Literature DB >> 23476494

catena-Poly[[(tetra-hydro-furan-κO)potas-sium]-di-μ-dimethyl-amido-κ(4) N:N-aluminium-di-μ-dimethyl-amido-κ(4) N:N-potassium-di-μ-dimethyl-amido-κ(4) N:N-aluminium-di-μ-dimethyl-amido-κ(4) N:N].

Andrew Purdy1, Damon Parrish.   

Abstract

The title compound, [Al2K2(C2H6N)8(C4H8O)] n , formed during the sonochemical reaction between Al(NMe2)3 and sodium-potassium alloy in the presence of tetra-hydro-furan (THF). Its asymmetric unit has two inequivalent K(+) sites. One site is coordinated by a THF ligand, and crystallizes as a one-dimensional polymer with a backbone of catenated AlN2K rings. A twofold rotation axis bis-ects one K(+) site and the THF ligand; the second K(+) site is situated on an inversion centre, resulting in a planar four-coordination by N atoms. The latter symmetry operation generates the second half of the THF mol-ecule and fills out the coordination sphere of the potassium sites. The chains extend along the c-axis direction and zigzag at the THF-coordinated K(+) sites by an angle of 106.02 (5)°.

Entities:  

Year:  2013        PMID: 23476494      PMCID: PMC3588537          DOI: 10.1107/S1600536813003553

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


Related literature

Several (RR′N)4AlM (M = Li, Na) compounds that have catenated AlN2 M chains have been reported previously (Eisler & Chivers, 2006 ▶); Rings et al. 2000 ▶). The structure of tris­(dimethyl­amino)­aluminium is a mol­ecular dimer, see: Ouzounis et al. (1983 ▶). Heavily solvated tetra­amino­alanates tend to have separated cations instead of catenated chain structures, see: Hensen et al. (1999 ▶). For details of the synthesis, see: Ruff (1960 ▶); Ouzounis et al. (1983 ▶).

Experimental

Crystal data

[Al2K2(C2H6N)8(C4H8O)] M = 278.44 Monoclinic, a = 13.247 (4) Å b = 12.075 (4) Å c = 20.822 (7) Å β = 90.979 (5)° V = 3330.1 (19) Å3 Z = 8 Mo Kα radiation μ = 0.36 mm−1 T = 173 K 0.74 × 0.57 × 0.42 mm

Data collection

Bruker SMART APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.776, T max = 0.863 18795 measured reflections 4928 independent reflections 3986 reflections with I > 2σ(I) R int = 0.023

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.107 S = 1.03 4928 reflections 155 parameters H-atom parameters constrained Δρmax = 0.25 e Å−3 Δρmin = −0.30 e Å−3 Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL. Click here for additional data file. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813003553/nk2195sup1.cif Click here for additional data file. Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813003553/nk2195Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Al2K2(C2H6N)8(C4H8O)]F(000) = 1216
Mr = 556.88Dx = 1.111 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
a = 13.247 (4) ÅCell parameters from 6485 reflections
b = 12.075 (4) Åθ = 2.3–30.2°
c = 20.822 (7) ŵ = 0.36 mm1
β = 90.979 (5)°T = 173 K
V = 3330.1 (19) Å3Chunk, orange
Z = 40.74 × 0.57 × 0.42 mm
Bruker SMART APEXII CCD diffractometer4928 independent reflections
Radiation source: fine-focus sealed tube3986 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
ω scansθmax = 30.9°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2008)h = −18→18
Tmin = 0.776, Tmax = 0.863k = −15→17
18795 measured reflectionsl = −29→29
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H-atom parameters constrained
S = 1.03w = 1/[σ2(Fo2) + (0.0567P)2 + 0.9926P] where P = (Fo2 + 2Fc2)/3
4928 reflections(Δ/σ)max = 0.001
155 parametersΔρmax = 0.25 e Å3
0 restraintsΔρmin = −0.30 e Å3
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.
xyzUiso*/Ueq
K10.50000.32471 (3)0.75000.03918 (11)
K20.50000.00000.50000.07103 (19)
Al0.52871 (2)0.22259 (3)0.595808 (16)0.02748 (9)
O1S0.50000.54941 (12)0.75000.0520 (3)
N10.50523 (8)0.23469 (9)0.50846 (5)0.0361 (2)
N20.60258 (8)0.34150 (9)0.62545 (5)0.0374 (2)
N30.59582 (7)0.09033 (8)0.61187 (5)0.0338 (2)
N40.40721 (7)0.21492 (9)0.63840 (5)0.0358 (2)
C1S0.57959 (13)0.61739 (15)0.77418 (9)0.0614 (4)
H1SA0.64450.59610.75470.074*
H1SB0.58620.60960.82140.074*
C2S0.55312 (18)0.73207 (19)0.75688 (16)0.1055 (10)
H2SA0.56920.78290.79290.127*
H2SB0.59100.75610.71880.127*
C110.40625 (11)0.24265 (14)0.47861 (7)0.0497 (3)
H11A0.40610.20360.43740.075*
H11B0.38930.32070.47150.075*
H11C0.35620.20900.50670.075*
C120.58075 (12)0.27839 (15)0.46587 (7)0.0543 (4)
H12A0.58370.23230.42720.081*
H12B0.64680.27810.48780.081*
H12C0.56290.35440.45370.081*
C210.59360 (13)0.44990 (12)0.59569 (8)0.0533 (4)
H21A0.65050.46170.56700.080*
H21B0.59420.50710.62910.080*
H21C0.53010.45400.57090.080*
C220.69696 (10)0.33235 (13)0.66072 (8)0.0501 (3)
H22A0.75310.33520.63070.075*
H22B0.69880.26190.68410.075*
H22C0.70300.39370.69130.075*
C310.68988 (10)0.06920 (12)0.57922 (7)0.0474 (3)
H31A0.6982−0.01080.57310.057*
H31B0.74630.09790.60520.057*
H31C0.68850.10610.53730.057*
C320.59875 (13)0.03606 (14)0.67380 (7)0.0561 (4)
H32A0.6057−0.04400.66770.084*
H32B0.53610.05160.69650.084*
H32C0.65640.06390.69910.084*
C410.34632 (11)0.11493 (15)0.63898 (8)0.0555 (4)
H41A0.30360.11230.60010.083*
H41B0.30360.11510.67690.083*
H41C0.39060.05000.64030.083*
C420.34249 (10)0.31184 (15)0.63825 (8)0.0526 (4)
H42A0.29790.31020.60020.079*
H42B0.38410.37890.63730.079*
H42C0.30170.31190.67710.079*
U11U22U33U12U13U23
K10.0424 (2)0.0394 (2)0.03566 (19)0.000−0.00112 (14)0.000
K20.1055 (4)0.0351 (2)0.0709 (3)0.0086 (3)−0.0445 (3)−0.0172 (2)
Al0.02602 (16)0.02410 (17)0.03224 (17)−0.00161 (12)−0.00140 (12)−0.00017 (12)
O1S0.0558 (8)0.0413 (8)0.0586 (9)0.000−0.0084 (7)0.000
N10.0381 (5)0.0367 (6)0.0335 (5)0.0005 (4)−0.0032 (4)0.0051 (4)
N20.0341 (5)0.0293 (5)0.0488 (6)−0.0068 (4)−0.0032 (4)−0.0014 (4)
N30.0348 (5)0.0297 (5)0.0369 (5)0.0023 (4)−0.0034 (4)0.0035 (4)
N40.0268 (4)0.0388 (6)0.0418 (5)−0.0039 (4)0.0001 (4)−0.0010 (4)
C1S0.0516 (8)0.0589 (10)0.0732 (11)−0.0001 (7)−0.0148 (7)−0.0021 (8)
C2S0.0924 (17)0.0547 (13)0.167 (3)−0.0215 (11)−0.0594 (17)0.0213 (14)
C110.0500 (8)0.0513 (8)0.0473 (7)0.0007 (6)−0.0152 (6)0.0074 (6)
C120.0571 (9)0.0629 (10)0.0433 (7)0.0029 (7)0.0091 (6)0.0151 (7)
C210.0656 (9)0.0294 (7)0.0650 (9)−0.0119 (6)0.0007 (7)0.0004 (6)
C220.0353 (6)0.0531 (9)0.0615 (9)−0.0094 (6)−0.0054 (6)−0.0121 (7)
C310.0379 (6)0.0431 (8)0.0611 (8)0.0102 (6)−0.0014 (6)0.0014 (6)
C320.0657 (10)0.0530 (9)0.0494 (8)0.0089 (7)−0.0050 (7)0.0171 (7)
C410.0431 (7)0.0640 (10)0.0593 (9)−0.0239 (7)0.0007 (6)0.0040 (7)
C420.0341 (6)0.0654 (10)0.0581 (9)0.0127 (6)−0.0050 (6)−0.0092 (7)
K1—O1S2.7133 (18)N3—C311.4521 (17)
K1—N4i2.9274 (12)N4—C421.4506 (18)
K1—N42.9275 (12)N4—C411.4522 (18)
K1—N22.9553 (14)C1S—C2S1.472 (3)
K1—N2i2.9553 (14)C1S—H1SA0.9900
K1—C42i3.1026 (16)C1S—H1SB0.9900
K1—C423.1026 (16)C2S—C2Si1.431 (4)
K1—C22i3.2306 (17)C2S—H2SA0.9900
K1—C223.2307 (17)C2S—H2SB0.9900
K1—Ali3.4662 (11)C11—H11A0.9800
K1—Al3.4662 (11)C11—H11B0.9800
K2—N12.8402 (14)C11—H11C0.9800
K2—N1ii2.8402 (14)C12—H12A0.9800
K2—N3ii2.8506 (12)C12—H12B0.9800
K2—N32.8506 (12)C12—H12C0.9800
K2—C31ii3.0990 (16)C21—H21A0.9800
K2—C313.0991 (16)C21—H21B0.9800
K2—C11ii3.2103 (18)C21—H21C0.9800
K2—C113.2103 (18)C22—H22A0.9800
K2—Alii3.3649 (9)C22—H22B0.9800
K2—Al3.3649 (9)C22—H22C0.9800
K2—H31A3.0156C31—H31A0.9807
K2—H31C2.9013C31—H31B0.9791
Al—N21.8383 (11)C31—H31C0.9800
Al—N11.8457 (12)C32—H32A0.9800
Al—N41.8533 (11)C32—H32B0.9800
Al—N31.8554 (11)C32—H32C0.9800
O1S—C1S1.4215 (19)C41—H41A0.9800
O1S—C1Si1.4215 (19)C41—H41B0.9800
N1—C111.4446 (17)C41—H41C0.9800
N1—C121.4478 (17)C42—H42A0.9800
N2—C221.4433 (17)C42—H42B0.9800
N2—C211.4522 (18)C42—H42C0.9800
N3—C321.4464 (17)
O1S—K1—N4i116.93 (2)H31A—K2—H31C31.3
O1S—K1—N4116.93 (2)N2—Al—N1110.41 (5)
N4i—K1—N4126.15 (5)N2—Al—N4109.88 (5)
O1S—K1—N286.06 (2)N1—Al—N4110.02 (5)
N4i—K1—N2122.31 (3)N2—Al—N3111.17 (5)
N4—K1—N261.81 (3)N1—Al—N3108.54 (5)
O1S—K1—N2i86.07 (2)N4—Al—N3106.74 (5)
N4i—K1—N2i61.81 (3)N2—Al—K2151.29 (4)
N4—K1—N2i122.31 (3)N1—Al—K257.56 (4)
N2—K1—N2i172.13 (4)N4—Al—K298.83 (4)
O1S—K1—C42i92.87 (3)N3—Al—K257.88 (4)
N4i—K1—C42i27.65 (4)N2—Al—K158.49 (4)
N4—K1—C42i147.19 (4)N1—Al—K1149.91 (4)
N2—K1—C42i110.37 (4)N4—Al—K157.63 (3)
N2i—K1—C42i70.05 (4)N3—Al—K1101.48 (4)
O1S—K1—C4292.87 (3)K2—Al—K1145.105 (13)
N4i—K1—C42147.19 (4)C1S—O1S—C1Si109.46 (18)
N4—K1—C4227.64 (4)C1S—O1S—K1125.27 (9)
N2—K1—C4270.05 (4)C1Si—O1S—K1125.27 (9)
N2i—K1—C42110.37 (4)C11—N1—C12110.11 (11)
C42i—K1—C42174.26 (7)C11—N1—Al124.45 (9)
O1S—K1—C22i88.36 (3)C12—N1—Al121.72 (9)
N4i—K1—C22i83.60 (4)C11—N1—K291.07 (8)
N4—K1—C22i97.90 (4)C12—N1—K2110.00 (9)
N2—K1—C22i152.99 (3)Al—N1—K289.18 (4)
N2i—K1—C22i26.51 (3)C22—N2—C21110.49 (11)
C42i—K1—C22i96.27 (4)C22—N2—Al124.23 (9)
C42—K1—C22i83.89 (5)C21—N2—Al121.43 (9)
O1S—K1—C2288.36 (3)C22—N2—K187.45 (8)
N4i—K1—C2297.90 (4)C21—N2—K1113.62 (9)
N4—K1—C2283.60 (4)Al—N2—K189.48 (4)
N2—K1—C2226.51 (3)C32—N3—C31109.13 (11)
N2i—K1—C22153.00 (3)C32—N3—Al123.79 (10)
C42i—K1—C2283.89 (5)C31—N3—Al118.63 (9)
C42—K1—C2296.27 (5)C32—N3—K2124.05 (9)
C22i—K1—C22176.73 (6)C31—N3—K285.63 (8)
O1S—K1—Ali110.839 (12)Al—N3—K288.67 (4)
N4i—K1—Ali32.32 (2)C42—N4—C41110.02 (12)
N4—K1—Ali121.53 (3)C42—N4—Al118.47 (10)
N2—K1—Ali153.72 (2)C41—N4—Al122.18 (10)
N2i—K1—Ali32.03 (2)C42—N4—K182.91 (8)
C42i—K1—Ali50.99 (3)C41—N4—K1126.56 (9)
C42—K1—Ali126.43 (4)Al—N4—K190.05 (4)
C22i—K1—Ali51.29 (3)O1S—C1S—C2S106.52 (14)
C22—K1—Ali130.21 (3)O1S—C1S—H1SA110.4
O1S—K1—Al110.838 (12)C2S—C1S—H1SA110.4
N4i—K1—Al121.53 (3)O1S—C1S—H1SB110.4
N4—K1—Al32.32 (2)C2S—C1S—H1SB110.4
N2—K1—Al32.03 (2)H1SA—C1S—H1SB108.6
N2i—K1—Al153.72 (3)C2Si—C2S—C1S106.16 (14)
C42i—K1—Al126.43 (4)C2Si—C2S—H2SA110.5
C42—K1—Al50.99 (3)C1S—C2S—H2SA110.5
C22i—K1—Al130.21 (3)C2Si—C2S—H2SB110.5
C22—K1—Al51.29 (3)C1S—C2S—H2SB110.5
Ali—K1—Al138.32 (2)H2SA—C2S—H2SB108.7
N1—K2—N1ii180.0N1—C11—K262.19 (7)
N1—K2—N3ii116.27 (3)N1—C11—H11A109.5
N1ii—K2—N3ii63.73 (3)K2—C11—H11A71.2
N1—K2—N363.73 (3)N1—C11—H11B109.5
N1ii—K2—N3116.26 (3)K2—C11—H11B170.5
N3ii—K2—N3179.999 (1)H11A—C11—H11B109.5
N1—K2—C31ii108.71 (3)N1—C11—H11C109.5
N1ii—K2—C31ii71.29 (3)K2—C11—H11C78.6
N3ii—K2—C31ii27.85 (3)H11A—C11—H11C109.5
N3—K2—C31ii152.15 (3)H11B—C11—H11C109.5
N1—K2—C3171.29 (3)N1—C12—H12A109.5
N1ii—K2—C31108.71 (3)N1—C12—H12B109.5
N3ii—K2—C31152.15 (3)H12A—C12—H12B109.5
N3—K2—C3127.85 (3)N1—C12—H12C109.5
C31ii—K2—C31180.0H12A—C12—H12C109.5
N1—K2—C11ii153.26 (3)H12B—C12—H12C109.5
N1ii—K2—C11ii26.74 (3)N2—C21—H21A109.5
N3ii—K2—C11ii85.98 (4)N2—C21—H21B109.5
N3—K2—C11ii94.02 (4)H21A—C21—H21B109.5
C31ii—K2—C11ii97.83 (4)N2—C21—H21C109.5
C31—K2—C11ii82.17 (4)H21A—C21—H21C109.5
N1—K2—C1126.74 (3)H21B—C21—H21C109.5
N1ii—K2—C11153.26 (3)N2—C22—K166.04 (7)
N3ii—K2—C1194.02 (4)N2—C22—H22A109.5
N3—K2—C1185.98 (4)K1—C22—H22A175.5
C31ii—K2—C1182.17 (4)N2—C22—H22B109.5
C31—K2—C1197.83 (4)K1—C22—H22B72.8
C11ii—K2—C11180.0H22A—C22—H22B109.5
N1—K2—Alii146.74 (2)N2—C22—H22C109.5
N1ii—K2—Alii33.26 (2)K1—C22—H22C72.9
N3ii—K2—Alii33.45 (2)H22A—C22—H22C109.5
N3—K2—Alii146.55 (2)H22B—C22—H22C109.5
C31ii—K2—Alii52.16 (3)N3—C31—K266.52 (7)
C31—K2—Alii127.84 (3)N3—C31—H31A109.5
C11ii—K2—Alii52.61 (3)K2—C31—H31A76.0
C11—K2—Alii127.39 (3)N3—C31—H31B109.4
N1—K2—Al33.26 (2)K2—C31—H31B174.3
N1ii—K2—Al146.74 (2)H31A—C31—H31B109.5
N3ii—K2—Al146.55 (2)N3—C31—H31C109.5
N3—K2—Al33.45 (2)K2—C31—H31C69.3
C31ii—K2—Al127.84 (3)H31A—C31—H31C109.4
C31—K2—Al52.16 (3)H31B—C31—H31C109.4
C11ii—K2—Al127.39 (3)N3—C32—H32A109.5
C11—K2—Al52.61 (3)N3—C32—H32B109.5
Alii—K2—Al180.0H32A—C32—H32B109.5
N1—K2—H31A89.5N3—C32—H32C109.5
N1ii—K2—H31A90.5H32A—C32—H32C109.5
N3ii—K2—H31A140.2H32B—C32—H32C109.5
N3—K2—H31A39.8N4—C41—H41A109.5
C31ii—K2—H31A161.6N4—C41—H41B109.5
C31—K2—H31A18.4H41A—C41—H41B109.5
C11ii—K2—H31A63.8N4—C41—H41C109.5
C11—K2—H31A116.2H41A—C41—H41C109.5
Alii—K2—H31A110.7H41B—C41—H41C109.5
Al—K2—H31A69.3N4—C42—K169.45 (7)
N1—K2—H31C61.5N4—C42—H42A109.5
N1ii—K2—H31C118.5K1—C42—H42A174.5
N3ii—K2—H31C139.2N4—C42—H42B109.5
N3—K2—H31C40.8K1—C42—H42B66.5
C31ii—K2—H31C161.6H42A—C42—H42B109.5
C31—K2—H31C18.4N4—C42—H42C109.5
C11ii—K2—H31C92.1K1—C42—H42C75.8
C11—K2—H31C87.9H42A—C42—H42C109.5
Alii—K2—H31C126.8H42B—C42—H42C109.5
Al—K2—H31C53.2
N1—K2—Al—N2−72.54 (9)K1—Al—N2—C21−117.65 (12)
N1ii—K2—Al—N2107.46 (9)N1—Al—N2—K1148.73 (4)
N3ii—K2—Al—N2−104.99 (9)N4—Al—N2—K127.20 (5)
N3—K2—Al—N275.01 (9)N3—Al—N2—K1−90.74 (5)
C31ii—K2—Al—N2−136.20 (9)K2—Al—N2—K1−152.06 (5)
C31—K2—Al—N243.80 (9)O1S—K1—N2—C2294.23 (7)
C11ii—K2—Al—N279.62 (9)N4i—K1—N2—C22−25.34 (9)
C11—K2—Al—N2−100.37 (9)N4—K1—N2—C22−142.28 (9)
Alii—K2—Al—N2−90.4 (6)N2i—K1—N2—C2294.24 (8)
N1ii—K2—Al—N1180.0C42i—K1—N2—C222.63 (9)
N3ii—K2—Al—N1−32.45 (6)C42—K1—N2—C22−171.27 (9)
N3—K2—Al—N1147.55 (6)C22i—K1—N2—C22172.81 (13)
C31ii—K2—Al—N1−63.66 (5)Ali—K1—N2—C22−37.53 (10)
C31—K2—Al—N1116.34 (5)Al—K1—N2—C22−124.29 (9)
C11ii—K2—Al—N1152.16 (5)O1S—K1—N2—C21−17.06 (9)
C11—K2—Al—N1−27.84 (5)N4i—K1—N2—C21−136.63 (9)
Alii—K2—Al—N1−17.8 (6)N4—K1—N2—C21106.44 (9)
N1—K2—Al—N4108.17 (5)N2i—K1—N2—C21−17.05 (9)
N1ii—K2—Al—N4−71.83 (5)C42i—K1—N2—C21−108.66 (9)
N3ii—K2—Al—N475.72 (5)C42—K1—N2—C2177.44 (9)
N3—K2—Al—N4−104.28 (5)C22i—K1—N2—C2161.52 (13)
C31ii—K2—Al—N444.51 (5)C22—K1—N2—C21−111.29 (12)
C31—K2—Al—N4−135.49 (5)Ali—K1—N2—C21−148.81 (8)
C11ii—K2—Al—N4−99.67 (5)Al—K1—N2—C21124.42 (10)
C11—K2—Al—N480.33 (5)O1S—K1—N2—Al−141.47 (4)
Alii—K2—Al—N490.3 (6)N4i—K1—N2—Al98.95 (5)
N1—K2—Al—N3−147.55 (6)N4—K1—N2—Al−17.98 (3)
N1ii—K2—Al—N332.45 (6)N2i—K1—N2—Al−141.47 (4)
N3ii—K2—Al—N3179.998 (1)C42i—K1—N2—Al126.92 (5)
C31ii—K2—Al—N3148.79 (5)C42—K1—N2—Al−46.98 (5)
C31—K2—Al—N3−31.21 (5)C22i—K1—N2—Al−62.89 (10)
C11ii—K2—Al—N34.61 (5)C22—K1—N2—Al124.29 (9)
C11—K2—Al—N3−175.39 (5)Ali—K1—N2—Al86.77 (6)
Alii—K2—Al—N3−165.4 (5)N2—Al—N3—C3278.67 (12)
N1—K2—Al—K1151.74 (5)N1—Al—N3—C32−159.71 (11)
N1ii—K2—Al—K1−28.26 (5)N4—Al—N3—C32−41.15 (12)
N3ii—K2—Al—K1119.29 (4)K2—Al—N3—C32−131.18 (12)
N3—K2—Al—K1−60.71 (4)K1—Al—N3—C3218.22 (11)
C31ii—K2—Al—K188.08 (4)N2—Al—N3—C31−65.87 (11)
C31—K2—Al—K1−91.92 (4)N1—Al—N3—C3155.76 (10)
C11ii—K2—Al—K1−56.10 (4)N4—Al—N3—C31174.31 (9)
C11—K2—Al—K1123.91 (4)K2—Al—N3—C3184.29 (10)
Alii—K2—Al—K1133.9 (5)K1—Al—N3—C31−126.31 (9)
O1S—K1—Al—N241.68 (4)N2—Al—N3—K2−150.16 (4)
N4i—K1—Al—N2−101.64 (5)N1—Al—N3—K2−28.53 (5)
N4—K1—Al—N2149.41 (6)N4—Al—N3—K290.02 (5)
N2i—K1—Al—N2168.89 (6)K1—Al—N3—K2149.395 (19)
C42i—K1—Al—N2−68.66 (6)N1—K2—N3—C32150.13 (11)
C42—K1—Al—N2117.83 (6)N1ii—K2—N3—C32−29.87 (11)
C22i—K1—Al—N2148.04 (6)N3ii—K2—N3—C3210 (12)
C22—K1—Al—N2−28.19 (5)C31ii—K2—N3—C3269.82 (13)
Ali—K1—Al—N2−138.33 (4)C31—K2—N3—C32−110.18 (13)
O1S—K1—Al—N1−34.33 (7)C11ii—K2—N3—C32−45.36 (11)
N4i—K1—Al—N1−177.64 (7)C11—K2—N3—C32134.65 (11)
N4—K1—Al—N173.41 (8)Alii—K2—N3—C32−49.03 (12)
N2—K1—Al—N1−76.00 (8)Al—K2—N3—C32130.97 (12)
N2i—K1—Al—N192.89 (9)N1—K2—N3—C31−99.69 (8)
C42i—K1—Al—N1−144.66 (8)N1ii—K2—N3—C3180.31 (8)
C42—K1—Al—N141.82 (8)N3ii—K2—N3—C31121 (12)
C22i—K1—Al—N172.04 (8)C31ii—K2—N3—C31180.0
C22—K1—Al—N1−104.20 (8)C11ii—K2—N3—C3164.83 (8)
Ali—K1—Al—N1145.67 (7)C11—K2—N3—C31−115.17 (8)
O1S—K1—Al—N4−107.73 (4)Alii—K2—N3—C3161.15 (8)
N4i—K1—Al—N4108.95 (6)Al—K2—N3—C31−118.84 (8)
N2—K1—Al—N4−149.41 (6)N1—K2—N3—Al19.16 (3)
N2i—K1—Al—N419.48 (7)N1ii—K2—N3—Al−160.84 (3)
C42i—K1—Al—N4141.93 (6)N3ii—K2—N3—Al−121 (12)
C42—K1—Al—N4−31.58 (6)C31ii—K2—N3—Al−61.15 (8)
C22i—K1—Al—N4−1.37 (6)C31—K2—N3—Al118.84 (8)
C22—K1—Al—N4−177.60 (6)C11ii—K2—N3—Al−176.33 (4)
Ali—K1—Al—N472.26 (4)C11—K2—N3—Al3.67 (4)
O1S—K1—Al—N3149.60 (3)Alii—K2—N3—Al180.0
N4i—K1—Al—N36.28 (4)N2—Al—N4—C4254.48 (11)
N4—K1—Al—N3−102.67 (5)N1—Al—N4—C42−67.29 (11)
N2—K1—Al—N3107.92 (6)N3—Al—N4—C42175.13 (9)
N2i—K1—Al—N3−83.18 (6)K2—Al—N4—C42−125.88 (9)
C42i—K1—Al—N339.26 (5)K1—Al—N4—C4281.96 (10)
C42—K1—Al—N3−134.25 (6)N2—Al—N4—C41−162.25 (10)
C22i—K1—Al—N3−104.04 (5)N1—Al—N4—C4175.98 (12)
C22—K1—Al—N379.73 (5)N3—Al—N4—C41−41.60 (12)
Ali—K1—Al—N3−30.40 (3)K2—Al—N4—C4117.39 (11)
O1S—K1—Al—K2−161.489 (17)K1—Al—N4—C41−134.78 (12)
N4i—K1—Al—K255.20 (4)N2—Al—N4—K1−27.47 (5)
N4—K1—Al—K2−53.75 (4)N1—Al—N4—K1−149.24 (4)
N2—K1—Al—K2156.84 (5)N3—Al—N4—K193.17 (5)
N2i—K1—Al—K2−34.27 (6)K2—Al—N4—K1152.17 (2)
C42i—K1—Al—K288.18 (4)O1S—K1—N4—C42−31.94 (8)
C42—K1—Al—K2−85.34 (5)N4i—K1—N4—C42148.06 (8)
C22i—K1—Al—K2−55.12 (4)N2—K1—N4—C42−100.87 (9)
C22—K1—Al—K2128.64 (4)N2i—K1—N4—C4271.36 (9)
Ali—K1—Al—K218.510 (17)C42i—K1—N4—C42175.00 (6)
N4i—K1—O1S—C1S37.19 (10)C22i—K1—N4—C4260.24 (8)
N4—K1—O1S—C1S−142.81 (10)C22—K1—N4—C42−116.82 (9)
N2—K1—O1S—C1S−87.28 (10)Ali—K1—N4—C42109.28 (8)
N2i—K1—O1S—C1S92.72 (10)Al—K1—N4—C42−118.70 (10)
C42i—K1—O1S—C1S22.96 (10)O1S—K1—N4—C41−141.66 (11)
C42—K1—O1S—C1S−157.04 (10)N4i—K1—N4—C4138.34 (11)
C22i—K1—O1S—C1S119.16 (10)N2—K1—N4—C41149.41 (12)
C22—K1—O1S—C1S−60.84 (10)N2i—K1—N4—C41−38.35 (12)
Ali—K1—O1S—C1S72.02 (10)C42i—K1—N4—C4165.28 (13)
Al—K1—O1S—C1S−107.98 (10)C42—K1—N4—C41−109.71 (14)
N4i—K1—O1S—C1Si−142.81 (10)C22i—K1—N4—C41−49.47 (12)
N4—K1—O1S—C1Si37.19 (10)C22—K1—N4—C41133.46 (12)
N2—K1—O1S—C1Si92.72 (10)Ali—K1—N4—C41−0.43 (12)
N2i—K1—O1S—C1Si−87.28 (10)Al—K1—N4—C41131.58 (13)
C42i—K1—O1S—C1Si−157.04 (10)O1S—K1—N4—Al86.76 (4)
C42—K1—O1S—C1Si22.96 (10)N4i—K1—N4—Al−93.24 (4)
C22i—K1—O1S—C1Si−60.84 (10)N2—K1—N4—Al17.83 (3)
C22—K1—O1S—C1Si119.16 (10)N2i—K1—N4—Al−169.94 (4)
Ali—K1—O1S—C1Si−107.98 (10)C42i—K1—N4—Al−66.30 (8)
Al—K1—O1S—C1Si72.02 (10)C42—K1—N4—Al118.70 (9)
N2—Al—N1—C11−118.54 (11)C22i—K1—N4—Al178.95 (4)
N4—Al—N1—C112.91 (13)C22—K1—N4—Al1.88 (5)
N3—Al—N1—C11119.37 (11)Ali—K1—N4—Al−132.01 (3)
K2—Al—N1—C1190.73 (11)C1Si—O1S—C1S—C2S−7.13 (16)
K1—Al—N1—C11−56.57 (15)K1—O1S—C1S—C2S172.87 (16)
N2—Al—N1—C1237.57 (12)O1S—C1S—C2S—C2Si19.0 (4)
N4—Al—N1—C12159.02 (11)C12—N1—C11—K2111.78 (11)
N3—Al—N1—C12−84.52 (12)Al—N1—C11—K2−89.74 (9)
K2—Al—N1—C12−113.16 (12)N1ii—K2—C11—N1180.0
K1—Al—N1—C1299.54 (12)N3ii—K2—C11—N1−147.85 (8)
N2—Al—N1—K2150.73 (4)N3—K2—C11—N132.15 (8)
N4—Al—N1—K2−87.82 (5)C31ii—K2—C11—N1−173.11 (8)
N3—Al—N1—K228.64 (5)C31—K2—C11—N16.88 (8)
K1—Al—N1—K2−147.30 (5)C11ii—K2—C11—N1−88 (10)
N1ii—K2—N1—C11−116 (15)Alii—K2—C11—N1−145.30 (6)
N3ii—K2—N1—C1136.29 (8)Al—K2—C11—N134.70 (6)
N3—K2—N1—C11−143.71 (8)C21—N2—C22—K1114.31 (10)
C31ii—K2—N1—C117.20 (9)Al—N2—C22—K1−87.64 (9)
C31—K2—N1—C11−172.80 (9)O1S—K1—C22—N2−84.46 (7)
C11ii—K2—N1—C11180.0N4i—K1—C22—N2158.58 (7)
Alii—K2—N1—C1155.55 (9)N4—K1—C22—N232.87 (7)
Al—K2—N1—C11−124.45 (9)N2i—K1—C22—N2−162.50 (10)
N1ii—K2—N1—C12132 (15)C42i—K1—C22—N2−177.52 (8)
N3ii—K2—N1—C12−75.59 (9)C42—K1—C22—N28.25 (8)
N3—K2—N1—C12104.41 (9)C22i—K1—C22—N2−84.45 (7)
C31ii—K2—N1—C12−104.68 (9)Ali—K1—C22—N2159.32 (6)
C31—K2—N1—C1275.32 (9)Al—K1—C22—N234.16 (6)
C11ii—K2—N1—C1268.11 (12)C32—N3—C31—K2124.60 (11)
C11—K2—N1—C12−111.88 (12)Al—N3—C31—K2−86.09 (7)
Alii—K2—N1—C12−56.33 (10)N1—K2—C31—N368.95 (7)
Al—K2—N1—C12123.67 (10)N1ii—K2—C31—N3−111.05 (7)
N1ii—K2—N1—Al8 (15)N3ii—K2—C31—N3180.0
N3ii—K2—N1—Al160.74 (3)C31ii—K2—C31—N3167 (13)
N3—K2—N1—Al−19.26 (3)C11ii—K2—C31—N3−114.31 (8)
C31ii—K2—N1—Al131.65 (4)C11—K2—C31—N365.69 (8)
C31—K2—N1—Al−48.35 (4)Alii—K2—C31—N3−142.31 (6)
C11ii—K2—N1—Al−55.56 (9)Al—K2—C31—N337.69 (6)
C11—K2—N1—Al124.45 (9)C41—N4—C42—K1126.41 (10)
Alii—K2—N1—Al180.0Al—N4—C42—K1−86.19 (7)
N1—Al—N2—C22−124.71 (11)O1S—K1—C42—N4151.82 (7)
N4—Al—N2—C22113.76 (11)N4i—K1—C42—N4−52.04 (12)
N3—Al—N2—C22−4.18 (12)N2—K1—C42—N467.05 (7)
K2—Al—N2—C22−65.50 (15)N2i—K1—C42—N4−121.32 (7)
K1—Al—N2—C2286.56 (11)C42i—K1—C42—N4−28.18 (8)
N1—Al—N2—C2131.07 (12)C22i—K1—C42—N4−120.14 (8)
N4—Al—N2—C21−90.46 (12)C22—K1—C42—N463.15 (8)
N3—Al—N2—C21151.60 (10)Ali—K1—C42—N4−89.52 (8)
K2—Al—N2—C2190.28 (13)Al—K1—C42—N437.12 (6)
  2 in total

1.  A short history of SHELX.

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

2.  Synthesis and Structural Characterization of (1,4-Dihydropyrid-1-yl)aluminum Complexes.

Authors:  Karl Hensen; Alexander Lemke; Thorsten Stumpf; Michael Bolte; Holger Fleischer; Colin R. Pulham; Robert O. Gould; Steven Harris
Journal:  Inorg Chem       Date:  1999-10-18       Impact factor: 5.165

  2 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.