I-4

Table 1 Crystal data and structure refinement for I-4.
Identification code I-4
Empirical formula C32H64Li4N4O8
Formula weight 660.63
Temperature/K 100.01
Crystal system tetragonal
Space group I-4
a/Å 9.8170(10)
b/Å 9.8170(10)
c/Å 19.541(4)
α/° 90
β/° 90
γ/° 90
Volume/Å3 1883.3(5)
Z 2
ρcalcg/cm3 1.165
μ/mm‑1 0.080
F(000) 720.0
Crystal size/mm3 ? × ? × ?
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.644 to 54.226
Index ranges -12 ≤ h ≤ 12, -12 ≤ k ≤ 12, -20 ≤ l ≤ 24
Reflections collected 7458
Independent reflections 2072 [Rint = 0.3131, Rsigma = 0.2428]
Data/restraints/parameters 2072/0/51
Goodness-of-fit on F2 2.155
Final R indexes [I>=2σ (I)] R1 = 0.3023, wR2 = 0.6100
Final R indexes [all data] R1 = 0.3681, wR2 = 0.6523
Largest diff. peak/hole / e Å-3 2.53/-1.03
Flack parameter-4.1(10)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for I-4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O1-6035(13)-3966(13)-4473(7)-1(3)
O2-1610(17)-1641(17)-3706(10)26(4)
C3-7560(20)-2480(30)-3880(13)14(5)
C5-2787(19)-3880(20)-3614(12)11(4)
C7-2390(20)-1070(20)-3167(13)20(5)
N1-3980(20)-2750(20)-3630(13)27(5)
C6-1370(40)-3090(40)-3630(20)59(9)
C1-6200(20)-2700(20)-4140(13)18(5)
C8-3590(30)-1660(30)-3230(19)41(8)
C4-5130(40)-2620(40)-3480(18)40(9)
Li1-5890(30)-5830(30)-4540(17)-1(6)
C2-5860(30)-1520(40)-4590(20)43(9)

 

Table 3 Bond Lengths for I-4.
AtomAtomLength/Å AtomAtomLength/Å
O1C11.41(3) N1C81.38(4)
O1Li111.94(4) N1C41.17(4)
O1Li11.84(3) N1Li122.26(4)
O1Li121.90(3) C1C41.67(4)
O2C71.42(3) C1Li122.63(4)
O2C61.45(4) C1C21.49(4)
C3C11.45(3) C4Li122.76(5)
C5N11.61(3) Li1Li112.47(6)
C5C61.59(4) Li1Li132.47(6)
C5Li122.25(4) Li1Li122.39(6)
C7C81.31(4)    

1+Y,-1-X,-1-Z; 2-1-X,-1-Y,+Z; 3-1-Y,+X,-1-Z

 

Table 4 Bond Angles for I-4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1O1Li1156.5(17) N1C4Li1153.3(19)
C1O1Li11103.8(15) C1C4Li1167.7(15)
C1O1Li12122.2(16) O1Li1O11100.2(14)
Li1O1Li1281.2(15) O1Li1O1399.6(16)
Li11O1Li1279.7(15) O11Li1O1397.6(15)
Li1O1Li1179.2(14) O1Li1N11123.5(18)
C7O2C6114(2) O11Li1N1186.4(14)
N1C5Li1169.5(15) O13Li1N11135.4(17)
C6C5N1107.7(18) O1Li1C11125.9(16)
C6C5Li11123(2) O11Li1C1131.5(8)
C8C7O2104(2) O13Li1C11107.3(15)
C5N1Li1168.5(15) O1Li1Li1251.2(9)
C8N1C5108(2) O1Li1Li1397.4(12)
C8N1Li11160(2) O11Li1Li1149.3(12)
C4N1C5140(3) O13Li1Li1347.6(14)
C4N1C892(3) O1Li1Li1151.5(12)
C4N1Li11102(2) O11Li1Li1350.9(9)
O2C6C5110(2) O13Li1Li1249.4(14)
O1C1C3113.3(19) O13Li1Li1197.2(9)
O1C1C4108.9(19) O11Li1Li1295.7(12)
O1C1Li1144.7(10) N11Li1C1158.1(10)
O1C1C2113(2) N11Li1Li11117.5(13)
C3C1C4108(2) N11Li1Li13126.7(18)
C3C1Li11155.0(18) N11Li1Li12175(2)
C3C1C2108(2) Li12Li1C11125.2(14)
C4C1Li1176.3(16) Li11Li1C1178.9(15)
C2C1C4106(2) Li13Li1C1170.8(12)
C2C1Li1194.4(19) Li11Li1Li1361.1(7)
C7C8N1130(3) Li12Li1Li1357.9(15)
N1C4C1114(3) Li11Li1Li1261.1(7)

1-1-X,-1-Y,+Z; 2+Y,-1-X,-1-Z; 3-1-Y,+X,-1-Z

 

Table 5 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for I-4.
AtomxyzU(eq)
H3A-8227.59-2738.66-4230.8320
H3B-7680.83-1518.81-3762.1220
H3C-7701.61-3042.23-3470.8320
H5A-2856.64-4435.88-3193.4614
H5B-2865.43-4490.54-4015.1614
H7A-1980.46-1270.55-2716.1224
H7B-2471.96-66.41-3219.6924
H6A-861.15-3269.62-3202.4771
H6B-812.26-3428.13-4019.1471
H8A-4215.01-912.48-3358.849
H8B-3841.39-1919.94-2757.9249
H4A-5239.22-1725.59-3250.1848
H4B-5372.59-3334.77-3146.1848
H2A-4907.43-1252.69-4514.0264
H2B-6456.06-748.83-4477.3264
H2C-5987.54-1775.36-5068.3664

Experimental

Single crystals of C32H64Li4N4O8 [I-4] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 100.01 K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program using Intrinsic Phasing and refined with the XL [3] refinement package using Least Squares minimisation.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
  2. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [I-4]

Crystal Data for C32H64Li4N4O8 (=660.63 g/mol): tetragonal, space group I-4 (no. 82), a = 9.8170(10) Å, c = 19.541(4) Å, = 1883.3(5) Å3, Z = 2, T = 100.01 K, μ(MoKα) = 0.080 mm-1, Dcalc = 1.165 g/cm3, 7458 reflections measured (4.644° ≤ 2Θ ≤ 54.226°), 2072 unique (Rint = 0.3131, Rsigma = 0.2428) which were used in all calculations. The final R1 was 0.3023 (I > 2σ(I)) and wR2 was 0.6523 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C8(H8A,H8B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)

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