mo_B0314_0m

Table 1 Crystal data and structure refinement for mo_B0314_0m.
Identification code mo_B0314_0m
Empirical formula C34H76Li5N3O8
Formula weight 689.67
Temperature/K 99.98
Crystal system monoclinic
Space group P21/c
a/Å 13.137(6)
b/Å 17.220(8)
c/Å 19.039(9)
α/° 90
β/° 96.585(12)
γ/° 90
Volume/Å3 4279(4)
Z 4
ρcalcg/cm3 1.071
μ/mm‑1 0.072
F(000) 1520.0
Crystal size/mm3 0.414 × 0.22 × 0.14
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.914 to 51.998
Index ranges -16 ≤ h ≤ 16, -21 ≤ k ≤ 20, -23 ≤ l ≤ 21
Reflections collected 41663
Independent reflections 8397 [Rint = 0.0417, Rsigma = 0.0388]
Data/restraints/parameters 8397/0/521
Goodness-of-fit on F2 1.031
Final R indexes [I>=2σ (I)] R1 = 0.0449, wR2 = 0.1106
Final R indexes [all data] R1 = 0.0629, wR2 = 0.1212
Largest diff. peak/hole / e Å-3 0.34/-0.29

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0314_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O37273.7(7)7560.4(6)2977.8(5)18.1(2)
O85010.1(7)6454.1(6)2550.2(5)18.7(2)
O55338.3(8)5635.5(6)4209.3(6)23.5(2)
O63216.9(8)7791.9(6)1941.9(6)22.7(2)
O29020.5(9)6137.6(6)3184.8(6)28.9(3)
O71209.6(8)5265.3(7)749.2(6)30.4(3)
O46614.2(8)8693.7(6)4436.5(6)25.6(2)
O111393.5(8)8842.1(7)3388.8(6)31.2(3)
N33548.4(9)6377.4(7)1300.3(6)19.4(3)
N25639.1(9)7254.0(7)3989.3(6)18.9(3)
N19319.2(9)7580.5(7)2577.6(7)19.9(3)
C325116.4(11)5873.3(8)2046.8(8)20.0(3)
C78395.9(11)7779.1(9)2088.7(8)20.0(3)
C107801.3(12)8876.6(8)2842.9(8)22.1(3)
C314649.6(11)6168.4(9)1323.0(8)20.4(3)
C282890.6(11)5747.6(9)983.2(8)21.7(3)
C263665.7(12)7813.3(9)1295.5(8)22.8(3)
C344592.0(12)5128.0(9)2256.6(8)23.6(3)
C87516.8(11)8103.7(8)2473.7(8)18.0(3)
C185698.8(13)6900.1(9)4681.0(8)23.1(3)
C253320.2(12)7093.1(9)885.5(8)21.9(3)
C291818.7(12)5775.1(9)1203.7(8)23.7(3)
C110071.6(11)8221.0(9)2646.6(8)23.0(3)
C196081.9(12)6075.9(9)4655.1(8)24.0(3)
C205629.3(14)4843.7(9)4173.8(9)29.8(4)
C155097.8(12)7992.3(9)3985.5(9)24.6(3)
C273297.5(13)8514.1(9)2307.8(9)27.8(4)
C96600.8(11)8232.0(9)1914.9(8)23.7(3)
C49831.7(12)6873.8(9)2353.6(9)26.0(4)
C336252.1(12)5703.7(10)2001.1(9)28.3(4)
C210662.6(11)8231.7(9)3372.8(8)24.4(3)
C165556.9(13)8582.0(9)4521.1(9)28.6(4)
C68740.9(14)5393.1(10)3416.6(11)37.7(4)
C59252.5(13)6136.6(9)2476.7(9)29.1(4)
C177164.8(15)9049.3(10)5037.2(9)33.7(4)
C212917.1(13)6624.1(11)3390.8(10)30.9(4)
C118630.3(12)7451.3(11)4569.4(9)28.3(4)
C30203.4(13)5192.5(12)938.2(10)39.2(4)
C129548.6(13)6917(1)4758.0(9)28.2(4)
C1310222.7(13)7073.5(12)5448.0(9)37.1(4)
C312018.2(13)8864.2(12)4045.4(10)38.5(4)
C241612.0(16)4793.4(12)4113.1(12)48.6(5)
C1411109.3(15)6513.0(13)5602.3(12)50.7(6)
C222086.6(19)6033.1(15)3489.0(12)22.9(7)
C232484.9(18)5358.6(15)3946.5(14)27.2(7)
Li53584.0(19)6761.2(14)2407.5(14)22.5(5)
Li44602.3(19)6386.3(15)3497.2(13)23.4(5)
Li18544.8(19)7177.8(15)3456.8(14)23.9(5)
Li27145.1(19)7745.3(15)3977.2(13)23.7(5)
Li36054.1(19)7042.9(15)3023.5(13)21.9(5)
C22A2619(7)5732(5)3617(5)42(2)
C23A1741(7)5616(5)3970(6)68(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0314_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
O319.3(5)16.8(5)18.7(5)0.9(4)3.7(4)-0.6(4)
O821.6(5)15.9(5)18.5(5)-3.5(4)2.4(4)-0.6(4)
O530.6(6)15.3(5)24.0(6)0.9(4)0.4(4)0.9(4)
O628.8(6)13.6(5)25.8(6)-0.4(4)4.2(4)-1.1(4)
O234.1(6)15.5(5)37.6(7)1.6(5)6.7(5)1.8(5)
O728.1(6)34.8(7)28.4(6)-9.3(5)3.5(5)-13.1(5)
O433.6(6)21.5(6)22.8(6)-6.3(5)7.2(5)-4.6(5)
O124.4(6)36.0(7)33.3(6)-7.8(5)3.9(5)-9.8(5)
N322.3(6)14.8(6)20.3(6)0.9(5)-1.2(5)-2.5(5)
N222.8(6)14.9(6)19.5(6)-0.1(5)4.7(5)1.5(5)
N117.5(6)17.8(6)24.5(7)-2.8(5)3.3(5)0.6(5)
C3222.7(7)17.2(7)20.3(7)-3.3(6)2.7(6)0.6(6)
C722.8(7)19.7(8)17.9(7)-0.9(6)3.8(6)-0.7(6)
C1024.0(7)17.0(8)25.7(8)-0.5(6)5.3(6)0.8(6)
C3124.0(7)16.9(7)20.6(8)-3.0(6)4.1(6)-1.4(6)
C2827.0(8)16.9(8)20.0(8)-1.0(6)-2.2(6)-2.6(6)
C2625.8(8)17.9(8)24.5(8)3.0(6)2.2(6)-1.8(6)
C3431.7(8)15.4(8)23.0(8)0.4(6)-0.2(6)1.5(6)
C819.3(7)16.0(7)19.0(7)0.7(6)3.5(6)0.1(6)
C1828.7(8)23.2(8)17.9(8)-1.6(6)5.1(6)-3.2(6)
C2526.5(8)18.6(8)19.9(8)3.8(6)-0.9(6)-1.9(6)
C2928.4(8)18.1(8)23.6(8)-2.0(6)-0.7(6)-4.5(6)
C119.2(7)23.3(8)27.2(8)0.8(7)6.0(6)-2.3(6)
C1926.9(8)24.8(8)19.8(8)3.6(7)-0.1(6)-0.6(6)
C2041.8(10)18.0(8)30.1(9)3.9(7)6.5(7)3.9(7)
C1524.5(8)20.7(8)29.3(9)-0.6(7)6.9(7)2.5(6)
C2734.2(9)16.4(8)32.3(9)-4.4(7)2.0(7)0.0(6)
C923.1(7)24.1(8)23.7(8)2.5(7)1.8(6)0.0(6)
C425.0(8)23.7(8)30.1(9)-3.8(7)6.2(7)5.6(6)
C3326.2(8)28.8(9)29.9(9)-5.5(7)3.3(7)4.2(7)
C219.2(7)25.7(8)28.5(8)-3.1(7)3.8(6)-0.6(6)
C1635.2(9)20.3(8)32.8(9)-3.6(7)14.2(7)2.3(7)
C637.4(10)21.1(9)52.0(12)9.1(8)-5.9(8)-3.0(7)
C533.5(9)20.5(8)33.0(9)-5.6(7)3.0(7)6.0(7)
C1750.8(11)24.2(9)25.4(9)-6.5(7)2.2(8)-6.3(8)
C2127.5(8)33.6(10)32.6(10)8.3(8)7.4(7)-2.2(7)
C1125.7(8)36.2(10)23.0(8)0.0(7)2.3(7)-0.9(7)
C3031.9(9)47.4(11)39(1)-9.7(9)6.9(8)-16.1(8)
C1228.1(8)29.6(9)25.5(9)5.4(7)-2.8(7)-5.1(7)
C1329.3(9)54.1(12)26.6(9)3.4(8)-3.2(7)-6.8(8)
C327.3(9)49.7(12)37.5(10)-15.5(9)-0.3(8)-3.1(8)
C2450.9(12)38.8(11)54.1(13)15.4(10)-2.9(10)-13.6(9)
C1442.4(11)50.3(13)53.6(13)20.0(11)-19.5(10)-9.0(9)
C2221.2(12)24.0(13)23.6(12)2.5(10)2.8(9)3(1)
C2325.3(14)24.9(14)31.4(13)6.3(11)3.6(10)-0.6(10)
Li522.6(12)17.0(12)27.9(14)0.9(11)2.9(10)0(1)
Li426.2(13)20.7(13)23.4(13)2.0(11)3.6(10)-0.9(10)
Li124.7(13)23.1(13)23.9(13)0.9(11)3.1(10)3.7(10)
Li225.3(13)24.4(13)21.6(13)-4.3(11)3.1(10)-1.2(10)
Li322.7(12)21.6(13)21.6(13)-1.8(10)3.2(10)-2.7(10)
C22A39(5)27(4)64(6)12(4)21(4)11(4)
C23A45(5)60(6)109(8)48(6)45(5)16(4)

 

Table 4 Bond Lengths for mo_B0314_0m.
AtomAtomLength/Å AtomAtomLength/Å
O3C81.4030(18) N1C71.482(2)
O3Li11.925(3) N1C11.4767(19)
O3Li21.956(3) N1C41.4771(19)
O3Li31.844(3) N1Li12.170(3)
O8C321.4033(18) C32C311.529(2)
O8Li51.936(3) C32C341.531(2)
O8Li41.942(3) C32C331.532(2)
O8Li31.854(3) C7C81.542(2)
O5C191.4352(19) C10C81.531(2)
O5C201.4197(19) C28C291.516(2)
O5Li42.036(3) C26C251.507(2)
O6C261.4248(19) C8C91.528(2)
O6C271.4235(19) C18C191.509(2)
O6Li52.018(3) C1C21.506(2)
O2C61.418(2) C15C161.514(2)
O2C51.416(2) C4C51.512(2)
O2Li11.985(3) C21C221.519(3)
O7C291.4145(19) C21Li52.169(3)
O7C301.415(2) C21Li42.238(3)
O4C161.429(2) C21C22A1.654(9)
O4C171.420(2) C11C121.527(2)
O4Li22.014(3) C11Li12.160(3)
O1C21.4217(19) C11Li22.198(3)
O1C31.415(2) C12C131.522(2)
N3C311.487(2) C13C141.515(3)
N3C281.4723(19) C24C231.564(3)
N3C251.4758(19) C24C23A1.455(9)
N3Li52.204(3) C22C231.509(4)
N2C181.445(2) Li5Li42.424(4)
N2C151.456(2) Li4Li32.475(4)
N2Li42.162(3) Li1Li22.395(4)
N2Li22.154(3) Li2Li32.493(4)
N2Li32.010(3) C22AC23A1.414(12)

 

Table 5 Bond Angles for mo_B0314_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C8O3Li1107.41(11) C22C21Li5123.10(15)
C8O3Li2127.50(12) C22C21Li4125.69(17)
C8O3Li3128.44(12) Li5C21Li466.71(11)
Li1O3Li276.22(11) C22AC21Li5117.2(3)
Li3O3Li1121.57(13) C22AC21Li493.9(4)
Li3O3Li281.97(11) C12C11Li192.87(12)
C32O8Li5105.63(11) C12C11Li2152.93(14)
C32O8Li4130.60(12) Li1C11Li266.67(11)
C32O8Li3126.56(12) C13C12C11117.53(15)
Li5O8Li477.36(11) C14C13C12114.39(17)
Li3O8Li5124.68(12) C23C22C21112.3(2)
Li3O8Li481.32(12) C22C23C24112.47(19)
C19O5Li4107.30(11) O8Li5O6118.73(13)
C20O5C19111.52(12) O8Li5N388.07(11)
C20O5Li4133.49(12) O8Li5C21109.23(13)
C26O6Li5107.49(11) O8Li5Li451.44(9)
C27O6C26112.65(12) O6Li5N382.29(10)
C27O6Li5123.57(12) O6Li5C21112.03(13)
C6O2Li1129.35(14) O6Li5Li4133.72(14)
C5O2C6112.76(13) N3Li5Li4133.46(13)
C5O2Li1110.98(12) C21Li5N3145.72(14)
C29O7C30112.27(13) C21Li5Li458.00(10)
C16O4Li2109.22(11) O8Li4O5119.73(13)
C17O4C16112.28(12) O8Li4N297.68(12)
C17O4Li2121.97(13) O8Li4C21106.28(13)
C3O1C2111.14(13) O8Li4Li551.19(9)
C31N3Li597.52(10) O8Li4Li347.79(8)
C28N3C31110.91(12) O5Li4N285.57(11)
C28N3C25108.78(12) O5Li4C21124.46(13)
C28N3Li5124.06(11) O5Li4Li5155.87(15)
C25N3C31110.79(11) O5Li4Li3101.88(12)
C25N3Li5104.02(11) N2Li4C21118.71(13)
C18N2C15110.37(12) N2Li4Li5116.45(13)
C18N2Li493.96(11) N2Li4Li350.84(9)
C18N2Li2102.79(12) C21Li4Li555.29(10)
C18N2Li3139.94(12) C21Li4Li3132.79(14)
C15N2Li4108.56(12) Li5Li4Li386.51(12)
C15N2Li296.06(12) O3Li1O2117.85(14)
C15N2Li3109.68(12) O3Li1N189.03(11)
Li2N2Li4143.19(11) O3Li1C11109.55(13)
Li3N2Li472.66(11) O3Li1Li252.47(9)
Li3N2Li273.47(11) O2Li1N184.13(11)
C7N1Li197.81(11) O2Li1C11118.03(14)
C1N1C7112.02(12) O2Li1Li2139.08(15)
C1N1C4108.57(12) N1Li1Li2129.71(14)
C1N1Li1122.57(12) C11Li1N1135.27(14)
C4N1C7112.10(12) C11Li1Li257.41(10)
C4N1Li1103.23(12) O3Li2O4128.84(14)
O8C32C31108.51(12) O3Li2N297.37(12)
O8C32C34109.65(12) O3Li2C11106.92(12)
O8C32C33110.39(12) O3Li2Li151.31(9)
C31C32C34111.57(12) O3Li2Li347.08(9)
C31C32C33107.73(12) O4Li2N287.11(11)
C34C32C33108.98(13) O4Li2C11107.18(13)
N1C7C8112.88(12) O4Li2Li1146.19(15)
N3C31C32113.26(12) O4Li2Li3120.71(13)
N3C28C29112.56(12) N2Li2C11131.80(14)
O6C26C25107.23(12) N2Li2Li1126.43(14)
O3C8C7108.97(12) N2Li2Li350.61(9)
O3C8C10109.17(12) C11Li2Li155.92(10)
O3C8C9110.48(12) C11Li2Li3131.62(14)
C10C8C7112.12(12) Li1Li2Li384.57(12)
C9C8C7107.11(12) O3Li3O8147.09(15)
C9C8C10108.97(12) O3Li3N2106.50(13)
N2C18C19110.51(13) O3Li3Li4161.46(15)
N3C25C26112.29(12) O3Li3Li250.95(9)
O7C29C28106.82(12) O8Li3N2106.28(13)
N1C1C2111.10(12) O8Li3Li450.89(9)
O5C19C18108.02(13) O8Li3Li2161.91(15)
N2C15C16115.18(14) N2Li3Li456.50(9)
N1C4C5113.13(13) N2Li3Li255.92(9)
O1C2C1107.73(13) Li4Li3Li2111.04(13)
O4C16C15109.35(12) C23AC22AC21119.0(7)
O2C5C4108.28(13) C22AC23AC24110.3(7)

 

Table 6 Torsion Angles for mo_B0314_0m.
ABCDAngle/˚ ABCDAngle/˚
O8C32C31N3-58.83(15) Li5O8Li3Li265.7(5)
O6C26C25N3-54.16(16) Li5O6C26C2553.44(15)
N3C28C29O7166.97(12) Li5N3C31C3231.58(14)
N2C18C19O5-64.27(16) Li5N3C28C2941.78(18)
N2C15C16O453.89(18) Li5N3C25C2626.16(15)
N1C7C8O3-56.90(15) Li5C21C22C23107.0(2)
N1C7C8C1064.07(16) Li5C21C22AC23A-144.9(8)
N1C7C8C9-176.44(12) Li4O8C32C31136.81(14)
N1C1C2O1177.83(11) Li4O8C32C3414.73(19)
N1C4C5O2-50.61(17) Li4O8C32C33-105.35(16)
C32O8Li3O338.2(3) Li4O8Li3O3173.1(3)
C32O8Li3N2-146.83(12) Li4O8Li3N2-11.89(13)
C32O8Li3Li4-134.94(15) Li4O8Li3Li2-2.2(5)
C32O8Li3Li2-137.2(4) Li4O5C19C1827.88(15)
C7N1C1C2148.51(12) Li4N2C18C1958.18(14)
C7N1C4C5-73.15(17) Li4N2C15C16159.26(13)
C31N3C28C29157.08(12) Li4C21C22C2323.5(3)
C31N3C25C26-77.67(15) Li4C21C22AC23A149.3(9)
C28N3C31C32-99.36(14) Li1O3C8C743.69(15)
C28N3C25C26160.15(12) Li1O3C8C10-79.06(14)
C34C32C31N362.07(16) Li1O3C8C9161.12(12)
C8O3Li3O849.6(3) Li1O3Li3O8-109.8(3)
C8O3Li3N2-125.43(14) Li1O3Li3N275.20(17)
C8O3Li3Li4-147.5(4) Li1O3Li3Li453.2(5)
C8O3Li3Li2-132.30(15) Li1O3Li3Li268.34(14)
C18N2C15C1657.58(17) Li1O2C5C442.82(17)
C25N3C31C32139.72(13) Li1N1C7C835.11(14)
C25N3C28C29-80.82(15) Li1N1C1C232.90(18)
C1N1C7C8-94.79(14) Li1N1C4C531.09(16)
C1N1C4C5162.57(13) Li1C11C12C13158.07(15)
C20O5C19C18-178.28(12) Li2O3C8C7129.44(14)
C15N2C18C19169.65(13) Li2O3C8C106.69(18)
C27O6C26C25-167.12(12) Li2O3C8C9-113.13(15)
C4N1C7C8142.87(12) Li2O3Li3O8-178.1(3)
C4N1C1C2-87.17(15) Li2O3Li3N26.86(13)
C33C32C31N3-178.35(12) Li2O3Li3Li4-15.2(5)
C6O2C5C4-163.36(13) Li2O4C16C15-24.00(17)
C17O4C16C15-162.47(13) Li2N2C18C19-88.82(14)
C21C22C23C24174.08(18) Li2N2C15C16-48.50(15)
C21C22AC23AC24179.4(6) Li2C11C12C13-162.6(3)
C11C12C13C14179.27(16) Li3O3C8C7-117.96(15)
C30O7C29C28175.33(14) Li3O3C8C10119.28(15)
C3O1C2C1-176.94(13) Li3O3C8C9-0.54(19)
Li5O8C32C3150.21(14) Li3O8C32C31-110.36(15)
Li5O8C32C34-71.86(14) Li3O8C32C34127.57(14)
Li5O8C32C33168.06(13) Li3O8C32C337.49(19)
Li5O8Li3O3-118.9(3) Li3N2C18C19-9.4(2)
Li5O8Li3N256.10(18) Li3N2C15C16-123.08(14)
Li5O8Li3Li467.99(14)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0314_0m.
AtomxyzU(eq)
H7A81537308182224
H7B85838169174424
H10A72129075306033
H10B79959253249533
H10C83798797321033
H31A50376631119524
H31B4724576296524
H28A32085242112626
H28B2847578546226
H26A44227823139227
H26B34398284102227
H34A49384936270735
H34B46304734188935
H34C38725237230835
H25A2573712574226
H25B3666706945126
H29A18275607170228
H29B15426310115828
H1A97108722255828
H1B105548159228728
H19A67516065446329
H19B61745851513729
H20A62684805395645
H20B50884554388945
H20C57334626465245
H27A40208665239842
H27B30108462275842
H27C29188913201942
H9A64037737168436
H9B67888603156136
H9C60248438214136
H4A105266841261631
H4B99116916184431
H33A65936178186642
H33B63145300164642
H33C65755525246242
H2A101928321373529
H2B110147728347229
H16A51859081445134
H16B54918395500634
H6A81715190309257
H6B85315434389357
H6C93285041342657
H5A86136113214835
H5B96765678239235
H17A68089522515751
H17B78569182493151
H17C72108689543851
H30A-191483960859
H30B-127570391859
H30C2324985141959
H13A105007607543445
H13B97927050584245
H3A125189286404158
H3B123808369412458
H3C115898953442658
H24A19074367441073
H24B11165076436373
H24C12664583367073
H24D10024720435873
H24E15304505366673
H24F22174601441273
H14A115796569524176
H14B108475980559776
H14C114756628606976
H22A15286292370827
H22B17965835302027
H23A28415560439633
H23B29915067370333
H15A4369(14)7930(10)4073(9)29(5)
H21A3160(16)6812(12)3898(12)52(6)
H21B2528(19)7085(15)3158(13)72(7)
H18A6173(12)7160(9)5050(9)21(4)
H15B5069(12)8226(10)3504(9)25(4)
H18B5008(12)6895(9)4876(8)20(4)
H12A10055(15)6918(11)4394(10)37(5)
H12B9307(14)6349(12)4784(10)39(5)
H11A8193(15)7393(11)4947(10)38(5)
H11B8896(15)8019(12)4632(11)48(6)
H22C25355415318051
H22D32155519392251
H23C11285813367382
H23D18155909442082

 

Table 8 Atomic Occupancy for mo_B0314_0m.
AtomOccupancy AtomOccupancy AtomOccupancy
H24A0.732(5) H24B0.732(5) H24C0.732(5)
H24D0.268(5) H24E0.268(5) H24F0.268(5)
C220.732(5) H22A0.732(5) H22B0.732(5)
C230.732(5) H23A0.732(5) H23B0.732(5)
C22A0.268(5) H22C0.268(5) H22D0.268(5)
C23A0.268(5) H23C0.268(5) H23D0.268(5)

Experimental

Single crystals of C34H76Li5N3O8 [mo_B0314_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_B0314_0m]

Crystal Data for C34H76Li5N3O8 (=689.67 g/mol): monoclinic, space group P21/c (no. 14), a = 13.137(6) Å, b = 17.220(8) Å, c = 19.039(9) Å, β = 96.585(12)°, = 4279(4) Å3, Z = 4, T = 99.98 K, μ(MoKα) = 0.072 mm-1, Dcalc = 1.071 g/cm3, 41663 reflections measured (4.914° ≤ 2Θ ≤ 51.998°), 8397 unique (Rint = 0.0417, Rsigma = 0.0388) which were used in all calculations. The final R1 was 0.0449 (I > 2σ(I)) and wR2 was 0.1212 (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, All C(H,H,H,H,H,H) groups
2. Others
Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C22A)=Sof(H22C)=Sof(H22D)=Sof(C23A)=
Sof(H23C)=Sof(H23D)=1-FVAR(1)
Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=
Sof(H23B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C7(H7A,H7B), C31(H31A,H31B), C28(H28A,H28B), C26(H26A,H26B), C25(H25A,H25B),
C29(H29A,H29B), C1(H1A,H1B), C19(H19A,H19B), C4(H4A,H4B), C2(H2A,H2B),
C16(H16A,H16B), C5(H5A,H5B), C13(H13A,H13B), C22(H22A,H22B), C23(H23A,H23B),
C22A(H22C,H22D), C23A(H23C,H23D)
3.b Me refined with riding coordinates:
C24(H24A,H24B,H24C), C24(H24D,H24E,H24F)
3.c Idealised Me refined as rotating group:
C10(H10A,H10B,H10C), C34(H34A,H34B,H34C), C20(H20A,H20B,H20C), C27(H27A,H27B,
H27C), C9(H9A,H9B,H9C), C33(H33A,H33B,H33C), C6(H6A,H6B,H6C), C17(H17A,H17B,
H17C), C30(H30A,H30B,H30C), C3(H3A,H3B,H3C), C14(H14A,H14B,H14C)

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