Literature DB >> 24764951

Bis(η(5)-penta-methyl-cyclo-penta-dien-yl)aluminium tetra-bromido-aluminate.

Andrew P Purdy1, Cherrelle Dugger1, Ray J Butcher2.   

Abstract

The title compound, [Al(C10H15)2][AlBr4], was formed during the reduction of a mixture of Cp*AlBr2 and AlBr3. The Al(III) atoms of the two crystallographically independent cations each lie on an inversion center, and the [AlBr4](-) anions are on general positions. At 123 K, the structure exhibits disorder in two of the Br atoms of the [AlBr4](-) ion, with a ratio occupancy of 0.733 (6): 0.267 (3). In the crystal, there is possible weak hydrogen bonding between some methyl groups and Br atoms. The interactions link the moieties in a three-dimensional array.

Entities:  

Year:  2014        PMID： 24764951      PMCID： PMC3998496          DOI： 10.1107/S1600536814002554

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For the tetra­chlorido­aluminate analog of the title compound, see: Macdonald et al. (2008 ▶); Schurko et al. (2002 ▶). For the formation of the Cp*2Al+ (deca­methyl­aluminocenium) cation starting from (AlCp*)4, see: Dohmeier et al. (1993 ▶); Üffing et al. (1998 ▶). For the formation of Cp*2Al+ starting from Cp*2AlX, see: Schurko et al. (2002 ▶). For other compounds containing this ion, see: Üffing et al. (1999 ▶); Kruczyński et al. (2012 ▶); Vollet et al. (2006 ▶); Burns et al. (1999 ▶). For the production of (Cp*Al)4 by alkali metal reduction of Cp*AlX 2, see: Schormann et al. (2001 ▶); Minasian & Arnold (2008 ▶). For larger Al clusters containing the Cp* ligand, which have so far only been obtained from reactions between "AlX" and Cp* organometallics, see: Vollet et al. (2004 ▶, 2005 ▶).

Experimental

Crystal data

[Al(C10H15)2][AlBr4] M = 644.04 Triclinic, a = 7.8152 (4) Å b = 9.2949 (4) Å c = 17.5420 (8) Å α = 85.394 (4)° β = 85.107 (4)° γ = 82.659 (4)° V = 1256.12 (10) Å3 Z = 2 Mo Kα radiation μ = 6.48 mm−1 T = 123 K 0.75 × 0.28 × 0.14 mm

Data collection

Agilent Xcalibur (Ruby, Gemini) diffractometer Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012 ▶) T min = 0.116, T max = 0.506 19757 measured reflections 9539 independent reflections 5959 reflections with I > 2σ(I) R int = 0.038

Refinement

R[F 2 > 2σ(F 2)] = 0.043 wR(F 2) = 0.072 S = 0.91 9539 reflections 256 parameters 24 restraints H-atom parameters constrained Δρmax = 1.58 e Å−3 Δρmin = −1.29 e Å−3 Data collection: CrysAlis PRO (Agilent, 2012 ▶); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536814002554/bh2490sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536814002554/bh2490Isup2.hkl CCDC reference: Additional supporting information: crystallographic information; 3D view; checkCIF report
[Al(C10H15)2][AlBr4]Z = 2
Mr = 644.04F(000) = 632
Triclinic, P1Dx = 1.703 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.8152 (4) ÅCell parameters from 5355 reflections
b = 9.2949 (4) Åθ = 3.1–40.9°
c = 17.5420 (8) ŵ = 6.48 mm−1
α = 85.394 (4)°T = 123 K
β = 85.107 (4)°Prism, colorless
γ = 82.659 (4)°0.75 × 0.28 × 0.14 mm
V = 1256.12 (10) Å3
Agilent Xcalibur (Ruby, Gemini) diffractometer9539 independent reflections
Radiation source: Enhance (Mo) X-ray Source5959 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
Detector resolution: 10.5081 pixels mm-1θmax = 33.1°, θmin = 3.1°
ω scansh = −12→9
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012)k = −14→14
Tmin = 0.116, Tmax = 0.506l = −23→26
19757 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.072w = 1/[σ2(Fo2)] where P = (Fo2 + 2Fc2)/3
S = 0.91(Δ/σ)max = 0.001
9539 reflectionsΔρmax = 1.58 e Å−3
256 parametersΔρmin = −1.29 e Å−3
24 restraintsExtinction correction: SHELXL2013 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 constraintsExtinction coefficient: 0.00092 (12)
Primary atom site location: structure-invariant direct methods
xyzUiso*/UeqOcc. (<1)
Br10.96698 (4)0.21881 (3)0.25435 (2)0.03406 (8)
Br20.65528 (4)0.55941 (4)0.27080 (2)0.03666 (9)
Br3A0.9871 (7)0.5256 (8)0.1151 (4)0.0541 (4)0.267 (6)
Br4A1.0853 (5)0.5280 (4)0.3398 (3)0.0544 (4)0.267 (6)
Br3B1.0273 (3)0.5371 (3)0.11613 (15)0.0541 (4)0.733 (6)
Br4B1.1204 (2)0.55802 (18)0.31528 (14)0.0544 (4)0.733 (6)
Al10.50001.00000.00000.0211 (2)
Al20.50000.00000.50000.0181 (2)
Al30.93792 (11)0.46832 (9)0.24082 (5)0.02554 (19)
C1A0.6158 (4)1.1583 (3)0.05506 (15)0.0267 (6)
C2A0.6105 (4)1.2014 (3)−0.02423 (15)0.0251 (6)
C3A0.7084 (4)1.0894 (3)−0.06667 (15)0.0243 (6)
C4A0.7753 (3)0.9763 (3)−0.01345 (15)0.0247 (6)
C5A0.7184 (4)1.0177 (3)0.06290 (15)0.0248 (6)
C6A0.5357 (4)1.2443 (3)0.12124 (16)0.0364 (8)
H6AA0.61881.30540.13620.055*
H6AB0.50481.17740.16480.055*
H6AC0.43151.30610.10570.055*
C7A0.5193 (4)1.3404 (3)−0.05916 (17)0.0338 (7)
H7AA0.60121.4122−0.06980.051*
H7AB0.42411.3781−0.02330.051*
H7AC0.47311.3213−0.10710.051*
C8A0.7364 (4)1.0949 (3)−0.15239 (15)0.0311 (7)
H8AA0.82851.1551−0.16940.047*
H8AB0.62921.1368−0.17500.047*
H8AC0.77000.9962−0.16880.047*
C9A0.8866 (4)0.8369 (3)−0.03221 (16)0.0298 (6)
H9AA1.00490.8411−0.01870.045*
H9AB0.88770.8244−0.08720.045*
H9AC0.83950.7547−0.00290.045*
C10A0.7629 (4)0.9341 (3)0.13688 (16)0.0320 (7)
H10D0.85950.97300.15700.048*
H10E0.79620.83130.12770.048*
H10F0.66210.94340.17420.048*
C1B0.6860 (3)0.0207 (3)0.58074 (15)0.0217 (5)
C2B0.6425 (3)−0.1248 (3)0.58812 (15)0.0230 (6)
C3B0.6905 (3)−0.1866 (3)0.51579 (15)0.0222 (5)
C4B0.7604 (3)−0.0790 (3)0.46392 (15)0.0217 (5)
C5B0.7598 (3)0.0501 (3)0.50399 (15)0.0215 (5)
C6B0.6614 (4)0.1239 (3)0.64341 (16)0.0324 (7)
H6BA0.75710.10210.67680.049*
H6BB0.55180.11310.67360.049*
H6BC0.65930.22400.62080.049*
C7B0.5666 (4)−0.1986 (3)0.65955 (16)0.0315 (7)
H7BA0.6585−0.23380.69350.047*
H7BB0.5110−0.28100.64620.047*
H7BC0.4805−0.12950.68570.047*
C8B0.6735 (4)−0.3398 (3)0.49793 (18)0.0327 (7)
H8BA0.7824−0.40190.50610.049*
H8BB0.6470−0.34050.44440.049*
H8BC0.5800−0.37670.53170.049*
C9B0.8314 (3)−0.0988 (3)0.38248 (15)0.0290 (6)
H9BA0.9574−0.12280.38090.043*
H9BB0.8025−0.00850.35090.043*
H9BC0.7804−0.17780.36260.043*
C10B0.8249 (4)0.1886 (3)0.47134 (17)0.0288 (6)
H10A0.95090.17210.46150.043*
H10B0.79440.26370.50800.043*
H10C0.77190.22050.42320.043*
U11U22U33U12U13U23
Br10.0522 (2)0.02018 (14)0.02845 (16)−0.00475 (13)0.00479 (14)−0.00135 (11)
Br20.02744 (15)0.04200 (19)0.03929 (19)0.00291 (14)0.00066 (13)−0.01010 (14)
Br3A0.0598 (9)0.0352 (4)0.0534 (3)0.0103 (6)0.0309 (7)0.0184 (3)
Br4A0.0404 (5)0.0323 (5)0.0970 (10)−0.0003 (4)−0.0318 (6)−0.0236 (6)
Br3B0.0598 (9)0.0352 (4)0.0534 (3)0.0103 (6)0.0309 (7)0.0184 (3)
Br4B0.0404 (5)0.0323 (5)0.0970 (10)−0.0003 (4)−0.0318 (6)−0.0236 (6)
Al10.0283 (6)0.0169 (5)0.0179 (6)−0.0012 (5)−0.0026 (4)−0.0020 (4)
Al20.0161 (5)0.0206 (5)0.0172 (5)−0.0002 (4)−0.0017 (4)−0.0013 (4)
Al30.0259 (4)0.0191 (4)0.0315 (5)−0.0011 (3)−0.0023 (3)−0.0029 (3)
C1A0.0390 (16)0.0183 (12)0.0230 (14)−0.0020 (12)−0.0037 (12)−0.0032 (11)
C2A0.0374 (15)0.0168 (12)0.0210 (13)−0.0038 (11)−0.0037 (11)0.0016 (10)
C3A0.0314 (14)0.0207 (13)0.0211 (13)−0.0052 (11)−0.0003 (11)−0.0015 (10)
C4A0.0288 (14)0.0223 (13)0.0228 (14)−0.0035 (11)−0.0005 (11)−0.0008 (11)
C5A0.0327 (14)0.0227 (13)0.0197 (13)−0.0026 (12)−0.0070 (11)−0.0008 (10)
C6A0.057 (2)0.0279 (15)0.0243 (15)0.0056 (15)−0.0104 (14)−0.0110 (12)
C7A0.0491 (19)0.0212 (14)0.0313 (16)−0.0014 (14)−0.0102 (14)−0.0004 (12)
C8A0.0373 (16)0.0341 (16)0.0209 (14)−0.0047 (13)0.0012 (12)0.0004 (12)
C9A0.0322 (15)0.0277 (15)0.0282 (15)0.0008 (12)0.0004 (12)−0.0043 (12)
C10A0.0412 (17)0.0301 (15)0.0245 (15)0.0008 (14)−0.0085 (13)−0.0016 (12)
C1B0.0197 (12)0.0250 (13)0.0206 (13)−0.0006 (11)−0.0047 (10)−0.0027 (10)
C2B0.0208 (12)0.0279 (14)0.0188 (13)0.0015 (11)−0.0022 (10)0.0015 (10)
C3B0.0196 (12)0.0218 (13)0.0237 (13)0.0026 (10)−0.0007 (10)−0.0009 (10)
C4B0.0189 (11)0.0248 (13)0.0208 (13)−0.0001 (10)0.0002 (10)−0.0040 (10)
C5B0.0185 (11)0.0247 (13)0.0212 (13)−0.0016 (10)−0.0021 (10)−0.0009 (10)
C6B0.0347 (15)0.0430 (18)0.0207 (14)−0.0030 (14)−0.0037 (12)−0.0103 (13)
C7B0.0306 (15)0.0385 (17)0.0219 (14)−0.0004 (13)0.0008 (12)0.0093 (12)
C8B0.0371 (16)0.0222 (14)0.0375 (17)−0.0003 (13)−0.0019 (13)−0.0007 (12)
C9B0.0276 (14)0.0335 (16)0.0241 (14)0.0008 (12)0.0050 (11)−0.0058 (12)
C10B0.0268 (14)0.0289 (15)0.0308 (16)−0.0069 (12)−0.0001 (12)−0.0003 (12)
Br1—Al32.2963 (9)C6A—H6AC0.9800
Br2—Al32.2952 (8)C7A—H7AA0.9800
Br3A—Al32.239 (7)C7A—H7AB0.9800
Br4A—Al32.304 (4)C7A—H7AC0.9800
Br3B—Al32.304 (2)C8A—H8AA0.9800
Br4B—Al32.2869 (14)C8A—H8AB0.9800
Al1—C4A2.129 (3)C8A—H8AC0.9800
Al1—C4Ai2.129 (3)C9A—H9AA0.9800
Al1—C3A2.139 (3)C9A—H9AB0.9800
Al1—C3Ai2.139 (3)C9A—H9AC0.9800
Al1—C5A2.140 (3)C10A—H10D0.9800
Al1—C5Ai2.140 (3)C10A—H10E0.9800
Al1—C1Ai2.153 (3)C10A—H10F0.9800
Al1—C1A2.153 (3)C1B—C2B1.429 (4)
Al1—C2A2.157 (3)C1B—C5B1.438 (4)
Al1—C2Ai2.157 (3)C1B—C6B1.501 (3)
Al2—C4Bii2.134 (2)C2B—C3B1.436 (3)
Al2—C4B2.134 (2)C2B—C7B1.494 (4)
Al2—C5Bii2.148 (3)C3B—C4B1.426 (4)
Al2—C5B2.148 (3)C3B—C8B1.507 (4)
Al2—C1B2.150 (3)C4B—C5B1.438 (3)
Al2—C1Bii2.150 (3)C4B—C9B1.504 (3)
Al2—C3Bii2.152 (2)C5B—C10B1.497 (4)
Al2—C3B2.152 (2)C6B—H6BA0.9800
Al2—C2Bii2.157 (3)C6B—H6BB0.9800
Al2—C2B2.157 (3)C6B—H6BC0.9800
C1A—C2A1.419 (4)C7B—H7BA0.9800
C1A—C5A1.447 (3)C7B—H7BB0.9800
C1A—C6A1.508 (3)C7B—H7BC0.9800
C2A—C3A1.431 (3)C8B—H8BA0.9800
C2A—C7A1.505 (4)C8B—H8BB0.9800
C3A—C4A1.427 (4)C8B—H8BC0.9800
C3A—C8A1.499 (4)C9B—H9BA0.9800
C4A—C5A1.441 (3)C9B—H9BB0.9800
C4A—C9A1.508 (3)C9B—H9BC0.9800
C5A—C10A1.502 (4)C10B—H10A0.9800
C6A—H6AA0.9800C10B—H10B0.9800
C6A—H6AB0.9800C10B—H10C0.9800
C4A—Al1—C4Ai180.0C3A—C2A—Al169.87 (16)
C4A—Al1—C3A39.05 (10)C7A—C2A—Al1125.4 (2)
C4Ai—Al1—C3A140.95 (10)C4A—C3A—C2A108.3 (2)
C4A—Al1—C3Ai140.95 (10)C4A—C3A—C8A127.0 (2)
C4Ai—Al1—C3Ai39.05 (10)C2A—C3A—C8A124.7 (2)
C3A—Al1—C3Ai180.0C4A—C3A—Al170.10 (17)
C4A—Al1—C5A39.46 (10)C2A—C3A—Al171.23 (16)
C4Ai—Al1—C5A140.54 (10)C8A—C3A—Al1125.4 (2)
C3A—Al1—C5A65.71 (11)C3A—C4A—C5A108.1 (2)
C3Ai—Al1—C5A114.29 (11)C3A—C4A—C9A126.9 (2)
C4A—Al1—C5Ai140.54 (10)C5A—C4A—C9A125.0 (2)
C4Ai—Al1—C5Ai39.46 (10)C3A—C4A—Al170.85 (16)
C3A—Al1—C5Ai114.29 (11)C5A—C4A—Al170.68 (15)
C3Ai—Al1—C5Ai65.71 (11)C9A—C4A—Al1124.2 (2)
C5A—Al1—C5Ai180.0C4A—C5A—C1A107.1 (2)
C4A—Al1—C1Ai114.31 (10)C4A—C5A—C10A126.7 (2)
C4Ai—Al1—C1Ai65.69 (10)C1A—C5A—C10A126.2 (2)
C3A—Al1—C1Ai114.91 (10)C4A—C5A—Al169.86 (15)
C3Ai—Al1—C1Ai65.09 (10)C1A—C5A—Al170.79 (16)
C5A—Al1—C1Ai140.62 (10)C10A—C5A—Al1126.4 (2)
C5Ai—Al1—C1Ai39.38 (10)C1A—C6A—H6AA109.5
C4A—Al1—C1A65.69 (10)C1A—C6A—H6AB109.5
C4Ai—Al1—C1A114.31 (10)H6AA—C6A—H6AB109.5
C3A—Al1—C1A65.09 (10)C1A—C6A—H6AC109.5
C3Ai—Al1—C1A114.90 (10)H6AA—C6A—H6AC109.5
C5A—Al1—C1A39.38 (10)H6AB—C6A—H6AC109.5
C5Ai—Al1—C1A140.62 (10)C2A—C7A—H7AA109.5
C1Ai—Al1—C1A180.00 (12)C2A—C7A—H7AB109.5
C4A—Al1—C2A65.39 (10)H7AA—C7A—H7AB109.5
C4Ai—Al1—C2A114.61 (10)C2A—C7A—H7AC109.5
C3A—Al1—C2A38.90 (9)H7AA—C7A—H7AC109.5
C3Ai—Al1—C2A141.10 (9)H7AB—C7A—H7AC109.5
C5A—Al1—C2A65.43 (11)C3A—C8A—H8AA109.5
C5Ai—Al1—C2A114.57 (11)C3A—C8A—H8AB109.5
C1Ai—Al1—C2A141.56 (10)H8AA—C8A—H8AB109.5
C1A—Al1—C2A38.44 (10)C3A—C8A—H8AC109.5
C4A—Al1—C2Ai114.61 (10)H8AA—C8A—H8AC109.5
C4Ai—Al1—C2Ai65.39 (10)H8AB—C8A—H8AC109.5
C3A—Al1—C2Ai141.10 (9)C4A—C9A—H9AA109.5
C3Ai—Al1—C2Ai38.90 (9)C4A—C9A—H9AB109.5
C5A—Al1—C2Ai114.57 (11)H9AA—C9A—H9AB109.5
C5Ai—Al1—C2Ai65.43 (11)C4A—C9A—H9AC109.5
C1Ai—Al1—C2Ai38.44 (10)H9AA—C9A—H9AC109.5
C1A—Al1—C2Ai141.56 (10)H9AB—C9A—H9AC109.5
C2A—Al1—C2Ai180.0C5A—C10A—H10D109.5
C4Bii—Al2—C4B180.0C5A—C10A—H10E109.5
C4Bii—Al2—C5Bii39.25 (9)H10D—C10A—H10E109.5
C4B—Al2—C5Bii140.75 (9)C5A—C10A—H10F109.5
C4Bii—Al2—C5B140.75 (9)H10D—C10A—H10F109.5
C4B—Al2—C5B39.25 (9)H10E—C10A—H10F109.5
C5Bii—Al2—C5B180.00 (14)C2B—C1B—C5B108.7 (2)
C4Bii—Al2—C1B114.57 (9)C2B—C1B—C6B125.4 (3)
C4B—Al2—C1B65.43 (9)C5B—C1B—C6B126.0 (3)
C5Bii—Al2—C1B140.90 (10)C2B—C1B—Al270.88 (14)
C5B—Al2—C1B39.10 (10)C5B—C1B—Al270.40 (14)
C4Bii—Al2—C1Bii65.43 (9)C6B—C1B—Al2125.53 (17)
C4B—Al2—C1Bii114.57 (9)C1B—C2B—C3B107.5 (2)
C5Bii—Al2—C1Bii39.10 (10)C1B—C2B—C7B125.5 (2)
C5B—Al2—C1Bii140.90 (10)C3B—C2B—C7B127.0 (3)
C1B—Al2—C1Bii180.0C1B—C2B—Al270.37 (14)
C4Bii—Al2—C3Bii38.87 (10)C3B—C2B—Al270.39 (15)
C4B—Al2—C3Bii141.13 (10)C7B—C2B—Al2126.15 (18)
C5Bii—Al2—C3Bii65.33 (10)C4B—C3B—C2B108.4 (2)
C5B—Al2—C3Bii114.67 (10)C4B—C3B—C8B125.7 (2)
C1B—Al2—C3Bii115.04 (9)C2B—C3B—C8B126.0 (3)
C1Bii—Al2—C3Bii64.96 (9)C4B—C3B—Al269.87 (14)
C4Bii—Al2—C3B141.13 (10)C2B—C3B—Al270.69 (13)
C4B—Al2—C3B38.87 (10)C8B—C3B—Al2126.13 (19)
C5Bii—Al2—C3B114.67 (10)C3B—C4B—C5B108.3 (2)
C5B—Al2—C3B65.33 (10)C3B—C4B—C9B126.2 (2)
C1B—Al2—C3B64.96 (9)C5B—C4B—C9B125.5 (3)
C1Bii—Al2—C3B115.04 (9)C3B—C4B—Al271.26 (13)
C3Bii—Al2—C3B180.0C5B—C4B—Al270.91 (13)
C4Bii—Al2—C2Bii65.48 (10)C9B—C4B—Al2125.92 (18)
C4B—Al2—C2Bii114.52 (10)C4B—C5B—C1B107.2 (2)
C5Bii—Al2—C2Bii65.51 (11)C4B—C5B—C10B126.0 (2)
C5B—Al2—C2Bii114.49 (11)C1B—C5B—C10B126.8 (2)
C1B—Al2—C2Bii141.24 (10)C4B—C5B—Al269.84 (15)
C1Bii—Al2—C2Bii38.76 (10)C1B—C5B—Al270.50 (15)
C3Bii—Al2—C2Bii38.92 (9)C10B—C5B—Al2125.03 (17)
C3B—Al2—C2Bii141.08 (9)C1B—C6B—H6BA109.5
C4Bii—Al2—C2B114.52 (10)C1B—C6B—H6BB109.5
C4B—Al2—C2B65.48 (10)H6BA—C6B—H6BB109.5
C5Bii—Al2—C2B114.49 (11)C1B—C6B—H6BC109.5
C5B—Al2—C2B65.51 (11)H6BA—C6B—H6BC109.5
C1B—Al2—C2B38.76 (10)H6BB—C6B—H6BC109.5
C1Bii—Al2—C2B141.24 (10)C2B—C7B—H7BA109.5
C3Bii—Al2—C2B141.08 (9)C2B—C7B—H7BB109.5
C3B—Al2—C2B38.92 (9)H7BA—C7B—H7BB109.5
C2Bii—Al2—C2B180.00 (10)C2B—C7B—H7BC109.5
Br3A—Al3—Br2105.36 (15)H7BA—C7B—H7BC109.5
Br4B—Al3—Br2111.17 (5)H7BB—C7B—H7BC109.5
Br3A—Al3—Br1105.60 (19)C3B—C8B—H8BA109.5
Br4B—Al3—Br1110.88 (6)C3B—C8B—H8BB109.5
Br2—Al3—Br1109.71 (4)H8BA—C8B—H8BB109.5
Br3A—Al3—Br4A127.9 (3)C3B—C8B—H8BC109.5
Br2—Al3—Br4A104.55 (10)H8BA—C8B—H8BC109.5
Br1—Al3—Br4A103.04 (10)H8BB—C8B—H8BC109.5
Br4B—Al3—Br3B105.47 (14)C4B—C9B—H9BA109.5
Br2—Al3—Br3B111.46 (7)C4B—C9B—H9BB109.5
Br1—Al3—Br3B108.05 (7)H9BA—C9B—H9BB109.5
C2A—C1A—C5A108.3 (2)C4B—C9B—H9BC109.5
C2A—C1A—C6A127.0 (2)H9BA—C9B—H9BC109.5
C5A—C1A—C6A124.7 (2)H9BB—C9B—H9BC109.5
C2A—C1A—Al170.94 (15)C5B—C10B—H10A109.5
C5A—C1A—Al169.83 (15)C5B—C10B—H10B109.5
C6A—C1A—Al1126.8 (2)H10A—C10B—H10B109.5
C1A—C2A—C3A108.3 (2)C5B—C10B—H10C109.5
C1A—C2A—C7A126.8 (2)H10A—C10B—H10C109.5
C3A—C2A—C7A125.0 (2)H10B—C10B—H10C109.5
C1A—C2A—Al170.62 (17)
C5A—C1A—C2A—C3A0.1 (3)C5B—C1B—C2B—C3B0.4 (3)
C6A—C1A—C2A—C3A177.9 (3)C6B—C1B—C2B—C3B−178.6 (2)
Al1—C1A—C2A—C3A−60.0 (2)Al2—C1B—C2B—C3B60.89 (17)
C5A—C1A—C2A—C7A−179.7 (3)C5B—C1B—C2B—C7B178.5 (2)
C6A—C1A—C2A—C7A−1.9 (5)C6B—C1B—C2B—C7B−0.5 (4)
Al1—C1A—C2A—C7A120.2 (3)Al2—C1B—C2B—C7B−121.0 (2)
C5A—C1A—C2A—Al160.1 (2)C5B—C1B—C2B—Al2−60.53 (17)
C6A—C1A—C2A—Al1−122.2 (3)C6B—C1B—C2B—Al2120.5 (2)
C1A—C2A—C3A—C4A−0.2 (3)C1B—C2B—C3B—C4B−0.9 (3)
C7A—C2A—C3A—C4A179.6 (3)C7B—C2B—C3B—C4B−179.0 (2)
Al1—C2A—C3A—C4A−60.6 (2)Al2—C2B—C3B—C4B59.97 (17)
C1A—C2A—C3A—C8A−179.0 (3)C1B—C2B—C3B—C8B177.9 (2)
C7A—C2A—C3A—C8A0.8 (5)C7B—C2B—C3B—C8B−0.1 (4)
Al1—C2A—C3A—C8A120.5 (3)Al2—C2B—C3B—C8B−121.2 (3)
C1A—C2A—C3A—Al160.5 (2)C1B—C2B—C3B—Al2−60.88 (16)
C7A—C2A—C3A—Al1−119.7 (3)C7B—C2B—C3B—Al2121.0 (3)
C2A—C3A—C4A—C5A0.1 (3)C2B—C3B—C4B—C5B1.1 (3)
C8A—C3A—C4A—C5A178.9 (3)C8B—C3B—C4B—C5B−177.7 (2)
Al1—C3A—C4A—C5A−61.2 (2)Al2—C3B—C4B—C5B61.60 (16)
C2A—C3A—C4A—C9A−179.7 (3)C2B—C3B—C4B—C9B178.2 (2)
C8A—C3A—C4A—C9A−0.9 (5)C8B—C3B—C4B—C9B−0.6 (4)
Al1—C3A—C4A—C9A118.9 (3)Al2—C3B—C4B—C9B−121.3 (3)
C2A—C3A—C4A—Al161.3 (2)C2B—C3B—C4B—Al2−60.49 (17)
C8A—C3A—C4A—Al1−119.9 (3)C8B—C3B—C4B—Al2120.7 (3)
C3A—C4A—C5A—C1A−0.1 (3)C3B—C4B—C5B—C1B−0.9 (3)
C9A—C4A—C5A—C1A179.8 (3)C9B—C4B—C5B—C1B−178.0 (2)
Al1—C4A—C5A—C1A−61.4 (2)Al2—C4B—C5B—C1B60.94 (17)
C3A—C4A—C5A—C10A−177.8 (3)C3B—C4B—C5B—C10B178.9 (2)
C9A—C4A—C5A—C10A2.1 (5)C9B—C4B—C5B—C10B1.8 (4)
Al1—C4A—C5A—C10A120.9 (3)Al2—C4B—C5B—C10B−119.3 (2)
C3A—C4A—C5A—Al161.3 (2)C3B—C4B—C5B—Al2−61.82 (17)
C9A—C4A—C5A—Al1−118.8 (3)C9B—C4B—C5B—Al2121.0 (3)
C2A—C1A—C5A—C4A0.0 (3)C2B—C1B—C5B—C4B0.3 (3)
C6A—C1A—C5A—C4A−177.8 (3)C6B—C1B—C5B—C4B179.2 (2)
Al1—C1A—C5A—C4A60.76 (19)Al2—C1B—C5B—C4B−60.52 (17)
C2A—C1A—C5A—C10A177.7 (3)C2B—C1B—C5B—C10B−179.5 (2)
C6A—C1A—C5A—C10A−0.1 (5)C6B—C1B—C5B—C10B−0.5 (4)
Al1—C1A—C5A—C10A−121.5 (3)Al2—C1B—C5B—C10B119.7 (2)
C2A—C1A—C5A—Al1−60.8 (2)C2B—C1B—C5B—Al260.83 (17)
C6A—C1A—C5A—Al1121.4 (3)C6B—C1B—C5B—Al2−120.2 (3)
D—H···AD—HH···AD···AD—H···A
C7A—H7AA···Br3Biii0.983.033.886 (4)146
C9A—H9AC···Br3A0.983.043.773 (8)133
C10A—H10E···Br3A0.983.054.007 (7)165
C9B—H9BB···Br10.982.953.770 (3)141
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
C7A—H7AA⋯Br3B i 0.983.033.886 (4)146
C9A—H9AC⋯Br3A 0.983.043.773 (8)133
C10A—H10E⋯Br3A 0.983.054.007 (7)165
C9B—H9BB⋯Br10.982.953.770 (3)141

Symmetry code: (i) .

  7 in total

1.  Al(50)C(120)H(180): a pseudofullerene shell of 60 carbon atoms and 60 methyl groups protecting a cluster core of 50 aluminum atoms.

Authors:  Jean Vollet; Jens R Hartig; Hansgeorg Schnöckel
Journal:  Angew Chem Int Ed Engl       Date:  2004-06-14       Impact factor: 15.336

2.  Al20Cp8*X10 (X=Cl, Br): snapshots of the formation of metalloid clusters from polyhedral AlnXm molecules?

Authors:  Jean Vollet; Ralf Burgert; Hansgeorg Schnöckel
Journal:  Angew Chem Int Ed Engl       Date:  2005-10-28       Impact factor: 15.336

3.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

4.  Anisotropic NMR interaction tensors in the decamethylaluminocenium cation.

Authors:  Robert W Schurko; Ivan Hung; Charles L B Macdonald; Alan H Cowley
Journal:  J Am Chem Soc       Date:  2002-11-06       Impact factor: 15.419

5.  Group 13 decamethylmetallocenium cations.

Authors:  Charles L B Macdonald; John D Gorden; Andreas Voigt; Silvia Filipponi; Alan H Cowley
Journal:  Dalton Trans       Date:  2007-12-18       Impact factor: 4.390

6.  Hunting for the magnesium(I) species: formation, structure, and reactivity of some donor-free Grignard compounds.

Authors:  Tomasz Kruczyński; Nikolay Pushkarevsky; Patrick Henke; Ralf Köppe; Elke Baum; Sergey Konchenko; Jerzy Pikies; Hansgeorg Schnöckel
Journal:  Angew Chem Int Ed Engl       Date:  2012-08-09       Impact factor: 15.336

7.  Synthesis and reactivity of bis-pentamethylcyclopentadienyl diiododialane (Cp*AlI)2: an aluminium(II) precursor to (Cp*Al)4.

Authors:  Stefan G Minasian; John Arnold
Journal:  Chem Commun (Camb)       Date:  2008-07-24       Impact factor: 6.222
  7 in total

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