3182

Table 1 Crystal data and structure refinement for 3182.
Identification code 3182
Empirical formula C28H68Li4O8Si4
Formula weight 672.94
Temperature/K 173.15
Crystal system monoclinic
Space group P21/c
a/Å 20.3421(14)
b/Å 10.7413(5)
c/Å 21.0670(16)
α/° 90
β/° 112.664(9)
γ/° 90
Volume/Å3 4247.7(5)
Z 4
ρcalcg/cm3 1.052
μ/mm‑1 0.176
F(000) 1472.0
Crystal size/mm3 0.3 × 0.23 × 0.21
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.19 to 50
Index ranges -24 ≤ h ≤ 24, -12 ≤ k ≤ 12, -25 ≤ l ≤ 24
Reflections collected 46058
Independent reflections 7469 [Rint = 0.0673, Rsigma = 0.0436]
Data/restraints/parameters 7469/0/409
Goodness-of-fit on F2 1.134
Final R indexes [I>=2σ (I)] R1 = 0.0710, wR2 = 0.1920
Final R indexes [all data] R1 = 0.0931, wR2 = 0.2057
Largest diff. peak/hole / e Å-3 0.43/-0.33

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3182. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Si311247.9(6)11341.2(10)1251.2(6)38.9(3)
Si113955.3(5)11197.5(9)3555.2(5)29.1(3)
Si413114.7(6)7435.0(11)1759.3(6)40.7(3)
Si211590.5(6)8726.2(11)3504.9(6)40.9(3)
O113230.9(12)10562(2)3054.8(12)28.7(6)
O412790.2(12)8379(2)2141.1(12)29.4(6)
O212010.6(13)9068(2)3027.7(12)33.4(6)
O311875.7(12)10591(2)1825.4(12)32.4(6)
O513587.3(15)7578(3)3815.9(13)42.9(7)
O713394.5(15)11062(3)1557.8(15)46.6(7)
O611867.5(15)12274(3)3145.1(17)54.6(8)
O811064.2(15)7714(3)1443.5(15)49.9(8)
C213965(2)11391(4)4450(2)44.7(10)
C910352(2)10930(5)1252(2)51.8(11)
C114757(2)10240(4)3641(2)43.3(10)
C1313512(3)6261(4)3691(2)54.3(12)
C314093(2)12777(4)3245(2)43.8(10)
C1613929(2)7795(4)4539(2)47.5(11)
C1514241(3)6554(5)4853(2)60.5(13)
C2113161(3)12290(4)1295(2)53.8(12)
C711219(3)11023(5)363(2)57.7(13)
C2610567(3)6453(5)466(3)61.7(14)
C2810734(3)6663(5)1614(3)58.8(13)
C1413735(3)5652(5)4388(3)66.9(15)
C611920(3)9654(5)4331(2)62.5(13)
C2314164(3)11771(5)1049(3)67.1(15)
C2710218(2)6151(4)941(3)59.5(13)
C2414078(3)10829(5)1537(3)59.3(13)
C1114112(2)7337(5)2204(3)63.9(14)
C1212917(3)7919(6)846(2)68.4(15)
C2012292(3)13326(5)3489(3)63.5(14)
C811341(3)13077(4)1383(3)66.8(15)
C2213777(3)12871(5)1171(3)67.4(15)
C411697(3)7038(5)3757(3)61.6(13)
C510605(2)9002(5)3059(3)59.4(13)
C1911993(3)13668(6)4011(3)72.9(16)
C1012754(3)5811(4)1707(3)67.1(15)
C2510897(3)7718(5)715(2)60.5(13)
C1811202(3)13495(7)3602(4)88(2)
C1711156(3)12523(6)3108(3)72.2(16)
Li411838(3)8820(6)2060(3)33.3(14)
Li312876(3)10199(6)2070(3)31.0(13)
Li212216(3)10782(6)2824(3)31.5(13)
Li112990(3)8805(6)3095(3)31.1(13)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3182. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Si329.6(6)38.1(6)36.3(6)6.3(5)-1.5(5)1.0(5)
Si122.4(5)35.2(5)23.9(5)-4.4(4)2.4(4)-3.3(4)
Si439.4(6)40.2(6)42.7(7)-12.9(5)16.3(5)-0.5(5)
Si234.4(6)51.5(7)38.4(6)2.3(5)15.8(5)-3.2(5)
O122.6(12)33.0(13)23.1(12)-4.9(10)0.8(10)-1.9(10)
O429.8(13)29.0(13)26.1(13)-2(1)7.2(11)-0.5(10)
O227.4(13)40.7(15)30.3(14)1.2(11)9.1(11)-2.1(11)
O327.9(13)32.9(13)27.5(13)-0.4(11)0.9(11)0.4(11)
O544.2(16)41.7(16)29.8(14)7.9(12)0.0(12)2.9(13)
O749.1(17)50.7(17)46.7(17)2.3(14)25.7(14)-11.7(14)
O636.2(16)55.1(19)69(2)-26.0(16)16.5(15)5.4(14)
O846.4(17)46.8(17)39.1(17)-3.8(13)-2.9(13)-16.1(14)
C246(2)54(3)26(2)-8.0(18)4.6(18)-4(2)
C932(2)62(3)49(3)-1(2)2(2)-1(2)
C131(2)51(2)43(2)5(2)8.2(18)4.2(18)
C1362(3)42(2)46(3)-1(2)7(2)-5(2)
C341(2)39(2)45(2)-4.5(19)8.6(19)-5.9(18)
C1651(3)48(3)34(2)2.1(19)7(2)-4(2)
C1555(3)70(3)42(3)21(2)3(2)0(2)
C2155(3)53(3)50(3)9(2)16(2)-8(2)
C749(3)74(3)36(2)10(2)1(2)-5(2)
C2666(3)54(3)45(3)-13(2)0(2)0(2)
C2862(3)57(3)61(3)-14(2)27(3)-22(2)
C1473(3)50(3)59(3)14(2)4(3)1(3)
C669(3)76(3)47(3)-4(3)26(3)-1(3)
C2370(3)84(4)57(3)6(3)35(3)-17(3)
C2740(2)46(3)79(4)-17(2)8(2)-14(2)
C2455(3)69(3)58(3)4(3)27(3)-4(2)
C1143(3)71(3)78(4)-6(3)25(3)14(2)
C1277(4)92(4)40(3)-22(3)27(3)-18(3)
C2048(3)59(3)82(4)-19(3)24(3)-2(2)
C857(3)41(3)78(4)13(2)-1(3)4(2)
C2285(4)61(3)67(3)11(3)40(3)-18(3)
C459(3)63(3)66(3)14(3)27(3)-2(2)
C539(2)70(3)69(3)-3(3)21(2)-2(2)
C1970(4)70(4)73(4)-30(3)21(3)-3(3)
C1071(3)40(3)85(4)-23(3)25(3)-3(2)
C2559(3)68(3)42(3)1(2)6(2)-10(3)
C1855(3)102(5)110(5)-56(4)35(3)-15(3)
C1740(3)80(4)91(4)-26(3)20(3)8(3)
Li427(3)34(3)29(3)0(3)0(3)-4(3)
Li329(3)38(3)22(3)-1(2)6(2)-3(3)
Li229(3)32(3)33(3)-5(3)12(3)5(3)
Li128(3)32(3)29(3)-3(3)6(3)-2(2)

 

Table 4 Bond Lengths for 3182.
AtomAtomLength/Å AtomAtomLength/Å
Si3O31.598(3) O5C161.429(5)
Si3C91.877(4) O5Li12.024(6)
Si3C71.881(5) O7C211.439(5)
Si3C81.884(5) O7C241.431(5)
Si1O11.597(2) O7Li32.003(7)
Si1C21.888(4) O6C201.438(6)
Si1C11.877(4) O6C171.444(5)
Si1C31.878(4) O6Li21.973(6)
Si4O41.588(3) O8C281.429(5)
Si4C111.881(5) O8C251.439(5)
Si4C121.881(5) O8Li41.999(6)
Si4C101.880(5) C13C141.510(6)
Si2O21.593(3) C16C151.515(6)
Si2C61.890(5) C15C141.477(7)
Si2C41.878(5) C21C221.509(7)
Si2C51.880(5) C26C271.470(7)
O1Li31.955(6) C26C251.516(7)
O1Li21.945(6) C28C271.506(6)
O1Li11.960(6) C23C241.500(7)
O4Li41.936(7) C23C221.496(8)
O4Li31.973(7) C20C191.492(7)
O4Li11.945(6) C19C181.517(7)
O2Li41.950(7) C18C171.451(7)
O2Li21.971(7) Li4Li32.573(8)
O2Li11.964(6) Li4Li22.584(8)
O3Li41.975(7) Li4Li12.513(8)
O3Li31.944(6) Li3Li22.523(8)
O3Li21.956(6) Li3Li12.563(8)
O5C131.436(5) Li2Li12.574(8)

 

Table 5 Bond Angles for 3182.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O3Si3C9111.96(18) O4Li4Li295.6(3)
O3Si3C7111.79(19) O4Li4Li149.8(2)
O3Si3C8112.44(18) O2Li4O396.9(3)
C9Si3C7107.4(2) O2Li4O8122.7(3)
C9Si3C8106.0(2) O2Li4Li395.5(3)
C7Si3C8106.8(3) O2Li4Li249.1(2)
O1Si1C2110.99(17) O2Li4Li150.3(2)
O1Si1C1112.06(17) O3Li4O8120.5(3)
O1Si1C3112.31(16) O3Li4Li348.4(2)
C1Si1C2106.83(19) O3Li4Li248.6(2)
C1Si1C3106.7(2) O3Li4Li196.3(3)
C3Si1C2107.6(2) O8Li4Li3141.8(3)
O4Si4C11111.25(19) O8Li4Li2149.3(3)
O4Si4C12112.0(2) O8Li4Li1142.9(3)
O4Si4C10113.1(2) Li3Li4Li258.6(2)
C12Si4C11106.8(3) Li1Li4Li360.5(2)
C10Si4C11107.4(2) Li1Li4Li260.7(2)
C10Si4C12105.8(3) O1Li3O497.2(3)
O2Si2C6111.9(2) O1Li3O7115.1(3)
O2Si2C4111.7(2) O1Li3Li495.2(3)
O2Si2C5112.06(19) O1Li3Li249.5(2)
C4Si2C6106.7(2) O1Li3Li149.2(2)
C4Si2C5106.1(2) O4Li3O7125.4(3)
C5Si2C6108.0(2) O4Li3Li448.2(2)
Si1O1Li3130.9(2) O4Li3Li296.5(3)
Si1O1Li2137.2(2) O4Li3Li148.7(2)
Si1O1Li1124.4(2) O3Li3O199.1(3)
Li3O1Li181.8(3) O3Li3O496.9(3)
Li2O1Li380.6(3) O3Li3O7118.1(3)
Li2O1Li182.5(3) O3Li3Li449.5(2)
Si4O4Li4135.1(2) O3Li3Li249.9(2)
Si4O4Li3121.9(2) O3Li3Li195.5(3)
Si4O4Li1135.3(2) O7Li3Li4149.6(3)
Li4O4Li382.3(3) O7Li3Li2138.0(3)
Li4O4Li180.7(3) O7Li3Li1146.0(3)
Li1O4Li381.7(3) Li2Li3Li460.9(2)
Si2O2Li4134.8(2) Li2Li3Li160.8(2)
Si2O2Li2124.2(2) Li1Li3Li458.6(2)
Si2O2Li1134.3(2) O1Li2O297.2(3)
Li4O2Li282.4(3) O1Li2O399.0(3)
Li4O2Li179.9(3) O1Li2O6120.0(3)
Li1O2Li281.7(3) O1Li2Li495.1(3)
Si3O3Li4125.3(2) O1Li2Li349.9(2)
Si3O3Li3139.5(2) O1Li2Li149.0(2)
Si3O3Li2127.6(2) O2Li2O6123.4(3)
Li3O3Li482.1(3) O2Li2Li448.4(2)
Li3O3Li280.6(3) O2Li2Li396.5(3)
Li2O3Li482.2(3) O2Li2Li149.0(2)
C13O5Li1120.8(3) O3Li2O296.8(3)
C16O5C13109.3(3) O3Li2O6115.4(3)
C16O5Li1126.8(3) O3Li2Li449.2(2)
C21O7Li3117.9(3) O3Li2Li349.5(2)
C24O7C21109.2(3) O3Li2Li194.8(3)
C24O7Li3130.9(3) O6Li2Li4144.7(3)
C20O6C17106.0(3) O6Li2Li3140.0(4)
C20O6Li2125.9(3) O6Li2Li1149.8(3)
C17O6Li2128.1(3) Li3Li2Li460.5(2)
C28O8C25109.2(3) Li3Li2Li160.4(2)
C28O8Li4129.4(3) Li1Li2Li458.3(2)
C25O8Li4119.6(3) O1Li1O297.0(3)
O5C13C14106.1(4) O1Li1O5124.9(3)
O5C16C15105.8(4) O1Li1Li497.0(3)
C14C15C16102.7(4) O1Li1Li349.0(2)
O7C21C22105.9(4) O1Li1Li248.5(2)
C27C26C25103.1(4) O4Li1O197.9(3)
O8C28C27106.0(4) O4Li1O299.0(3)
C15C14C13103.4(4) O4Li1O5116.7(3)
C22C23C24102.0(4) O4Li1Li449.5(2)
C26C27C28102.5(4) O4Li1Li349.6(2)
O7C24C23105.9(4) O4Li1Li295.6(3)
O6C20C19103.3(4) O2Li1O5116.5(3)
C23C22C21103.3(4) O2Li1Li449.8(2)
C20C19C18101.3(4) O2Li1Li395.5(3)
O8C25C26105.0(4) O2Li1Li249.3(2)
C17C18C19104.8(4) O5Li1Li4138.2(3)
O6C17C18108.0(4) O5Li1Li3147.8(3)
O4Li4O299.8(3) O5Li1Li2147.4(3)
O4Li4O397.1(3) Li4Li1Li360.9(2)
O4Li4O8115.0(3) Li4Li1Li261.0(2)
O4Li4Li349.5(2) Li3Li1Li258.8(2)

 

Table 6 Torsion Angles for 3182.
ABCDAngle/˚ ABCDAngle/˚
O5C13C14C15-27.3(6) C11Si4O4Li374.7(3)
O5C16C15C14-31.2(5) C11Si4O4Li1-38.1(4)
O7C21C22C2326.4(5) C12Si4O4Li468.8(4)
O6C20C19C18-40.3(6) C12Si4O4Li3-44.8(3)
O8C28C27C2631.2(5) C12Si4O4Li1-157.6(3)
C2Si1O1Li3176.2(3) C20O6C17C18-17.3(7)
C2Si1O1Li248.0(4) C20C19C18C1729.7(7)
C2Si1O1Li1-72.4(3) C8Si3O3Li4159.8(3)
C9Si3O3Li440.5(3) C8Si3O3Li3-75.5(4)
C9Si3O3Li3165.3(4) C8Si3O3Li250.2(4)
C9Si3O3Li2-69.0(3) C22C23C24O733.7(5)
C1Si1O1Li3-64.5(3) C4Si2O2Li477.6(4)
C1Si1O1Li2167.3(3) C4Si2O2Li2-165.7(3)
C1Si1O1Li146.9(3) C4Si2O2Li1-50.8(4)
C13O5C16C1514.5(5) C5Si2O2Li4-41.4(4)
C3Si1O1Li355.7(3) C5Si2O2Li275.4(3)
C3Si1O1Li2-72.6(4) C5Si2O2Li1-169.8(3)
C3Si1O1Li1167.0(3) C19C18C17O6-8.5(7)
C16O5C13C147.8(5) C10Si4O4Li4-50.6(4)
C16C15C14C1335.1(6) C10Si4O4Li3-164.3(3)
C21O7C24C23-17.9(5) C10Si4O4Li182.9(4)
C7Si3O3Li4-80.1(3) C25O8C28C27-12.0(5)
C7Si3O3Li344.7(4) C25C26C27C28-37.2(5)
C7Si3O3Li2170.4(3) C17O6C20C1936.4(6)
C28O8C25C26-11.4(5) Li4O8C28C27-176.8(4)
C6Si2O2Li4-162.8(3) Li4O8C25C26155.1(4)
C6Si2O2Li2-46.1(3) Li3O7C21C22160.4(4)
C6Si2O2Li168.8(4) Li3O7C24C23178.8(4)
C27C26C25O830.8(5) Li2O6C20C19-141.8(4)
C24O7C21C22-5.4(5) Li2O6C17C18160.7(5)
C24C23C22C21-36.2(5) Li1O5C13C14-153.6(4)
C11Si4O4Li4-171.6(4) Li1O5C16C15174.5(4)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3182.
AtomxyzU(eq)
H2A1357411940443267
H2B1442011758475067
H2C1390710576463167
H9A1025710043114678
H9B99841142790478
H9C1034611104170678
H1A147099406380865
H1B1518710640396865
H1C1479310172319265
H13A138215980345265
H13B130126049340265
H3A1418112688282166
H3B1450313181359866
H3C1366613286315366
H16A135808091472857
H16B143098428463557
H15A147266440485873
H15B142616477532973
H21A1304312785163365
H21B127351224486165
H7A116531134432587
H7B10802114352287
H7C111861012327887
H26A102176495-1574
H26B10937583049674
H28A104806917191071
H28B110966029186171
H14A133215523451780
H14B139694840439680
H6A124299496458394
H6B116569405461494
H6C1184410544422494
H23A1467211964116180
H23B139431148056680
H27A10157524096971
H27B9748656180071
H24A141019974137271
H24B1445910927200071
H11A143218154219496
H11B142966727196896
H11C142387078268396
H12A124027883581103
H12B131597355641103
H12C130868771840103
H20A1224114020316476
H20B1280213097371276
H8A11453132711868100
H8B10894134841097100
H8C11726133801253100
H22A136051342676481
H22B1408613353157681
H4A115296521334192
H4B114166854403392
H4C122006860402692
H5A105139899300389
H5B103588649333589
H5C104318603260589
H19A1210814540416787
H19B1216913106441487
H10A1289654672172101
H10B1294452871437101
H10C1223358311486101
H25A11333783561973
H25B10556839248673
H18A10957132393906106
H18B10983142763364106
H17A1094811760321887
H17B1084812796263887

Experimental

Single crystals of C28H68Li4O8Si4 [3182] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 K during data collection. Using Olex2 [1], the structure was solved with the SIR2004 [2] structure solution program using Direct Methods and refined with the ShelXL [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. Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R. (2007). J. Appl. Cryst. 40, 609-613.
  3. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [3182]

Crystal Data for C28H68Li4O8Si4 (=672.94 g/mol): monoclinic, space group P21/c (no. 14), a = 20.3421(14) Å, b = 10.7413(5) Å, c = 21.0670(16) Å, β = 112.664(9)°, = 4247.7(5) Å3, Z = 4, T = 173.15 K, μ(MoKα) = 0.176 mm-1, Dcalc = 1.052 g/cm3, 46058 reflections measured (4.19° ≤ 2Θ ≤ 50°), 7469 unique (Rint = 0.0673, Rsigma = 0.0436) which were used in all calculations. The final R1 was 0.0710 (I > 2σ(I)) and wR2 was 0.2057 (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:
C13(H13A,H13B), C16(H16A,H16B), C15(H15A,H15B), C21(H21A,H21B), C26(H26A,
H26B), C28(H28A,H28B), C14(H14A,H14B), C23(H23A,H23B), C27(H27A,H27B),
C24(H24A,H24B), C20(H20A,H20B), C22(H22A,H22B), C19(H19A,H19B), C25(H25A,H25B),
C18(H18A,H18B), C17(H17A,H17B)
2.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C7(H7A,
H7B,H7C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C8(H8A,
H8B,H8C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)

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