mo_B0321_0m

Table 1 Crystal data and structure refinement for mo_B0321_0m.
Identification code mo_B0321_0m
Empirical formula C24H56Li4N4O4
Formula weight 492.48
Temperature/K 99.98
Crystal system monoclinic
Space group P21/n
a/Å 18.0767(15)
b/Å 10.0888(9)
c/Å 18.548(2)
α/° 90
β/° 108.538(4)
γ/° 90
Volume/Å3 3207.1(5)
Z 4
ρcalcg/cm3 1.020
μ/mm‑1 0.066
F(000) 1088.0
Crystal size/mm3 0.41 × 0.33 × 0.32
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.686 to 56
Index ranges -23 ≤ h ≤ 23, -13 ≤ k ≤ 13, -24 ≤ l ≤ 24
Reflections collected 70347
Independent reflections 7736 [Rint = 0.0243, Rsigma = 0.0142]
Data/restraints/parameters 7736/0/342
Goodness-of-fit on F2 1.027
Final R indexes [I>=2σ (I)] R1 = 0.0348, wR2 = 0.0916
Final R indexes [all data] R1 = 0.0388, wR2 = 0.0944
Largest diff. peak/hole / e Å-3 0.34/-0.17

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0321_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O42052.2(3)2246.6(6)5371.1(3)14.31(13)
O21723.9(3)4524.8(6)4362.7(3)13.38(12)
O13093.0(3)4524.9(6)5751.2(3)13.92(12)
O33074.9(3)2908.6(6)4463.7(3)13.21(12)
N41208.4(4)1102.3(7)3906.8(4)15.83(15)
N34091.9(4)1383.7(8)5704.7(4)19.46(16)
N11847.0(4)5420.9(8)6287.3(4)19.65(16)
N22745.3(4)6421.8(7)4009.2(4)17.56(15)
C191462.3(5)1340.2(9)5335.4(5)17.61(17)
C211686.7(7)448.0(12)6041.7(6)34.0(3)
C221348.4(5)412.9(8)4642.7(5)17.86(17)
C164071.4(5)1256.5(9)4901.5(5)19.62(18)
C133788.2(5)2498.7(9)4404.9(5)15.67(16)
C91512.0(5)4406.0(9)3018.4(5)21.25(18)
C23413.0(5)3901.5(10)7059.0(5)21.16(18)
C42638.9(5)6009.1(9)6531.5(5)19.68(18)
C13288.4(5)5044.7(9)6484.3(5)15.79(16)
C101883.9(5)6567.1(8)3765.5(5)18.48(17)
C154380.5(5)3642.2(10)4628.3(6)25.6(2)
C184856.4(6)1841.5(12)6195.8(6)31.0(2)
C8572.8(5)5583.2(10)3530.9(6)26.9(2)
C71438.2(5)5239.2(8)3689.0(5)15.63(16)
C20710.4(6)2092.9(12)5305.7(6)31.6(2)
C24376.1(5)1330.8(12)3523.3(6)30.3(2)
C123035.6(6)6424.6(11)3354.2(6)28.0(2)
C34046.9(5)5856.1(10)6672.1(5)25.3(2)
C51639.0(6)4907.0(12)6938.9(6)29.1(2)
C113123.3(6)7502.6(10)4521.3(6)28.2(2)
C143699.9(6)2097.5(11)3581.9(5)28.1(2)
C61261.0(6)6410.8(11)5898.9(6)31.6(2)
C173927.3(7)96.0(11)5988.9(7)33.3(2)
C231506.8(7)316.0(11)3395.7(6)33.5(2)
Li22872.7(8)4704.9(14)4694.9(8)15.4(3)
Li33115.0(8)2658.9(14)5534.5(8)15.9(3)
Li11954.0(8)4151.7(15)5411.8(8)16.6(3)
Li41995.2(8)2693.7(14)4320.4(8)15.2(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0321_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
O412.4(3)16.5(3)13.4(3)1.9(2)3.2(2)-3.0(2)
O211.8(3)15.3(3)12.2(3)3.5(2)2.6(2)1.4(2)
O113.2(3)17.2(3)10.5(3)-3.6(2)2.6(2)0.0(2)
O39.5(3)16.5(3)13.9(3)-2.2(2)4.2(2)1.5(2)
N414.9(3)16.7(3)14.1(3)0.5(3)2.0(3)-2.0(3)
N317.1(3)20.2(4)18.0(3)-0.7(3)1.1(3)5.1(3)
N116.3(3)25.6(4)17.4(3)-1.9(3)5.9(3)6.2(3)
N216.5(3)17.2(3)17.7(3)1.4(3)3.7(3)-4.3(3)
C1916.9(4)21.2(4)15.0(4)2.5(3)5.3(3)-5.4(3)
C2145.1(6)35.3(6)18.9(5)9.5(4)6.1(4)-16.4(5)
C2218.9(4)15.3(4)17.3(4)3.3(3)2.7(3)-3.7(3)
C1617.7(4)19.1(4)20.5(4)-5.3(3)3.8(3)5.4(3)
C1311.6(3)20.0(4)15.9(4)-3.9(3)5.2(3)1.4(3)
C925.6(4)22.3(4)13.0(4)1.8(3)2.1(3)-6.5(3)
C221.6(4)27.0(5)13.0(4)-0.3(3)2.8(3)5.8(3)
C420.8(4)20.2(4)17.7(4)-6.1(3)5.5(3)2.3(3)
C114.3(4)19.5(4)12.3(4)-4.3(3)2.5(3)0.4(3)
C1017.5(4)15.1(4)20.5(4)4.3(3)2.7(3)1.0(3)
C1514.0(4)27.9(5)34.4(5)0.9(4)7.0(4)-3.6(3)
C1817.7(4)45.4(6)22.7(5)-5.3(4)-3.8(4)6.9(4)
C813.8(4)29.7(5)33.3(5)11.8(4)1.8(4)4.0(4)
C712.3(4)17.0(4)15.2(4)4.6(3)1.1(3)-0.1(3)
C2018.9(4)42.9(6)37.3(6)-10.7(5)15.0(4)-6.5(4)
C2416.3(4)41.9(6)25.7(5)9.2(4)-3.3(4)-5.6(4)
C1224.4(5)37.6(6)23.4(5)6.5(4)9.6(4)-7.5(4)
C319.7(4)29.9(5)23.8(4)-10.5(4)3.3(3)-6.7(4)
C523.4(5)44.9(6)22.7(5)-1.6(4)12.5(4)3.4(4)
C1125.6(5)19.6(4)32.2(5)-1.7(4)-0.9(4)-5.7(4)
C1425.2(5)41.8(6)19.3(4)-6.4(4)10.0(4)8.1(4)
C625.5(5)35.1(6)32.1(5)-0.5(4)6.1(4)15.1(4)
C1743.4(6)24.3(5)34.3(6)6.8(4)15.2(5)8.8(4)
C2352.0(7)27.0(5)25.5(5)-2.4(4)17.7(5)5.0(5)
Li214.4(6)16.5(7)15.4(6)-0.1(5)4.8(5)-0.1(5)
Li313.9(6)17.9(7)14.5(6)-0.4(5)2.5(5)1.5(5)
Li114.8(6)19.9(7)15.5(6)-0.8(5)5.6(5)1.1(5)
Li413.5(6)16.5(7)14.4(6)-0.3(5)3.0(5)-1.5(5)

 

Table 4 Bond Lengths for mo_B0321_0m.
AtomAtomLength/Å AtomAtomLength/Å
O4C191.3902(10) N1C51.4697(12)
O4Li31.8936(15) N1C61.4674(12)
O4Li11.9339(16) N1Li12.1246(16)
O4Li41.9708(15) N2C101.4843(11)
O2C71.3917(10) N2C121.4686(12)
O2Li21.9777(15) N2C111.4647(12)
O2Li11.8938(15) N2Li22.1176(16)
O2Li41.9194(16) C19C211.5340(12)
O1C11.3940(9) C19C221.5493(12)
O1Li21.8799(15) C19C201.5424(13)
O1Li31.9281(16) C16C131.5431(12)
O1Li11.9883(15) C13C151.5385(12)
O3C131.3909(9) C13C141.5377(12)
O3Li21.9239(15) C9C71.5418(12)
O3Li31.9802(15) C2C11.5377(12)
O3Li41.8966(15) C4C11.5485(12)
N4C221.4802(11) C1C31.5388(12)
N4C241.4637(11) C10C71.5464(12)
N4C231.4644(12) C8C71.5369(12)
N4Li42.1202(16) Li2Li32.538(2)
N3C161.4839(11) Li2Li12.498(2)
N3C181.4671(12) Li2Li42.533(2)
N3C171.4676(13) Li3Li12.534(2)
N3Li32.1258(16) Li3Li42.504(2)
N1C41.4813(12) Li1Li42.522(2)

 

Table 5 Bond Angles for mo_B0321_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C19O4Li3151.16(7) O1Li2O299.75(7)
C19O4Li1125.24(7) O1Li2O398.57(7)
C19O4Li4107.78(6) O1Li2N2130.65(8)
Li3O4Li182.90(6) O1Li2Li349.01(5)
Li3O4Li480.76(6) O1Li2Li151.70(5)
Li1O4Li480.48(6) O1Li2Li496.61(7)
C7O2Li2106.57(6) O3Li2O295.69(7)
C7O2Li1157.37(7) O3Li2N2128.96(8)
C7O2Li4119.24(7) O3Li2Li350.41(5)
Li1O2Li280.34(6) O3Li2Li196.53(7)
Li1O2Li482.83(6) O3Li2Li448.02(5)
Li4O2Li281.05(6) N2Li2Li3176.49(8)
C1O1Li2152.16(7) N2Li2Li1122.59(7)
C1O1Li3123.71(7) N2Li2Li4123.47(7)
C1O1Li1107.20(6) Li1Li2Li360.40(6)
Li2O1Li383.60(6) Li1Li2Li460.18(6)
Li2O1Li180.40(6) Li4Li2Li359.18(6)
Li3O1Li180.62(6) O4Li3O199.25(7)
C13O3Li2122.96(6) O4Li3O398.96(7)
C13O3Li3107.55(6) O4Li3N3130.05(8)
C13O3Li4153.29(7) O4Li3Li296.43(7)
Li2O3Li381.10(6) O4Li3Li149.23(5)
Li4O3Li283.04(6) O4Li3Li450.97(5)
Li4O3Li380.44(6) O1Li3O395.07(7)
C22N4Li497.11(6) O1Li3N3129.14(8)
C24N4C22111.73(7) O1Li3Li247.39(5)
C24N4C23107.70(8) O1Li3Li150.73(5)
C24N4Li4121.62(7) O1Li3Li496.28(7)
C23N4C22110.62(7) O3Li3N389.41(6)
C23N4Li4107.55(7) O3Li3Li248.48(5)
C16N3Li398.56(6) O3Li3Li193.97(6)
C18N3C16111.62(7) O3Li3Li448.32(5)
C18N3C17108.31(8) N3Li3Li2123.81(7)
C18N3Li3118.40(7) N3Li3Li1176.62(8)
C17N3C16109.92(8) N3Li3Li4122.54(7)
C17N3Li3109.60(7) Li1Li3Li259.01(6)
C4N1Li199.28(6) Li4Li3Li260.30(6)
C5N1C4111.41(7) Li4Li3Li160.08(6)
C5N1Li1121.68(8) O4Li1O195.85(7)
C6N1C4110.74(8) O4Li1N1131.35(8)
C6N1C5108.07(8) O4Li1Li296.69(7)
C6N1Li1105.19(7) O4Li1Li347.87(5)
C10N2Li299.61(6) O4Li1Li450.40(5)
C12N2C10111.36(7) O2Li1O498.65(7)
C12N2Li2119.94(7) O2Li1O198.91(7)
C11N2C10110.60(7) O2Li1N1128.45(8)
C11N2C12108.62(8) O2Li1Li251.30(5)
C11N2Li2106.28(7) O2Li1Li396.64(7)
O4C19C21110.78(7) O2Li1Li449.02(5)
O4C19C22109.53(7) O1Li1N188.89(6)
O4C19C20109.37(8) O1Li1Li247.90(5)
C21C19C22106.45(8) O1Li1Li348.65(5)
C21C19C20108.07(8) O1Li1Li494.17(6)
C20C19C22112.61(7) N1Li1Li2120.64(8)
N4C22C19114.81(7) N1Li1Li3124.31(7)
N3C16C13115.25(7) N1Li1Li4176.31(8)
O3C13C16109.55(7) Li2Li1Li360.59(6)
O3C13C15109.82(7) Li2Li1Li460.59(6)
O3C13C14110.48(7) Li4Li1Li359.37(6)
C15C13C16112.20(7) O4Li4N490.15(6)
C14C13C16106.78(7) O4Li4Li294.64(6)
C14C13C15107.97(8) O4Li4Li348.28(5)
N1C4C1114.04(7) O4Li4Li149.12(5)
O1C1C2109.26(7) O2Li4O496.52(7)
O1C1C4109.27(6) O2Li4N4126.36(7)
O1C1C3110.61(7) O2Li4Li250.48(5)
C2C1C4112.25(7) O2Li4Li396.94(7)
C2C1C3108.57(7) O2Li4Li148.15(5)
C3C1C4106.86(7) O3Li4O499.18(7)
N2C10C7114.07(7) O3Li4O298.58(7)
O2C7C9109.84(7) O3Li4N4132.79(8)
O2C7C10109.42(7) O3Li4Li248.94(5)
O2C7C8110.66(7) O3Li4Li351.24(5)
C9C7C10111.72(7) O3Li4Li196.46(7)
C8C7C9108.25(7) N4Li4Li2174.53(8)
C8C7C10106.91(7) N4Li4Li3124.91(7)
O2Li2N289.15(6) N4Li4Li1122.98(7)
O2Li2Li394.34(6) Li3Li4Li260.52(6)
O2Li2Li148.36(5) Li3Li4Li160.54(6)
O2Li2Li448.47(5) Li1Li4Li259.23(6)

 

Table 6 Torsion Angles for mo_B0321_0m.
ABCDAngle/˚ ABCDAngle/˚
O4C19C22N4-54.09(9) Li2O3Li4Li1-38.62(7)
N3C16C13O3-52.46(9) Li2N2C10C7-31.50(9)
N3C16C13C1569.77(9) Li3O4C19C2148.67(17)
N3C16C13C14-172.13(7) Li3O4C19C22-68.46(15)
N1C4C1O154.23(10) Li3O4C19C20167.68(12)
N1C4C1C2-67.14(9) Li3O1C1C2-7.18(10)
N1C4C1C3173.94(7) Li3O1C1C4-130.35(8)
N2C10C7O253.35(9) Li3O1C1C3112.29(9)
N2C10C7C9-68.51(9) Li3O1Li2O287.27(7)
N2C10C7C8173.23(7) Li3O1Li2O3-10.06(6)
C19O4Li3O1-159.16(11) Li3O1Li2N2-175.39(10)
C19O4Li3O3104.17(13) Li3O1Li2Li181.52(6)
C19O4Li3N37.3(2) Li3O1Li2Li438.37(6)
C19O4Li3Li2153.06(12) Li3O3C13C1638.60(8)
C19O4Li3Li1-168.32(15) Li3O3C13C15-85.05(8)
C19O4Li3Li4110.23(14) Li3O3C13C14155.96(8)
C21C19C22N4-173.91(7) Li3O3Li4O4-6.06(6)
C13O3Li4O4104.16(14) Li3O3Li4O292.03(7)
C13O3Li4O2-157.74(12) Li3O3Li4N4-104.88(11)
C13O3Li4N45.3(2) Li3O3Li4Li282.10(6)
C13O3Li4Li2-167.68(16) Li3O3Li4Li143.48(7)
C13O3Li4Li3110.23(15) Li3N3C16C1333.48(9)
C13O3Li4Li1153.71(13) Li1O4C19C21-117.09(9)
C1O1Li2O2-103.05(14) Li1O4C19C22125.78(8)
C1O1Li2O3159.62(11) Li1O4C19C201.92(11)
C1O1Li2N2-5.7(2) Li1O4Li3O19.16(7)
C1O1Li2Li3169.68(15) Li1O4Li3O3-87.51(7)
C1O1Li2Li1-108.80(14) Li1O4Li3N3175.66(10)
C1O1Li2Li4-151.95(12) Li1O4Li3Li2-38.62(6)
C18N3C16C13-91.77(9) Li1O4Li3Li4-81.45(6)
C7O2Li1O4158.23(14) Li1O2C7C9-174.38(15)
C7O2Li1O1-104.40(17) Li1O2C7C1062.63(19)
C7O2Li1N1-8.7(2) Li1O2C7C8-54.92(19)
C7O2Li1Li2-110.10(17) Li1O1C1C282.90(8)
C7O2Li1Li3-153.49(15) Li1O1C1C4-40.27(9)
C7O2Li1Li4167.80(18) Li1O1C1C3-157.63(7)
C20C19C22N467.84(10) Li1O1Li2O25.75(6)
C24N4C22C19-89.84(9) Li1O1Li2O3-91.58(7)
C12N2C10C796.08(9) Li1O1Li2N2103.09(10)
C5N1C4C194.93(9) Li1O1Li2Li3-81.52(6)
C11N2C10C7-143.05(8) Li1O1Li2Li4-43.15(6)
C6N1C4C1-144.76(8) Li1N1C4C1-34.54(9)
C17N3C16C13148.02(8) Li4O4C19C21152.12(8)
C23N4C22C19150.19(8) Li4O4C19C2234.99(9)
Li2O2C7C980.61(8) Li4O4C19C20-88.87(8)
Li2O2C7C10-42.37(8) Li4O4Li3O190.61(7)
Li2O2C7C8-159.92(7) Li4O4Li3O3-6.06(6)
Li2O2Li1O4-91.67(7) Li4O4Li3N3-102.89(10)
Li2O2Li1O15.70(6) Li4O4Li3Li242.83(6)
Li2O2Li1N1101.40(10) Li4O4Li3Li181.45(6)
Li2O2Li1Li3-43.39(6) Li4O2C7C9-8.28(9)
Li2O2Li1Li4-82.09(6) Li4O2C7C10-131.26(7)
Li2O1C1C2-174.82(12) Li4O2C7C8111.19(8)
Li2O1C1C462.01(16) Li4O2Li1O4-9.58(6)
Li2O1C1C3-55.35(16) Li4O2Li1O187.79(7)
Li2O3C13C16129.27(8) Li4O2Li1N1-176.51(10)
Li2O3C13C155.62(10) Li4O2Li1Li282.09(6)
Li2O3C13C14-113.36(9) Li4O2Li1Li338.71(6)
Li2O3Li4O4-88.16(7) Li4O3C13C16-65.35(16)
Li2O3Li4O29.93(6) Li4O3C13C15171.00(13)
Li2O3Li4N4173.03(11) Li4O3C13C1452.01(18)
Li2O3Li4Li3-82.10(6) Li4N4C22C1938.36(8)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0321_0m.
AtomxyzU(eq)
H21A2157-57606551
H21B1258-166601251
H21C1789997649951
H22A1819-149473821
H22B901-181460221
H16A3726506466824
H16B46031034489524
H9A20534108313032
H9B13634947255532
H9C11673634294332
H2A29533325691632
H2B34934263756832
H2C38733388705832
H4A27626321706324
H4B26396792621024
H10A17107030326922
H10B17447132413922
H15A42224349424838
H15B48983316465338
H15C43983990512738
H18A52621228615547
H18B48581873672447
H18C49602729603647
H8A2704764348640
H8B3836086305640
H8C5146118395040
H20A7792519579847
H20B2731468519447
H20C6012770490747
H24A99481343945
H24B3051766303345
H24C1671899384145
H12A27855708300542
H12B36026291353142
H12C29137277308942
H3A44715287663138
H3B41796203719138
H3C39746595631338
H5A20304257721444
H5B11254482675744
H5C16235640728044
H11A29938351425342
H11B36907375468942
H11C29397505496542
H14A33271364342842
H14B42071816355042
H14C35092856324442
H6A12697144624847
H6B7436000573747
H6C13806749545347
H17A3409-209568050
H17B3943187652050
H17C4320-550595750
H23A2067165363450
H23B1418795291650
H23C1235-538329550

Experimental

Single crystals of C24H56Li4N4O4 [mo_B0321_0m] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 99.98 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 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. 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. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [mo_B0321_0m]

Crystal Data for C24H56Li4N4O4 (=492.48 g/mol): monoclinic, space group P21/n (no. 14), a = 18.0767(15) Å, b = 10.0888(9) Å, c = 18.548(2) Å, β = 108.538(4)°, = 3207.1(5) Å3, Z = 4, T = 99.98 K, μ(MoKα) = 0.066 mm-1, Dcalc = 1.020 g/cm3, 70347 reflections measured (4.686° ≤ 2Θ ≤ 56°), 7736 unique (Rint = 0.0243, Rsigma = 0.0142) which were used in all calculations. The final R1 was 0.0348 (I > 2σ(I)) and wR2 was 0.0944 (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:
C22(H22A,H22B), C16(H16A,H16B), C4(H4A,H4B), C10(H10A,H10B)
2.b Idealised Me refined as rotating group:
C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C2(H2A,H2B,H2C), C15(H15A,H15B,H15C),
C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C),
C12(H12A,H12B,H12C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C),
C14(H14A,H14B,H14C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C)

This report has been created with Olex2, compiled on 2015.09.30 svn.r3233 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.