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The novel title compound, [(CH3)4N]2[Ta6Br12(H2O)6]Br4·2H2O, with a [Ta6Br12]2+ cluster unit, has been prepared and structurally characterized. The compound crystallizes in space group C2/c, with a twofold axis passing through the cluster and the centre of symmetry located between the clusters. The nearest neighbouring cluster units are aligned along the crystallographic c axis, forming a one-dimensional chain pattern.
Supporting information
CCDC reference: 184461
Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO-SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO-SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2001) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: PLATON (Spek, 1990).
Hexaaquadodecabromohexatantalum(I,II) bis(tetramethylammonium) tetrabromide
dihydrate
top
Crystal data top
(C4H12N)2[Ta6Br12(H2O)6]Br4·2H2O | F(000) = 4656 |
Mr = 2656.52 | DENZO-SMN software |
Monoclinic, C2/c | Dx = 3.982 Mg m−3 |
Hall symbol: -C 2yc | Mo Kα radiation, λ = 0.71073 Å |
a = 24.388 (5) Å | Cell parameters from 12960 reflections |
b = 12.470 (2) Å | θ = 2.1–30.5° |
c = 18.425 (4) Å | µ = 29.21 mm−1 |
β = 127.74 (3)° | T = 200 K |
V = 4431 (2) Å3 | Prism, dark green |
Z = 4 | 0.10 × 0.07 × 0.05 mm |
Data collection top
Nonius KappaCCD area-detector diffractometer | 6770 independent reflections |
Radiation source: fine-focus sealed tube | 5864 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
Detector resolution: 18.4 pixels mm-1 | θmax = 30.5°, θmin = 2.1° |
ω scans | h = −34→34 |
Absorption correction: multi-scan DENZO-SCALEPACK (Otwinowski & Minor, 1997) | k = −17→17 |
Tmin = 0.054, Tmax = 0.232 | l = −26→26 |
12960 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.028 | w = 1/[σ2(Fo2) + (0.0172P)2 + 7.5089P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.069 | (Δ/σ)max = 0.001 |
S = 1.07 | Δρmax = 2.50 e Å−3 |
6770 reflections | Δρmin = −2.94 e Å−3 |
219 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
12 restraints | Extinction coefficient: 0.000407 (10) |
Primary atom site location: structure-invariant direct methods | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All e.s.d.'s are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors R are based on F, with F set to zero for
negative F2. The threshold expression of F2 >
σ(F2) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F2 are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ta1 | 0.08007 (1) | 0.03713 (2) | 0.38898 (1) | 0.0085 (1) | |
Ta2 | 0.04972 (1) | −0.07905 (2) | 0.23122 (1) | 0.0080 (1) | |
Ta3 | 0.05025 (1) | 0.15270 (2) | 0.23201 (1) | 0.0073 (1) | |
Br1 | 0.16010 (2) | −0.11177 (4) | 0.39981 (3) | 0.0155 (1) | |
Br2 | 0.16237 (2) | 0.18203 (4) | 0.40035 (3) | 0.0151 (1) | |
Br3 | 0.12420 (3) | 0.03649 (4) | 0.20262 (3) | 0.0131 (1) | |
Br4 | −0.03680 (3) | −0.10527 (4) | 0.05444 (3) | 0.0160 (1) | |
Br5 | −0.03692 (3) | 0.18220 (4) | 0.05530 (3) | 0.0146 (1) | |
Br6 | 0.00000 | −0.25283 (6) | 0.25000 | 0.0134 (2) | |
Br7 | 0.00000 | 0.32656 (5) | 0.25000 | 0.0119 (2) | |
O1 | 0.1667 (2) | 0.0369 (3) | 0.5383 (3) | 0.0219 (11) | |
O2 | 0.1033 (2) | −0.2068 (3) | 0.2090 (3) | 0.0204 (11) | |
O3 | 0.10595 (18) | 0.2794 (3) | 0.2107 (3) | 0.0154 (10) | |
N1 | 0.1340 (3) | 0.4643 (4) | 0.0194 (3) | 0.0275 (14) | |
C1 | 0.1998 (4) | 0.4732 (9) | 0.1129 (5) | 0.056 (3) | |
C2 | 0.0934 (6) | 0.5634 (10) | 0.0011 (8) | 0.084 (4) | |
C3 | 0.1439 (6) | 0.4505 (12) | −0.0519 (7) | 0.100 (6) | |
C4 | 0.0941 (6) | 0.3718 (10) | 0.0179 (8) | 0.094 (5) | |
O4 | 0.2440 (3) | 0.1275 (5) | 0.1384 (3) | 0.0461 (16) | |
Br8 | 0.09383 (4) | 0.53616 (5) | 0.21614 (6) | 0.0376 (2) | |
Br9 | 0.27148 (3) | 0.27570 (5) | 0.30937 (4) | 0.0245 (2) | |
H11 | 0.174 (5) | 0.084 (5) | 0.583 (4) | 0.08 (3)* | |
H12 | 0.193 (4) | −0.025 (4) | 0.570 (4) | 0.05 (2)* | |
H21 | 0.098 (4) | −0.280 (3) | 0.219 (6) | 0.08 (3)* | |
H22 | 0.139 (3) | −0.210 (6) | 0.202 (5) | 0.05 (2)* | |
H31 | 0.1538 (14) | 0.275 (6) | 0.239 (5) | 0.07 (3)* | |
H32 | 0.096 (3) | 0.352 (2) | 0.215 (5) | 0.05 (2)* | |
H1A | 0.22212 | 0.40441 | 0.13253 | 0.0843* | |
H1B | 0.19075 | 0.49730 | 0.15411 | 0.0843* | |
H1C | 0.22959 | 0.52376 | 0.11302 | 0.0843* | |
H2A | 0.08764 | 0.57212 | 0.04782 | 0.1259* | |
H2B | 0.04877 | 0.55777 | −0.05776 | 0.1259* | |
H2C | 0.11771 | 0.62421 | 0.00143 | 0.1259* | |
H3A | 0.10029 | 0.45989 | −0.11157 | 0.1506* | |
H3B | 0.16134 | 0.37979 | −0.04737 | 0.1506* | |
H3C | 0.17641 | 0.50279 | −0.04293 | 0.1506* | |
H4A | 0.11609 | 0.30577 | 0.02195 | 0.1407* | |
H4B | 0.04755 | 0.37300 | −0.03830 | 0.1407* | |
H4C | 0.09305 | 0.37721 | 0.06901 | 0.1407* | |
H41 | 0.283 (4) | 0.085 (8) | 0.155 (6) | 0.08 (4)* | |
H42 | 0.251 (4) | 0.133 (8) | 0.194 (3) | 0.08 (3)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ta1 | 0.0083 (1) | 0.0074 (1) | 0.0096 (1) | −0.0002 (1) | 0.0054 (1) | 0.0009 (1) |
Ta2 | 0.0091 (1) | 0.0049 (1) | 0.0140 (1) | 0.0008 (1) | 0.0092 (1) | 0.0005 (1) |
Ta3 | 0.0080 (1) | 0.0047 (1) | 0.0119 (1) | 0.0002 (1) | 0.0075 (1) | 0.0009 (1) |
Br1 | 0.0108 (2) | 0.0141 (3) | 0.0196 (2) | 0.0049 (2) | 0.0082 (2) | 0.0048 (2) |
Br2 | 0.0102 (2) | 0.0141 (3) | 0.0171 (2) | −0.0047 (2) | 0.0063 (2) | −0.0007 (2) |
Br3 | 0.0156 (2) | 0.0089 (2) | 0.0245 (2) | 0.0014 (2) | 0.0172 (2) | 0.0021 (2) |
Br4 | 0.0204 (2) | 0.0153 (3) | 0.0162 (2) | 0.0007 (2) | 0.0132 (2) | −0.0046 (2) |
Br5 | 0.0177 (2) | 0.0152 (3) | 0.0132 (2) | 0.0012 (2) | 0.0107 (2) | 0.0034 (2) |
Br6 | 0.0178 (3) | 0.0049 (3) | 0.0259 (3) | 0.0000 | 0.0176 (3) | 0.0000 |
Br7 | 0.0153 (3) | 0.0051 (3) | 0.0210 (3) | 0.0000 | 0.0141 (3) | 0.0000 |
O1 | 0.0204 (19) | 0.020 (2) | 0.0113 (16) | 0.0001 (17) | 0.0025 (15) | 0.0009 (15) |
O2 | 0.028 (2) | 0.0076 (19) | 0.043 (2) | 0.0033 (16) | 0.0306 (19) | −0.0006 (17) |
O3 | 0.0146 (16) | 0.0080 (18) | 0.0289 (19) | −0.0003 (14) | 0.0160 (15) | 0.0044 (15) |
N1 | 0.024 (2) | 0.025 (3) | 0.023 (2) | 0.000 (2) | 0.009 (2) | −0.002 (2) |
C1 | 0.030 (4) | 0.088 (8) | 0.034 (4) | 0.009 (4) | 0.011 (3) | −0.007 (4) |
C2 | 0.069 (7) | 0.066 (7) | 0.077 (7) | 0.043 (6) | 0.024 (6) | 0.015 (6) |
C3 | 0.069 (7) | 0.194 (17) | 0.042 (5) | 0.026 (8) | 0.036 (5) | −0.001 (7) |
C4 | 0.092 (8) | 0.062 (8) | 0.091 (8) | −0.038 (7) | 0.037 (7) | 0.001 (6) |
O4 | 0.049 (3) | 0.041 (3) | 0.029 (2) | −0.014 (3) | 0.014 (2) | −0.018 (2) |
Br8 | 0.0523 (4) | 0.0093 (3) | 0.0723 (5) | 0.0009 (3) | 0.0489 (4) | 0.0013 (3) |
Br9 | 0.0192 (2) | 0.0244 (3) | 0.0347 (3) | −0.0047 (2) | 0.0189 (2) | −0.0080 (2) |
Geometric parameters (Å, º) top
Ta1—Ta3 | 2.8975 (7) | Ta3—O3 | 2.269 (5) |
Ta1—Ta2i | 2.9054 (7) | O1—H11 | 0.94 (7) |
Ta1—Ta2 | 2.9090 (7) | O1—H12 | 0.94 (6) |
Ta1—Ta3i | 2.9111 (7) | O2—H21 | 0.96 (5) |
Ta2—Ta3 | 2.8899 (7) | O2—H22 | 0.96 (9) |
Ta2—Ta2i | 2.9008 (7) | O3—H31 | 0.94 (7) |
Ta2—Ta1i | 2.9054 (7) | O3—H32 | 0.95 (3) |
Ta2—Ta1 | 2.9090 (7) | O4—H41 | 0.96 (11) |
Ta3—Ta2 | 2.8899 (7) | O4—H42 | 0.93 (6) |
Ta3—Ta1 | 2.8975 (7) | N1—C1 | 1.473 (9) |
Ta3—Ta3i | 2.9045 (7) | N1—C4 | 1.498 (16) |
Ta3—Ta1i | 2.9111 (7) | N1—C3 | 1.484 (15) |
Ta1—Br1 | 2.6115 (8) | N1—C2 | 1.487 (15) |
Ta1—Br2 | 2.6120 (8) | C1—H1B | 0.9595 |
Ta1—O1 | 2.218 (4) | C1—H1A | 0.9602 |
Ta1—Br4i | 2.5885 (9) | C1—H1C | 0.9609 |
Ta1—Br5i | 2.5993 (9) | C2—H2B | 0.9596 |
Ta2—Br1 | 2.6126 (7) | C2—H2A | 0.9595 |
Ta2—Br3 | 2.6124 (10) | C2—H2C | 0.9603 |
Ta2—Br4 | 2.5990 (7) | C3—H3B | 0.9602 |
Ta2—Br6 | 2.6076 (9) | C3—H3C | 0.9595 |
Ta2—O2 | 2.251 (5) | C3—H3A | 0.9603 |
Ta3—Br2 | 2.6170 (7) | C4—H4C | 0.9600 |
Ta3—Br3 | 2.6156 (10) | C4—H4A | 0.9603 |
Ta3—Br5 | 2.6043 (7) | C4—H4B | 0.9603 |
Ta3—Br7 | 2.6095 (8) | | |
| | | |
Ta1···Ta1i | 4.1227 (9) | O1···H41ii | 2.74 (10) |
Ta2···Ta3i | 4.0960 (10) | O3···H4C | 2.7197 |
Ta3···Ta2i | 4.0960 (10) | O4···H12xiii | 1.69 (6) |
Br1···O4ii | 3.541 (5) | C1···Br1x | 3.719 (11) |
Br1···C1iii | 3.719 (11) | C1···Br3x | 3.569 (9) |
Br3···C1iii | 3.569 (9) | C2···Br5v | 3.360 (13) |
Br4···Br5iv | 3.5625 (13) | C3···Br8xiv | 3.660 (11) |
Br4···C4iv | 3.535 (13) | C4···Br4iv | 3.535 (13) |
Br5···Br4iv | 3.5625 (13) | H1A···H4A | 2.4293 |
Br5···C2v | 3.360 (13) | H1A···Br9 | 3.1369 |
Br6···Br8vi | 3.7811 (14) | H1B···Br8 | 3.2303 |
Br6···Br8vii | 3.7811 (14) | H1B···H2A | 2.2362 |
Br7···Br8i | 3.7689 (13) | H1B···H4C | 2.4093 |
Br7···Br8 | 3.7689 (13) | H1C···H3C | 2.3334 |
Br8···Br7 | 3.7689 (13) | H1C···Br3x | 3.0742 |
Br8···C3viii | 3.660 (11) | H1C···H2C | 2.5246 |
Br8···Br7 | 3.7689 (13) | H2A···Br8 | 3.0445 |
Br8···O2ix | 3.222 (4) | H2A···H4C | 2.4524 |
Br8···O3 | 3.223 (4) | H2A···H1B | 2.2362 |
Br8···O4x | 3.339 (7) | H2B···H4B | 2.3348 |
Br8···Br6xi | 3.7811 (14) | H2B···H3A | 2.3614 |
Br8···Br6ix | 3.7811 (14) | H2B···Br8v | 3.0917 |
Br9···O3 | 3.259 (5) | H2C···Br5v | 2.8777 |
Br9···O4 | 3.347 (6) | H2C···H1C | 2.5246 |
Br9···O2x | 3.279 (6) | H2C···H3C | 2.5382 |
Br9···O1xii | 3.230 (4) | H3A···H2B | 2.3614 |
Br3···H1Ciii | 3.0742 | H3A···Br8xiv | 3.0809 |
Br4···H4Aiv | 2.9393 | H3B···H4A | 2.3295 |
Br5···H2Cv | 2.8777 | H3C···H2C | 2.5382 |
Br8···H2A | 3.0445 | H3C···H1C | 2.3334 |
Br8···H41x | 2.51 (10) | H4A···H3B | 2.3295 |
Br8···H3Aviii | 3.0809 | H4A···Br4iv | 2.9393 |
Br8···H32 | 2.30 (3) | H4A···H1A | 2.4293 |
Br8···H1B | 3.2303 | H4B···H2B | 2.3348 |
Br8···H4Bv | 3.1746 | H4B···Br8v | 3.1746 |
Br8···H2Bv | 3.0917 | H4C···O3 | 2.7197 |
Br8···H21ix | 2.29 (4) | H4C···H1B | 2.4093 |
Br9···H31 | 2.32 (7) | H4C···H2A | 2.4524 |
Br9···H42 | 2.58 (8) | H11···Br9xii | 2.35 (6) |
Br9···H11xii | 2.35 (6) | H12···O4ii | 1.69 (6) |
Br9···H22x | 2.32 (9) | H12···H41ii | 1.90 (13) |
Br9···H1A | 3.1369 | H12···H42ii | 2.25 (9) |
O1···O4ii | 2.627 (7) | H21···Br8vi | 2.29 (4) |
O1···Br9xii | 3.230 (4) | H22···Br9iii | 2.32 (9) |
O2···Br9iii | 3.279 (6) | H31···Br9 | 2.32 (7) |
O2···Br8vi | 3.222 (4) | H32···Br8 | 2.30 (3) |
O3···Br9 | 3.259 (5) | H41···H12xiii | 1.90 (13) |
O3···Br8 | 3.223 (4) | H41···O1xiii | 2.74 (10) |
O4···O1xiii | 2.627 (7) | H41···Br8iii | 2.51 (10) |
O4···Br9 | 3.347 (6) | H42···Br9 | 2.58 (8) |
O4···Br1xiii | 3.541 (5) | H42···H12xiii | 2.25 (9) |
O4···Br8iii | 3.339 (7) | | |
| | | |
Br1—Ta1—Br2 | 89.09 (4) | H11—O1—H12 | 106 (5) |
Br1—Ta1—O1 | 78.72 (13) | Ta2—O2—H21 | 119 (7) |
Br1—Ta1—Br4i | 87.21 (4) | Ta2—O2—H22 | 137 (5) |
Br1—Ta1—Br5i | 158.27 (3) | H21—O2—H22 | 103 (8) |
Br2—Ta1—O1 | 78.44 (13) | Ta3—O3—H31 | 122 (4) |
Br2—Ta1—Br4i | 157.66 (3) | Ta3—O3—H32 | 116 (5) |
Br2—Ta1—Br5i | 87.93 (4) | H31—O3—H32 | 108 (7) |
Br4i—Ta1—O1 | 79.23 (13) | H41—O4—H42 | 102 (8) |
Br5i—Ta1—O1 | 79.60 (13) | C1—N1—C3 | 113.1 (9) |
Br4i—Ta1—Br5i | 87.42 (4) | C1—N1—C4 | 108.0 (7) |
Br1—Ta2—Br3 | 89.33 (3) | C2—N1—C3 | 110.0 (8) |
Br1—Ta2—Br4 | 157.78 (4) | C2—N1—C4 | 107.5 (10) |
Br1—Ta2—Br6 | 86.38 (3) | C3—N1—C4 | 110.5 (8) |
Br1—Ta2—O2 | 79.36 (12) | C1—N1—C2 | 107.5 (7) |
Br3—Ta2—Br4 | 87.02 (4) | N1—C1—H1A | 109.50 |
Br3—Ta2—Br6 | 157.27 (4) | N1—C1—H1B | 109.60 |
Br3—Ta2—O2 | 78.52 (13) | H1A—C1—H1B | 109.49 |
Br4—Ta2—Br6 | 88.57 (3) | H1A—C1—H1C | 109.38 |
Br4—Ta2—O2 | 78.43 (12) | H1B—C1—H1C | 109.42 |
Br6—Ta2—O2 | 78.75 (13) | N1—C1—H1C | 109.45 |
Br2—Ta3—Br3 | 88.29 (3) | N1—C2—H2B | 109.43 |
Br2—Ta3—Br5 | 157.40 (4) | N1—C2—H2C | 109.38 |
Br2—Ta3—Br7 | 87.97 (3) | N1—C2—H2A | 109.48 |
Br2—Ta3—O3 | 78.81 (12) | H2A—C2—H2C | 109.49 |
Br3—Ta3—Br5 | 87.60 (4) | H2B—C2—H2C | 109.50 |
Br3—Ta3—Br7 | 157.45 (4) | H2A—C2—H2B | 109.55 |
Br3—Ta3—O3 | 77.78 (12) | N1—C3—H3A | 109.46 |
Br5—Ta3—Br7 | 87.36 (3) | N1—C3—H3B | 109.45 |
Br5—Ta3—O3 | 78.60 (12) | H3A—C3—H3B | 109.44 |
Br7—Ta3—O3 | 79.68 (12) | H3A—C3—H3C | 109.49 |
Ta1—Br1—Ta2 | 67.67 (3) | N1—C3—H3C | 109.50 |
Ta1—Br2—Ta3 | 67.30 (3) | H3B—C3—H3C | 109.50 |
Ta2—Br3—Ta3 | 67.12 (4) | N1—C4—H4B | 109.49 |
Ta1i—Br4—Ta2 | 68.12 (3) | N1—C4—H4C | 109.56 |
Ta1i—Br5—Ta3 | 68.03 (3) | N1—C4—H4A | 109.46 |
Ta2—Br6—Ta2i | 67.59 (4) | H4A—C4—H4C | 109.45 |
Ta3—Br7—Ta3i | 67.63 (3) | H4B—C4—H4C | 109.45 |
Ta1—O1—H11 | 128 (5) | H4A—C4—H4B | 109.42 |
Ta1—O1—H12 | 123 (3) | | |
| | | |
Br2—Ta1—Br1—Ta2 | −100.16 (3) | Br3—Ta2—Br4—Ta1i | −101.75 (4) |
O1—Ta1—Br1—Ta2 | −178.56 (14) | Br6—Ta2—Br4—Ta1i | 100.56 (3) |
Br4i—Ta1—Br1—Ta2 | 101.87 (3) | O2—Ta2—Br4—Ta1i | 179.37 (13) |
Br5i—Ta1—Br1—Ta2 | 177.75 (6) | Br1—Ta2—Br6—Ta2i | 100.77 (3) |
Br1—Ta1—Br2—Ta3 | 100.93 (3) | Br3—Ta2—Br6—Ta2i | −179.68 (4) |
O1—Ta1—Br2—Ta3 | 179.60 (13) | Br4—Ta2—Br6—Ta2i | −100.89 (3) |
Br4i—Ta1—Br2—Ta3 | −178.68 (6) | O2—Ta2—Br6—Ta2i | −179.37 (12) |
Br5i—Ta1—Br2—Ta3 | −100.60 (3) | Br3—Ta3—Br2—Ta1 | −101.38 (3) |
Br1—Ta1—Br4i—Ta2i | −100.10 (3) | Br5—Ta3—Br2—Ta1 | 179.03 (6) |
Br2—Ta1—Br4i—Ta2i | 179.14 (6) | Br7—Ta3—Br2—Ta1 | 100.86 (3) |
O1—Ta1—Br4i—Ta2i | −179.14 (13) | O3—Ta3—Br2—Ta1 | −179.26 (13) |
Br1—Ta1—Br5i—Ta3i | −176.26 (6) | Br2—Ta3—Br3—Ta2 | 101.11 (3) |
Br2—Ta1—Br5i—Ta3i | 101.43 (3) | Br5—Ta3—Br3—Ta2 | −101.12 (3) |
O1—Ta1—Br5i—Ta3i | −179.95 (12) | Br7—Ta3—Br3—Ta2 | −178.34 (4) |
Br3—Ta2—Br1—Ta1 | 100.43 (3) | O3—Ta3—Br3—Ta2 | −179.97 (12) |
Br4—Ta2—Br1—Ta1 | −179.14 (6) | Br2—Ta3—Br5—Ta1i | −179.23 (6) |
Br6—Ta2—Br1—Ta1 | −101.91 (3) | Br3—Ta3—Br5—Ta1i | 101.05 (4) |
O2—Ta2—Br1—Ta1 | 178.87 (13) | Br7—Ta3—Br5—Ta1i | −100.93 (3) |
Br1—Ta2—Br3—Ta3 | −100.96 (3) | O3—Ta3—Br5—Ta1i | 179.06 (12) |
Br4—Ta2—Br3—Ta3 | 100.98 (3) | Br2—Ta3—Br7—Ta3i | −101.44 (3) |
Br6—Ta2—Br3—Ta3 | −179.93 (4) | Br3—Ta3—Br7—Ta3i | 177.95 (4) |
O2—Ta2—Br3—Ta3 | 179.77 (12) | Br5—Ta3—Br7—Ta3i | 100.68 (3) |
Br1—Ta2—Br4—Ta1i | 177.37 (6) | O3—Ta3—Br7—Ta3i | 179.57 (12) |
Symmetry codes: (i) −x, y, −z+1/2; (ii) x, −y, z+1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) −x, −y, −z; (v) −x, −y+1, −z; (vi) x, y−1, z; (vii) −x, y−1, −z+1/2; (viii) x, −y+1, z+1/2; (ix) x, y+1, z; (x) −x+1/2, y+1/2, −z+1/2; (xi) −x, y+1, −z+1/2; (xii) −x+1/2, −y+1/2, −z+1; (xiii) x, −y, z−1/2; (xiv) x, −y+1, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H11···Br9xii | 0.94 (7) | 2.35 (6) | 3.230 (4) | 156 (10) |
O1—H12···O4ii | 0.94 (6) | 1.69 (6) | 2.627 (7) | 173 (8) |
O2—H21···Br8vi | 0.96 (5) | 2.29 (4) | 3.222 (4) | 164 (8) |
O2—H22···Br9iii | 0.96 (9) | 2.32 (9) | 3.279 (6) | 177 (6) |
O3—H31···Br9 | 0.94 (7) | 2.32 (7) | 3.259 (5) | 176 (3) |
O3—H32···Br8 | 0.95 (3) | 2.30 (3) | 3.223 (4) | 163 (8) |
O4—H41···Br8iii | 0.96 (11) | 2.51 (10) | 3.339 (7) | 144 (7) |
O4—H42···Br9 | 0.93 (6) | 2.58 (8) | 3.347 (6) | 140 (8) |
C2—H2C···Br5v | 0.96 | 2.88 | 3.360 (13) | 112 |
Symmetry codes: (ii) x, −y, z+1/2; (iii) −x+1/2, y−1/2, −z+1/2; (v) −x, −y+1, −z; (vi) x, y−1, z; (xii) −x+1/2, −y+1/2, −z+1. |
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