phw1308

Table 1 Crystal data and structure refinement for phw1308
Identification code phw1308
Empirical formula C30H24F9N3
Formula weight 597.52
Temperature/K 110.05(10)
Crystal system orthorhombic
Space group Pbca
a/Å 19.0875(3)
b/Å 12.10177(17)
c/Å 24.0122(3)
α/° 90.00
β/° 90.00
γ/° 90.00
Volume/Å3 5546.65(15)
Z 8
ρcalcmg/mm3 1.431
m/mm‑1 0.127
F(000) 2448.0
Crystal size/mm3 0.2777 × 0.1474 × 0.0697
2Θ range for data collection 6.4 to 56.06°
Index ranges -24 ≤ h ≤ 13, -15 ≤ k ≤ 10, -31 ≤ l ≤ 18
Reflections collected 14716
Independent reflections 5708[R(int) = 0.0213]
Data/restraints/parameters 5708/37/406
Goodness-of-fit on F2 1.059
Final R indexes [I>=2σ (I)] R1 = 0.0445, wR2 = 0.0958
Final R indexes [all data] R1 = 0.0601, wR2 = 0.1041
Largest diff. peak/hole / e Å-3 0.23/-0.43

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1308. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C15755.9(10)3960.9(14)2299.9(7)20.3(4)
C25864.7(10)2895.2(15)1970.0(7)22.7(4)
C35211.8(10)2555.2(15)1644.5(7)21.8(4)
C44591.2(10)2434.6(15)2039.6(7)21.8(4)
C54466.8(10)3504.3(14)2360.4(7)20.2(4)
C65122.1(10)3846.3(14)2683.6(7)20.2(4)
C76651.9(10)5115.8(14)2625.5(7)20.7(4)
C87279.9(10)5394.2(14)2953.5(7)19.5(4)
C97597.7(10)4622.6(14)3303.2(7)21.9(4)
C108210.1(10)4871.6(14)3580.9(7)21.8(4)
C118513.1(10)5911.2(14)3513.2(7)20.0(4)
C128194.2(10)6696.7(14)3180.6(7)21.3(4)
C137578.8(10)6439.9(14)2902.3(7)22.1(4)
C145468.8(10)1537.4(15)848.1(7)23.1(4)
C155689(1)572.1(15)519.3(7)22.8(4)
C165978.1(11)742.9(16)-4.6(8)29.0(5)
C176235.0(12)-132.2(16)-316.6(8)30.7(5)
C186185.6(11)-1188.3(16)-108.5(8)26.3(4)
C195879.3(11)-1379.0(16)407.9(8)28.4(4)
C205636.7(11)-501.1(16)720.4(8)25.7(4)
C213570.0(9)4233.5(14)2895.3(7)19.6(4)
C223030.8(9)4252.5(14)3332.3(7)18.9(4)
C232797.3(10)3281.4(14)3581.4(7)21.4(4)
C242324.9(10)3317.8(15)4017.8(7)23.0(4)
C252080.7(10)4331.0(15)4205.9(7)22.4(4)
C262303.6(11)5302.3(15)3956.0(8)26.6(4)
C272775.8(10)5261.7(15)3521.3(8)24.2(4)
C289206.2(10)6168.3(15)3769.7(8)24.9(4)
C296469.3(12)-2149.8(17)-428.9(8)33.7(5)
C301587.9(10)4397.8(14)4684.7(8)30.8(5)
F19722.2(6)6174.4(10)3385.8(5)35.4(3)
F29403.7(6)5451.4(10)4158.6(5)36.6(3)
F39224.7(7)7176.2(10)4003.0(5)39.6(3)
F45984.7(7)-2927(1)-519.8(6)48.7(4)
F56989.6(7)-2660.8(12)-159.4(6)52.0(4)
F66716.5(9)-1877.2(12)-927.4(6)60.0(4)
F7A1913.0(16)4798(5)5137.8(10)43.3(9)
F7B1670(5)5255(6)5011(3)59.0(15)
F7C1220(20)5300(30)4560(30)65.4(13)
F8A1336(4)3442(2)4853(2)59.0(15)
F8B1590(5)3461(6)4977(4)65.4(13)
F8C1941(13)4280(40)5159(6)52.3(18)
F9A1060(2)5100(5)4609(2)65.4(13)
F9B923(2)4419(8)4500(3)52.3(18)
F9C1024(13)3760(30)4634(13)43.3(9)
N16374.5(8)4165.8(12)2642.0(6)21.0(3)
N25363.2(8)1500.1(12)1369.0(6)23.9(3)
N33893.5(8)3361.2(12)2760.2(6)20.7(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1308. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
C120.9(9)19.2(8)20.8(8)2.1(7)-0.6(8)2.3(7)
C220.5(9)25.6(9)22.0(9)-1.7(7)2.6(8)2.4(8)
C325.7(10)21.2(9)18.6(8)-2.2(7)0.1(8)3.1(8)
C421.5(9)24.5(9)19.6(8)-2.1(7)-1.1(8)0.3(8)
C521.3(9)19.9(9)19.5(8)2.0(7)2.5(8)2.7(8)
C622.6(9)18.1(8)20.0(8)-1.1(7)1.4(8)2.1(8)
C721.9(10)19.4(8)20.7(9)1.6(7)3.0(8)4.2(8)
C821.8(9)16.7(8)19.8(8)-1.7(7)5.7(8)1.8(7)
C926.7(10)16.4(8)22.6(9)1.0(7)3.2(8)-3.2(8)
C1027.7(10)17.4(8)20.3(8)1.9(7)1.6(8)0.6(8)
C1123.5(10)19.4(8)17.1(8)-2.8(7)5.6(8)-0.8(8)
C1226.3(10)14.5(8)23.1(9)-2.0(7)6.9(8)-1.4(8)
C1327(1)16.0(8)23.3(9)2.3(7)5.1(8)2.9(8)
C1423.6(10)24.1(9)21.7(9)-1.3(7)-2.3(8)2.2(8)
C1522.4(10)26.9(9)19.0(8)-2.8(7)-3.3(8)1.9(8)
C1639.2(12)24.8(10)22.9(9)0.1(8)1.3(9)-0.7(9)
C1737.7(12)33.1(11)21.3(9)-3.2(8)5.3(9)2(1)
C1825.9(10)30.7(10)22.3(9)-6.9(8)-5.1(8)5.4(9)
C1933.3(11)25.7(10)26.2(10)-0.2(8)-4.8(9)3.0(9)
C2029.1(11)29.3(10)18.5(8)-1.0(8)-0.1(8)1.1(9)
C2119.2(9)20.3(8)19.3(8)1.9(7)-3.2(8)-0.7(8)
C2219.2(9)20.4(8)17.0(8)0.7(7)-3.1(7)0.8(7)
C2322.8(9)18.2(8)23.2(9)-2.0(7)-1.7(8)0.6(8)
C2424.2(10)21.3(9)23.3(9)1.9(7)-1.0(8)-4.1(8)
C2522.7(10)25.8(9)18.6(8)-2.4(7)-0.1(8)-4.3(8)
C2632.0(11)19.6(9)28.2(10)-4.4(8)5.3(9)0.7(8)
C2728.6(10)19.4(9)24.7(9)1.7(7)2.8(8)-0.4(8)
C2829.1(11)23.0(9)22.6(9)-1.7(8)4.8(8)-2.5(8)
C2936.5(12)35.8(11)28.8(10)-9.0(9)-5.5(10)8.7(10)
C3034.2(12)28.6(10)29.4(10)-2.8(9)7.5(9)-3.4(9)
F127.0(6)46.0(7)33.1(6)-4.2(5)9.2(5)-9.0(6)
F231.1(7)42.1(7)36.7(7)11.2(6)-7.8(6)-6.9(6)
F342.2(8)33.2(6)43.3(7)-17.6(6)-4.8(6)-6.1(6)
F444.6(8)37.9(7)63.5(9)-26.1(7)-8.3(7)5.8(6)
F546.8(8)54.0(8)55.1(8)-23.6(7)-18.0(7)28.1(7)
F691.6(12)50.4(8)38.0(7)-12.0(6)24.0(8)14.4(8)
F7A56.2(17)49(2)24.8(11)-18.5(11)10.5(11)-6.5(17)
F7B86(3)28.5(12)63(2)-13.8(13)53(2)-25.7(17)
F7C48(2)89(3)59.3(19)26.1(18)33.7(16)29(2)
F8A86(3)28.5(12)63(2)-13.8(13)53(2)-25.7(17)
F8B48(2)89(3)59.3(19)26.1(18)33.7(16)29(2)
F8C30(3)63(5)63(4)15(4)21(3)13(3)
F9A48(2)89(3)59.3(19)26.1(18)33.7(16)29(2)
F9B30(3)63(5)63(4)15(4)21(3)13(3)
F9C56.2(17)49(2)24.8(11)-18.5(11)10.5(11)-6.5(17)
N120.8(8)19.7(7)22.4(8)-0.1(6)1.5(7)1.4(6)
N225.2(9)24.2(8)22.3(8)-3.9(6)0.2(7)2.8(7)
N320.5(8)22.5(8)19.2(7)0.2(6)0.7(6)1.1(7)

 

Table 4 Bond Lengths for phw1308.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.528(2) C19C201.381(3)
C1C61.527(2) C21C221.470(2)
C1N11.459(2) C21N31.265(2)
C2C31.528(3) C22C231.392(2)
C3C41.525(3) C22C271.391(2)
C3N21.467(2) C23C241.383(3)
C4C51.525(2) C24C251.387(3)
C5C61.529(3) C25C261.387(3)
C5N31.466(2) C25C301.488(3)
C7C81.473(3) C26C271.380(3)
C7N11.266(2) C28F11.349(2)
C8C91.395(2) C28F21.329(2)
C8C131.393(2) C28F31.343(2)
C9C101.379(3) C29F41.337(3)
C10C111.394(2) C29F51.337(2)
C11C121.383(2) C29F61.328(2)
C11C281.492(3) C30F7A1.343(2)
C12C131.387(3) C30F7B1.310(3)
C14C151.471(2) C30F7C1.332(4)
C14N21.268(2) C30F8A1.316(3)
C15C161.389(3) C30F8B1.334(4)
C15C201.389(3) C30F8C1.331(4)
C16C171.387(3) C30F9A1.330(3)
C17C181.375(3) C30F9B1.344(4)
C18C191.390(3) C30F9C1.329(4)
C18C291.496(3)    

 

Table 5 Bond Angles for phw1308.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C6C1C2110.12(15) C24C23C22120.50(17)
N1C1C2108.98(14) C23C24C25119.59(17)
N1C1C6108.46(14) C24C25C30120.81(16)
C3C2C1112.45(15) C26C25C24120.35(17)
C4C3C2109.95(14) C26C25C30118.83(16)
N2C3C2107.73(15) C27C26C25119.84(17)
N2C3C4110.51(15) C26C27C22120.43(17)
C3C4C5110.74(15) F1C28C11111.50(15)
C4C5C6111.02(15) F2C28C11113.92(15)
N3C5C4110.29(14) F2C28F1106.06(16)
N3C5C6108.07(14) F2C28F3106.99(15)
C1C6C5111.49(14) F3C28C11112.64(16)
N1C7C8122.08(16) F3C28F1105.12(15)
C9C8C7121.50(16) F4C29C18112.37(18)
C13C8C7119.57(16) F5C29C18112.30(16)
C13C8C9118.89(17) F5C29F4105.51(17)
C10C9C8120.89(16) F6C29C18113.50(18)
C9C10C11119.50(17) F6C29F4105.87(17)
C10C11C28120.51(16) F6C29F5106.69(18)
C12C11C10120.34(17) F7AC30C25110.71(18)
C12C11C28119.04(16) F7BC30C25115.5(3)
C11C12C13119.81(16) F7BC30F8B110.9(5)
C12C13C8120.52(17) F7BC30F9B107.2(5)
N2C14C15123.14(17) F7CC30C25102(2)
C16C15C14118.77(17) F8AC30C25114.9(2)
C16C15C20118.85(17) F8AC30F7A103.7(2)
C20C15C14122.36(17) F8BC30C25111.0(4)
C17C16C15121.06(18) F8BC30F9B101.1(5)
C18C17C16119.28(18) F8CC30C25109.6(12)
C17C18C19120.48(18) F9AC30C25114.1(2)
C17C18C29120.72(18) F9AC30F7A103.3(3)
C19C18C29118.79(18) F9BC30C25110.1(3)
C20C19C18119.87(18) F9CC30C25114.2(10)
C19C20C15120.42(18) F9CC30F7C91(3)
N3C21C22122.53(16) F9CC30F8C115.4(18)
C23C22C21121.18(16) C7N1C1118.35(15)
C27C22C21119.45(16) C14N2C3116.44(16)
C27C22C23119.28(16) C21N3C5115.69(15)

 

Table 6 Torsion Angles for phw1308.
ABCDAngle/˚ ABCDAngle/˚
C1C2C3C4-56.6(2) C19C18C29F6176.73(19)
C1C2C3N2-177.12(14) C20C15C16C17-2.3(3)
C2C1C6C5-54.57(19) C21C22C23C24175.59(16)
C2C1N1C7130.36(17) C21C22C27C26-175.75(17)
C2C3C4C556.83(19) C22C21N3C5-173.66(15)
C2C3N2C14-105.64(19) C22C23C24C250.3(3)
C3C4C5C6-57.22(19) C23C22C27C260.9(3)
C3C4C5N3-176.98(14) C23C24C25C260.5(3)
C4C3N2C14134.22(18) C23C24C25C30-178.27(17)
C4C5C6C156.25(19) C24C25C26C27-0.6(3)
C4C5N3C21-154.59(16) C24C25C30F7A107.9(3)
C6C1C2C355.35(19) C24C25C30F7B144.9(6)
C6C1N1C7-109.75(17) C24C25C30F7C-149(3)
C6C5N3C2183.88(18) C24C25C30F8A-9.2(5)
C7C8C9C10175.90(16) C24C25C30F8B17.5(6)
C7C8C13C12-175.99(16) C24C25C30F8C79(2)
C8C7N1C1-179.55(15) C24C25C30F9A-136.1(4)
C8C9C10C110.4(3) C24C25C30F9B-93.6(5)
C9C8C13C122.1(3) C24C25C30F9C-52(2)
C9C10C11C121.5(3) C25C26C27C22-0.1(3)
C9C10C11C28-174.75(16) C26C25C30F7A-71.0(4)
C10C11C12C13-1.6(3) C26C25C30F7B-33.9(7)
C10C11C28F1104.56(19) C26C25C30F7C32(3)
C10C11C28F2-15.4(2) C26C25C30F8A172.0(4)
C10C11C28F3-137.53(17) C26C25C30F8B-161.3(6)
C11C12C13C8-0.2(3) C26C25C30F8C-100(2)
C12C11C28F1-71.7(2) C26C25C30F9A45.1(4)
C12C11C28F2168.27(16) C26C25C30F9B87.6(5)
C12C11C28F346.2(2) C26C25C30F9C129(2)
C13C8C9C10-2.1(3) C27C22C23C24-1.0(3)
C14C15C16C17175.85(19) C28C11C12C13174.74(16)
C14C15C20C19-177.03(18) C29C18C19C20177.65(18)
C15C14N2C3174.29(17) C30C25C26C27178.20(18)
C15C16C17C181.7(3) N1C1C2C3174.22(14)
C16C15C20C191.1(3) N1C1C6C5-173.75(14)
C16C17C18C190.3(3) N1C7C8C9-0.5(3)
C16C17C18C29-178.85(19) N1C7C8C13177.49(17)
C17C18C19C20-1.5(3) N2C3C4C5175.63(14)
C17C18C29F4-124.2(2) N2C14C15C16-162.19(19)
C17C18C29F5117.0(2) N2C14C15C2015.9(3)
C17C18C29F6-4.1(3) N3C5C6C1177.32(13)
C18C19C20C150.8(3) N3C21C22C23-6.7(3)
C19C18C29F456.6(2) N3C21C22C27169.86(17)
C19C18C29F5-62.1(3)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1308.
AtomxyzU(eq)
H156824592203824
H2A62592999170727
H2B59942294223027
H351033129135726
H4A46841826230526
H4B41662245182426
H543414104209224
H6A50354560287324
H6B52243286297324
H764495666239425
H973893916335126
H1084244339381726
H1283967410314326
H1373596981267526
H145403222166128
H1660001471-15135
H176443-4-67037
H195837-211254534
H205433-632107531
H2136804902270723
H2329642588345126
H2421682653418828
H2621325994408432
H2729285928335029

Experimental

Single crystals of C30H24F9N3 [phw1308] were []. A suitable crystal was selected and [oil on loop] on a Oxford Diffraction Supernova diffractometer. The crystal was kept at 110.05(10) K during data collection. Using Olex2 [1], the structure was solved with the Superflip [2] structure solution program using Charge Flipping and refined with the ShelXL [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. SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790
  3. SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122

Crystal structure determination of [phw1308]

Crystal Data for C30H24F9N3 (=597.52): orthorhombic, space group Pbca (no. 61), a = 19.0875(3) Å, b = 12.10177(17) Å, c = 24.0122(3) Å, = 5546.65(15) Å3, Z = 8, T = 110.05(10) K, μ(Mo Kα) = 0.127 mm-1, Dcalc = 1.431 g/mm3, 14716 reflections measured (6.4 ≤ 2Θ ≤ 56.06), 5708 unique (Rint = 0.0213) which were used in all calculations. The final R1 was 0.0445 (>2sigma(I)) and wR2 was 0.1041 (all data).

This report has been created with Olex2, compiled on Apr 23 2013 17:59:47. Please let us know if there are any errors or if you would like to have additional featrues.