phw1117

Table 1 Crystal data and structure refinement for phw1117
Identification code phw1117
Empirical formula C27H33N3O3
Formula weight 447.56
Temperature/K 110.00(10)
Crystal system trigonal
Space group P31c
a/Å 13.4860(5)
b/Å 13.4860(5)
c/Å 7.7069(7)
α/° 90.00
β/° 90.00
γ/° 120.00
Volume/Å3 1213.87(12)
Z 2
ρcalcmg/mm3 1.225
m/mm‑1 0.080
F(000) 480
Crystal size/mm3 0.2907 × 0.068 × 0.0524
2Θ range for data collection 6.04 to 60.78°
Index ranges -6 ≤ h ≤ 17, -19 ≤ k ≤ 15, -10 ≤ l ≤ 9
Reflections collected 2916
Independent reflections 1846[R(int) = 0.0235]
Data/restraints/parameters 1846/1/108
Goodness-of-fit on F2 1.194
Final R indexes [I>=2σ (I)] R1 = 0.0510, wR2 = 0.1450
Final R indexes [all data] R1 = 0.0697, wR2 = 0.1578
Largest diff. peak/hole / e Å-3 0.217/-0.284
Flack Parameter 0(3)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1117. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
O1-6093.5(19)-5118.4(17)-5385(3)40.4(5)
N1-5310.1(19)-6417.7(18)-4305(4)34.0(6)
C5-7132(2)-5916(2)-4734(4)35.1(7)
C4-7371(2)-7031(2)-4375(4)35.5(7)
C1-4374(2)-6579(2)-4974(4)31.3(7)
C6-7963(3)-5605(3)-4466(5)39.5(7)
C2-4453(2)-7696(2)-4393(4)31.9(6)
C7-9020(3)-6396(3)-3806(5)51.8(10)
C9-8443(2)-7808(3)-3712(6)48.3(9)
C3-6472(2)-7376(2)-4697(5)39.1(8)
C8-9269(3)-7498(3)-3405(6)54.5(10)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1117. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
O131.5(11)25(1)66.9(14)6(1)0.6(10)15.7(9)
N119.7(11)22.9(11)59.2(17)1.2(11)-0.6(10)10.5(9)
C526.0(13)23.3(13)55.2(18)-2.9(12)-7.2(13)11.7(12)
C423.2(13)23.6(13)62.4(19)-4.7(12)-6.3(12)13.8(11)
C118.6(12)18.9(12)56.1(19)0.3(11)-0.2(12)9.2(11)
C634.8(16)30.8(15)61.4(19)-8.6(14)-15.6(14)22.7(13)
C221.7(12)22.0(12)52.2(17)-0.4(12)-1.3(12)11(1)
C727.1(14)39.3(18)99(3)-10.7(17)-17.0(17)24.0(14)
C921.8(14)21.2(13)99(3)-0.7(15)-8.2(16)8.9(11)
C322.0(13)22.1(13)73(2)1.5(14)-2.3(14)11.2(11)
C819.2(14)33.2(17)107(3)-4.6(18)-7.7(16)10.1(12)

 

Table 4 Bond Lengths for phw1117.
AtomAtomLength/Å AtomAtomLength/Å
O1C51.365(3) C1C211.530(4)
N1C11.477(3) C1C21.523(4)
N1C31.481(4) C6C71.381(5)
C5C41.398(4) C2C121.530(4)
C5C61.396(4) C7C81.385(5)
C4C91.391(4) C9C81.391(4)
C4C31.521(4)    

1+Y-X,-1-X,+Z; 2-1-Y,-1+X-Y,+Z

 

Table 5 Bond Angles for phw1117.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1N1C3114.2(2) N1C1C21107.5(2)
O1C5C4121.0(3) C2C1C21111.0(3)
O1C5C6118.6(3) C7C6C5119.7(3)
C6C5C4120.4(3) C1C2C12112.6(2)
C5C4C3120.4(3) C6C7C8121.0(3)
C9C4C5118.4(3) C8C9C4121.5(3)
C9C4C3121.1(3) N1C3C4110.9(2)
N1C1C2113.6(2) C7C8C9118.9(3)

1+Y-X,-1-X,+Z; 2-1-Y,-1+X-Y,+Z

 

Table 6 Hydrogen Bonds for phw1117.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1N10.92(5)1.73(5)2.594(3)155(4)

 

Table 7 Torsion Angles for phw1117.
ABCDAngle/˚
O1C5C4C9179.9(3)
O1C5C4C30.2(4)
O1C5C6C7-179.9(3)
N1C1C2C11-175.1(2)
C5C4C9C80.0(5)
C5C4C3N135.8(4)
C5C6C7C8-0.1(5)
C4C5C6C71.4(5)
C4C9C8C71.3(6)
C1N1C3C4-166.0(3)
C6C5C4C9-1.4(5)
C6C5C4C3178.9(3)
C6C7C8C9-1.3(6)
C22C1C2C11-53.8(4)
C9C4C3N1-143.9(3)
C3N1C1C22-177.5(3)
C3N1C1C2-54.3(3)
C3C4C9C8179.7(4)

1-1-Y,-1+X-Y,+Z; 2+Y-X,-1-X,+Z

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1117.
AtomxyzU(eq)
H1B-4402-6577-624538
H6-7807-4867-473147
H2A-5145-8333-486638
H2B-4508-7746-313838
H7-9572-6185-362862
H9-8612-8551-346758
H3A-6633-8028-397447
H3B-6507-7603-590047
H8-9976-8022-293965
H1A-5280(20)-6330(20)-3040(40)20(7)
H1-5630(40)-5380(40)-4960(50)65(13)

[RSC Journal Format]

Experimental

Single crystals of C27H33N3O3 [phw1117] were []. A suitable crystal was selected and on a Oxford Diffraction SuperNova 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 [phw1117]

Crystal Data. C27H33N3O3, =447.56, trigonal, a = 13.4860(5) Å, c = 7.7069(7) Å, = 1213.87(12) Å3, T = 110.00(10), space group P31c (no. 159), Z = 2, μ(Mo Kα) = 0.080, 2916 reflections measured, 1846 unique (Rint = 0.0235) which were used in all calculations. The final wR(F2) was 0.1578 (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.