phw1118

Table 1 Crystal data and structure refinement for phw1118
Identification code phw1118
Empirical formula C30H39N3O3
Formula weight 489.64
Temperature/K 110.00(10)
Crystal system trigonal
Space group P31c
a/Å 14.2781(7)
b/Å 14.2781(7)
c/Å 7.8801(4)
α/° 90.00
β/° 90.00
γ/° 120.00
Volume/Å3 1391.26(12)
Z 2
ρcalcmg/mm3 1.169
m/mm‑1 0.076
F(000) 528
Crystal size/mm3 0.3155 × 0.1659 × 0.1467
2Θ range for data collection 5.7 to 64.32°
Index ranges -18 ≤ h ≤ 8, -20 ≤ k ≤ 19, -11 ≤ l ≤ 9
Reflections collected 4801
Independent reflections 2325[R(int) = 0.0314]
Data/restraints/parameters 2325/1/118
Goodness-of-fit on F2 1.089
Final R indexes [I>=2σ (I)] R1 = 0.0622, wR2 = 0.1793
Final R indexes [all data] R1 = 0.0739, wR2 = 0.1929
Largest diff. peak/hole / e Å-3 0.405/-0.208
Flack Parameter -1(2)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1118. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C13525.6(18)-2224.2(19)4892(3)29.5(5)
C24433.1(18)-2426.0(18)5456(3)30.7(5)
C32922(2)-887(2)5216(4)36.6(5)
C43308(2)294(2)5512(3)31.7(5)
C54358.5(19)1085(2)5040(3)32.4(5)
C64690(2)2177(2)5271(4)39.2(6)
C73987(3)2479(2)5955(4)43.5(6)
C82952(3)1720(2)6439(4)44.0(6)
C92626(2)625(2)6213(4)38.7(6)
C102184(4)2040(4)7212(6)69.1(10)
N13780.8(17)-1147.2(17)5522(3)31.2(4)
O15059.3(15)804.3(16)4337(3)38.3(4)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1118. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
C127.9(10)26.4(10)34.7(12)1.2(9)-1.5(8)14.0(9)
C226.5(10)27.1(10)38.3(12)0.6(9)0.3(9)13.3(8)
C329.4(11)29.4(12)50.3(15)-0.7(10)-6.3(10)14.1(9)
C429.9(10)29.6(11)36.8(13)0.8(9)-6.0(8)15.8(9)
C532.3(12)33.8(12)31.5(12)2.9(9)-3.0(9)16.9(9)
C641.2(13)30.3(12)40.9(13)6.2(10)-4.3(10)14.0(11)
C758.2(17)33.1(12)44.0(15)2.8(10)-10.1(12)26.5(12)
C855.5(17)46.1(15)45.0(15)6.5(11)-1.7(12)36.2(13)
C932.2(12)39.8(13)49.0(15)4.7(11)0.8(10)21.6(11)
C1081(3)71(3)84(2)7.4(19)11(2)60(2)
N129.2(10)26.7(9)38.7(11)0.0(7)-3.4(8)14.6(8)
O131.9(9)35.9(10)44.0(11)4.9(7)3.9(7)14.7(8)

 

Table 4 Bond Lengths for phw1118.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.527(3) C4C91.392(4)
C1C211.524(3) C5C61.397(4)
C1N11.478(3) C5O11.367(3)
C2C121.524(3) C6C71.385(4)
C3C41.508(4) C7C81.380(4)
C3N11.468(3) C8C91.402(4)
C4C51.403(3) C8C101.511(5)

1-Y,-1+X-Y,+Z; 21+Y-X,-X,+Z

 

Table 5 Bond Angles for phw1118.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C21C1C2111.1(2) O1C5C4121.1(2)
N1C1C2107.90(18) O1C5C6119.4(2)
N1C1C21114.08(19) C7C6C5120.3(2)
C12C2C1112.6(2) C8C7C6121.5(3)
N1C3C4111.9(2) C7C8C9117.9(3)
C5C4C3120.3(2) C7C8C10121.9(3)
C9C4C3120.9(2) C9C8C10120.2(3)
C9C4C5118.7(2) C4C9C8122.0(3)
C6C5C4119.5(2) C3N1C1113.94(19)

1-Y,-1+X-Y,+Z; 21+Y-X,-X,+Z

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1118.
AtomxyzU(eq)
H13529-2201362335
H2A5127-1853498237
H2B4490-2379670937
H3A2305-1328598044
H3B2664-1076403244
H654022715495747
H742233226609452
H9191792654846
H10A145315696771104
H10B242027936918104
H10C218119678449104
H1A3860(30)-1110(30)6630(50)36(8)
H1B4690(40)30(40)4480(60)78(14)

[RSC Journal Format]

Experimental

Single crystals of C30H39N3O3 [phw1118] were [DMSO/H2O]. A suitable crystal was selected and oil on loop on a SuperNova, Single source at offset), Eos diffractometer. The crystal was kept at 110.00(10) K during data collection. Using Olex2 [1], the structure was solved with the XS [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.

  1. O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341.
  2. XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
  3. XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122

Crystal structure determination of [phw1118]

Crystal Data. C30H39N3O3, =489.64, trigonal, a = 14.2781(7) Å, c = 7.8801(4) Å, = 1391.26(12) Å3, T = 110.00(10), space group P31c (no. 159), Z = 2, μ(Mo Kα) = 0.076, 4801 reflections measured, 2325 unique (Rint = 0.0314) which were used in all calculations. The final wR(F2) was 0.1929 (all data).

This report has been created with Olex2, compiled on 2011.09.07 svn.r1971. Please let us know if there are any errors or if you would like to have additional featrues.