phw1101

Crystal Submitted by:
LC
Crystal Submitted on:
31/1/2011
Data Collected on:
Structure Solved by:
NCS

Table 1: Crystal data and structure refinement for phw1101
Identification code phw1101
Empirical formula C27H27N3O3
Formula weight 441.52
Temperature / K 120.0
Crystal system monoclinic
Space group P21/c
a / Å, b / Å, c / Å 5.9979(2), 24.6161(8), 15.3079(6)
α/°, β/°, γ/° 90.00, 91.843(2), 90.00
Volume / Å3 2258.96(14)
Z 4
ρcalc / mg mm-3 1.298
μ / mm‑1 0.086
F(000) 936
Crystal size / mm3 0.32 × 0.05 × 0.04
2Θ range for data collection 6.28 to 55.14°
Index ranges -7 ≤ h ≤ 7, -29 ≤ k ≤ 31, -19 ≤ l ≤ 19
Reflections collected 18092
Independent reflections 5165[R(int) = 0.0524]
Data/restraints/parameters 5165/0/311
Goodness-of-fit on F2 1.114
Final R indexes [I>2σ (I)] R1 = 0.0679, wR2 = 0.1184
Final R indexes [all data] R1 = 0.1034, wR2 = 0.1352
Largest diff. peak/hole / e Å-3 0.265/-0.239

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1101. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C15935(4)5439.9(9)-2045.5(15)20.2(5)
C24433(3)5080.0(9)-1513.4(15)19.5(5)
C35719(3)4626.7(9)-1036.1(15)19.6(5)
C47114(4)4300.5(9)-1669.5(15)19.5(5)
C58600(3)4679.2(9)-2185.3(15)19.7(5)
C67242(4)5102.7(9)-2694.7(15)20.8(5)
C75127(4)6343.3(9)-2490.8(16)20.5(5)
C83721(4)6765.0(9)-2886.6(15)20.3(5)
C91608(4)6637.4(9)-3269.9(16)22.3(5)
C10258(4)7049.5(10)-3607.4(17)28.4(6)
C11965(4)7584.3(11)-3561.0(18)32.1(6)
C123038(4)7715(1)-3182.8(17)28.9(6)
C134399(4)7308.7(9)-2852.3(16)24.3(5)
C144365(4)3808.1(9)-383.8(15)20.6(5)
C152753(4)3499.8(9)112.3(15)20.7(5)
C16777(4)3745.4(9)397.9(15)21.0(5)
C17-715(4)3446.5(10)882.1(16)24.9(5)
C18-263(4)2908.9(10)1079.5(17)28.2(6)
C191658(4)2656(1)796.4(17)28.0(6)
C203150(4)2952.2(10)316.2(16)25.0(5)
C2110698(4)4474.4(11)-3458.1(17)29.9(6)
C2212438(4)4178.8(11)-3903.7(17)30.5(6)
C2313525(4)3731.4(10)-3507.1(17)24.9(5)
C2415328(4)3491.7(11)-3914.2(18)31.7(6)
C2516022(5)3683.3(13)-4702.9(19)43.0(8)
C2614945(6)4117.9(16)-5108(2)61.3(11)
C2713176(5)4362.5(15)-4701(2)54.8(10)
N14536(3)5842.4(7)-2504.1(13)20.6(4)
N24069(3)4310.7(7)-554.5(13)20.2(4)
N310136(3)4344.7(8)-2688.9(13)21.8(4)
O1864(3)6117.4(7)-3309.0(12)28.1(4)
O2294(3)4274.1(7)211.9(11)24.2(4)
O312879(3)3533.2(7)-2734.4(13)32.4(4)

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1101. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
C118.9(10)19.7(11)21.8(13)-0.1(9)-1.8(9)-0.8(9)
C216.7(10)21.9(11)20.0(12)-1.8(9)1.4(8)1.6(9)
C317.6(10)19.4(11)21.7(12)-1.7(9)0.5(9)-0.4(9)
C419.5(10)19.3(11)19.6(12)-0.4(9)1.2(9)1.1(9)
C517.7(10)20.8(11)20.5(12)-3.3(9)2.0(9)3.0(9)
C619.8(10)20.0(11)22.8(12)0.7(9)3.4(9)-1.6(9)
C720(1)21.9(11)19.8(12)0.4(9)3.8(9)-0.2(9)
C821.2(11)23.3(12)16.6(12)2.6(9)3.0(9)2.2(9)
C924.1(11)22.9(12)20.2(12)0.1(10)5.4(9)0.8(9)
C1025.8(12)32.2(14)27.0(14)3.4(11)-0.5(10)5.2(10)
C1136.5(14)31.1(14)28.6(15)7.2(11)-0.9(11)11.7(11)
C1239.1(14)19.5(12)28.2(15)4.1(10)4.1(11)1.2(10)
C1328.2(12)22.7(12)22.0(13)0.9(10)1(1)-2.9(10)
C1420.0(11)23.3(12)18.6(12)-3.0(9)2.5(9)1.9(9)
C1521.1(11)22.5(11)18.4(12)-0.5(9)0.5(9)-2.0(9)
C1622.1(11)22.8(12)18.0(12)0.4(9)-1.8(9)-0.3(9)
C1720.1(11)29.9(13)25.0(14)-0.7(10)3.4(9)-1.2(10)
C1828.2(12)30.5(13)25.9(14)1.4(11)3.5(10)-8.7(10)
C1931.6(13)23.1(12)29.3(14)2.6(11)-0.4(11)-1.7(10)
C2027.7(12)22.8(12)24.3(13)-0.4(10)0.8(10)3.2(10)
C2126.7(12)40.4(15)22.6(14)0.6(11)-0.1(10)10.6(11)
C2228.8(12)42.4(15)20.3(13)-2.4(11)0.9(10)8.5(11)
C2321.8(11)27.8(12)25.1(13)-7.1(10)2.1(9)-2.5(10)
C2426.4(12)36.4(14)32.4(15)-4.9(12)1.0(11)7.7(11)
C2537.2(15)64(2)28.7(16)-7.0(14)7.5(12)19.4(14)
C2668(2)93(3)24.3(17)11.1(17)17.4(15)40(2)
C2760(2)77(2)28.0(17)14.3(16)10.0(14)38.9(18)
N120.1(9)19.9(10)22.0(11)1.3(8)3.8(8)1.3(7)
N219.7(9)20.5(10)20.4(10)0.4(8)2.0(7)-2.0(8)
N317.3(9)22.5(10)25.8(11)-3.5(8)0.8(8)0.1(8)
O124.1(8)24.3(9)35.6(11)3.2(8)-5.0(7)-3.6(7)
O222.2(8)22.8(9)27.7(10)2.4(7)3.1(7)4.2(7)
O332.2(10)27.2(9)38.7(12)5.4(8)13.2(8)5.6(8)

Table 4 Bond Lengths for phw1101.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.519(3) C14C151.461(3)
C1C61.530(3) C14N21.276(3)
C1N11.463(3) C15C161.412(3)
C2C31.529(3) C15C201.402(3)
C3C41.529(3) C16C171.390(3)
C3N21.475(3) C16O21.361(3)
C4C51.527(3) C17C181.382(3)
C5C61.522(3) C18C191.391(3)
C5N31.472(3) C19C201.384(3)
C7C81.457(3) C21C221.460(3)
C7N11.283(3) C21N31.276(3)
C8C91.414(3) C22C231.407(4)
C8C131.399(3) C22C271.387(4)
C9C101.388(3) C23C241.396(3)
C9O11.357(3) C23O31.348(3)
C10C111.384(4) C24C251.373(4)
C11C121.392(4) C25C261.386(4)
C12C131.377(3) C26C271.386(4)

Table 5 Bond Angles for phw1101.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2C1C6110.91(18) C16C15C14121.0(2)
N1C1C2108.17(17) C20C15C14120.3(2)
N1C1C6110.70(19) C20C15C16118.8(2)
C1C2C3112.55(17) C17C16C15120.0(2)
C2C3C4110.99(19) O2C16C15121.3(2)
N2C3C2106.73(17) O2C16C17118.8(2)
N2C3C4115.45(18) C18C17C16119.9(2)
C5C4C3110.35(18) C17C18C19121.2(2)
C6C5C4111.79(18) C20C19C18119.1(2)
N3C5C4108.35(18) C19C20C15121.1(2)
N3C5C6116.64(19) N3C21C22121.4(2)
C5C6C1108.40(19) C23C22C21121.1(2)
N1C7C8121.5(2) C27C22C21120.1(2)
C9C8C7120.9(2) C27C22C23118.6(2)
C13C8C7120.2(2) C24C23C22119.5(2)
C13C8C9118.9(2) O3C23C22121.3(2)
C10C9C8119.8(2) O3C23C24119.2(2)
O1C9C8121.1(2) C25C24C23120.6(3)
O1C9C10119.1(2) C24C25C26120.5(3)
C11C10C9120.1(2) C27C26C25119.1(3)
C10C11C12120.6(2) C26C27C22121.6(3)
C13C12C11119.7(2) C7N1C1119.31(19)
C12C13C8120.9(2) C14N2C3121.54(19)
N2C14C15121.4(2) C21N3C5122.1(2)

Table 6 Hydrogen Bonds for phw1101.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1AN11.01(4)1.67(4)2.580(3)147(3)
O2H2N20.96(3)1.72(3)2.585(2)149(3)
O3H3AN31.02(4)1.69(4)2.591(3)145(3)

Table 7 Torsion Angles for phw1101.
ABCDAngle/˚
C1C2C3C4-53.1(2)
C1C2C3N2-179.72(18)
C2C1C6C5-58.0(2)
C2C1N1C7133.3(2)
C2C3C4C553.3(2)
C2C3N2C14151.9(2)
C3C4C5C6-58.2(2)
C3C4C5N3171.90(18)
C4C3N2C1428.0(3)
C4C5C6C159.9(2)
C4C5N3C21142.6(2)
C6C1C2C355.9(3)
C6C1N1C7-105.0(2)
C6C5N3C2115.4(3)
C7C8C9C10177.1(2)
C7C8C9O1-2.4(3)
C7C8C13C12-176.6(2)
C8C7N1C1-175.8(2)
C8C9C10C11-0.7(4)
C9C8C13C120.2(4)
C9C10C11C120.5(4)
C10C11C12C130.1(4)
C11C12C13C8-0.4(4)
C13C8C9C100.4(3)
C13C8C9O1-179.2(2)
C14C15C16C17-178.9(2)
C14C15C16O20.8(3)
C14C15C20C19179.0(2)
C15C14N2C3178.5(2)
C15C16C17C18-0.3(4)
C16C15C20C19-0.7(4)
C16C17C18C19-0.5(4)
C17C18C19C200.7(4)
C18C19C20C15-0.1(4)
C20C15C16C170.9(3)
C20C15C16O2-179.4(2)
C21C22C23C24-173.7(2)
C21C22C23O35.4(4)
C21C22C27C26174.7(3)
C22C21N3C5171.9(2)
C22C23C24C25-1.1(4)
C23C22C27C26-0.2(5)
C23C24C25C260.0(5)
C24C25C26C270.9(6)
C25C26C27C22-0.9(6)
C27C22C23C241.1(4)
C27C22C23O3-179.8(3)
N1C1C2C3177.50(18)
N1C1C6C5-178.06(17)
N1C7C8C92.5(3)
N1C7C8C13179.2(2)
N2C3C4C5174.87(18)
N2C14C15C161.9(3)
N2C14C15C20-177.9(2)
N3C5C6C1-174.64(18)
N3C21C22C231.4(4)
N3C21C22C27-173.3(3)
O1C9C10C11178.9(2)
O2C16C17C18180.0(2)
O3C23C24C25179.8(3)

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1101.
AtomxyzU(eq)
H170115632-164024
H2A32764916-190723
H2B36695306-108023
H367654800-59723
H4A80524036-133923
H4B61154096-207823
H595424883-174524
H6A62004922-311725
H6B82455341-302425
H765136442-221725
H10-11556965-387134
H11287865-378939
H1235128083-315335
H1358167399-259829
H1456593631-58325
H17-20413612107730
H18-12852708141534
H191942228593134
H204466278212230
H2199684770-374736
H24160813194-364338
H25172513516-497352
H26154144246-565874
H27124504664-497466
H1A 2030.0(6)5881(14)-3000.0(2)67(11)
H2 1530.0(5)4416(13)-100.0(2)55(10)
H3A 11610.0(6)3767(15)-2520.0(3)83(13)

[RSC Journal Format]

Experimental

Single crystals of C27H27N3O3 [phw1101] were recrystallised from [solvents] mounted in inert oil and transferred to the cold gas stream of the diffractometer.

Crystal structure determination of [phw1101]

Crystal Data. C27H27N3O3, =441.52, monoclinic, a = 5.9979(2) Å, b = 24.6161(8) Å, c = 15.3079(6) Å, β = 91.843(2)°, = 2258.96(14) Å3, T = 120.0, space group P21/c (no. 14), Z = 4, μ(MO Kα) = 0.086, 18092 reflections measured, 5165 unique (Rint = 0.0524) which were used in all calculations. The final wR(F2) was 0.1352 (all data).

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