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) |
Atom | x | y | z | U(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) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O1 | C1 | 1.41(3) | N1 | C8 | 1.38(4) | |
O1 | Li11 | 1.94(4) | N1 | C4 | 1.17(4) | |
O1 | Li1 | 1.84(3) | N1 | Li12 | 2.26(4) | |
O1 | Li12 | 1.90(3) | C1 | C4 | 1.67(4) | |
O2 | C7 | 1.42(3) | C1 | Li12 | 2.63(4) | |
O2 | C6 | 1.45(4) | C1 | C2 | 1.49(4) | |
C3 | C1 | 1.45(3) | C4 | Li12 | 2.76(5) | |
C5 | N1 | 1.61(3) | Li1 | Li11 | 2.47(6) | |
C5 | C6 | 1.59(4) | Li1 | Li13 | 2.47(6) | |
C5 | Li12 | 2.25(4) | Li1 | Li12 | 2.39(6) | |
C7 | C8 | 1.31(4) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C1 | O1 | Li1 | 156.5(17) | N1 | C4 | Li11 | 53.3(19) | |
C1 | O1 | Li11 | 103.8(15) | C1 | C4 | Li11 | 67.7(15) | |
C1 | O1 | Li12 | 122.2(16) | O1 | Li1 | O11 | 100.2(14) | |
Li1 | O1 | Li12 | 81.2(15) | O1 | Li1 | O13 | 99.6(16) | |
Li11 | O1 | Li12 | 79.7(15) | O11 | Li1 | O13 | 97.6(15) | |
Li1 | O1 | Li11 | 79.2(14) | O1 | Li1 | N11 | 123.5(18) | |
C7 | O2 | C6 | 114(2) | O11 | Li1 | N11 | 86.4(14) | |
N1 | C5 | Li11 | 69.5(15) | O13 | Li1 | N11 | 135.4(17) | |
C6 | C5 | N1 | 107.7(18) | O1 | Li1 | C11 | 125.9(16) | |
C6 | C5 | Li11 | 123(2) | O11 | Li1 | C11 | 31.5(8) | |
C8 | C7 | O2 | 104(2) | O13 | Li1 | C11 | 107.3(15) | |
C5 | N1 | Li11 | 68.5(15) | O1 | Li1 | Li12 | 51.2(9) | |
C8 | N1 | C5 | 108(2) | O1 | Li1 | Li13 | 97.4(12) | |
C8 | N1 | Li11 | 160(2) | O11 | Li1 | Li11 | 49.3(12) | |
C4 | N1 | C5 | 140(3) | O13 | Li1 | Li13 | 47.6(14) | |
C4 | N1 | C8 | 92(3) | O1 | Li1 | Li11 | 51.5(12) | |
C4 | N1 | Li11 | 102(2) | O11 | Li1 | Li13 | 50.9(9) | |
O2 | C6 | C5 | 110(2) | O13 | Li1 | Li12 | 49.4(14) | |
O1 | C1 | C3 | 113.3(19) | O13 | Li1 | Li11 | 97.2(9) | |
O1 | C1 | C4 | 108.9(19) | O11 | Li1 | Li12 | 95.7(12) | |
O1 | C1 | Li11 | 44.7(10) | N11 | Li1 | C11 | 58.1(10) | |
O1 | C1 | C2 | 113(2) | N11 | Li1 | Li11 | 117.5(13) | |
C3 | C1 | C4 | 108(2) | N11 | Li1 | Li13 | 126.7(18) | |
C3 | C1 | Li11 | 155.0(18) | N11 | Li1 | Li12 | 175(2) | |
C3 | C1 | C2 | 108(2) | Li12 | Li1 | C11 | 125.2(14) | |
C4 | C1 | Li11 | 76.3(16) | Li11 | Li1 | C11 | 78.9(15) | |
C2 | C1 | C4 | 106(2) | Li13 | Li1 | C11 | 70.8(12) | |
C2 | C1 | Li11 | 94.4(19) | Li11 | Li1 | Li13 | 61.1(7) | |
C7 | C8 | N1 | 130(3) | Li12 | Li1 | Li13 | 57.9(15) | |
N1 | C4 | C1 | 114(3) | Li11 | Li1 | Li12 | 61.1(7) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H3A | -8227.59 | -2738.66 | -4230.83 | 20 |
H3B | -7680.83 | -1518.81 | -3762.12 | 20 |
H3C | -7701.61 | -3042.23 | -3470.83 | 20 |
H5A | -2856.64 | -4435.88 | -3193.46 | 14 |
H5B | -2865.43 | -4490.54 | -4015.16 | 14 |
H7A | -1980.46 | -1270.55 | -2716.12 | 24 |
H7B | -2471.96 | -66.41 | -3219.69 | 24 |
H6A | -861.15 | -3269.62 | -3202.47 | 71 |
H6B | -812.26 | -3428.13 | -4019.14 | 71 |
H8A | -4215.01 | -912.48 | -3358.8 | 49 |
H8B | -3841.39 | -1919.94 | -2757.92 | 49 |
H4A | -5239.22 | -1725.59 | -3250.18 | 48 |
H4B | -5372.59 | -3334.77 | -3146.18 | 48 |
H2A | -4907.43 | -1252.69 | -4514.02 | 64 |
H2B | -6456.06 | -748.83 | -4477.32 | 64 |
H2C | -5987.54 | -1775.36 | -5068.36 | 64 |
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.
Crystal structure determination of [I-4]
Crystal Data for C32H64Li4N4O8 (M =660.63 g/mol): tetragonal, space group I-4 (no. 82), a = 9.8170(10) Å, c = 19.541(4) Å, V = 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)
This report has been created with Olex2, compiled on 2018.04.18 svn.r3501 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.