7—F45 | 114.3 (8) | F67—F55—Ta8 | 60.1 (6) |
F47—Ta7—F45 | 76.7 (4) | Ta88—F55—Ta8 | 13.26 (9) |
F46—Ta7—F54 | 84.3 (7) | F68—F56—F65 | 89.2 (11) |
F53—Ta7—F54 | 89.3 (10) | F68—F56—Ta88 | 73.4 (9) |
F47—Ta7—F54 | 49.3 (7) | F65—F56—Ta88 | 73.9 (8) |
F45—Ta7—F54 | 29.3 (6) | F68—F56—Ta8 | 78.0 (9) |
F46—Ta7—F51 | 62.2 (5) | F65—F56—Ta8 | 83.1 (8) |
F53—Ta7—F51 | 103.8 (8) | Ta88—F56—Ta8 | 10.47 (13) |
F47—Ta7—F51 | 131.1 (5) | F68—F57—Ta8 | 79.0 (9) |
F45—Ta7—F51 | 138.1 (5) | F68—F57—Ta88 | 65.6 (8) |
F54—Ta7—F51 | 144.4 (7) | Ta8—F57—Ta88 | 13.48 (10) |
F46—Ta7—F44 | 152.3 (4) | Ta88—F58—Ta8 | 9.92 (13) |
F53—Ta7—F44 | 72.7 (7) | F64—F59—F61 | 123.6 (12) |
F47—Ta7—F44 | 77.5 (3) | F64—F59—Ta88 | 82.8 (8) |
F45—Ta7—F44 | 78.1 (3) | F61—F59—Ta88 | 63.9 (8) |
F54—Ta7—F44 | 83.5 (6) | F64—F59—Ta8 | 70.3 (8) |
F51—Ta7—F44 | 131.8 (4) | F61—F59—Ta8 | 68.8 (8) |
F46—Ta7—F48 | 119.6 (4) | Ta88—F59—Ta8 | 13.98 (10) |
F53—Ta7—F48 | 75.0 (8) | F64—F60—Ta8 | 69.5 (8) |
F47—Ta7—F48 | 114.6 (4) | F64—F60—Ta88 | 73.2 (8) |
F45—Ta7—F48 | 146.8 (4) | Ta8—F60—Ta88 | 12.32 (17) |
F54—Ta7—F48 | 156.0 (7) | F55—F61—F59 | 142.0 (15) |
F51—Ta7—F48 | 58.7 (5) | F55—F61—Ta88 | 77.0 (10) |
F44—Ta7—F48 | 74.7 (3) | F59—F61—Ta88 | 69.8 (8) |
F46—Ta7—F50 | 78.5 (5) | F55—F61—Ta8 | 76.3 (10) |
F53—Ta7—F50 | 60.3 (8) | F59—F61—Ta8 | 67.0 (8) |
F47—Ta7—F50 | 78.8 (5) | Ta88—F61—Ta8 | 13.60 (14) |
F45—Ta7—F50 | 137.4 (4) | F66—F62—F67 | 91.7 (13) |
F54—Ta7—F50 | 112.5 (7) | F66—F62—Ta8 | 72.8 (11) |
F51—Ta7—F50 | 52.3 (6) | F67—F62—Ta8 | 69.8 (8) |
F44—Ta7—F50 | 129.1 (4) | F66—F62—Ta88 | 79.1 (10) |
F48—Ta7—F50 | 75.5 (4) | F67—F62—Ta88 | 68.2 (7) |
F46—Ta7—F43 | 80.6 (4) | Ta8—F62—Ta88 | 6.31 (17) |
F53—Ta7—F43 | 145.3 (7) | F67—F63—Ta8 | 67.3 (8) |
F47—Ta7—F43 | 149.8 (3) | F67—F63—Ta88 | 71.8 (9) |
F45—Ta7—F43 | 79.3 (3) | Ta8—F63—Ta88 | 12.50 (17) |
F54—Ta7—F43 | 108.6 (6) | F59—F64—F60 | 108.7 (11) |
F51—Ta7—F43 | 79.1 (4) | F59—F64—Ta8 | 68.4 (8) |
F44—Ta7—F43 | 79.9 (3) | F60—F64—Ta8 | 58.1 (7) |
F48—Ta7—F43 | 77.6 (3) | F59—F64—Ta88 | 59.0 (7) |
F50—Ta7—F43 | 131.3 (4) | F60—F64—Ta88 | 60.8 (7) |
F46—Ta7—F49 | 61.2 (4) | Ta8—F64—Ta88 | 11.01 (15) |
F53—Ta7—F49 | 70.9 (7) | F56—F65—Ta88 | 55.7 (7) |
F47—Ta7—F49 | 62.1 (4) | F56—F65—Ta8 | 56.1 (7) |
F45—Ta7—F49 | 99.6 (4) | Ta88—F65—Ta8 | 4.20 (13) |
F54—Ta7—F49 | 77.0 (7) | F62—F66—Ta8 | 60.7 (10) |
F51—Ta7—F49 | 76.5 (5) | F62—F66—Ta88 | 63.9 (10) |
F44—Ta7—F49 | 138.6 (4) | Ta8—F66—Ta88 | 3.27 (17) |
F48—Ta7—F49 | 113.3 (4) | F63—F67—F62 | 100.4 (13) |
F50—Ta7—F49 | 37.8 (5) | F63—F67—F55 | 108.9 (11) |
F43—Ta7—F49 | 141.0 (4) | F62—F67—F55 | 97.8 (10) |
F46—Ta7—F52 | 18.4 (4) | F63—F67—Ta8 | 64.6 (9) |
F53—Ta7—F52 | 142.7 (8) | F62—F67—Ta8 | 59.5 (7) |
F47—Ta7—F52 | 111.4 (5) | F55—F67—Ta8 | 68.1 (7) |
F45—Ta7—F52 | 62.0 (5) | F63—F67—Ta88 | 65.5 (8) |
F54—Ta7—F52 | 72.7 (7) | F62—F67—Ta88 | 69.2 (7) |
F51—Ta7—F52 | 77.3 (6) | F55—F67—Ta88 | 58.8 (6) |
F44—Ta7—F52 | 134.3 (5) | Ta8—F67—Ta88 | 11.34 (15) |
F48—Ta7—F52 | 130.3 (5) | F56—F68—F57 | 97.0 (12) |
F50—Ta7—F52 | 96.3 (5) | F56—F68—Ta88 | 56.2 (7) |
F43—Ta7—F52 | 72.0 (4) | F57—F68—Ta88 | 66.2 (8) |
F49—Ta7—F52 | 73.3 (5) | F56—F68—Ta8 | 59.6 (7) |
F62—Ta8—F60 | 87.4 (8) | F57—F68—Ta8 | 57.4 (7) |
F62—Ta8—F63 | 82.6 (8) | Ta88—F68—Ta8 | 8.90 (15) |
Subscribe to Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.