Ammonium tantalum oxide fluorides: new features of dynamic disorder

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, (NH₄)₃TaOF₆, 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 24e and two 96j). The tantalum atom is seven-coordinated in the form of a pentagonal bipyramid (PB) and occupies the 4a 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 8c into the 32f site), while the other group in the 4b site forms eight spatial orientations due to disordering of hydrogen atoms in the 96k and 32f positions. Strong dynamic disorder of [TaOF₆]^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.

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.

(I)

Crystal data

(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) Å^3	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

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.006	H-atom parameters not refined
wR(F^2) = 0.014	w = 1/[σ^2(Fo^2) + (0.0081P)^2 + 0.0421P] where P = (Fo^2 + 2Fc^2)/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+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0082 (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)
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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Ta1—F1	1.888 (11)	N2—F1^xv	2.777 (11)
Ta1—F1^i	1.888 (11)	N2—F1^xvi	2.777 (11)
Ta1—F1^ii	1.888 (11)	N2—F2^xvii	2.826 (18)
Ta1—F2^iii	1.974 (13)	N2—F2^x	2.826 (18)
Ta1—F2^iv	1.974 (13)	N2—H2	0.9018
Ta1—F3^v	2.091 (8)	N2—H3	0.8970
Ta1—F3^vi	2.091 (8)	F1—F2^xviii	2.32 (2)
N1—N1^vii	0.31 (2)	F1—F2^xix	2.32 (2)
N1—N1^viii	0.31 (2)	F1—F1^i	2.671 (15)
N1—N1^ix	0.31 (2)	F1—F1^xx	2.671 (15)
N1—F3^x	2.559 (9)	F1—F2^i	2.732 (7)
N1—F3^xi	2.559 (9)	F1—F2^v	2.732 (7)
N1—F3^xii	2.606 (6)	F1—F2^xxi	2.732 (7)
N1—F3^xiii	2.606 (6)	F1—F2^xxii	2.732 (7)
N1—F3^xiv	2.606 (6)	F1—F3^v	2.817 (7)
N1—H11	0.8844	F1—F3^i	2.817 (7)
N1—H12	0.8904	F1—F3^xxi	2.817 (7)
N1—H13	0.8904	F1—F3^xxii	2.817 (7)
N1—H14	0.8904	F1—F3^xxiii	2.817 (7)
F1—Ta1—F1^i	90.0	F1^xxv—Ta1—F2^iii	90.0
F1—Ta1—F1^ii	90.0	F2^xxvi—Ta1—F3^xxvii	72.1 (8)
F1^xxiv—Ta1—F2^iii	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.

(II)

Crystal data

(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) Å^3	T = 296 K
Z = 6	Prism, colourless
F(000) = 2118	0.30 × 0.22 × 0.16 mm

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.035	H-atom parameters not refined
wR(F^2) = 0.101	w = 1/[σ^2(Fo^2) + (0.052P)^2 + 12.6611P] where P = (Fo^2 + 2Fc^2)/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+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00028 (8)

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)
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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Ta1—Ta11^i	0.381 (11)	Ta2—F5^vii	2.028 (7)
Ta1—Ta11^ii	0.381 (11)	Ta22—F5	1.917 (11)
Ta1—Ta11^iii	0.381 (11)	Ta22—F5^vi	1.917 (11)
Ta1—Ta11^iv	0.381 (11)	Ta22—F5^vii	1.917 (11)
Ta1—Ta11^v	0.381 (11)	Ta22—F6	1.975 (7)
Ta1—F1	1.835 (12)	Ta22—F6^vi	1.975 (7)
Ta1—F3^ii	2.003 (7)	Ta22—F6^vii	1.975 (7)
Ta1—F3	2.003 (7)	Ta22—F7	2.070 (18)
Ta1—F3^iii	2.003 (7)	F1—Ta11^i	2.10 (2)
Ta1—F2	2.201 (19)	F1—Ta11^iii	2.10 (2)
Ta1—F4^ii	2.079 (9)	F1—Ta11^ii	2.10 (2)
Ta1—F4	2.079 (9)	F1—Ta11^iv	2.10 (2)
Ta11—Ta11^iv	0.26 (4)	F1—Ta11^v	2.10 (2)
Ta11—Ta11^v	0.32 (3)	F2—Ta11^ii	1.97 (2)
Ta11—Ta11^iii	0.499 (16)	F2—Ta11^i	1.97 (2)
Ta11—Ta11^ii	0.499 (16)	F2—Ta11^iv	1.97 (2)
Ta11—Ta11^i	0.575 (19)	F2—Ta11^iii	1.97 (2)
Ta11—F4^iii	1.77 (2)	F2—Ta11^v	1.97 (2)
Ta11—F2	1.97 (2)	F3—Ta11^iv	1.839 (13)
Ta11—F3	1.839 (13)	F3—Ta11^v	2.11 (2)
Ta11—F4	1.99 (2)	F3—Ta11^ii	2.11 (2)
Ta11—F3^iii	2.11 (2)	F3—Ta11^iii	2.307 (18)
Ta11—F1	2.10 (2)	F3—Ta11^i	2.307 (18)
Ta11—F4^ii	2.243 (12)	F4—Ta11^iv	1.77 (2)
Ta2—F7	1.901 (12)	F4—Ta11^ii	1.77 (2)
Ta2—F6	1.933 (6)	F4—Ta11^i	1.99 (2)
Ta2—F6^vi	1.933 (6)	F4—Ta11^v	2.243 (12)
Ta2—F6^vii	1.933 (6)	F4—Ta11^iii	2.243 (12)
Ta2—F5	2.028 (7)	N1—H1	0.9462
Ta2—F5^vi	2.028 (7)
Ta11^i—Ta1—Ta11^ii	39 (6)	Ta11^iv—Ta11—F3	86.0 (6)
Ta11^i—Ta1—Ta11^iii	50 (5)	Ta11^v—Ta11—F3	146.2 (6)
Ta11^ii—Ta1—Ta11^iii	82 (3)	Ta11^iii—Ta11—F3	157.2 (6)
Ta11^i—Ta1—Ta11^iv	82 (3)	Ta11^ii—Ta11—F3	117 (4)
Ta11^ii—Ta1—Ta11^iv	50 (5)	Ta11^i—Ta11—F3	139.6 (6)
Ta11^iii—Ta1—Ta11^iv	98 (4)	F4^iii—Ta11—F3	80.1 (4)
Ta11^i—Ta1—Ta11^v	82 (3)	F2—Ta11—F3	119.9 (8)
Ta11^ii—Ta1—Ta11^v	98 (4)	Ta11^iv—Ta11—F4	27.1 (5)
Ta11^iii—Ta1—Ta11^v	39 (6)	Ta11^v—Ta11—F4	138.2 (3)
Ta11^iv—Ta1—Ta11^v	82 (3)	Ta11^iii—Ta11—F4	114 (4)
Ta11^i—Ta1—F1	130.8 (18)	Ta11^ii—Ta11—F4	57 (4)
Ta11^ii—Ta1—F1	130.8 (18)	Ta11^i—Ta11—F4	81.7 (3)
Ta11^iii—Ta1—F1	130.8 (18)	F4^iii—Ta11—F4	122.0 (8)
Ta11^iv—Ta1—F1	130.8 (18)	F2—Ta11—F4	72.3 (7)
Ta11^v—Ta1—F1	130.8 (18)	F3—Ta11—F4	74.5 (6)
Ta11^i—Ta1—F3^ii	59 (2)	Ta11^iv—Ta11—F3^iii	137.6 (4)
Ta11^ii—Ta1—F3^ii	59 (2)	Ta11^v—Ta11—F3^iii	29.0 (3)
Ta11^iii—Ta1—F3^ii	101 (3)	Ta11^iii—Ta11—F3^iii	51 (3)
Ta11^iv—Ta1—F3^ii	101 (3)	Ta11^ii—Ta11—F3^iii	107 (4)
Ta11^v—Ta1—F3^ii	140 (3)	Ta11^i—Ta11—F3^iii	82.2 (3)
F1—Ta1—F3^ii	76.6 (3)	F4^iii—Ta11—F3^iii	72.9 (8)
Ta11^i—Ta1—F3	140 (3)	F2—Ta11—F3^iii	107.8 (8)
Ta11^ii—Ta1—F3	101 (3)	F3—Ta11—F3^iii	117.2 (9)
Ta11^iii—Ta1—F3	140 (3)	F4—Ta11—F3^iii	163.7 (6)
Ta11^iv—Ta1—F3	59 (2)	Ta11^iv—Ta11—F1	86.5 (5)
Ta11^v—Ta1—F3	101 (3)	Ta11^v—Ta11—F1	85.6 (4)
F1—Ta1—F3	76.6 (3)	Ta11^iii—Ta11—F1	83.2 (2)
F3^ii—Ta1—F3	114.8 (2)	Ta11^ii—Ta11—F1	83.2 (2)
Ta11^i—Ta1—F3^iii	101 (3)	Ta11^i—Ta11—F1	82.1 (3)
Ta11^ii—Ta1—F3^iii	140 (3)	F4^iii—Ta11—F1	115.4 (9)
Ta11^iii—Ta1—F3^iii	59 (2)	F2—Ta11—F1	163.7 (5)
Ta11^iv—Ta1—F3^iii	140 (3)	F3—Ta11—F1	74.0 (6)
Ta11^v—Ta1—F3^iii	59 (2)	F4—Ta11—F1	106.3 (9)
F1—Ta1—F3^iii	76.6 (3)	F3^iii—Ta11—F1	68.8 (6)
F3^ii—Ta1—F3^iii	114.8 (2)	Ta11^iv—Ta11—F4^ii	86.7 (5)
F3—Ta1—F3^iii	114.8 (2)	Ta11^v—Ta11—F4^ii	36.3 (5)
Ta11^i—Ta1—F2	49.2 (18)	Ta11^iii—Ta11—F4^ii	16.8 (15)
Ta11^ii—Ta1—F2	49.2 (18)	Ta11^ii—Ta11—F4^ii	54 (3)
Ta11^iii—Ta1—F2	49.2 (18)	Ta11^i—Ta11—F4^ii	30.4 (5)
Ta11^iv—Ta1—F2	49.2 (18)	F4^iii—Ta11—F4^ii	109.8 (9)
Ta11^v—Ta1—F2	49.2 (18)	F2—Ta11—F4^ii	67.1 (5)
F1—Ta1—F2	180.0	F3—Ta11—F4^ii	169.5 (11)
F3^ii—Ta1—F2	103.4 (3)	F4—Ta11—F4^ii	101.9 (7)
F3—Ta1—F2	103.4 (3)	F3^iii—Ta11—F4^ii	64.4 (4)
F3^iii—Ta1—F2	103.4 (3)	F1—Ta11—F4^ii	98.0 (6)
Ta11^i—Ta1—F4^ii	33 (3)	F7—Ta2—F6	78.4 (3)
Ta11^ii—Ta1—F4^ii	72 (3)	F7—Ta2—F6^vi	78.4 (3)
Ta11^iii—Ta1—F4^ii	33 (3)	F6—Ta2—F6^vi	116.0 (2)
Ta11^iv—Ta1—F4^ii	110.9 (19)	F7—Ta2—F6^vii	78.4 (3)
Ta11^v—Ta1—F4^ii	72 (3)	F6—Ta2—F6^vii	116.0 (2)
F1—Ta1—F4^ii	113.8 (3)	F6^vi—Ta2—F6^vii	116.0 (2)
F3^ii—Ta1—F4^ii	69.40 (15)	F7—Ta2—F5	132.9 (2)
F3—Ta1—F4^ii	169.6 (5)	F6—Ta2—F5	77.20 (19)
F3^iii—Ta1—F4^ii	69.40 (15)	F6^vi—Ta2—F5	77.21 (19)
F2—Ta1—F4^ii	66.2 (3)	F6^vii—Ta2—F5	148.7 (5)
Ta11^i—Ta1—F4	72 (3)	F7—Ta2—F5^vi	132.9 (2)
Ta11^ii—Ta1—F4	33 (3)	F6—Ta2—F5^vi	148.7 (5)
Ta11^iii—Ta1—F4	110.9 (19)	F6^vi—Ta2—F5^vi	77.21 (19)
Ta11^iv—Ta1—F4	33 (3)	F6^vii—Ta2—F5^vi	77.21 (19)
Ta11^v—Ta1—F4	110.9 (19)	F5—Ta2—F5^vi	78.7 (4)
F1—Ta1—F4	113.8 (3)	F7—Ta2—F5^vii	132.9 (2)
F3^ii—Ta1—F4	69.40 (15)	F6—Ta2—F5^vii	77.20 (19)
F3—Ta1—F4	69.40 (15)	F6^vi—Ta2—F5^vii	148.7 (5)
F3^iii—Ta1—F4	169.6 (5)	F6^vii—Ta2—F5^vii	77.21 (19)
F2—Ta1—F4	66.2 (3)	F5—Ta2—F5^vii	78.7 (4)
F4^ii—Ta1—F4	104.8 (4)	F5^vi—Ta2—F5^vii	78.7 (4)
Ta11^iv—Ta11—Ta11^v	120.00 (14)	F5—Ta22—F5^vi	84.3 (6)
Ta11^iv—Ta11—Ta11^iii	94 (4)	F5—Ta22—F5^vii	84.3 (6)
Ta11^v—Ta11—Ta11^iii	26 (4)	F5^vi—Ta22—F5^vii	84.3 (6)
Ta11^iv—Ta11—Ta11^ii	34 (4)	F5—Ta22—F6	78.9 (2)
Ta11^v—Ta11—Ta11^ii	86 (4)	F5^vi—Ta22—F6	157.3 (8)
Ta11^iii—Ta11—Ta11^ii	60.000 (3)	F5^vii—Ta22—F6	78.9 (2)
Ta11^iv—Ta11—Ta11^i	60.00 (6)	F5—Ta22—F6^vi	78.9 (2)
Ta11^v—Ta11—Ta11^i	60.00 (2)	F5^vi—Ta22—F6^vi	78.9 (2)
Ta11^iii—Ta11—Ta11^i	34 (4)	F5^vii—Ta22—F6^vi	157.3 (8)
Ta11^ii—Ta11—Ta11^i	26 (4)	F6—Ta22—F6^vi	112.3 (4)
Ta11^iv—Ta11—F4^iii	149.1 (6)	F5—Ta22—F6^vii	157.3 (8)
Ta11^v—Ta11—F4^iii	84.8 (5)	F5^vi—Ta22—F6^vii	78.9 (2)
Ta11^iii—Ta11—F4^iii	110 (4)	F5^vii—Ta22—F6^vii	78.9 (2)
Ta11^ii—Ta11—F4^iii	158.6 (18)	F6—Ta22—F6^vii	112.3 (4)
Ta11^i—Ta11—F4^iii	140.2 (4)	F6^vi—Ta22—F6^vii	112.3 (4)
Ta11^iv—Ta11—F2	86.3 (6)	F5—Ta22—F7	129.2 (4)
Ta11^v—Ta11—F2	85.4 (5)	F5^vi—Ta22—F7	129.2 (4)
Ta11^iii—Ta11—F2	82.7 (3)	F5^vii—Ta22—F7	129.2 (4)
Ta11^ii—Ta11—F2	82.7 (3)	F6—Ta22—F7	73.5 (5)
Ta11^i—Ta11—F2	81.6 (3)	F6^vi—Ta22—F7	73.5 (5)
F4^iii—Ta11—F2	77.2 (8)	F6^vii—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.

(III)

Crystal data

(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) Å^3	Plate, colourless
Z = 4	0.25 × 0.22 × 0.05 mm
F(000) = 2750

Data collection

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

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)] = 0.033	w = 1/[σ^2(Fo^2) + (0.045P)^2 + 8.7205P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 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+0.001xFc^2λ^3/sin(2θ)]^-1/4
7 restraints	Extinction coefficient: 0.00053 (5)

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)
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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Ta1—F1	1.837 (10)	Ta33—F14^i	2.189 (5)
Ta1—F3	1.913 (6)	Ta33—F13^i	2.367 (7)
Ta1—F3^i	1.913 (6)	Ta4—F23	1.93 (3)
Ta1—F2^i	1.927 (5)	Ta4—F22^i	1.904 (15)
Ta1—F2	1.927 (5)	Ta4—F22	1.904 (15)
Ta1—F5	2.020 (8)	Ta4—F25^i	1.903 (7)
Ta1—F4	2.049 (9)	Ta4—F25	1.903 (7)
Ta11—F4	1.851 (8)	Ta4—F24^i	1.94 (2)
Ta11—F5	1.874 (7)	Ta4—F24	1.94 (2)
Ta11—F2^i	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—F3^i	1.985 (5)	Ta4—F18	1.963 (7)
Ta11—F1	2.055 (9)	Ta4—F18^i	1.963 (7)
Ta2—F9	1.786 (11)	Ta44—F21	1.81 (2)
Ta2—F6	1.827 (8)	Ta44—F22	1.825 (17)
Ta2—F6^i	1.827 (8)	Ta44—F22^i	1.825 (17)
Ta2—F7	2.034 (10)	Ta44—F20	1.857 (18)
Ta2—F8^i	2.037 (8)	Ta44—F18	1.893 (10)
Ta2—F8	2.037 (8)	Ta44—F18^i	1.893 (10)
Ta2—F10	2.055 (9)	Ta44—F24^i	1.99 (2)
Ta22—F8^i	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—F25^i	2.030 (11)
Ta22—F6	2.000 (6)	F11—Ta33^i	1.973 (5)
Ta22—F6^i	2.000 (6)	F12—Ta33^i	2.009 (7)
Ta3—Ta33	0.524 (10)	F13—Ta33^i	2.367 (7)
Ta3—Ta33^i	0.524 (10)	F14—Ta33^i	2.189 (5)
Ta3—F12	1.687 (11)	F15—Ta33^i	1.941 (6)
Ta3—F16	1.860 (14)	F16—Ta33^i	2.121 (10)
Ta3—F13^i	1.944 (9)	F17—F24	1.77 (3)
Ta3—F13	1.944 (9)	F17—F24^i	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—F14^i	2.278 (10)	F19—F22^i	1.77 (3)
Ta33—Ta33^i	0.4149 (17)	F19—F22	1.77 (3)
Ta33—F14	1.827 (5)	F20—F22	1.64 (2)
Ta33—F15	1.941 (6)	F20—F22^i	1.64 (2)
Ta33—F11	1.973 (5)	F23—F25	1.64 (2)
Ta33—F12	2.009 (7)	F23—F25^i	1.64 (2)
Ta33—F13	2.040 (7)	F24—F25	1.65 (3)
Ta33—F16	2.121 (10)
F1—Ta1—F3	81.3 (4)	F13^i—Ta3—F14^i	66.5 (2)
F1—Ta1—F3^i	81.3 (4)	F11—Ta3—F14^i	63.6 (3)
F3—Ta1—F3^i	97.6 (4)	F15—Ta3—F14^i	64.4 (3)
F1—Ta1—F2^i	81.2 (4)	F14—Ta33—F15	79.5 (2)
F3^i—Ta1—F2^i	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)
F2^i—Ta1—F2	97.3 (4)	F14—Ta33—F13	73.9 (2)
F3—Ta1—F5	75.9 (2)	F15—Ta33—F13	112.8 (2)
F3^i—Ta1—F5	75.9 (2)	F11—Ta33—F13	118.9 (2)
F2^i—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—F2^i	79.3 (2)	F15—Ta33—F14^i	71.19 (16)
F4—Ta11—F2	79.3 (2)	F11—Ta33—F14^i	69.62 (14)
F2^i—Ta11—F2	96.1 (4)	F16—Ta33—F13^i	61.05 (19)
F5—Ta11—F3	77.7 (2)	F14^i—Ta33—F13^i	61.44 (19)
F2^i—Ta11—F3	150.0 (4)	F23—Ta4—F22^i	86.6 (12)
F2—Ta11—F3	77.7 (2)	F23—Ta4—F22	86.6 (12)
F4—Ta11—F3^i	127.0 (3)	F22^i—Ta4—F22	83.1 (16)
F5—Ta11—F3^i	77.6 (2)	F22^i—Ta4—F25^i	77.1 (7)
F2^i—Ta11—F3^i	77.7 (2)	F25^i—Ta4—F25	86.5 (6)
F3—Ta11—F3^i	93.0 (4)	F22^i—Ta4—F24^i	83.3 (13)
F2^i—Ta11—F1	75.5 (3)	F22—Ta4—F24	83.3 (13)
F2—Ta11—F1	75.5 (3)	F25^i—Ta4—F17	86.4 (4)
F3—Ta11—F1	74.5 (3)	F25—Ta4—F17	86.4 (4)
F3^i—Ta11—F1	74.5 (3)	F25^i—Ta4—F19	79.4 (4)
F9—Ta2—F6	85.5 (5)	F25—Ta4—F19	79.4 (4)
F9—Ta2—F6^i	85.5 (5)	F22^i—Ta4—F21	86.2 (8)
F6—Ta2—F6^i	91.4 (6)	F22—Ta4—F21	86.2 (8)
F6—Ta2—F7	86.4 (4)	F24^i—Ta4—F21	84.4 (10)
F6^i—Ta2—F7	86.4 (4)	F24—Ta4—F21	84.4 (10)
F6^i—Ta2—F8^i	76.6 (2)	F17—Ta4—F21	75.0 (7)
F7—Ta2—F8^i	72.5 (4)	F25^i—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)	F25^i—Ta4—F18^i	79.0 (4)
F8^i—Ta2—F10	70.1 (3)	F17—Ta4—F18^i	80.3 (3)
F8—Ta2—F10	70.1 (3)	F21—Ta44—F22	92.8 (10)
F8^i—Ta22—F10	76.6 (2)	F21—Ta44—F22^i	92.8 (10)
F8—Ta22—F10	76.6 (2)	F22—Ta44—F22^i	87.5 (17)
F8^i—Ta22—F7	78.7 (2)	F20—Ta44—F18	78.0 (6)
F8—Ta22—F7	78.7 (2)	F20—Ta44—F18^i	78.0 (6)
F10—Ta22—F7	129.4 (5)	F21—Ta44—F24^i	86.7 (11)
F10—Ta22—F9	75.6 (3)	F22^i—Ta44—F24^i	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)
F8^i—Ta22—F6^i	76.3 (2)	F20—Ta44—F19	72.6 (8)
F7—Ta22—F6^i	85.1 (4)	F21—Ta44—F17	76.5 (9)
F9—Ta22—F6^i	76.1 (3)	F18—Ta44—F17	80.4 (5)
F6—Ta22—F6^i	81.6 (4)	F18^i—Ta44—F17	80.4 (5)
F12—Ta3—F13^i	80.2 (4)	F22—Ta44—F23	85.0 (12)
F16—Ta3—F13^i	74.0 (4)	F22^i—Ta44—F23	85.0 (12)
F12—Ta3—F13	80.2 (4)	F24^i—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)	F22^i—Ta44—F25^i	75.7 (8)
F13—Ta3—F14	66.5 (2)	F18^i—Ta44—F25^i	77.6 (4)
F11—Ta3—F14	63.6 (3)	F19—Ta44—F25^i	76.3 (6)
F15—Ta3—F14	64.4 (3)	F17—Ta44—F25^i	81.3 (5)

Symmetry code: (i) x, −y+1/2, z.

(IV)

Crystal data

(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) Å^3	Plate, colourless
Z = 4	0.31 × 0.27 × 0.08 mm

Data collection

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

Refinement on F^2	4 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.037	Secondary atom site location: difference Fourier map
wR(F^2) = 0.086	w = 1/[σ^2(Fo^2) + (0.0332P)^2 + 37.7647P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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)