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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102001841/sk1533sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102001841/sk1533Isup2.hkl
Contains datablock I

CCDC reference: 184461

Computing details top

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]Br4·2H2OF(000) = 4656
Mr = 2656.52DENZO-SMN software
Monoclinic, C2/cDx = 3.982 Mg m3
Hall symbol: -C 2ycMo Kα radiation, λ = 0.71073 Å
a = 24.388 (5) ÅCell parameters from 12960 reflections
b = 12.470 (2) Åθ = 2.1–30.5°
c = 18.425 (4) ŵ = 29.21 mm1
β = 127.74 (3)°T = 200 K
V = 4431 (2) Å3Prism, dark green
Z = 40.10 × 0.07 × 0.05 mm
Data collection top
Nonius KappaCCD area-detector
diffractometer
6770 independent reflections
Radiation source: fine-focus sealed tube5864 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
Detector resolution: 18.4 pixels mm-1θmax = 30.5°, θmin = 2.1°
ω scansh = 3434
Absorption correction: multi-scan
DENZO-SCALEPACK (Otwinowski & Minor, 1997)
k = 1717
Tmin = 0.054, Tmax = 0.232l = 2626
12960 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullH 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 = 1.07Δρmax = 2.50 e Å3
6770 reflectionsΔρmin = 2.94 e Å3
219 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
12 restraintsExtinction 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
xyzUiso*/Ueq
Ta10.08007 (1)0.03713 (2)0.38898 (1)0.0085 (1)
Ta20.04972 (1)0.07905 (2)0.23122 (1)0.0080 (1)
Ta30.05025 (1)0.15270 (2)0.23201 (1)0.0073 (1)
Br10.16010 (2)0.11177 (4)0.39981 (3)0.0155 (1)
Br20.16237 (2)0.18203 (4)0.40035 (3)0.0151 (1)
Br30.12420 (3)0.03649 (4)0.20262 (3)0.0131 (1)
Br40.03680 (3)0.10527 (4)0.05444 (3)0.0160 (1)
Br50.03692 (3)0.18220 (4)0.05530 (3)0.0146 (1)
Br60.000000.25283 (6)0.250000.0134 (2)
Br70.000000.32656 (5)0.250000.0119 (2)
O10.1667 (2)0.0369 (3)0.5383 (3)0.0219 (11)
O20.1033 (2)0.2068 (3)0.2090 (3)0.0204 (11)
O30.10595 (18)0.2794 (3)0.2107 (3)0.0154 (10)
N10.1340 (3)0.4643 (4)0.0194 (3)0.0275 (14)
C10.1998 (4)0.4732 (9)0.1129 (5)0.056 (3)
C20.0934 (6)0.5634 (10)0.0011 (8)0.084 (4)
C30.1439 (6)0.4505 (12)0.0519 (7)0.100 (6)
C40.0941 (6)0.3718 (10)0.0179 (8)0.094 (5)
O40.2440 (3)0.1275 (5)0.1384 (3)0.0461 (16)
Br80.09383 (4)0.53616 (5)0.21614 (6)0.0376 (2)
Br90.27148 (3)0.27570 (5)0.30937 (4)0.0245 (2)
H110.174 (5)0.084 (5)0.583 (4)0.08 (3)*
H120.193 (4)0.025 (4)0.570 (4)0.05 (2)*
H210.098 (4)0.280 (3)0.219 (6)0.08 (3)*
H220.139 (3)0.210 (6)0.202 (5)0.05 (2)*
H310.1538 (14)0.275 (6)0.239 (5)0.07 (3)*
H320.096 (3)0.352 (2)0.215 (5)0.05 (2)*
H1A0.222120.404410.132530.0843*
H1B0.190750.497300.154110.0843*
H1C0.229590.523760.113020.0843*
H2A0.087640.572120.047820.1259*
H2B0.048770.557770.057760.1259*
H2C0.117710.624210.001430.1259*
H3A0.100290.459890.111570.1506*
H3B0.161340.379790.047370.1506*
H3C0.176410.502790.042930.1506*
H4A0.116090.305770.021950.1407*
H4B0.047550.373000.038300.1407*
H4C0.093050.377210.069010.1407*
H410.283 (4)0.085 (8)0.155 (6)0.08 (4)*
H420.251 (4)0.133 (8)0.194 (3)0.08 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ta10.0083 (1)0.0074 (1)0.0096 (1)0.0002 (1)0.0054 (1)0.0009 (1)
Ta20.0091 (1)0.0049 (1)0.0140 (1)0.0008 (1)0.0092 (1)0.0005 (1)
Ta30.0080 (1)0.0047 (1)0.0119 (1)0.0002 (1)0.0075 (1)0.0009 (1)
Br10.0108 (2)0.0141 (3)0.0196 (2)0.0049 (2)0.0082 (2)0.0048 (2)
Br20.0102 (2)0.0141 (3)0.0171 (2)0.0047 (2)0.0063 (2)0.0007 (2)
Br30.0156 (2)0.0089 (2)0.0245 (2)0.0014 (2)0.0172 (2)0.0021 (2)
Br40.0204 (2)0.0153 (3)0.0162 (2)0.0007 (2)0.0132 (2)0.0046 (2)
Br50.0177 (2)0.0152 (3)0.0132 (2)0.0012 (2)0.0107 (2)0.0034 (2)
Br60.0178 (3)0.0049 (3)0.0259 (3)0.00000.0176 (3)0.0000
Br70.0153 (3)0.0051 (3)0.0210 (3)0.00000.0141 (3)0.0000
O10.0204 (19)0.020 (2)0.0113 (16)0.0001 (17)0.0025 (15)0.0009 (15)
O20.028 (2)0.0076 (19)0.043 (2)0.0033 (16)0.0306 (19)0.0006 (17)
O30.0146 (16)0.0080 (18)0.0289 (19)0.0003 (14)0.0160 (15)0.0044 (15)
N10.024 (2)0.025 (3)0.023 (2)0.000 (2)0.009 (2)0.002 (2)
C10.030 (4)0.088 (8)0.034 (4)0.009 (4)0.011 (3)0.007 (4)
C20.069 (7)0.066 (7)0.077 (7)0.043 (6)0.024 (6)0.015 (6)
C30.069 (7)0.194 (17)0.042 (5)0.026 (8)0.036 (5)0.001 (7)
C40.092 (8)0.062 (8)0.091 (8)0.038 (7)0.037 (7)0.001 (6)
O40.049 (3)0.041 (3)0.029 (2)0.014 (3)0.014 (2)0.018 (2)
Br80.0523 (4)0.0093 (3)0.0723 (5)0.0009 (3)0.0489 (4)0.0013 (3)
Br90.0192 (2)0.0244 (3)0.0347 (3)0.0047 (2)0.0189 (2)0.0080 (2)
Geometric parameters (Å, º) top
Ta1—Ta32.8975 (7)Ta3—O32.269 (5)
Ta1—Ta2i2.9054 (7)O1—H110.94 (7)
Ta1—Ta22.9090 (7)O1—H120.94 (6)
Ta1—Ta3i2.9111 (7)O2—H210.96 (5)
Ta2—Ta32.8899 (7)O2—H220.96 (9)
Ta2—Ta2i2.9008 (7)O3—H310.94 (7)
Ta2—Ta1i2.9054 (7)O3—H320.95 (3)
Ta2—Ta12.9090 (7)O4—H410.96 (11)
Ta3—Ta22.8899 (7)O4—H420.93 (6)
Ta3—Ta12.8975 (7)N1—C11.473 (9)
Ta3—Ta3i2.9045 (7)N1—C41.498 (16)
Ta3—Ta1i2.9111 (7)N1—C31.484 (15)
Ta1—Br12.6115 (8)N1—C21.487 (15)
Ta1—Br22.6120 (8)C1—H1B0.9595
Ta1—O12.218 (4)C1—H1A0.9602
Ta1—Br4i2.5885 (9)C1—H1C0.9609
Ta1—Br5i2.5993 (9)C2—H2B0.9596
Ta2—Br12.6126 (7)C2—H2A0.9595
Ta2—Br32.6124 (10)C2—H2C0.9603
Ta2—Br42.5990 (7)C3—H3B0.9602
Ta2—Br62.6076 (9)C3—H3C0.9595
Ta2—O22.251 (5)C3—H3A0.9603
Ta3—Br22.6170 (7)C4—H4C0.9600
Ta3—Br32.6156 (10)C4—H4A0.9603
Ta3—Br52.6043 (7)C4—H4B0.9603
Ta3—Br72.6095 (8)
Ta1···Ta1i4.1227 (9)O1···H41ii2.74 (10)
Ta2···Ta3i4.0960 (10)O3···H4C2.7197
Ta3···Ta2i4.0960 (10)O4···H12xiii1.69 (6)
Br1···O4ii3.541 (5)C1···Br1x3.719 (11)
Br1···C1iii3.719 (11)C1···Br3x3.569 (9)
Br3···C1iii3.569 (9)C2···Br5v3.360 (13)
Br4···Br5iv3.5625 (13)C3···Br8xiv3.660 (11)
Br4···C4iv3.535 (13)C4···Br4iv3.535 (13)
Br5···Br4iv3.5625 (13)H1A···H4A2.4293
Br5···C2v3.360 (13)H1A···Br93.1369
Br6···Br8vi3.7811 (14)H1B···Br83.2303
Br6···Br8vii3.7811 (14)H1B···H2A2.2362
Br7···Br8i3.7689 (13)H1B···H4C2.4093
Br7···Br83.7689 (13)H1C···H3C2.3334
Br8···Br73.7689 (13)H1C···Br3x3.0742
Br8···C3viii3.660 (11)H1C···H2C2.5246
Br8···Br73.7689 (13)H2A···Br83.0445
Br8···O2ix3.222 (4)H2A···H4C2.4524
Br8···O33.223 (4)H2A···H1B2.2362
Br8···O4x3.339 (7)H2B···H4B2.3348
Br8···Br6xi3.7811 (14)H2B···H3A2.3614
Br8···Br6ix3.7811 (14)H2B···Br8v3.0917
Br9···O33.259 (5)H2C···Br5v2.8777
Br9···O43.347 (6)H2C···H1C2.5246
Br9···O2x3.279 (6)H2C···H3C2.5382
Br9···O1xii3.230 (4)H3A···H2B2.3614
Br3···H1Ciii3.0742H3A···Br8xiv3.0809
Br4···H4Aiv2.9393H3B···H4A2.3295
Br5···H2Cv2.8777H3C···H2C2.5382
Br8···H2A3.0445H3C···H1C2.3334
Br8···H41x2.51 (10)H4A···H3B2.3295
Br8···H3Aviii3.0809H4A···Br4iv2.9393
Br8···H322.30 (3)H4A···H1A2.4293
Br8···H1B3.2303H4B···H2B2.3348
Br8···H4Bv3.1746H4B···Br8v3.1746
Br8···H2Bv3.0917H4C···O32.7197
Br8···H21ix2.29 (4)H4C···H1B2.4093
Br9···H312.32 (7)H4C···H2A2.4524
Br9···H422.58 (8)H11···Br9xii2.35 (6)
Br9···H11xii2.35 (6)H12···O4ii1.69 (6)
Br9···H22x2.32 (9)H12···H41ii1.90 (13)
Br9···H1A3.1369H12···H42ii2.25 (9)
O1···O4ii2.627 (7)H21···Br8vi2.29 (4)
O1···Br9xii3.230 (4)H22···Br9iii2.32 (9)
O2···Br9iii3.279 (6)H31···Br92.32 (7)
O2···Br8vi3.222 (4)H32···Br82.30 (3)
O3···Br93.259 (5)H41···H12xiii1.90 (13)
O3···Br83.223 (4)H41···O1xiii2.74 (10)
O4···O1xiii2.627 (7)H41···Br8iii2.51 (10)
O4···Br93.347 (6)H42···Br92.58 (8)
O4···Br1xiii3.541 (5)H42···H12xiii2.25 (9)
O4···Br8iii3.339 (7)
Br1—Ta1—Br289.09 (4)H11—O1—H12106 (5)
Br1—Ta1—O178.72 (13)Ta2—O2—H21119 (7)
Br1—Ta1—Br4i87.21 (4)Ta2—O2—H22137 (5)
Br1—Ta1—Br5i158.27 (3)H21—O2—H22103 (8)
Br2—Ta1—O178.44 (13)Ta3—O3—H31122 (4)
Br2—Ta1—Br4i157.66 (3)Ta3—O3—H32116 (5)
Br2—Ta1—Br5i87.93 (4)H31—O3—H32108 (7)
Br4i—Ta1—O179.23 (13)H41—O4—H42102 (8)
Br5i—Ta1—O179.60 (13)C1—N1—C3113.1 (9)
Br4i—Ta1—Br5i87.42 (4)C1—N1—C4108.0 (7)
Br1—Ta2—Br389.33 (3)C2—N1—C3110.0 (8)
Br1—Ta2—Br4157.78 (4)C2—N1—C4107.5 (10)
Br1—Ta2—Br686.38 (3)C3—N1—C4110.5 (8)
Br1—Ta2—O279.36 (12)C1—N1—C2107.5 (7)
Br3—Ta2—Br487.02 (4)N1—C1—H1A109.50
Br3—Ta2—Br6157.27 (4)N1—C1—H1B109.60
Br3—Ta2—O278.52 (13)H1A—C1—H1B109.49
Br4—Ta2—Br688.57 (3)H1A—C1—H1C109.38
Br4—Ta2—O278.43 (12)H1B—C1—H1C109.42
Br6—Ta2—O278.75 (13)N1—C1—H1C109.45
Br2—Ta3—Br388.29 (3)N1—C2—H2B109.43
Br2—Ta3—Br5157.40 (4)N1—C2—H2C109.38
Br2—Ta3—Br787.97 (3)N1—C2—H2A109.48
Br2—Ta3—O378.81 (12)H2A—C2—H2C109.49
Br3—Ta3—Br587.60 (4)H2B—C2—H2C109.50
Br3—Ta3—Br7157.45 (4)H2A—C2—H2B109.55
Br3—Ta3—O377.78 (12)N1—C3—H3A109.46
Br5—Ta3—Br787.36 (3)N1—C3—H3B109.45
Br5—Ta3—O378.60 (12)H3A—C3—H3B109.44
Br7—Ta3—O379.68 (12)H3A—C3—H3C109.49
Ta1—Br1—Ta267.67 (3)N1—C3—H3C109.50
Ta1—Br2—Ta367.30 (3)H3B—C3—H3C109.50
Ta2—Br3—Ta367.12 (4)N1—C4—H4B109.49
Ta1i—Br4—Ta268.12 (3)N1—C4—H4C109.56
Ta1i—Br5—Ta368.03 (3)N1—C4—H4A109.46
Ta2—Br6—Ta2i67.59 (4)H4A—C4—H4C109.45
Ta3—Br7—Ta3i67.63 (3)H4B—C4—H4C109.45
Ta1—O1—H11128 (5)H4A—C4—H4B109.42
Ta1—O1—H12123 (3)
Br2—Ta1—Br1—Ta2100.16 (3)Br3—Ta2—Br4—Ta1i101.75 (4)
O1—Ta1—Br1—Ta2178.56 (14)Br6—Ta2—Br4—Ta1i100.56 (3)
Br4i—Ta1—Br1—Ta2101.87 (3)O2—Ta2—Br4—Ta1i179.37 (13)
Br5i—Ta1—Br1—Ta2177.75 (6)Br1—Ta2—Br6—Ta2i100.77 (3)
Br1—Ta1—Br2—Ta3100.93 (3)Br3—Ta2—Br6—Ta2i179.68 (4)
O1—Ta1—Br2—Ta3179.60 (13)Br4—Ta2—Br6—Ta2i100.89 (3)
Br4i—Ta1—Br2—Ta3178.68 (6)O2—Ta2—Br6—Ta2i179.37 (12)
Br5i—Ta1—Br2—Ta3100.60 (3)Br3—Ta3—Br2—Ta1101.38 (3)
Br1—Ta1—Br4i—Ta2i100.10 (3)Br5—Ta3—Br2—Ta1179.03 (6)
Br2—Ta1—Br4i—Ta2i179.14 (6)Br7—Ta3—Br2—Ta1100.86 (3)
O1—Ta1—Br4i—Ta2i179.14 (13)O3—Ta3—Br2—Ta1179.26 (13)
Br1—Ta1—Br5i—Ta3i176.26 (6)Br2—Ta3—Br3—Ta2101.11 (3)
Br2—Ta1—Br5i—Ta3i101.43 (3)Br5—Ta3—Br3—Ta2101.12 (3)
O1—Ta1—Br5i—Ta3i179.95 (12)Br7—Ta3—Br3—Ta2178.34 (4)
Br3—Ta2—Br1—Ta1100.43 (3)O3—Ta3—Br3—Ta2179.97 (12)
Br4—Ta2—Br1—Ta1179.14 (6)Br2—Ta3—Br5—Ta1i179.23 (6)
Br6—Ta2—Br1—Ta1101.91 (3)Br3—Ta3—Br5—Ta1i101.05 (4)
O2—Ta2—Br1—Ta1178.87 (13)Br7—Ta3—Br5—Ta1i100.93 (3)
Br1—Ta2—Br3—Ta3100.96 (3)O3—Ta3—Br5—Ta1i179.06 (12)
Br4—Ta2—Br3—Ta3100.98 (3)Br2—Ta3—Br7—Ta3i101.44 (3)
Br6—Ta2—Br3—Ta3179.93 (4)Br3—Ta3—Br7—Ta3i177.95 (4)
O2—Ta2—Br3—Ta3179.77 (12)Br5—Ta3—Br7—Ta3i100.68 (3)
Br1—Ta2—Br4—Ta1i177.37 (6)O3—Ta3—Br7—Ta3i179.57 (12)
Symmetry codes: (i) x, y, z+1/2; (ii) x, y, z+1/2; (iii) x+1/2, y1/2, z+1/2; (iv) x, y, z; (v) x, y+1, z; (vi) x, y1, z; (vii) x, y1, 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, z1/2; (xiv) x, y+1, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H11···Br9xii0.94 (7)2.35 (6)3.230 (4)156 (10)
O1—H12···O4ii0.94 (6)1.69 (6)2.627 (7)173 (8)
O2—H21···Br8vi0.96 (5)2.29 (4)3.222 (4)164 (8)
O2—H22···Br9iii0.96 (9)2.32 (9)3.279 (6)177 (6)
O3—H31···Br90.94 (7)2.32 (7)3.259 (5)176 (3)
O3—H32···Br80.95 (3)2.30 (3)3.223 (4)163 (8)
O4—H41···Br8iii0.96 (11)2.51 (10)3.339 (7)144 (7)
O4—H42···Br90.93 (6)2.58 (8)3.347 (6)140 (8)
C2—H2C···Br5v0.962.883.360 (13)112
Symmetry codes: (ii) x, y, z+1/2; (iii) x+1/2, y1/2, z+1/2; (v) x, y+1, z; (vi) x, y1, z; (xii) x+1/2, y+1/2, z+1.
 

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