mo_B0636_0m

Table 1 Crystal data and structure refinement for mo_B0636_0m.
Identification code mo_B0636_0m
Empirical formula C14H34NNaO4
Formula weight 303.41
Temperature/K 99.99
Crystal system triclinic
Space group P-1
a/Å 9.939(5)
b/Å 10.302(6)
c/Å 11.094(6)
α/° 103.433(15)
β/° 108.200(14)
γ/° 111.747(19)
Volume/Å3 921.0(8)
Z 2
ρcalcg/cm3 1.094
μ/mm‑1 0.097
F(000) 336.0
Crystal size/mm3 0.31 × 0.29 × 0.14
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.632 to 51.994
Index ranges -12 ≤ h ≤ 12, -12 ≤ k ≤ 12, -13 ≤ l ≤ 13
Reflections collected 18203
Independent reflections 3605 [Rint = 0.0343, Rsigma = 0.0233]
Data/restraints/parameters 3605/0/197
Goodness-of-fit on F2 1.206
Final R indexes [I>=2σ (I)] R1 = 0.0375, wR2 = 0.1125
Final R indexes [all data] R1 = 0.0528, wR2 = 0.1354
Largest diff. peak/hole / e Å-3 0.44/-0.37

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0636_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Na15657.3(7)3614.0(6)4137.0(6)12.88(18)
O13163.4(13)2651.0(11)4130.2(11)13.2(3)
O47753.2(14)5405.9(13)6377.4(11)18.0(3)
O36255.2(15)5654.6(13)3498.8(12)22.0(3)
O27028.3(13)2203.2(12)3815.8(12)18.4(3)
N13791.4(16)1124.9(14)1978.6(13)15.0(3)
C12355.8(19)1057.6(16)3534.7(16)14.1(3)
C127928(2)5373.3(18)7692.9(16)19.4(4)
C97122(2)6357.4(18)2823.0(17)21.0(4)
C23229(2)455.3(18)4472.5(17)19.2(4)
C64538(2)131.8(17)2040.1(17)18.9(4)
C3606(2)412.0(19)3344.8(19)24.3(4)
C76338(2)991.0(18)2513.5(17)19.5(4)
C88747(2)2889(2)4479(2)26.3(4)
C42247.9(19)499.6(17)2071.0(16)16.9(3)
C106128(3)6793(2)1834(2)32.3(5)
C147656(2)3806.1(19)7627.6(19)27.3(4)
C53559(2)1413(2)717.4(17)24.1(4)
C139595(2)6591(2)8811.8(19)33.0(5)
C117579(2)5276(2)2081(2)33.6(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0636_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Na116.9(3)9.1(3)13.5(3)4.8(2)7.0(3)6.5(3)
O118.2(6)7.8(5)14.7(6)4.7(4)8.1(4)6.4(4)
O424.0(6)14.6(6)14.8(6)5.6(5)4.9(5)11.9(5)
O338.7(7)12.0(6)15.4(6)7.3(5)14.9(5)8.5(5)
O218.1(6)16.1(6)20.3(6)4.0(5)8.5(5)9.5(5)
N121.2(7)13.3(6)12.6(7)5.4(5)8.7(5)9.0(6)
C117.0(8)9.0(7)15.8(8)4.3(6)7.9(6)5.4(6)
C1224.4(9)16.8(8)14.2(8)5.6(6)4.3(7)11.1(7)
C921.7(8)16.9(8)16.9(8)6.5(7)7.3(7)3.2(7)
C232.1(9)13.3(8)17.8(8)9.1(6)12.8(7)12.9(7)
C627.9(9)11.5(7)18.9(8)3.8(6)12.7(7)10.5(7)
C320.7(9)18.3(8)29.0(10)5.6(7)13.3(8)4.9(7)
C727.8(9)15.5(8)22.4(9)6.9(7)16.0(7)13.6(7)
C819.3(9)27.1(9)33.1(10)11.1(8)10.9(8)12.7(8)
C417.6(8)14.1(8)13.2(8)2.5(6)4.3(6)5.7(7)
C1051.9(13)29.4(10)23.4(10)16.2(8)17.9(9)22.5(10)
C1432.8(10)18.7(9)23.9(9)10.5(7)5.5(8)10.5(8)
C532.8(10)27.5(9)16.8(8)11.4(7)13.3(7)15.4(8)
C1337.5(11)19.8(9)21.4(9)5.0(7)-3.4(8)9.8(8)
C1129.6(10)42.7(12)32.2(11)14.4(9)14.7(9)20.2(9)

 

Table 4 Bond Lengths for mo_B0636_0m.
AtomAtomLength/Å AtomAtomLength/Å
Na1Na113.9135(18) O2C71.423(2)
Na1O12.3002(17) O2C81.427(2)
Na1O113.419(2) N1C61.471(2)
Na1O42.3894(17) N1C41.475(2)
Na1O413.799(2) N1C51.463(2)
Na1O32.3026(16) C1C21.535(2)
Na1O22.3719(15) C1C31.537(2)
Na1N12.5685(19) C1C41.546(2)
Na1C13.092(2) C12C141.515(2)
O1C11.401(2) C12C131.520(2)
O4C121.425(2) C9C101.504(3)
O3Na113.7839(19) C9C111.519(3)
O3C91.422(2) C6C71.511(2)

11-X,1-Y,1-Z

 

Table 5 Bond Angles for mo_B0636_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O11Na1Na1135.77(3) C1Na1O4163.28(6)
O1Na1Na1160.31(4) C1O1Na1110.94(9)
O1Na1O1196.07(4) C12O4Na1129.03(10)
O1Na1O4111.87(6) Na1O3Na1175.70(4)
O1Na1O4141.87(4) C9O3Na11142.17(10)
O11Na1O4164.89(4) C9O3Na1141.13(11)
O1Na1O3113.48(5) C7O2Na1118.36(10)
O1Na1O2124.94(6) C7O2C8112.23(13)
O1Na1N173.20(5) C8O2Na1121.82(10)
O1Na1C125.05(4) C6N1Na1107.75(10)
O41Na1Na1136.06(3) C6N1C4112.57(13)
O4Na1Na1169.36(5) C4N1Na1104.77(9)
O4Na1O1149.14(4) C5N1Na1111.05(10)
O4Na1O41105.41(5) C5N1C6110.33(13)
O4Na1N1160.79(5) C5N1C4110.23(13)
O4Na1C1125.52(6) O1C1Na144.02(7)
O3Na1Na1169.54(5) O1C1C2109.54(13)
O3Na1O1148.07(5) O1C1C3111.15(12)
O3Na1O4171.81(5) O1C1C4109.68(12)
O3Na1O485.63(6) C2C1Na189.66(10)
O3Na1O2116.44(6) C2C1C3108.52(13)
O3Na1N1109.83(7) C2C1C4111.93(13)
O3Na1C1130.10(5) C3C1Na1154.36(10)
O2Na1Na11162.15(4) C3C1C4105.99(13)
O2Na1O11134.77(5) C4C1Na182.52(9)
O2Na1O41159.90(4) O4C12C14108.27(13)
O2Na1O493.78(6) O4C12C13110.53(15)
O2Na1N169.43(6) C14C12C13110.83(14)
O2Na1C1100.75(6) O3C9C10110.36(15)
N1Na1Na11125.96(5) O3C9C11109.16(15)
N1Na1O11150.07(4) C10C9C11111.18(15)
N1Na1O4190.63(5) N1C6C7112.29(13)
N1Na1C152.75(5) O2C7C6108.13(13)
C1Na1Na1185.31(6) N1C4C1115.67(13)
C1Na1O11121.06(5)     

11-X,1-Y,1-Z

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0636_0m.
AtomxyzU(eq)
H1270945564790223
H981327299353525
H2A4356879462329
H2B2697-657403229
H2C3191759536129
H6A4032-686111423
H6B4328-351268323
H3A602684425136
H3B47-698286736
H3C51838279636
H7A6809303260023
H7B65641399183323
H8A91783176384339
H8B90632164474339
H8C91793799530639
H4A1759-623170120
H4B1508758146820
H10A51295879113548
H10B67437284138348
H10C58627500234148
H14A65813039689541
H14B77343750851541
H14C84763615743141
H5A3225220075836
H5B2723475-8536
H5C4574175963436
H13A104176389863149
H13B96806579971349
H13C97617591881349
H11A81924983274250
H11B82435783166850
H11C65984367135350
H36490(30)6360(30)4250(30)52(7)
H47620(30)6160(30)6350(20)38(6)

Experimental

Single crystals of C14H34NNaO4 [mo_B0636_0m] were []. A suitable crystal was selected and [] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 99.99 K during data collection. Using Olex2 [1], the structure was solved with the olex2.solve [2] structure solution program using Charge Flipping and refined with the ShelXL [3] refinement package using Least Squares minimisation.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
  2. Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H. (2015). Acta Cryst. A71, 59-75.
  3. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [mo_B0636_0m]

Crystal Data for C14H34NNaO4 (=303.41 g/mol): triclinic, space group P-1 (no. 2), a = 9.939(5) Å, b = 10.302(6) Å, c = 11.094(6) Å, α = 103.433(15)°, β = 108.200(14)°, γ = 111.747(19)°, = 921.0(8) Å3, Z = 2, T = 99.99 K, μ(MoKα) = 0.097 mm-1, Dcalc = 1.094 g/cm3, 18203 reflections measured (4.632° ≤ 2Θ ≤ 51.994°), 3605 unique (Rint = 0.0343, Rsigma = 0.0233) which were used in all calculations. The final R1 was 0.0375 (I > 2σ(I)) and wR2 was 0.1354 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C12(H12), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
C6(H6A,H6B), C7(H7A,H7B), C4(H4A,H4B)
2.c Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
C14(H14A,H14B,H14C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C)

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