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The title compound, (C6H22N4)[Al2F10]·H2O, was obtained by the reaction of aluminium oxide, tris(2-aminoethyl)amine (tren), HF and ethanol at 463 K for 1 h. It consists of (Al2F10)4- dimers, located on inversion centers, water molecules and tetraprotonated tren cations. A network of hydrogen bonds ensures the three-dimensional cohesion.
Supporting information
CCDC reference: 252752
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.043
- wR factor = 0.123
- Data-to-parameter ratio = 20.1
checkCIF/PLATON results
No syntax errors found
Alert level C
DIFMX01_ALERT_2_C The maximum difference density is > 0.1*ZMAX*0.75
_refine_diff_density_max given = 1.217
Test value = 0.975
DIFMX02_ALERT_1_C The minimum difference density is > 0.1*ZMAX*0.75
The relevant atom site should be identified.
PLAT097_ALERT_2_C Maximum (Positive) Residual Density ............ 1.22 e/A 3
PLAT432_ALERT_2_C Short Inter X...Y Contact F5 .. C5 .. 2.91 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1
PLAT751_ALERT_4_C Bond Calc 0.89524, Rep 0.895(3) ...... Senseless su
OW -H1W 1.555 1.555
PLAT751_ALERT_4_C Bond Calc 0.92635, Rep 0.927(3) ...... Senseless su
OW -H2W 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 108.03, Rep 108.0(3) ...... Senseless su
H1W -OW -H2W 1.555 1.555 1.555
PLAT755_ALERT_4_C D-H Calc 0.89524, Rep 0.895(3) ...... Senseless su
O1# -H1W 1.555 1.555
PLAT755_ALERT_4_C D-H Calc 0.92635, Rep 0.927(3) ...... Senseless su
O1# -H2W 1.555 1.555
PLAT756_ALERT_4_C H...A Calc 1.69233, Rep 1.6924(15) ...... Senseless su
H1W -F8 1.555 1.556
PLAT756_ALERT_4_C H...A Calc 1.87122, Rep 1.8713(16) ...... Senseless su
H2W -F8 1.555 2.665
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 2.71 Ratio
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
Al2 F10
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
14 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
10 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: Stadi4 (Stoe, 1998); cell refinement: Stadi4; data reduction: X-RED32 (Stoe, 1998); program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: enCIFer (Allen et al. (2004).
Crystal data top
C6H22N44+·Al2F104−·H2O | Z = 2 |
Mr = 412.23 | F(000) = 424.0 |
Triclinic, P1 | Dx = 1.836 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 7.6996 (16) Å | Cell parameters from 32 reflections |
b = 8.838 (2) Å | θ = 28–32° |
c = 12.197 (4) Å | µ = 0.31 mm−1 |
α = 105.87 (2)° | T = 293 K |
β = 97.74 (3)° | Parallepiped, colorless |
γ = 106.317 (15)° | 0.14 × 0.10 × 0.09 mm |
V = 745.8 (4) Å3 | |
Data collection top
Siemens AED2 diffractometer | 3119 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 30.0°, θmin = 1.8° |
2θ/ω scans | h = −10→10 |
Absorption correction: gaussian (SHELX76; Sheldrick, 1976) | k = −12→11 |
Tmin = 0.934, Tmax = 0.967 | l = 0→17 |
4283 measured reflections | 3 standard reflections every 120 min |
4283 independent reflections | intensity decay: 15% |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.123 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0562P)2 + 0.5017P] where P = (Fo2 + 2Fc2)/3 |
4269 reflections | (Δ/σ)max < 0.001 |
212 parameters | Δρmax = 1.22 e Å−3 |
0 restraints | Δρmin = −0.73 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
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 | |
Al1 | 0.64711 (9) | 0.10387 (8) | −0.03968 (6) | 0.01633 (14) | |
Al2 | 0.13806 (9) | 0.16839 (8) | −0.43328 (6) | 0.01701 (14) | |
F1 | 0.50347 (17) | 0.11929 (15) | 0.07394 (11) | 0.0185 (3) | |
F2 | 0.47946 (19) | 0.13192 (18) | −0.13743 (12) | 0.0237 (3) | |
F3 | 0.7706 (2) | 0.05726 (19) | −0.15113 (13) | 0.0284 (3) | |
F4 | 0.7824 (2) | 0.31966 (17) | 0.01730 (13) | 0.0276 (3) | |
F5 | 0.81633 (18) | 0.07178 (17) | 0.06038 (12) | 0.0239 (3) | |
F6 | −0.02659 (17) | −0.01903 (16) | −0.41057 (11) | 0.0197 (3) | |
F7 | 0.2119 (2) | 0.27790 (18) | −0.28188 (12) | 0.0295 (3) | |
F8 | 0.2803 (2) | 0.32431 (19) | −0.47908 (13) | 0.0295 (3) | |
F9 | 0.30964 (18) | 0.06826 (18) | −0.43321 (13) | 0.0265 (3) | |
F10 | −0.04581 (19) | 0.25217 (17) | −0.44759 (12) | 0.0240 (3) | |
N1 | 0.0976 (2) | 0.3777 (2) | 0.17887 (16) | 0.0179 (3) | |
H1A | −0.0065 | 0.3262 | 0.1199 | 0.0400 (18)* | |
C1 | 0.2498 (3) | 0.3213 (3) | 0.1338 (2) | 0.0236 (4) | |
H1B | 0.2190 | 0.2027 | 0.1213 | 0.0400 (18)* | |
H1C | 0.3646 | 0.3784 | 0.1935 | 0.0400 (18)* | |
C2 | 0.2821 (3) | 0.3530 (3) | 0.0209 (2) | 0.0245 (5) | |
H2D | 0.2606 | 0.4559 | 0.0205 | 0.0400 (18)* | |
H2E | 0.4106 | 0.3670 | 0.0177 | 0.0400 (18)* | |
N2 | 0.1587 (3) | 0.2149 (3) | −0.08402 (18) | 0.0241 (4) | |
H2A | 0.1776 | 0.1202 | −0.0838 | 0.0400 (18)* | |
H2B | 0.1837 | 0.2370 | −0.1483 | 0.0400 (18)* | |
H2C | 0.0406 | 0.2047 | −0.0830 | 0.0400 (18)* | |
C3 | 0.1333 (3) | 0.5622 (3) | 0.20895 (19) | 0.0186 (4) | |
H3D | 0.0367 | 0.5900 | 0.2452 | 0.0400 (18)* | |
H3E | 0.1270 | 0.5907 | 0.1375 | 0.0400 (18)* | |
C4 | 0.3216 (3) | 0.6652 (3) | 0.2914 (2) | 0.0256 (5) | |
H4D | 0.3398 | 0.6215 | 0.3552 | 0.0400 (18)* | |
H4E | 0.4193 | 0.6585 | 0.2497 | 0.0400 (18)* | |
N3 | 0.3309 (3) | 0.8409 (2) | 0.33845 (17) | 0.0219 (4) | |
H3A | 0.2514 | 0.8483 | 0.3847 | 0.0400 (18)* | |
H3B | 0.3013 | 0.8770 | 0.2795 | 0.0400 (18)* | |
H3C | 0.4457 | 0.9033 | 0.3795 | 0.0400 (18)* | |
C5 | 0.0564 (3) | 0.3155 (3) | 0.2787 (2) | 0.0256 (5) | |
H5A | 0.1567 | 0.3792 | 0.3475 | 0.0400 (18)* | |
H5B | 0.0491 | 0.1994 | 0.2585 | 0.0400 (18)* | |
C6 | −0.1256 (4) | 0.3314 (3) | 0.3062 (2) | 0.0282 (5) | |
H6A | −0.0996 | 0.4212 | 0.3793 | 0.0400 (18)* | |
H6B | −0.1902 | 0.3598 | 0.2449 | 0.0400 (18)* | |
N4 | −0.2461 (3) | 0.1757 (3) | 0.31569 (19) | 0.0263 (4) | |
H4A | −0.2815 | 0.0961 | 0.2462 | 0.0400 (18)* | |
H4B | −0.3459 | 0.1922 | 0.3390 | 0.0400 (18)* | |
H4C | −0.1837 | 0.1448 | 0.3676 | 0.0400 (18)* | |
OW | 0.5195 (4) | 0.3353 (4) | 0.3911 (3) | 0.0755 (9) | |
H1W | 0.4355 | 0.3238 | 0.4350 | 0.0400 (18)* | |
H2W | 0.5840 | 0.4481 | 0.4103 | 0.0400 (18)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Al1 | 0.0143 (3) | 0.0191 (3) | 0.0176 (3) | 0.0061 (2) | 0.0036 (2) | 0.0085 (2) |
Al2 | 0.0152 (3) | 0.0213 (3) | 0.0151 (3) | 0.0058 (2) | 0.0041 (2) | 0.0068 (2) |
F1 | 0.0195 (6) | 0.0174 (6) | 0.0183 (6) | 0.0063 (5) | 0.0056 (5) | 0.0045 (5) |
F2 | 0.0230 (7) | 0.0311 (7) | 0.0227 (7) | 0.0131 (6) | 0.0040 (5) | 0.0140 (6) |
F3 | 0.0264 (7) | 0.0383 (8) | 0.0298 (7) | 0.0155 (6) | 0.0147 (6) | 0.0170 (6) |
F4 | 0.0266 (7) | 0.0207 (7) | 0.0325 (8) | 0.0028 (6) | −0.0011 (6) | 0.0130 (6) |
F5 | 0.0181 (6) | 0.0242 (7) | 0.0304 (7) | 0.0074 (5) | −0.0006 (5) | 0.0131 (6) |
F6 | 0.0198 (6) | 0.0233 (6) | 0.0157 (6) | 0.0052 (5) | 0.0053 (5) | 0.0075 (5) |
F7 | 0.0346 (8) | 0.0326 (8) | 0.0159 (6) | 0.0067 (6) | 0.0027 (6) | 0.0058 (6) |
F8 | 0.0283 (7) | 0.0301 (8) | 0.0297 (8) | 0.0031 (6) | 0.0118 (6) | 0.0138 (6) |
F9 | 0.0165 (6) | 0.0298 (7) | 0.0317 (8) | 0.0089 (6) | 0.0022 (5) | 0.0080 (6) |
F10 | 0.0233 (7) | 0.0255 (7) | 0.0261 (7) | 0.0114 (6) | 0.0069 (5) | 0.0089 (6) |
N1 | 0.0178 (8) | 0.0198 (8) | 0.0174 (8) | 0.0070 (7) | 0.0040 (7) | 0.0071 (7) |
C1 | 0.0241 (11) | 0.0259 (11) | 0.0262 (11) | 0.0143 (9) | 0.0082 (9) | 0.0092 (9) |
C2 | 0.0262 (11) | 0.0231 (11) | 0.0305 (12) | 0.0118 (9) | 0.0140 (9) | 0.0111 (9) |
N2 | 0.0263 (10) | 0.0282 (10) | 0.0259 (10) | 0.0142 (8) | 0.0101 (8) | 0.0140 (8) |
C3 | 0.0180 (9) | 0.0188 (10) | 0.0199 (10) | 0.0071 (8) | 0.0039 (8) | 0.0072 (8) |
C4 | 0.0175 (10) | 0.0216 (11) | 0.0327 (12) | 0.0044 (8) | 0.0010 (9) | 0.0058 (9) |
N3 | 0.0181 (9) | 0.0237 (9) | 0.0204 (9) | 0.0049 (7) | 0.0038 (7) | 0.0042 (7) |
C5 | 0.0272 (11) | 0.0308 (12) | 0.0266 (12) | 0.0113 (10) | 0.0094 (9) | 0.0182 (10) |
C6 | 0.0309 (12) | 0.0253 (11) | 0.0329 (13) | 0.0090 (10) | 0.0162 (10) | 0.0130 (10) |
N4 | 0.0253 (10) | 0.0262 (10) | 0.0277 (10) | 0.0055 (8) | 0.0060 (8) | 0.0123 (8) |
OW | 0.0619 (18) | 0.077 (2) | 0.087 (2) | 0.0266 (15) | 0.0436 (17) | 0.0093 (17) |
Geometric parameters (Å, º) top
Al1—F2 | 1.7538 (15) | F8—F10 | 2.520 (2) |
Al1—F4 | 1.7802 (16) | F8—F9 | 2.536 (2) |
Al1—F3 | 1.7842 (16) | F8—F6ii | 2.693 (2) |
Al1—F5 | 1.7989 (15) | F9—F6ii | 2.543 (2) |
Al1—F1i | 1.8821 (15) | F9—F10ii | 2.825 (2) |
Al1—F1 | 1.8859 (15) | F10—F6ii | 2.550 (2) |
Al2—F7 | 1.7610 (17) | F10—F9ii | 2.825 (2) |
Al2—F8 | 1.7742 (15) | N1—C5 | 1.502 (3) |
Al2—F10 | 1.7822 (15) | N1—C3 | 1.505 (3) |
Al2—F9 | 1.7848 (15) | N1—C1 | 1.508 (3) |
Al2—F6 | 1.8955 (15) | N1—H1A | 0.9100 |
Al2—F6ii | 1.9117 (16) | C1—C2 | 1.517 (3) |
F1—Al1i | 1.8821 (15) | C1—H1B | 0.9700 |
F1—F1i | 2.352 (3) | C1—H1C | 0.9700 |
F1—F2i | 2.5734 (19) | C2—N2 | 1.482 (3) |
F1—F5 | 2.5776 (19) | C2—H2D | 0.9700 |
F1—F5i | 2.581 (2) | C2—H2E | 0.9700 |
F1—F2 | 2.595 (2) | N2—H2A | 0.8900 |
F1—F4 | 2.675 (2) | N2—H2B | 0.8900 |
F1—F3i | 2.695 (2) | N2—H2C | 0.8900 |
F2—F3 | 2.522 (2) | C3—C4 | 1.519 (3) |
F2—F1i | 2.5734 (19) | C3—H3D | 0.9700 |
F2—F4 | 2.585 (2) | C3—H3E | 0.9700 |
F2—F5i | 2.917 (2) | C4—N3 | 1.478 (3) |
F3—F5 | 2.519 (2) | C4—H4D | 0.9700 |
F3—F4 | 2.614 (2) | C4—H4E | 0.9700 |
F3—F1i | 2.695 (2) | N3—H3A | 0.8900 |
F4—F5 | 2.4611 (19) | N3—H3B | 0.8900 |
F5—F1i | 2.581 (2) | N3—H3C | 0.8900 |
F5—F2i | 2.917 (2) | C5—C6 | 1.520 (3) |
F6—Al2ii | 1.9117 (16) | C5—H5A | 0.9700 |
F6—F6ii | 2.367 (3) | C5—H5B | 0.9700 |
F6—F9ii | 2.543 (2) | C6—N4 | 1.472 (3) |
F6—F10ii | 2.550 (2) | C6—H6A | 0.9700 |
F6—F9 | 2.5613 (19) | C6—H6B | 0.9700 |
F6—F10 | 2.597 (2) | N4—H4A | 0.8900 |
F6—F7 | 2.643 (2) | N4—H4B | 0.8900 |
F6—F8ii | 2.693 (2) | N4—H4C | 0.8900 |
F7—F10 | 2.547 (2) | OW—H1W | 0.895 (3) |
F7—F9 | 2.587 (2) | OW—H2W | 0.927 (3) |
F7—F8 | 2.644 (2) | | |
| | | |
F2—Al1—F4 | 94.02 (8) | C1—C2—H2E | 109.2 |
F2—Al1—F3 | 90.91 (8) | H2D—C2—H2E | 107.9 |
F4—Al1—F3 | 94.33 (8) | C2—N2—H2A | 109.5 |
F2—Al1—F5 | 179.04 (7) | C2—N2—H2B | 109.5 |
F4—Al1—F5 | 86.89 (7) | H2A—N2—H2B | 109.5 |
F3—Al1—F5 | 89.34 (8) | C2—N2—H2C | 109.5 |
F2—Al1—F1i | 90.03 (7) | H2A—N2—H2C | 109.5 |
F4—Al1—F1i | 170.15 (7) | H2B—N2—H2C | 109.5 |
F3—Al1—F1i | 94.58 (7) | N1—C3—C4 | 112.31 (18) |
F5—Al1—F1i | 89.02 (7) | N1—C3—H3D | 109.1 |
F2—Al1—F1 | 90.88 (7) | C4—C3—H3D | 109.1 |
F4—Al1—F1 | 93.69 (7) | N1—C3—H3E | 109.1 |
F3—Al1—F1 | 171.64 (7) | C4—C3—H3E | 109.1 |
F5—Al1—F1 | 88.75 (7) | H3D—C3—H3E | 107.9 |
F1i—Al1—F1 | 77.26 (7) | N3—C4—C3 | 109.57 (19) |
F7—Al2—F8 | 96.81 (8) | N3—C4—H4D | 109.8 |
F7—Al2—F10 | 91.94 (8) | C3—C4—H4D | 109.8 |
F8—Al2—F10 | 90.26 (7) | N3—C4—H4E | 109.8 |
F7—Al2—F9 | 93.71 (8) | C3—C4—H4E | 109.8 |
F8—Al2—F9 | 90.88 (8) | H4D—C4—H4E | 108.2 |
F10—Al2—F9 | 174.06 (8) | C4—N3—H3A | 109.5 |
F7—Al2—F6 | 92.51 (7) | C4—N3—H3B | 109.5 |
F8—Al2—F6 | 170.67 (7) | H3A—N3—H3B | 109.5 |
F10—Al2—F6 | 89.78 (7) | C4—N3—H3C | 109.5 |
F9—Al2—F6 | 88.15 (7) | H3A—N3—H3C | 109.5 |
F7—Al2—F6ii | 169.37 (7) | H3B—N3—H3C | 109.5 |
F8—Al2—F6ii | 93.79 (7) | N1—C5—C6 | 111.04 (19) |
F10—Al2—F6ii | 87.26 (7) | N1—C5—H5A | 109.4 |
F9—Al2—F6ii | 86.85 (7) | C6—C5—H5A | 109.4 |
F6—Al2—F6ii | 76.89 (7) | N1—C5—H5B | 109.4 |
C5—N1—C3 | 112.54 (18) | C6—C5—H5B | 109.4 |
C5—N1—C1 | 109.66 (17) | H5A—C5—H5B | 108.0 |
C3—N1—C1 | 114.30 (17) | N4—C6—C5 | 111.6 (2) |
C5—N1—H1A | 106.6 | N4—C6—H6A | 109.3 |
C3—N1—H1A | 106.6 | C5—C6—H6A | 109.3 |
C1—N1—H1A | 106.6 | N4—C6—H6B | 109.3 |
N1—C1—C2 | 114.29 (18) | C5—C6—H6B | 109.3 |
N1—C1—H1B | 108.7 | H6A—C6—H6B | 108.0 |
C2—C1—H1B | 108.7 | C6—N4—H4A | 109.5 |
N1—C1—H1C | 108.7 | C6—N4—H4B | 109.5 |
C2—C1—H1C | 108.7 | H4A—N4—H4B | 109.5 |
H1B—C1—H1C | 107.6 | C6—N4—H4C | 109.5 |
N2—C2—C1 | 112.21 (19) | H4A—N4—H4C | 109.5 |
N2—C2—H2D | 109.2 | H4B—N4—H4C | 109.5 |
C1—C2—H2D | 109.2 | H1W—OW—H2W | 108.0 (3) |
N2—C2—H2E | 109.2 | | |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x, −y, −z−1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···F4iii | 0.91 | 1.89 | 2.738 (2) | 154 |
N1—H1A···F5iii | 0.91 | 2.14 | 2.796 (2) | 129 |
N2—H2A···F5i | 0.89 | 1.81 | 2.683 (2) | 167 |
N2—H2B···F7 | 0.89 | 1.79 | 2.678 (3) | 175 |
N2—H2C···F3iii | 0.89 | 2.03 | 2.814 (3) | 146 |
N3—H3A···F10iv | 0.89 | 1.95 | 2.764 (2) | 152 |
N3—H3B···F3v | 0.89 | 1.88 | 2.771 (3) | 177 |
N3—H3C···F9v | 0.89 | 1.83 | 2.650 (2) | 152 |
N4—H4A···F2vi | 0.89 | 2.10 | 2.884 (3) | 146 |
N4—H4B···OWiii | 0.89 | 1.88 | 2.694 (4) | 150 |
N4—H4C···F10vii | 0.89 | 2.17 | 2.884 (3) | 136 |
N4—H4C···F9vi | 0.89 | 2.27 | 2.869 (3) | 125 |
OW—H1W···F8vii | 0.895 (3) | 1.6924 (15) | 2.584 (3) | 173.8 (2) |
OW—H2W···F8v | 0.927 (3) | 1.8713 (16) | 2.786 (4) | 168.8 (2) |
Symmetry codes: (i) −x+1, −y, −z; (iii) x−1, y, z; (iv) −x, −y+1, −z; (v) −x+1, −y+1, −z; (vi) −x, −y, −z; (vii) x, y, z+1. |
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