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The dimeric title coordination compound, [Al2(C4H9)2Cl2(C3H8N)2], comprises tetrahedral Al atoms each bonded to two N atoms of the amide ligands, one C atom of the tert-butyl group and one Cl atom. The Al atoms are bridged by amide moieties, creating a planar four-membered Al2N2 ring, which may be considered as the main structural feature. A twofold rotation axis passes through the centre of the ring. The Al—N bond distance are 1.943 (4) and 1.962 (4) Å. Pseudosymmetry in space group P42/nmc was considered but the space group P\overline 421c was confirmed by the structure solution and refinement.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804021622/bt6510sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804021622/bt6510Isup2.hkl
Contains datablock I

CCDC reference: 252755

Key indicators

  • Single-crystal X-ray study
  • T = 213 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.060
  • wR factor = 0.124
  • Data-to-parameter ratio = 23.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 90 PerFit
Author Response: See PLAT_113.

PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem...          4
PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem...          m
PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem...          m
PLAT113_ALERT_2_B ADDSYM Suggests Possible Pseudo/New Spacegroup .    P42/nmc
Author Response: Refinement in suggested new space group was checked and proofed to be unstable.

Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.500 From the CIF: _refine_ls_abs_structure_Flack_su 0.200 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.50 PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C1 PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.20 Ratio
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.22 From the CIF: _reflns_number_total 2162 Count of symmetry unique reflns 1330 Completeness (_total/calc) 162.56% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 832 Fraction of Friedel pairs measured 0.626 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 5 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

Bis(µ-N-methylethylamido)bis[tert-butylchloroaluminium] top
Crystal data top
[Al2(C4H9)2Cl2(C3H8N)2]Dx = 1.130 Mg m3
Mr = 355.29Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P421cCell parameters from 8923 reflections
Hall symbol: P-42nθ = 2–25°
a = 12.0110 (1) ŵ = 0.39 mm1
c = 14.4768 (3) ÅT = 213 K
V = 2088.48 (5) Å3Block, colourless
Z = 40.40 × 0.30 × 0.20 mm
F(000) = 768
Data collection top
BRUKER smart CCD
diffractometer
2162 independent reflections
Radiation source: fine-focus sealed tube1693 reflections with i > 2Σ(I)
Graphite monochromatorRint = 0.094
ω scansθmax = 27.2°, θmin = 2.2°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 614
Tmin = 0.860, Tmax = 0.926k = 1414
8923 measured reflectionsl = 1815
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.060H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.124 w = 1/[σ2(Fo2) + (0.0324P)2 + 1.7272P]
where P = (Fo2 + 2Fc2)/3
S = 1.17(Δ/σ)max < 0.001
2162 reflectionsΔρmax = 0.35 e Å3
92 parametersΔρmin = 0.37 e Å3
0 restraintsAbsolute structure: Flack (1983), 832 Friedel reflections [CHECK]
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.5 (2)
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
xyzUiso*/Ueq
Al10.38453 (7)0.00653 (12)0.10112 (6)0.0302 (2)
Cl10.33940 (8)0.00943 (15)0.04225 (6)0.0572 (3)
N10.4947 (3)0.1123 (2)0.11765 (15)0.0339 (6)
C10.2489 (3)0.0085 (5)0.1792 (2)0.0427 (9)
C20.1823 (4)0.0962 (5)0.1546 (4)0.0668 (18)
H2A0.17250.10010.08820.077 (3)*
H2B0.22220.16160.17570.077 (3)*
H2C0.11000.09320.18430.077 (3)*
C30.2624 (3)0.0111 (7)0.2842 (2)0.0689 (15)
H3A0.30400.07690.30190.077 (3)*
H3B0.18960.01280.31310.077 (3)*
H3C0.30220.05490.30430.077 (3)*
C40.1795 (5)0.1105 (6)0.1513 (5)0.0722 (19)
H4A0.22030.17780.16610.077 (3)*
H4B0.16490.10810.08540.077 (3)*
H4C0.10950.10990.18470.077 (3)*
C50.4924 (5)0.1571 (3)0.2144 (2)0.0487 (9)
H5A0.50020.09610.25780.077 (3)*
H5B0.42210.19470.22510.077 (3)*
H5C0.55320.20920.22270.077 (3)*
C60.4827 (4)0.2076 (3)0.0511 (3)0.0541 (12)
H6A0.47710.17720.01160.077 (3)*
H6B0.41270.24630.06450.077 (3)*
C70.5751 (5)0.2906 (4)0.0532 (4)0.0843 (18)
H7A0.56030.34900.00860.077 (3)*
H7B0.64470.25400.03780.077 (3)*
H7C0.58050.32270.11450.077 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Al10.0287 (4)0.0368 (5)0.0252 (4)0.0013 (6)0.0020 (4)0.0004 (7)
Cl10.0565 (6)0.0843 (8)0.0307 (4)0.0047 (8)0.0116 (4)0.0018 (8)
N10.0397 (15)0.0310 (12)0.0309 (12)0.003 (2)0.000 (2)0.0009 (10)
C10.0306 (16)0.057 (2)0.0401 (17)0.000 (2)0.0043 (14)0.005 (3)
C20.046 (3)0.083 (4)0.072 (5)0.020 (3)0.010 (3)0.007 (3)
C30.049 (2)0.116 (4)0.042 (2)0.003 (4)0.0167 (18)0.011 (4)
C40.048 (3)0.086 (4)0.083 (5)0.018 (3)0.016 (3)0.001 (4)
C50.052 (2)0.048 (2)0.0461 (18)0.006 (3)0.007 (3)0.0208 (16)
C60.061 (3)0.038 (2)0.064 (2)0.002 (2)0.008 (3)0.0164 (19)
C70.091 (4)0.059 (3)0.103 (5)0.020 (3)0.014 (4)0.029 (3)
Geometric parameters (Å, º) top
Al1—N1i1.943 (4)C3—H3B0.9700
Al1—N11.962 (4)C3—H3C0.9700
Al1—C11.983 (3)C4—H4A0.9700
Al1—Cl12.1455 (12)C4—H4B0.9700
Al1—Al1i2.7782 (18)C4—H4C0.9700
N1—C51.500 (4)C5—H5A0.9700
N1—C61.502 (4)C5—H5B0.9700
N1—Al1i1.943 (4)C5—H5C0.9700
C1—C31.530 (5)C6—C71.493 (7)
C1—C21.533 (7)C6—H6A0.9800
C1—C41.535 (8)C6—H6B0.9800
C2—H2A0.9700C7—H7A0.9700
C2—H2B0.9700C7—H7B0.9700
C2—H2C0.9700C7—H7C0.9700
C3—H3A0.9700
N1i—Al1—N187.56 (12)C1—C3—H3B109.5
N1i—Al1—C1122.36 (18)H3A—C3—H3B109.5
N1—Al1—C1119.58 (19)C1—C3—H3C109.5
N1i—Al1—Cl1107.28 (10)H3A—C3—H3C109.5
N1—Al1—Cl1107.48 (10)H3B—C3—H3C109.5
C1—Al1—Cl1110.08 (11)C1—C4—H4A109.5
N1i—Al1—Al1i44.91 (10)C1—C4—H4B109.5
N1—Al1—Al1i44.37 (11)H4A—C4—H4B109.5
C1—Al1—Al1i145.19 (10)C1—C4—H4C109.5
Cl1—Al1—Al1i104.67 (4)H4A—C4—H4C109.5
C5—N1—C6108.9 (3)H4B—C4—H4C109.5
C5—N1—Al1i111.3 (3)N1—C5—H5A109.5
C6—N1—Al1i119.4 (3)N1—C5—H5B109.5
C5—N1—Al1111.2 (3)H5A—C5—H5B109.5
C6—N1—Al1114.3 (3)N1—C5—H5C109.5
Al1i—N1—Al190.71 (11)H5A—C5—H5C109.5
C3—C1—C2107.6 (5)H5B—C5—H5C109.5
C3—C1—C4107.7 (5)C7—C6—N1115.1 (4)
C2—C1—C4108.1 (3)C7—C6—H6A108.5
C3—C1—Al1118.6 (2)N1—C6—H6A108.5
C2—C1—Al1106.7 (3)C7—C6—H6B108.5
C4—C1—Al1107.8 (3)N1—C6—H6B108.5
C1—C2—H2A109.5H6A—C6—H6B107.5
C1—C2—H2B109.5C6—C7—H7A109.5
H2A—C2—H2B109.5C6—C7—H7B109.5
C1—C2—H2C109.5H7A—C7—H7B109.5
H2A—C2—H2C109.5C6—C7—H7C109.5
H2B—C2—H2C109.5H7A—C7—H7C109.5
C1—C3—H3A109.5H7B—C7—H7C109.5
N1i—Al1—N1—C599.2 (3)Cl1—Al1—C1—C3177.8 (5)
C1—Al1—N1—C527.1 (3)Al1i—Al1—C1—C35.6 (8)
Cl1—Al1—N1—C5153.4 (3)N1i—Al1—C1—C2172.1 (3)
Al1i—Al1—N1—C5113.3 (3)N1—Al1—C1—C264.5 (3)
N1i—Al1—N1—C6137.0 (3)Cl1—Al1—C1—C260.6 (4)
C1—Al1—N1—C696.7 (3)Al1i—Al1—C1—C2115.9 (3)
Cl1—Al1—N1—C629.7 (3)N1i—Al1—C1—C472.0 (4)
Al1i—Al1—N1—C6123.0 (3)N1—Al1—C1—C4179.6 (3)
N1i—Al1—N1—Al1i14.05 (14)Cl1—Al1—C1—C455.3 (4)
C1—Al1—N1—Al1i140.34 (16)Al1i—Al1—C1—C4128.2 (4)
Cl1—Al1—N1—Al1i93.31 (10)C5—N1—C6—C763.6 (6)
N1i—Al1—C1—C350.5 (6)Al1i—N1—C6—C765.8 (5)
N1—Al1—C1—C357.1 (6)Al1—N1—C6—C7171.4 (4)
Symmetry code: (i) x+1, y, z.
 

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