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The crystal structure of diethylaminoalane, [H2Al—N(C2H5)2]2, was determined by X-ray powder diffraction in conjunction with DFT calculations. Diethylaminoalane crystallizes in the monoclinic space group P21/c with a = 7.4020 (2), b = 12.9663 (3), c = 7.2878 (2) Å and β = 90.660 (2)° at 293 K. The crystal structure was confirmed by DFT calculations and Raman spectroscopy. The molecular structure of diethylaminoalane consists of dimers of [H2Al—N(CH2CH3)2] in which an Al2N2 four-membered ring is formed by a center of inversion. Such an arrangement of the aminoalane moieties in the crystal structure is well known for this class of compound, as shown by the comparison with ethylmethylaminoalane and diisopropylaminoalane.
Supporting information
Data collection: Stoe; program(s) used to solve structure: EXPO2009; program(s) used to refine structure: GSAS.
Crystal data top
C4H12AlN | V = 699.41 (3) Å3 |
Mr = 101.13 | Z = 4 |
Monoclinic, P21/c | Dx = 0.960 Mg m−3 |
a = 7.40203 (19) Å | Mo Kα1 radiation, λ = 0.7093 Å |
b = 12.9663 (3) Å | T = 293 K |
c = 7.28776 (17) Å | white |
β = 90.660 (2)° | |
Data collection top
Stoe StadiP diffractometer | 2θmin = 2.966°, 2θmax = 60.071°, 2θstep = 0.015° |
Scan method: step | |
Refinement top
Least-squares matrix: full | 74 parameters |
Rp = 0.053 | 45 restraints |
Rwp = 0.067 | H atoms treated by a mixture of independent and constrained refinement |
Rexp = 0.057 | (Δ/σ)max = 0.08 |
R(F2) = 0.28094 | Background function: GSAS Background function number 1 with 20 terms. |
3808 data points | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
N1 | 0.6344 (3) | 0.9908 (2) | 0.1284 (3) | 0.0601 (14)* | |
C1 | 0.78016 (19) | 0.91096 (11) | 0.1319 (2) | 0.0601 (14)* | |
C2 | 0.65640 (19) | 1.06186 (11) | 0.28800 (19) | 0.0601 (14)* | |
C3 | 0.83310 (18) | 1.12205 (11) | 0.29266 (19) | 0.0601 (14)* | |
C4 | 0.76494 (19) | 0.84991 (11) | 0.30853 (19) | 0.0601 (14)* | |
Al1 | 0.3907 (3) | 0.9387 (2) | 0.1042 (4) | 0.0849 (14)* | |
H1 | 0.285 | 0.972 | 0.262 | 0.0721 (17)* | |
H2 | 0.39331 | 0.8337 | 0.04098 | 0.0721 (17)* | |
H3 | 0.6492 (4) | 1.0168 (2) | 0.4114 (6) | 0.0721 (17)* | |
H4 | 0.5449 (5) | 1.1165 (3) | 0.2865 (4) | 0.0721 (17)* | |
H5 | 0.8594 (4) | 1.1529 (2) | 0.1581 (8) | 0.0721 (17)* | |
H6 | 0.9437 (5) | 1.0707 (3) | 0.3340 (4) | 0.0721 (17)* | |
H7 | 0.8230 (4) | 1.1851 (3) | 0.3909 (5) | 0.0721 (17)* | |
H8 | 0.9115 (8) | 0.9482 (2) | 0.1264 (4) | 0.0721 (17)* | |
H9 | 0.7637 (3) | 0.8601 (3) | 0.0163 (6) | 0.0721 (17)* | |
H10 | 0.8284 (4) | 0.7754 (4) | 0.2917 (4) | 0.0721 (17)* | |
H11 | 0.6213 (12) | 0.8391 (2) | 0.3417 (4) | 0.0721 (17)* | |
H12 | 0.8328 (4) | 0.8921 (2) | 0.4207 (5) | 0.0721 (17)* | |
Geometric parameters (Å, º) top
N1—C1 | 1.495 (3) | Al1—N1 | 1.933 (4) |
N1—C2 | 1.491 (3) | N1—C1 | 1.495 (3) |
N1—Al1 | 1.932 (3) | N1—C2 | 1.491 (3) |
N1—Al1 | 1.933 (4) | N1—Al1 | 1.932 (3) |
C1—C4 | 1.516 (2) | C1—C4 | 1.516 (2) |
C1—H8 | 1.086 (6) | C1—H8 | 1.086 (6) |
C1—H9 | 1.076 (4) | C1—H9 | 1.076 (4) |
C2—C3 | 1.523 (2) | C2—C3 | 1.523 (2) |
C2—H3 | 1.075 (4) | C2—H3 | 1.075 (4) |
C2—H4 | 1.088 (4) | C2—H4 | 1.088 (4) |
C3—H5 | 1.079 (6) | C3—H5 | 1.079 (6) |
C3—H6 | 1.095 (4) | C3—H6 | 1.095 (4) |
C3—H7 | 1.090 (4) | C3—H7 | 1.090 (4) |
C4—H10 | 1.082 (5) | C4—H10 | 1.082 (5) |
C4—H11 | 1.102 (9) | C4—H11 | 1.102 (9) |
C4—H12 | 1.100 (4) | C4—H12 | 1.100 (4) |
Al1—H1 | 1.464 | Al1—H1 | 1.464 |
Al1—H2 | 1.437 | Al1—H2 | 1.437 |
| | | |
C1—N1—C2 | 110.0 (2) | Al1—N1—Al1 | 90.3 (1) |
C1—N1—Al1 | 115.6 (2) | C1—N1—C2 | 110.0 (2) |
C2—N1—Al1 | 112.4 (2) | C1—N1—Al1 | 115.6 (2) |
Al1—N1—Al1 | 90.3 (1) | C2—N1—Al1 | 112.4 (2) |
N1—C1—C4 | 108.4 (1) | N1—C1—C4 | 108.4 (1) |
N1—C1—H8 | 109.7 (2) | N1—C1—H8 | 109.7 (2) |
N1—C1—H9 | 109.6 (2) | N1—C1—H9 | 109.6 (2) |
C4—C1—H8 | 109.8 (2) | C4—C1—H8 | 109.8 (2) |
C4—C1—H9 | 109.6 (2) | C4—C1—H9 | 109.6 (2) |
H8—C1—H9 | 109.7 (3) | H8—C1—H9 | 109.7 (3) |
N1—C2—C3 | 114.8 (1) | N1—C2—C3 | 114.8 (1) |
N1—C2—H3 | 108.1 (2) | N1—C2—H3 | 108.1 (2) |
N1—C2—H4 | 108.6 (2) | N1—C2—H4 | 108.6 (2) |
C3—C2—H3 | 108.1 (2) | C3—C2—H3 | 108.1 (2) |
C3—C2—H4 | 108.5 (2) | C3—C2—H4 | 108.5 (2) |
H3—C2—H4 | 108.5 (3) | H3—C2—H4 | 108.5 (3) |
C2—C3—H5 | 109.5 (2) | C2—C3—H5 | 109.5 (2) |
C2—C3—H6 | 109.5 (2) | C2—C3—H6 | 109.5 (2) |
C2—C3—H7 | 109.5 (2) | C2—C3—H7 | 109.5 (2) |
H5—C3—H6 | 109.5 (3) | H5—C3—H6 | 109.5 (3) |
H5—C3—H7 | 109.5 (3) | H5—C3—H7 | 109.5 (3) |
H6—C3—H7 | 109.4 (3) | H6—C3—H7 | 109.4 (3) |
C1—C4—H10 | 109.5 (2) | C1—C4—H10 | 109.5 (2) |
C1—C4—H11 | 109.5 (3) | C1—C4—H11 | 109.5 (3) |
C1—C4—H12 | 109.5 (2) | C1—C4—H12 | 109.5 (2) |
H10—C4—H11 | 109.5 (3) | H10—C4—H11 | 109.5 (3) |
H10—C4—H12 | 109.5 (3) | H10—C4—H12 | 109.5 (3) |
H11—C4—H12 | 109.5 (3) | H11—C4—H12 | 109.5 (3) |
N1—Al1—H1 | 109.4 | N1—Al1—N1 | 89.7 (1) |
N1—Al1—H2 | 110.2 | N1—Al1—H1 | 120.1 |
N1—Al1—N1 | 89.7 (1) | N1—Al1—H2 | 99.7 |
H1—Al1—H2 | 122.7 | N1—Al1—H1 | 109.4 |
H1—Al1—N1 | 120.1 | N1—Al1—H2 | 110.2 |
H2—Al1—N1 | 99.7 | H1—Al1—H2 | 122.7 |
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