phw1115

Table 1 Crystal data and structure refinement for phw1115
Identification code phw1115
Empirical formula C27H30Cl3N3O3
Formula weight 550.89
Temperature/K 110.00(10)
Crystal system trigonal
Space group P31c
a/Å 13.8281(3)
b/Å 13.8281(3)
c/Å 8.2311(2)
α/° 90.00
β/° 90.00
γ/° 120.00
Volume/Å3 1363.07(6)
Z 2
ρcalcmg/mm3 1.342
m/mm‑1 0.370
F(000) 576
Crystal size/mm3 0.3051 × 0.1453 × 0.116
2Θ range for data collection 5.9 to 64.54°
Index ranges -19 ≤ h ≤ 20, -20 ≤ k ≤ 20, -12 ≤ l ≤ 12
Reflections collected 8234
Independent reflections 2940[R(int) = 0.0270]
Data/restraints/parameters 2940/1/117
Goodness-of-fit on F2 1.111
Final R indexes [I>=2σ (I)] R1 = 0.0404, wR2 = 0.1014
Final R indexes [all data] R1 = 0.0463, wR2 = 0.1057
Largest diff. peak/hole / e Å-3 0.324/-0.241
Flack Parameter 0.02(7)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1115. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C14301.7(14)13113.2(14)2162.2(19)24.1(3)
C24678.6(16)12364.0(15)2439(2)30.9(4)
C34004.2(17)11366.8(15)3264(2)33.7(4)
C42961.3(17)11131.0(14)3769(2)31.7(4)
C52559.5(15)11859.4(14)3480(2)28.4(3)
C63232.8(14)12863.0(13)2677.9(19)23.7(3)
C72830.1(13)13675.3(14)2348(2)25.7(3)
C83501.1(12)15700.4(12)2060.6(17)20.7(3)
C92375.2(12)15541.4(12)2612(2)22.6(3)
Cl12137.5(5)9920.5(4)4896.4(8)47.85(16)
N13729.3(11)14832.8(11)2668.1(18)22.2(3)
O14981.7(10)14094.3(11)1378.3(16)28.4(2)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1115. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
C125.3(7)23.4(7)25.3(7)-5.6(6)-4.3(6)13.3(6)
C230.7(8)29.3(8)39.2(9)-11.4(7)-7.5(7)19.9(7)
C347.9(10)29.3(8)32.9(9)-9.2(7)-10.2(8)26.0(8)
C443.8(10)19.4(7)29.6(8)-3.4(6)-6.1(7)13.9(7)
C530.4(8)23.2(7)29.5(7)-4.5(6)-2.4(7)11.9(6)
C624.2(7)20.2(7)26.6(7)-4.9(5)-4.8(6)11.0(6)
C720.1(7)19.9(7)36.5(8)-2.1(6)-5.1(6)9.5(6)
C820.5(6)19.4(6)22.7(7)-0.7(5)-0.8(5)10.4(6)
C919.8(6)20.6(7)27.5(7)0.4(6)-0.6(5)10.2(6)
Cl168.0(4)24.6(2)44.5(3)5.3(2)0.6(3)18.3(2)
N122.3(6)20.0(6)25.0(6)-1.7(5)-2.9(5)11.1(5)
O124.9(6)27.9(6)34.0(6)-1.8(5)1.9(5)14.3(5)

 

Table 4 Bond Lengths for phw1115.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.392(2) C5C61.392(2)
C1C61.405(2) C6C71.507(2)
C1O11.366(2) C7N11.479(2)
C2C31.395(3) C8C91.528(2)
C3C41.374(3) C8C911.530(2)
C4C51.393(2) C8N11.4723(19)
C4Cl11.7477(18) C9C821.530(2)

12-Y,3+X-Y,+Z; 2-1+Y-X,2-X,+Z

 

Table 5 Bond Angles for phw1115.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2C1C6120.45(16) C1C6C7119.83(15)
O1C1C2119.26(16) C5C6C1119.07(15)
O1C1C6120.29(14) C5C6C7121.10(16)
C1C2C3120.10(18) N1C7C6110.52(13)
C4C3C2119.03(16) C9C8C91110.91(14)
C3C4C5121.85(17) N1C8C9113.57(12)
C3C4Cl1119.47(14) N1C8C91107.80(12)
C5C4Cl1118.60(15) C8C9C82112.26(14)
C6C5C4119.50(17) C8N1C7114.49(13)

12-Y,3+X-Y,+Z; 2-1+Y-X,2-X,+Z

 

Table 6 Hydrogen Bonds for phw1115.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1AN10.78(3)1.91(3)2.6340(19)154(3)

 

Table 7 Torsion Angles for phw1115.
ABCDAngle/˚
C1C2C3C41.1(2)
C1C6C7N1-42.5(2)
C2C1C6C50.5(2)
C2C1C6C7-179.13(15)
C2C3C4C50.0(3)
C2C3C4Cl1-176.62(14)
C3C4C5C6-0.9(3)
C4C5C6C10.6(2)
C4C5C6C7-179.78(15)
C5C6C7N1137.89(16)
C6C1C2C3-1.3(2)
C6C7N1C8167.77(13)
C91C8C9C8254.4(2)
C91C8N1C7175.32(13)
C9C8N1C752.02(17)
Cl1C4C5C6175.78(13)
N1C8C9C82175.99(11)
O1C1C2C3178.85(15)
O1C1C6C5-179.73(14)
O1C1C6C70.7(2)

12-Y,3+X-Y,+Z; 2-1+Y-X,2-X,+Z

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1115.
AtomxyzU(eq)
H2539612532206737
H3426210858347340
H5183111673382834
H7A258813607120131
H7B218013495305031
H835041568084625
H9A233115489381227
H9B176914830216627
H13862(16)14918(15)3590(20)11(4)
H1A4760(20)14490(20)1630(30)32(6)

[RSC Journal Format]

Experimental

Single crystals of C27H30Cl3N3O3 [phw1115] were []. A suitable crystal was selected and 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 [phw1115]

Crystal Data. C27H30Cl3N3O3, =550.89, trigonal, a = 13.8281(3) Å, c = 8.2311(2) Å, = 1363.07(6) Å3, T = 110.00(10), space group P31c (no. 159), Z = 2, μ(Mo Kα) = 0.370, 8234 reflections measured, 2940 unique (Rint = 0.0270) which were used in all calculations. The final wR(F2) was 0.1057 (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.