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 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Na1 | 5657.3(7) | 3614.0(6) | 4137.0(6) | 12.88(18) |
O1 | 3163.4(13) | 2651.0(11) | 4130.2(11) | 13.2(3) |
O4 | 7753.2(14) | 5405.9(13) | 6377.4(11) | 18.0(3) |
O3 | 6255.2(15) | 5654.6(13) | 3498.8(12) | 22.0(3) |
O2 | 7028.3(13) | 2203.2(12) | 3815.8(12) | 18.4(3) |
N1 | 3791.4(16) | 1124.9(14) | 1978.6(13) | 15.0(3) |
C1 | 2355.8(19) | 1057.6(16) | 3534.7(16) | 14.1(3) |
C12 | 7928(2) | 5373.3(18) | 7692.9(16) | 19.4(4) |
C9 | 7122(2) | 6357.4(18) | 2823.0(17) | 21.0(4) |
C2 | 3229(2) | 455.3(18) | 4472.5(17) | 19.2(4) |
C6 | 4538(2) | 131.8(17) | 2040.1(17) | 18.9(4) |
C3 | 606(2) | 412.0(19) | 3344.8(19) | 24.3(4) |
C7 | 6338(2) | 991.0(18) | 2513.5(17) | 19.5(4) |
C8 | 8747(2) | 2889(2) | 4479(2) | 26.3(4) |
C4 | 2247.9(19) | 499.6(17) | 2071.0(16) | 16.9(3) |
C10 | 6128(3) | 6793(2) | 1834(2) | 32.3(5) |
C14 | 7656(2) | 3806.1(19) | 7627.6(19) | 27.3(4) |
C5 | 3559(2) | 1413(2) | 717.4(17) | 24.1(4) |
C13 | 9595(2) | 6591(2) | 8811.8(19) | 33.0(5) |
C11 | 7579(2) | 5276(2) | 2081(2) | 33.6(5) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Na1 | 16.9(3) | 9.1(3) | 13.5(3) | 4.8(2) | 7.0(3) | 6.5(3) |
O1 | 18.2(6) | 7.8(5) | 14.7(6) | 4.7(4) | 8.1(4) | 6.4(4) |
O4 | 24.0(6) | 14.6(6) | 14.8(6) | 5.6(5) | 4.9(5) | 11.9(5) |
O3 | 38.7(7) | 12.0(6) | 15.4(6) | 7.3(5) | 14.9(5) | 8.5(5) |
O2 | 18.1(6) | 16.1(6) | 20.3(6) | 4.0(5) | 8.5(5) | 9.5(5) |
N1 | 21.2(7) | 13.3(6) | 12.6(7) | 5.4(5) | 8.7(5) | 9.0(6) |
C1 | 17.0(8) | 9.0(7) | 15.8(8) | 4.3(6) | 7.9(6) | 5.4(6) |
C12 | 24.4(9) | 16.8(8) | 14.2(8) | 5.6(6) | 4.3(7) | 11.1(7) |
C9 | 21.7(8) | 16.9(8) | 16.9(8) | 6.5(7) | 7.3(7) | 3.2(7) |
C2 | 32.1(9) | 13.3(8) | 17.8(8) | 9.1(6) | 12.8(7) | 12.9(7) |
C6 | 27.9(9) | 11.5(7) | 18.9(8) | 3.8(6) | 12.7(7) | 10.5(7) |
C3 | 20.7(9) | 18.3(8) | 29.0(10) | 5.6(7) | 13.3(8) | 4.9(7) |
C7 | 27.8(9) | 15.5(8) | 22.4(9) | 6.9(7) | 16.0(7) | 13.6(7) |
C8 | 19.3(9) | 27.1(9) | 33.1(10) | 11.1(8) | 10.9(8) | 12.7(8) |
C4 | 17.6(8) | 14.1(8) | 13.2(8) | 2.5(6) | 4.3(6) | 5.7(7) |
C10 | 51.9(13) | 29.4(10) | 23.4(10) | 16.2(8) | 17.9(9) | 22.5(10) |
C14 | 32.8(10) | 18.7(9) | 23.9(9) | 10.5(7) | 5.5(8) | 10.5(8) |
C5 | 32.8(10) | 27.5(9) | 16.8(8) | 11.4(7) | 13.3(7) | 15.4(8) |
C13 | 37.5(11) | 19.8(9) | 21.4(9) | 5.0(7) | -3.4(8) | 9.8(8) |
C11 | 29.6(10) | 42.7(12) | 32.2(11) | 14.4(9) | 14.7(9) | 20.2(9) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Na1 | Na11 | 3.9135(18) | O2 | C7 | 1.423(2) | |
Na1 | O1 | 2.3002(17) | O2 | C8 | 1.427(2) | |
Na1 | O11 | 3.419(2) | N1 | C6 | 1.471(2) | |
Na1 | O4 | 2.3894(17) | N1 | C4 | 1.475(2) | |
Na1 | O41 | 3.799(2) | N1 | C5 | 1.463(2) | |
Na1 | O3 | 2.3026(16) | C1 | C2 | 1.535(2) | |
Na1 | O2 | 2.3719(15) | C1 | C3 | 1.537(2) | |
Na1 | N1 | 2.5685(19) | C1 | C4 | 1.546(2) | |
Na1 | C1 | 3.092(2) | C12 | C14 | 1.515(2) | |
O1 | C1 | 1.401(2) | C12 | C13 | 1.520(2) | |
O4 | C12 | 1.425(2) | C9 | C10 | 1.504(3) | |
O3 | Na11 | 3.7839(19) | C9 | C11 | 1.519(3) | |
O3 | C9 | 1.422(2) | C6 | C7 | 1.511(2) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
O11 | Na1 | Na11 | 35.77(3) | C1 | Na1 | O41 | 63.28(6) | |
O1 | Na1 | Na11 | 60.31(4) | C1 | O1 | Na1 | 110.94(9) | |
O1 | Na1 | O11 | 96.07(4) | C12 | O4 | Na1 | 129.03(10) | |
O1 | Na1 | O4 | 111.87(6) | Na1 | O3 | Na11 | 75.70(4) | |
O1 | Na1 | O41 | 41.87(4) | C9 | O3 | Na11 | 142.17(10) | |
O11 | Na1 | O41 | 64.89(4) | C9 | O3 | Na1 | 141.13(11) | |
O1 | Na1 | O3 | 113.48(5) | C7 | O2 | Na1 | 118.36(10) | |
O1 | Na1 | O2 | 124.94(6) | C7 | O2 | C8 | 112.23(13) | |
O1 | Na1 | N1 | 73.20(5) | C8 | O2 | Na1 | 121.82(10) | |
O1 | Na1 | C1 | 25.05(4) | C6 | N1 | Na1 | 107.75(10) | |
O41 | Na1 | Na11 | 36.06(3) | C6 | N1 | C4 | 112.57(13) | |
O4 | Na1 | Na11 | 69.36(5) | C4 | N1 | Na1 | 104.77(9) | |
O4 | Na1 | O11 | 49.14(4) | C5 | N1 | Na1 | 111.05(10) | |
O4 | Na1 | O41 | 105.41(5) | C5 | N1 | C6 | 110.33(13) | |
O4 | Na1 | N1 | 160.79(5) | C5 | N1 | C4 | 110.23(13) | |
O4 | Na1 | C1 | 125.52(6) | O1 | C1 | Na1 | 44.02(7) | |
O3 | Na1 | Na11 | 69.54(5) | O1 | C1 | C2 | 109.54(13) | |
O3 | Na1 | O11 | 48.07(5) | O1 | C1 | C3 | 111.15(12) | |
O3 | Na1 | O41 | 71.81(5) | O1 | C1 | C4 | 109.68(12) | |
O3 | Na1 | O4 | 85.63(6) | C2 | C1 | Na1 | 89.66(10) | |
O3 | Na1 | O2 | 116.44(6) | C2 | C1 | C3 | 108.52(13) | |
O3 | Na1 | N1 | 109.83(7) | C2 | C1 | C4 | 111.93(13) | |
O3 | Na1 | C1 | 130.10(5) | C3 | C1 | Na1 | 154.36(10) | |
O2 | Na1 | Na11 | 162.15(4) | C3 | C1 | C4 | 105.99(13) | |
O2 | Na1 | O11 | 134.77(5) | C4 | C1 | Na1 | 82.52(9) | |
O2 | Na1 | O41 | 159.90(4) | O4 | C12 | C14 | 108.27(13) | |
O2 | Na1 | O4 | 93.78(6) | O4 | C12 | C13 | 110.53(15) | |
O2 | Na1 | N1 | 69.43(6) | C14 | C12 | C13 | 110.83(14) | |
O2 | Na1 | C1 | 100.75(6) | O3 | C9 | C10 | 110.36(15) | |
N1 | Na1 | Na11 | 125.96(5) | O3 | C9 | C11 | 109.16(15) | |
N1 | Na1 | O11 | 150.07(4) | C10 | C9 | C11 | 111.18(15) | |
N1 | Na1 | O41 | 90.63(5) | N1 | C6 | C7 | 112.29(13) | |
N1 | Na1 | C1 | 52.75(5) | O2 | C7 | C6 | 108.13(13) | |
C1 | Na1 | Na11 | 85.31(6) | N1 | C4 | C1 | 115.67(13) | |
C1 | Na1 | O11 | 121.06(5) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H12 | 7094 | 5564 | 7902 | 23 |
H9 | 8132 | 7299 | 3535 | 25 |
H2A | 4356 | 879 | 4623 | 29 |
H2B | 2697 | -657 | 4032 | 29 |
H2C | 3191 | 759 | 5361 | 29 |
H6A | 4032 | -686 | 1114 | 23 |
H6B | 4328 | -351 | 2683 | 23 |
H3A | 602 | 684 | 4251 | 36 |
H3B | 47 | -698 | 2867 | 36 |
H3C | 51 | 838 | 2796 | 36 |
H7A | 6809 | 303 | 2600 | 23 |
H7B | 6564 | 1399 | 1833 | 23 |
H8A | 9178 | 3176 | 3843 | 39 |
H8B | 9063 | 2164 | 4743 | 39 |
H8C | 9179 | 3799 | 5306 | 39 |
H4A | 1759 | -623 | 1701 | 20 |
H4B | 1508 | 758 | 1468 | 20 |
H10A | 5129 | 5879 | 1135 | 48 |
H10B | 6743 | 7284 | 1383 | 48 |
H10C | 5862 | 7500 | 2341 | 48 |
H14A | 6581 | 3039 | 6895 | 41 |
H14B | 7734 | 3750 | 8515 | 41 |
H14C | 8476 | 3615 | 7431 | 41 |
H5A | 3225 | 2200 | 758 | 36 |
H5B | 2723 | 475 | -85 | 36 |
H5C | 4574 | 1759 | 634 | 36 |
H13A | 10417 | 6389 | 8631 | 49 |
H13B | 9680 | 6579 | 9713 | 49 |
H13C | 9761 | 7591 | 8813 | 49 |
H11A | 8192 | 4983 | 2742 | 50 |
H11B | 8243 | 5783 | 1668 | 50 |
H11C | 6598 | 4367 | 1353 | 50 |
H3 | 6490(30) | 6360(30) | 4250(30) | 52(7) |
H4 | 7620(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.
Crystal structure determination of [mo_B0636_0m]
Crystal Data for C14H34NNaO4 (M =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)°, V = 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)
This report has been created with Olex2, compiled on 2018.04.18 svn.r3501 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.