mo_B1032_0m

Table 1 Crystal data and structure refinement for mo_B1032_0m.
Identification code mo_B1032_0m
Empirical formula C28H68Li4O3Si4
Formula weight 592.94
Temperature/K 100.01
Crystal system monoclinic
Space group P21/c
a/Å 9.8606(18)
b/Å 19.160(2)
c/Å 20.638(3)
α/° 90
β/° 91.536(6)
γ/° 90
Volume/Å3 3897.8(10)
Z 4
ρcalcg/cm3 1.010
μ/mm‑1 0.176
F(000) 1312.0
Crystal size/mm3 0.34 × 0.25 × 0.15
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.484 to 54
Index ranges -12 ≤ h ≤ 12, -24 ≤ k ≤ 24, -25 ≤ l ≤ 26
Reflections collected 38837
Independent reflections 8504 [Rint = 0.0304, Rsigma = 0.0268]
Data/restraints/parameters 8504/0/396
Goodness-of-fit on F2 1.059
Final R indexes [I>=2σ (I)] R1 = 0.0315, wR2 = 0.0774
Final R indexes [all data] R1 = 0.0403, wR2 = 0.0814
Largest diff. peak/hole / e Å-3 0.47/-0.29

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B1032_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Si31672.5(3)8115.3(2)1193.9(2)12.85(8)
Si43773.4(3)8948.6(2)3592.4(2)13.92(8)
Si26291.5(3)6976.6(2)1872.1(2)12.86(8)
Si11596.0(3)5485.7(2)3463.7(2)13.77(8)
O11710.4(8)6038.3(4)1531.7(4)14.54(18)
O25343.3(9)6459.9(5)3911.2(4)18.8(2)
O395.5(8)7882.4(5)3536.8(4)15.59(19)
C91596.7(12)7778.5(7)2028.4(6)14.0(2)
C87738.3(13)6672.2(7)2409.2(7)20.4(3)
C133771.1(12)7997.3(6)3467.4(6)13.8(2)
C11834.1(13)6423.6(6)3276.7(6)14.8(2)
C102631.8(14)7519.3(7)640.6(6)19.7(3)
C4637.8(17)5018.4(8)2796.6(7)28.3(3)
C28-1023.4(12)8272.4(7)3248.5(6)18.2(3)
C112559.0(14)8984.5(7)1179.3(7)22.0(3)
C144621.2(15)9246.0(8)4375.3(7)25.4(3)
C76361.1(14)7958.4(7)1829.5(7)23.5(3)
C19540.0(14)5679.4(7)578.4(7)22.7(3)
C172552.4(13)5531.2(7)1213.1(7)21.3(3)
C181609.4(14)5132.5(7)752.7(7)24.1(3)
C54642.5(12)6699.8(7)2176.5(7)15.2(3)
C216441.5(14)5957.2(7)3925.7(7)22.1(3)
C12-45.7(13)8248.0(7)786.0(7)20.0(3)
C20384.5(12)6055.0(7)1217.3(6)17.1(3)
C236098.1(17)6313.5(8)5005.5(7)29.4(3)
C66656.1(14)6654.6(9)1030.0(7)26.5(3)
C27-2203.5(13)8171.6(8)3701.1(7)25.9(3)
C23249.5(15)5016.4(7)3589.8(8)26.7(3)
C226522.3(14)5680.5(7)4612.6(7)22.2(3)
C154632.2(15)9414.7(7)2914.2(7)24.3(3)
C162011.8(14)9323.2(7)3616.2(8)27.5(3)
C26-1495.9(14)8058.8(8)4355.0(7)24.9(3)
C25-258.8(15)7642.4(8)4172.7(7)24.7(3)
C3617.1(16)5345.2(8)4221.6(7)28.2(3)
C245012.2(16)6640.5(8)4571.7(7)28.5(3)
Li31762(2)7606.0(11)3114.5(10)15.3(4)
Li12338(2)6631.4(11)2250.1(10)15.9(4)
Li24044(2)6761.4(11)3219.5(11)17.6(4)
Li43733(2)7743.9(11)2410.5(11)16.4(4)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B1032_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Si313.67(16)13.29(16)11.53(17)2.44(13)-0.68(13)-1.96(12)
Si413.19(16)12.21(16)16.25(18)-3.43(13)-1.87(13)-0.35(12)
Si210.41(16)16.45(17)11.80(17)-0.73(13)2.23(12)-0.47(12)
Si117.32(17)11.94(16)12.09(17)-0.41(13)0.83(13)-0.59(12)
O112.0(4)16.7(4)14.7(4)-3.8(4)-2.6(3)0.7(3)
O221.4(5)21.3(5)13.7(5)0.1(4)-2.2(4)10.1(4)
O313.1(4)19.2(4)14.6(4)4.6(4)3.0(3)5.0(3)
C915.2(6)14.7(6)12.1(6)1.7(5)1.2(5)0.2(5)
C814.7(6)25.9(7)20.4(7)-0.1(6)0.5(5)1.4(5)
C1311.4(6)13.5(6)16.5(6)-1.0(5)-0.8(5)1.0(5)
C115.5(6)12.9(6)15.9(7)-2.1(5)-2.8(5)2.1(5)
C1021.8(7)22.1(7)15.4(7)1.8(5)5.0(5)-1.9(5)
C443.6(9)20.1(7)20.7(7)2.7(6)-6.8(6)-12.5(6)
C2812.7(6)23.0(7)18.8(7)0.1(5)-3.3(5)4.5(5)
C1123.8(7)18.5(7)23.7(7)4.1(6)-2.4(6)-4.9(5)
C1425.7(7)28.3(8)22.1(7)-10.4(6)-2.7(6)-0.5(6)
C722.3(7)20.7(7)27.4(8)5.4(6)0.7(6)-2.6(5)
C1923.4(7)24.8(7)19.6(7)-5.8(6)-6.9(5)0.1(5)
C1718.5(6)20.6(7)24.4(7)-9.1(6)-4.4(5)5.6(5)
C1825.1(7)20.1(7)26.9(8)-9.3(6)-4.5(6)1.7(5)
C512.2(6)17.0(6)16.4(7)-2.2(5)1.9(5)-1.1(5)
C2118.0(6)27.3(7)21.2(7)4.8(6)3.0(5)10.6(5)
C1219.3(6)21.6(7)18.8(7)3.6(5)-4.1(5)-0.9(5)
C2012.2(6)19.1(6)19.9(7)-2.3(5)-3.7(5)-0.9(5)
C2340.6(9)29.6(8)17.5(7)-0.1(6)-8.4(6)8.3(7)
C621.1(7)42.2(9)16.5(7)-5.0(6)4.7(5)-0.3(6)
C2713.5(6)34.2(8)30.2(8)-8.0(6)3.5(6)2.6(6)
C227.0(7)16.9(7)36.2(9)2.8(6)0.1(6)5.0(5)
C2221.1(7)24.6(7)20.9(7)6.2(6)0.5(5)6.8(5)
C1530.8(8)18.6(7)23.3(7)0.7(6)-1.6(6)-6.9(6)
C1618.2(7)17.6(7)46.3(10)-6.1(6)-4.4(6)3.8(5)
C2624.8(7)27.7(7)22.8(7)-1.8(6)9.6(6)3.5(6)
C2528.7(7)28.4(8)17.5(7)6.2(6)8.5(6)7.9(6)
C336.4(8)24.6(7)24.1(8)1.1(6)11.9(6)-5.2(6)
C2438.8(9)32.2(8)14.3(7)-3.6(6)-2.1(6)16.9(7)
Li312.8(10)17.1(10)15.9(11)-0.4(8)1.2(8)1.0(8)
Li114.8(10)18.1(11)14.6(11)-2.1(8)-0.2(8)-1.8(8)
Li216.8(10)19.9(11)15.9(11)1.0(9)-2.2(8)1.0(8)
Li416(1)16(1)17.1(11)1.1(8)1.5(8)-2.4(8)

 

Table 4 Bond Lengths for mo_B1032_0m.
AtomAtomLength/Å AtomAtomLength/Å
Si3C91.8424(13) C9Li12.357(2)
Si3C101.8869(13) C9Li42.230(2)
Si3C111.8816(13) C13Li32.223(2)
Si3C121.8888(14) C13Li22.439(3)
Si4C131.8408(13) C13Li42.234(3)
Si4C141.8872(14) C1Li32.291(2)
Si4C151.8808(14) C1Li12.225(3)
Si4C161.8814(14) C1Li22.280(3)
Si2C81.8760(14) C28C271.5238(18)
Si2C71.8846(14) C19C181.5228(19)
Si2C51.8370(13) C19C201.5136(18)
Si2C61.8879(14) C17C181.5178(19)
Si2Li43.149(2) C5Li12.285(2)
Si1C11.8543(13) C5Li22.250(3)
Si1C41.8762(15) C5Li42.250(3)
Si1C21.8739(14) C21C221.5136(19)
Si1C31.8793(14) C23C221.524(2)
O1C171.4474(15) C23C241.513(2)
O1C201.4443(15) C27C261.518(2)
O1Li11.955(2) C26C251.5135(19)
O2C211.4490(15) Li3Li12.654(3)
O2C241.4520(16) Li3Li22.776(3)
O2Li21.978(2) Li3Li42.471(3)
O3C281.4473(15) Li1Li22.591(3)
O3C251.4424(16) Li1Li42.553(3)
O3Li31.954(2) Li2Li42.529(3)
C9Li32.267(2)    

 

Table 5 Bond Angles for mo_B1032_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C9Si3C10112.78(6) C9Li3C1106.84(10)
C9Si3C11110.83(6) C9Li3Li156.57(7)
C9Si3C12113.91(6) C9Li3Li2101.47(9)
C10Si3C12105.66(6) C9Li3Li455.95(8)
C11Si3C10106.58(6) C13Li3C9108.34(10)
C11Si3C12106.57(6) C13Li3C1105.18(10)
C13Si4C14114.69(6) C13Li3Li1104.64(9)
C13Si4C15111.39(6) C13Li3Li257.14(7)
C13Si4C16112.56(6) C13Li3Li456.54(8)
C15Si4C14107.21(7) C1Li3Li152.86(7)
C15Si4C16105.82(7) C1Li3Li252.42(7)
C16Si4C14104.51(7) C1Li3Li499.78(9)
C8Si2C7108.05(6) Li1Li3Li256.96(8)
C8Si2C6106.37(6) Li4Li3Li159.62(8)
C8Si2Li4122.73(6) Li4Li3Li257.29(8)
C7Si2C6105.97(7) O1Li1C9107.73(10)
C7Si2Li465.22(6) O1Li1C1122.94(11)
C5Si2C8111.98(6) O1Li1C5106.14(10)
C5Si2C7109.74(6) O1Li1Li3148.14(11)
C5Si2C6114.37(6) O1Li1Li2145.79(12)
C5Si2Li444.69(6) O1Li1Li4137.89(12)
C6Si2Li4130.66(6) C9Li1Li353.40(7)
C1Si1C4111.95(6) C9Li1Li2104.59(10)
C1Si1C2112.29(6) C9Li1Li453.84(7)
C1Si1C3112.51(6) C1Li1C9106.01(9)
C4Si1C3106.42(7) C1Li1C5108.75(10)
C2Si1C4106.99(7) C1Li1Li355.16(7)
C2Si1C3106.26(7) C1Li1Li255.88(8)
C17O1Li1124.11(10) C1Li1Li499.16(10)
C20O1C17109.52(9) C5Li1C9103.73(9)
C20O1Li1126.31(9) C5Li1Li3103.62(9)
C21O2C24109.01(10) C5Li1Li254.52(7)
C21O2Li2132.69(10) C5Li1Li455.09(7)
C24O2Li2116.76(10) Li2Li1Li363.88(8)
C28O3Li3126.70(10) Li4Li1Li356.62(8)
C25O3C28109.76(9) Li4Li1Li258.90(8)
C25O3Li3123.13(10) O2Li2C13101.84(10)
Si3C9Li3166.28(9) O2Li2C1118.75(11)
Si3C9Li1119.20(8) O2Li2C5119.59(11)
Si3C9Li4106.22(8) O2Li2Li3137.26(11)
Li3C9Li170.03(8) O2Li2Li1157.43(12)
Li4C9Li366.66(8) O2Li2Li4139.34(12)
Li4C9Li167.58(8) C13Li2Li349.94(7)
Si4C13Li3112.19(8) C13Li2Li1100.50(9)
Si4C13Li2172.28(9) C13Li2Li453.40(7)
Si4C13Li4110.61(8) C1Li2C1398.84(9)
Li3C13Li272.92(8) C1Li2Li352.79(7)
Li3C13Li467.35(8) C1Li2Li153.90(7)
Li4C13Li265.37(8) C1Li2Li498.40(10)
Si1C1Li3170.13(9) C5Li2C13106.55(10)
Si1C1Li1113.85(8) C5Li2C1108.06(10)
Si1C1Li2114.37(8) C5Li2Li3100.87(10)
Li1C1Li371.98(8) C5Li2Li155.79(7)
Li1C1Li270.22(9) C5Li2Li455.80(8)
Li2C1Li374.79(8) Li1Li2Li359.16(8)
O3C28C27105.59(11) Li4Li2Li355.29(8)
C20C19C18101.95(11) Li4Li2Li159.80(8)
O1C17C18105.84(10) C9Li4Si2130.34(9)
C17C18C19102.14(11) C9Li4C13109.27(10)
Si2C5Li1158.46(10) C9Li4C5109.19(10)
Si2C5Li2124.68(9) C9Li4Li357.39(8)
Si2C5Li4100.28(8) C9Li4Li158.58(8)
Li2C5Li169.69(8) C9Li4Li2110.64(10)
Li2C5Li468.40(9) C13Li4Si2116.95(9)
Li4C5Li168.52(8) C13Li4C5113.98(10)
O2C21C22105.82(10) C13Li4Li356.10(8)
O1C20C19105.62(10) C13Li4Li1107.64(10)
C24C23C22102.40(12) C13Li4Li261.23(8)
C26C27C28102.87(11) C5Li4Si235.03(4)
C21C22C23102.20(11) C5Li4Li3110.82(10)
C25C26C27102.03(11) C5Li4Li156.39(7)
O3C25C26105.93(11) C5Li4Li255.80(8)
O2C24C23106.47(11) Li3Li4Si2143.87(10)
O3Li3C9111.25(10) Li3Li4Li163.75(8)
O3Li3C13121.02(11) Li3Li4Li267.42(9)
O3Li3C1103.06(10) Li1Li4Si289.90(8)
O3Li3Li1133.48(11) Li2Li4Si278.52(7)
O3Li3Li2144.40(11) Li2Li4Li161.30(8)
O3Li3Li4156.52(12)     

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B1032_0m.
AtomxyzU(eq)
H8A8592.96853.812245.6431
H8B77656160.882411.3531
H8C7612.926842.82851.2431
H10A3590.417507.84778.3630
H10B2551.217693.19194.6830
H10C2251.957047.47661.4630
H4A-248.535240.712724.642
H4B508.684529.212919.1442
H4C1152.755041.162397.5242
H28A-1258.058092.052810.222
H28B-787.518773.033213.6722
H11A2076.969316.881451.1733
H11B2568.79159.06733.1333
H11C3492.978930.441346.133
H14A4144.259046.44742.4238
H14B4591.89756.54400.3238
H14C5567.679089.444389.8338
H7A6283.128153.222265.9535
H7B5610.678129.511551.935
H7C7225.628103.141648.3535
H19A857.145999.89238.0227
H19B-322.785459.91430.3127
H17A2981.155211.081534.6526
H17B3274.645767.33971.3326
H18A1203.264724.43968.7429
H18B2089.454973.24364.2829
H21A7305.76183.613812.0427
H21B6251.315573.743614.8527
H12A-508.727797.25741.4230
H12B69.368453.13356.0430
H12C-589.358562.351049.0430
H20A85.26542.481143.9421
H20B-290.125815.191485.6921
H23A5729.76172.315427.3635
H23B6868.486637.055082.1435
H6A7530.116840.77895.0240
H6B5937.036812.56727.4340
H6C6690.346143.471030.340
H27A-2792.248589.943706.2231
H27B-2756.967760.653572.831
H2A3806.495079.543208.0340
H2B3077.214517.873654.8340
H2C3729.375206.333972.640
H22A7455.655530.284733.8127
H22B5892.035284.564670.3827
H15A5578.159260.742896.136
H15B4604.979919.242990.8836
H15C4160.869307.092502.1636
H16A1551.129256.473194.0741
H16B2065.529822.953714.7941
H16C1501.19085.413952.0441
H26A-1236.848507.964560.4730
H26B-2075.097792.544651.6830
H25A498.27724.744488.2530
H25B-467.997137.044164.1730
H3A1096.95567.484588.7942
H3B532.444843.584304.1842
H3C-288.415551.164166.9742
H24A4107.046455.934677.7534
H24B5005.047153.624627.8734
H13A3366(17)7801(9)3849(8)31(4)
H1A1995(18)6623(9)3710(9)39(5)
H9A1220(18)8192(10)2259(9)39(5)
H13B4709(18)7863(9)3514(8)34(5)
H9B852(17)7440(9)2025(8)29(4)
H5A4125(18)6648(10)1782(9)41(5)
H1B891(18)6584(9)3175(9)40(5)
H5B4775(19)6231(10)2316(9)44(5)

Experimental

Single crystals of C28H68Li4O3Si4 [mo_B1032_0m] 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 XT [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 [mo_B1032_0m]

Crystal Data for C28H68Li4O3Si4 (=592.94 g/mol): monoclinic, space group P21/c (no. 14), a = 9.8606(18) Å, b = 19.160(2) Å, c = 20.638(3) Å, β = 91.536(6)°, = 3897.8(10) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 0.176 mm-1, Dcalc = 1.010 g/cm3, 38837 reflections measured (4.484° ≤ 2Θ ≤ 54°), 8504 unique (Rint = 0.0304, Rsigma = 0.0268) which were used in all calculations. The final R1 was 0.0315 (I > 2σ(I)) and wR2 was 0.0814 (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:
C28(H28A,H28B), C19(H19A,H19B), C17(H17A,H17B), C18(H18A,H18B), C21(H21A,
H21B), C20(H20A,H20B), C23(H23A,H23B), C27(H27A,H27B), C22(H22A,H22B),
C26(H26A,H26B), C25(H25A,H25B), C24(H24A,H24B)
2.b Idealised Me refined as rotating group:
C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C),
C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C6(H6A,H6B,H6C),
C2(H2A,H2B,H2C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C)

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