Identification code | mo_B0747_0m_4 |
Empirical formula | C19H47KLi3N3O5Si |
Formula weight | 485.60 |
Temperature/K | 100.03 |
Crystal system | triclinic |
Space group | P-1 |
a/Å | 10.740(3) |
b/Å | 11.012(3) |
c/Å | 14.879(4) |
α/° | 86.695(9) |
β/° | 78.411(9) |
γ/° | 68.404(9) |
Volume/Å3 | 1602.5(7) |
Z | 2 |
ρcalcg/cm3 | 1.006 |
μ/mm‑1 | 0.229 |
F(000) | 528.0 |
Crystal size/mm3 | 0.55 × 0.21 × 0.18 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.538 to 51.998 |
Index ranges | -12 ≤ h ≤ 13, -13 ≤ k ≤ 13, 0 ≤ l ≤ 18 |
Reflections collected | 6289 |
Independent reflections | 6289 [Rint = 0.0000, Rsigma = 0.0474] |
Data/restraints/parameters | 6289/1/328 |
Goodness-of-fit on F2 | 1.057 |
Final R indexes [I>=2σ (I)] | R1 = 0.0645, wR2 = 0.1621 |
Final R indexes [all data] | R1 = 0.0901, wR2 = 0.1728 |
Largest diff. peak/hole / e Å-3 | 0.57/-0.40 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
C1 | 7381(5) | 4307(4) | 838(3) | 70.4(11) |
C2 | 7478(4) | 6938(3) | 1171(3) | 63.4(10) |
C3 | 9853(4) | 4517(4) | 1396(3) | 73.9(12) |
C4 | 7111(3) | 5602(3) | 5225(2) | 34.3(6) |
C5 | 8045(3) | 6237(3) | 4638(2) | 38.7(7) |
C6 | 8246(3) | 7773(3) | 3443(2) | 46.9(8) |
C7 | 6321(3) | 8450(3) | 4705(2) | 46.7(8) |
C8 | 3513(3) | 8105(3) | 3348(2) | 46.2(8) |
C12 | 2784(3) | 8454(3) | 6137(2) | 38.7(7) |
C13 | 1300(3) | 8678(3) | 6609(2) | 42.0(8) |
C14 | 745(4) | 7923(3) | 5292(3) | 49.4(9) |
C15 | -596(3) | 7949(3) | 6782(3) | 54.1(10) |
C16 | 5560(4) | 8230(4) | 7449(3) | 73.7(11) |
C17 | 4752(7) | 9168(5) | 8190(4) | 116(2) |
C18 | 5487(9) | 8633(6) | 8967(5) | 152(3) |
C19 | 6122(5) | 7180(5) | 8785(3) | 84.8(13) |
K1 | 5138.2(6) | 5298.4(6) | 7134.2(4) | 37.82(19) |
Li1 | 7458(4) | 3949(4) | 3642(3) | 33.4(10) |
Li2 | 6183(4) | 6385(4) | 3595(3) | 34.6(10) |
Li3 | 4329(4) | 6265(4) | 4949(3) | 29.5(9) |
N1 | 7285(2) | 7339(2) | 4103.4(16) | 36.2(6) |
N2 | 3033(3) | 6950(3) | 2132.8(19) | 60.4(8) |
N3 | 784(2) | 7763(2) | 6279.6(17) | 37.6(6) |
O1 | 7260.8(19) | 5131.9(17) | 2654.0(13) | 35.1(4) |
O2 | 6383.8(17) | 5195.5(15) | 4701.5(12) | 27.8(4) |
O3 | 4277.9(18) | 6988.0(17) | 3761.2(13) | 34.6(4) |
O4 | 3639.5(17) | 7140.1(16) | 6133.7(12) | 31.6(4) |
O5 | 5985(3) | 6985(2) | 7907(2) | 76.8(8) |
Si1 | 7943.6(8) | 5214.6(8) | 1607.1(6) | 39.6(2) |
C9A | 2435(6) | 7822(5) | 2903(4) | 50.5(16) |
C10A | 1897(6) | 6427(7) | 1983(4) | 62.2(14) |
C9B | 3579(8) | 8123(7) | 2400(5) | 39(2) |
C10B | 1734(10) | 7303(11) | 2531(8) | 64(2) |
C2AA | 3356(13) | 7000(13) | 1110(9) | 64(2) |
C1AA | 3484(8) | 7443(8) | 1283(5) | 62.2(14) |
C0AA | 1590(40) | 8660(40) | 5800(30) | 42.0(8) |
C10 | 350(40) | 8260(40) | 7370(30) | 54.1(10) |
C3AA | -350(40) | 7850(40) | 5850(30) | 49.4(9) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
C1 | 105(3) | 71(3) | 41(2) | -4.6(18) | -4(2) | -43(2) |
C2 | 68(2) | 53(2) | 61(2) | 14.5(17) | 5.8(19) | -24.0(18) |
C3 | 47(2) | 93(3) | 55(2) | 15(2) | 13.4(17) | -9(2) |
C4 | 32.9(14) | 29.4(14) | 39.8(16) | -0.2(11) | 1.6(12) | -14.8(12) |
C5 | 32.3(15) | 35.2(15) | 51.0(18) | -5.0(13) | 0.2(13) | -18.3(12) |
C6 | 47.9(18) | 42.2(17) | 54(2) | -4.6(14) | 11.1(15) | -30.2(15) |
C7 | 51.6(19) | 31.9(15) | 52.5(19) | -7.7(13) | 12.2(15) | -20.7(14) |
C8 | 39.2(17) | 38.6(16) | 51(2) | 13.6(14) | -0.9(14) | -9.3(13) |
C12 | 41.0(16) | 25.5(13) | 49.5(18) | -2.5(12) | -0.7(13) | -15.9(12) |
C13 | 37.6(17) | 25.3(15) | 54(2) | -6.1(14) | 3.1(15) | -6.3(13) |
C14 | 47(2) | 42.7(19) | 59(2) | 7.8(16) | -11.8(17) | -17.9(16) |
C15 | 29.9(17) | 43.7(19) | 76(3) | 0.8(18) | 10.0(16) | -9.1(15) |
C16 | 73(3) | 61(2) | 86(3) | -3(2) | -6(2) | -28(2) |
C17 | 142(5) | 60(3) | 105(4) | -12(3) | 13(4) | -7(3) |
C18 | 237(9) | 91(4) | 124(5) | -43(4) | -65(6) | -35(5) |
C19 | 94(3) | 82(3) | 77(3) | -10(2) | -29(3) | -22(3) |
K1 | 39.4(4) | 34.8(3) | 41.0(4) | 1.3(3) | -3.8(3) | -17.6(3) |
Li1 | 35(2) | 24(2) | 37(3) | -1.9(18) | 3(2) | -10.6(18) |
Li2 | 33(2) | 28(2) | 38(3) | -1.9(19) | 10(2) | -14.1(19) |
Li3 | 29(2) | 24(2) | 33(2) | -2.5(17) | 3.3(18) | -11.2(17) |
N1 | 36.4(13) | 26.1(11) | 43.6(14) | -5.3(10) | 9.9(10) | -17(1) |
N2 | 53.1(18) | 64.2(19) | 42.3(17) | -5.6(14) | -6.9(13) | 3.2(14) |
N3 | 30.3(12) | 28.0(12) | 47.2(15) | -0.6(10) | 6.5(10) | -9.2(10) |
O1 | 36.5(10) | 31(1) | 33.6(11) | -1.9(8) | 8.6(8) | -15.1(8) |
O2 | 26.9(9) | 22.4(8) | 33.9(10) | -2.6(7) | 2.8(7) | -12.9(7) |
O3 | 30.3(10) | 28.9(9) | 39.6(11) | 5.3(8) | 1.7(8) | -10.3(8) |
O4 | 32.1(10) | 21.3(9) | 37.4(11) | -4.1(7) | 5.3(8) | -10.8(7) |
O5 | 103(2) | 50.2(15) | 86(2) | -5.5(14) | -50.2(17) | -21.1(15) |
Si1 | 39.9(5) | 36.1(4) | 34.4(5) | -0.2(3) | 8.6(3) | -12.2(4) |
C9A | 51(3) | 41(3) | 46(3) | -1(2) | -1(2) | -5(2) |
C10A | 54(3) | 78(3) | 53(3) | 0(2) | -8(2) | -24(2) |
C9B | 34(4) | 37(4) | 40(5) | 6(3) | -1(3) | -8(3) |
C10B | 53(4) | 72(6) | 65(5) | -13(4) | -8(4) | -20(4) |
C2AA | 53(4) | 72(6) | 65(5) | -13(4) | -8(4) | -20(4) |
C1AA | 54(3) | 78(3) | 53(3) | 0(2) | -8(2) | -24(2) |
C0AA | 37.6(17) | 25.3(15) | 54(2) | -6.1(14) | 3.1(15) | -6.3(13) |
C10 | 29.9(17) | 43.7(19) | 76(3) | 0.8(18) | 10.0(16) | -9.1(15) |
C3AA | 47(2) | 42.7(19) | 59(2) | 7.8(16) | -11.8(17) | -17.9(16) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
C1 | Si1 | 1.879(4) | Li1 | Li31 | 2.606(6) | |
C2 | Si1 | 1.887(3) | Li1 | N31 | 2.139(5) | |
C3 | Si1 | 1.872(4) | Li1 | O1 | 1.899(5) | |
C4 | C5 | 1.534(4) | Li1 | O2 | 2.013(5) | |
C4 | O2 | 1.399(3) | Li1 | O41 | 1.943(5) | |
C5 | N1 | 1.480(4) | Li2 | K11 | 3.067(5) | |
C6 | N1 | 1.469(3) | Li2 | Li3 | 2.567(6) | |
C7 | N1 | 1.480(4) | Li2 | N1 | 2.109(5) | |
C8 | O3 | 1.392(3) | Li2 | O1 | 1.897(5) | |
C8 | C9A | 1.572(7) | Li2 | O2 | 2.039(5) | |
C8 | C9B | 1.396(8) | Li2 | O3 | 1.871(5) | |
C12 | C13 | 1.541(4) | Li3 | K11 | 3.475(5) | |
C12 | O4 | 1.399(3) | Li3 | Li11 | 2.606(6) | |
C12 | C0AA | 1.41(4) | Li3 | Li31 | 2.636(8) | |
C13 | N3 | 1.463(4) | Li3 | O2 | 2.050(4) | |
C14 | N3 | 1.477(4) | Li3 | O21 | 2.024(4) | |
C15 | N3 | 1.466(4) | Li3 | O3 | 1.898(5) | |
C16 | C17 | 1.457(6) | Li3 | O4 | 1.931(5) | |
C16 | O5 | 1.451(5) | N2 | K11 | 2.854(3) | |
C17 | C18 | 1.501(9) | N2 | C9A | 1.424(6) | |
C18 | C19 | 1.507(7) | N2 | C10A | 1.585(7) | |
C19 | O5 | 1.381(5) | N2 | C9B | 1.698(9) | |
K1 | Li11 | 3.046(5) | N2 | C10B | 1.320(10) | |
K1 | Li21 | 3.068(5) | N2 | C2AA | 1.494(14) | |
K1 | Li31 | 3.475(5) | N2 | C1AA | 1.413(8) | |
K1 | Li3 | 3.538(5) | N3 | Li11 | 2.139(5) | |
K1 | N21 | 2.854(3) | N3 | C0AA | 1.58(4) | |
K1 | O11 | 2.742(2) | N3 | C10 | 1.67(5) | |
K1 | O31 | 2.720(2) | N3 | C3AA | 1.465(19) | |
K1 | O4 | 2.671(2) | O1 | K11 | 2.742(2) | |
K1 | O5 | 2.740(3) | O1 | Si1 | 1.5956(19) | |
K1 | Si11 | 3.6802(12) | O2 | Li31 | 2.024(4) | |
K1 | C9A1 | 3.461(5) | O3 | K11 | 2.720(2) | |
Li1 | C121 | 2.747(5) | O4 | Li11 | 1.943(5) | |
Li1 | C131 | 2.715(5) | Si1 | K11 | 3.6803(13) | |
Li1 | K11 | 3.046(5) | C10A | K11 | 3.524(6) | |
Li1 | Li2 | 2.528(6) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
O2 | C4 | C5 | 112.3(2) | O3 | Li2 | K11 | 61.29(14) | |
N1 | C5 | C4 | 112.0(2) | O3 | Li2 | Li1 | 117.8(2) | |
O3 | C8 | C9A | 110.4(3) | O3 | Li2 | Li3 | 47.53(15) | |
O3 | C8 | C9B | 120.4(4) | O3 | Li2 | N1 | 124.7(2) | |
O4 | C12 | C13 | 112.3(2) | O3 | Li2 | O1 | 119.5(3) | |
O4 | C12 | C0AA | 113.7(16) | O3 | Li2 | O2 | 97.33(19) | |
N3 | C13 | C12 | 112.4(2) | K11 | Li3 | K1 | 135.85(12) | |
O5 | C16 | C17 | 104.1(4) | Li11 | Li3 | K11 | 121.64(17) | |
C16 | C17 | C18 | 102.5(5) | Li11 | Li3 | K1 | 57.04(13) | |
C17 | C18 | C19 | 104.7(4) | Li11 | Li3 | Li31 | 87.8(2) | |
O5 | C19 | C18 | 106.2(4) | Li2 | Li3 | K1 | 120.46(18) | |
Li11 | K1 | Li21 | 48.85(12) | Li2 | Li3 | K11 | 58.74(14) | |
Li11 | K1 | Li3 | 45.90(11) | Li2 | Li3 | Li11 | 177.1(2) | |
Li11 | K1 | Li31 | 67.39(11) | Li2 | Li3 | Li31 | 89.8(2) | |
Li11 | K1 | Si11 | 57.56(8) | Li31 | Li3 | K11 | 69.18(18) | |
Li11 | K1 | C9A1 | 125.20(13) | Li31 | Li3 | K1 | 66.67(18) | |
Li21 | K1 | Li31 | 45.67(10) | O21 | Li3 | K1 | 75.59(14) | |
Li21 | K1 | Li3 | 67.13(11) | O2 | Li3 | K1 | 74.72(14) | |
Li21 | K1 | Si11 | 56.16(8) | O21 | Li3 | K11 | 76.51(14) | |
Li21 | K1 | C9A1 | 76.83(13) | O2 | Li3 | K11 | 76.88(13) | |
Li31 | K1 | Li3 | 44.15(12) | O21 | Li3 | Li11 | 49.61(14) | |
Li31 | K1 | Si11 | 101.52(7) | O2 | Li3 | Li11 | 126.2(2) | |
Li3 | K1 | Si11 | 102.76(7) | O21 | Li3 | Li2 | 129.3(2) | |
N21 | K1 | Li11 | 138.38(11) | O2 | Li3 | Li2 | 50.94(15) | |
N21 | K1 | Li21 | 90.84(11) | O21 | Li3 | Li31 | 50.11(14) | |
N21 | K1 | Li3 | 136.05(9) | O2 | Li3 | Li31 | 49.24(14) | |
N21 | K1 | Li31 | 93.03(9) | O21 | Li3 | O2 | 99.35(19) | |
N21 | K1 | Si11 | 94.05(7) | O3 | Li3 | K1 | 163.9(2) | |
N21 | K1 | C9A1 | 23.65(11) | O3 | Li3 | K11 | 51.10(12) | |
O11 | K1 | Li11 | 37.85(9) | O3 | Li3 | Li11 | 136.1(2) | |
O11 | K1 | Li21 | 37.60(9) | O3 | Li3 | Li2 | 46.65(15) | |
O11 | K1 | Li3 | 80.59(8) | O3 | Li3 | Li31 | 117.5(3) | |
O11 | K1 | Li31 | 80.38(8) | O3 | Li3 | O21 | 119.5(2) | |
O11 | K1 | N21 | 105.22(8) | O3 | Li3 | O2 | 96.12(19) | |
O11 | K1 | Si11 | 23.44(4) | O3 | Li3 | O4 | 129.2(2) | |
O11 | K1 | C9A1 | 103.19(11) | O4 | Li3 | K11 | 167.7(2) | |
O31 | K1 | Li11 | 81.79(9) | O4 | Li3 | K1 | 48.17(11) | |
O31 | K1 | Li21 | 37.12(9) | O4 | Li3 | Li11 | 47.90(14) | |
O31 | K1 | Li31 | 32.91(8) | O4 | Li3 | Li2 | 132.1(2) | |
O31 | K1 | Li3 | 75.74(8) | O4 | Li3 | Li31 | 113.1(3) | |
O31 | K1 | N21 | 65.14(8) | O4 | Li3 | O2 | 114.1(2) | |
O31 | K1 | O11 | 73.20(6) | O4 | Li3 | O21 | 95.60(19) | |
O31 | K1 | O5 | 150.09(8) | C5 | N1 | Li2 | 97.16(19) | |
O31 | K1 | Si11 | 86.09(4) | C6 | N1 | C5 | 109.9(2) | |
O31 | K1 | C9A1 | 44.43(10) | C6 | N1 | C7 | 109.8(2) | |
O4 | K1 | Li11 | 39.04(9) | C6 | N1 | Li2 | 118.3(2) | |
O4 | K1 | Li21 | 83.09(10) | C7 | N1 | C5 | 111.8(2) | |
O4 | K1 | Li31 | 75.88(8) | C7 | N1 | Li2 | 109.3(2) | |
O4 | K1 | Li3 | 32.60(8) | C9A | N2 | K11 | 102.8(3) | |
O4 | K1 | N21 | 168.66(7) | C9A | N2 | C10A | 106.1(4) | |
O4 | K1 | O11 | 75.61(6) | C10A | N2 | K11 | 101.2(3) | |
O4 | K1 | O31 | 104.92(6) | C9B | N2 | K11 | 100.7(3) | |
O4 | K1 | O5 | 93.90(7) | C10B | N2 | K11 | 115.7(5) | |
O4 | K1 | Si11 | 90.53(5) | C10B | N2 | C9B | 106.8(6) | |
O4 | K1 | C9A1 | 145.03(10) | C10B | N2 | C2AA | 117.4(7) | |
O5 | K1 | Li11 | 125.75(10) | C2AA | N2 | K11 | 113.4(5) | |
O5 | K1 | Li21 | 172.56(11) | C2AA | N2 | C9B | 99.5(6) | |
O5 | K1 | Li31 | 140.11(10) | C1AA | N2 | K11 | 119.7(4) | |
O5 | K1 | Li3 | 113.46(9) | C1AA | N2 | C9A | 118.3(5) | |
O5 | K1 | N21 | 93.21(9) | C1AA | N2 | C10A | 106.7(4) | |
O5 | K1 | O11 | 135.04(8) | C13 | N3 | C14 | 111.6(2) | |
O5 | K1 | Si11 | 117.25(8) | C13 | N3 | C15 | 111.1(2) | |
O5 | K1 | C9A1 | 109.01(12) | C13 | N3 | Li11 | 96.0(2) | |
C9A1 | K1 | Li3 | 112.44(11) | C14 | N3 | Li11 | 105.2(2) | |
C9A1 | K1 | Li31 | 69.58(12) | C15 | N3 | C14 | 108.2(3) | |
C9A1 | K1 | Si11 | 101.30(10) | C15 | N3 | Li11 | 124.1(2) | |
C121 | Li1 | K11 | 84.15(14) | C0AA | N3 | Li11 | 96.6(14) | |
C131 | Li1 | C121 | 32.78(10) | C0AA | N3 | C10 | 103(2) | |
C131 | Li1 | K11 | 105.69(16) | C10 | N3 | Li11 | 99.5(16) | |
Li2 | Li1 | C121 | 145.4(2) | C3AA | N3 | Li11 | 126.2(18) | |
Li2 | Li1 | C131 | 169.5(3) | C3AA | N3 | C0AA | 113(2) | |
Li2 | Li1 | K11 | 66.03(15) | C3AA | N3 | C10 | 115(3) | |
Li2 | Li1 | Li31 | 91.32(19) | Li1 | O1 | K11 | 79.79(15) | |
Li31 | Li1 | C121 | 63.96(14) | Li2 | O1 | K11 | 80.56(15) | |
Li31 | Li1 | C131 | 93.03(17) | Li2 | O1 | Li1 | 83.5(2) | |
Li31 | Li1 | K11 | 77.06(15) | Si1 | O1 | K11 | 113.45(10) | |
N31 | Li1 | C121 | 59.95(13) | Si1 | O1 | Li1 | 140.06(17) | |
N31 | Li1 | C131 | 32.40(11) | Si1 | O1 | Li2 | 134.41(17) | |
N31 | Li1 | K11 | 137.8(2) | C4 | O2 | Li1 | 117.8(2) | |
N31 | Li1 | Li2 | 154.2(2) | C4 | O2 | Li2 | 106.25(19) | |
N31 | Li1 | Li31 | 102.9(2) | C4 | O2 | Li3 | 113.82(19) | |
O1 | Li1 | C121 | 131.9(2) | C4 | O2 | Li31 | 124.4(2) | |
O1 | Li1 | C131 | 122.9(2) | Li1 | O2 | Li2 | 77.17(19) | |
O1 | Li1 | K11 | 62.37(14) | Li1 | O2 | Li3 | 126.9(2) | |
O1 | Li1 | Li2 | 48.22(15) | Li1 | O2 | Li31 | 80.42(18) | |
O1 | Li1 | Li31 | 130.7(2) | Li2 | O2 | Li3 | 77.76(18) | |
O1 | Li1 | N31 | 125.7(2) | Li31 | O2 | Li2 | 129.3(2) | |
O1 | Li1 | O2 | 100.1(2) | Li31 | O2 | Li3 | 80.65(19) | |
O1 | Li1 | O41 | 119.5(3) | C8 | O3 | K11 | 115.17(18) | |
O2 | Li1 | C121 | 113.38(19) | C8 | O3 | Li2 | 123.1(2) | |
O2 | Li1 | C131 | 136.8(2) | C8 | O3 | Li3 | 138.9(2) | |
O2 | Li1 | K11 | 88.68(16) | Li2 | O3 | K11 | 81.59(15) | |
O2 | Li1 | Li2 | 51.88(15) | Li2 | O3 | Li3 | 85.8(2) | |
O2 | Li1 | Li31 | 49.97(14) | Li3 | O3 | K11 | 95.99(14) | |
O2 | Li1 | N31 | 124.2(2) | C12 | O4 | K1 | 143.75(17) | |
O41 | Li1 | C121 | 28.69(10) | C12 | O4 | Li11 | 109.5(2) | |
O41 | Li1 | C131 | 60.65(14) | C12 | O4 | Li3 | 116.0(2) | |
O41 | Li1 | K11 | 59.99(13) | Li11 | O4 | K1 | 80.97(15) | |
O41 | Li1 | Li2 | 116.7(2) | Li3 | O4 | K1 | 99.22(14) | |
O41 | Li1 | Li31 | 47.53(14) | Li3 | O4 | Li11 | 84.57(19) | |
O41 | Li1 | N31 | 88.44(18) | C16 | O5 | K1 | 108.8(2) | |
O41 | Li1 | O2 | 95.6(2) | C19 | O5 | C16 | 109.5(3) | |
Li1 | Li2 | K11 | 65.13(15) | C19 | O5 | K1 | 134.1(3) | |
Li1 | Li2 | Li3 | 91.05(19) | C1 | Si1 | C2 | 106.15(19) | |
Li3 | Li2 | K11 | 75.58(15) | C1 | Si1 | K11 | 71.19(13) | |
N1 | Li2 | K11 | 173.3(2) | C2 | Si1 | K11 | 109.95(12) | |
N1 | Li2 | Li1 | 108.3(2) | C3 | Si1 | C1 | 107.6(2) | |
N1 | Li2 | Li3 | 106.1(2) | C3 | Si1 | C2 | 105.54(18) | |
O1 | Li2 | K11 | 61.85(14) | C3 | Si1 | K11 | 143.32(13) | |
O1 | Li2 | Li1 | 48.27(15) | O1 | Si1 | C1 | 110.76(14) | |
O1 | Li2 | Li3 | 129.7(2) | O1 | Si1 | C2 | 113.45(14) | |
O1 | Li2 | N1 | 113.5(2) | O1 | Si1 | C3 | 112.92(15) | |
O1 | Li2 | O2 | 99.2(2) | O1 | Si1 | K11 | 43.11(7) | |
O2 | Li2 | K11 | 87.61(15) | N2 | C9A | C8 | 113.4(4) | |
O2 | Li2 | Li1 | 50.95(15) | N2 | C10A | K11 | 52.6(2) | |
O2 | Li2 | Li3 | 51.30(14) | C8 | C9B | N2 | 107.7(5) | |
O2 | Li2 | N1 | 88.6(2) | C12 | C0AA | N3 | 113(3) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H1A | 7576 | 3407 | 1047 | 106 |
H1B | 7875 | 4300 | 207 | 106 |
H1C | 6398 | 4740 | 859 | 106 |
H2A | 7901 | 6920 | 522 | 95 |
H2B | 7808 | 7441 | 1524 | 95 |
H2C | 6484 | 7348 | 1242 | 95 |
H3A | 10174 | 4882 | 1850 | 111 |
H3B | 10219 | 4740 | 778 | 111 |
H3C | 10167 | 3565 | 1452 | 111 |
H4A | 7670 | 4839 | 5538 | 41 |
H4B | 6458 | 6236 | 5702 | 41 |
H5A | 8491 | 6558 | 5042 | 46 |
H5B | 8770 | 5572 | 4211 | 46 |
H6A | 8792 | 8062 | 3774 | 70 |
H6B | 7736 | 8498 | 3089 | 70 |
H6C | 8850 | 7046 | 3025 | 70 |
H7A | 5638 | 8174 | 5111 | 70 |
H7B | 5864 | 9172 | 4327 | 70 |
H7C | 6822 | 8740 | 5074 | 70 |
H8AA | 4127 | 8391 | 2869 | 55 |
H8AB | 3038 | 8818 | 3812 | 55 |
H8BC | 3774 | 8828 | 3504 | 55 |
H8BD | 2545 | 8317 | 3644 | 55 |
H12A | 2799 | 8755 | 5496 | 46 |
H12B | 3137 | 8983 | 6458 | 46 |
H12C | 3296 | 8949 | 5755 | 46 |
H12D | 2528 | 8808 | 6772 | 46 |
H13A | 1251 | 8582 | 7280 | 50 |
H13B | 709 | 9582 | 6497 | 50 |
H14A | 170 | 8823 | 5183 | 74 |
H14B | 366 | 7319 | 5099 | 74 |
H14C | 1672 | 7734 | 4940 | 74 |
H15A | -605 | 7909 | 7443 | 81 |
H15B | -875 | 7259 | 6602 | 81 |
H15C | -1232 | 8803 | 6637 | 81 |
H16A | 5005 | 8223 | 6995 | 88 |
H16B | 6360 | 8436 | 7134 | 88 |
H17A | 3800 | 9199 | 8343 | 139 |
H17B | 4747 | 10055 | 8029 | 139 |
H18A | 4842 | 8834 | 9564 | 182 |
H18B | 6197 | 9004 | 8972 | 182 |
H19A | 7098 | 6849 | 8831 | 102 |
H19B | 5647 | 6719 | 9234 | 102 |
H9AA | 1891 | 7447 | 3373 | 61 |
H9AB | 1804 | 8658 | 2708 | 61 |
H10A | 2270 | 5787 | 1475 | 93 |
H10B | 1111 | 7159 | 1837 | 93 |
H10C | 1606 | 6011 | 2544 | 93 |
H9BA | 4528 | 7947 | 2073 | 47 |
H9BB | 2991 | 8990 | 2217 | 47 |
H10D | 1379 | 6645 | 2398 | 96 |
H10E | 1214 | 8148 | 2295 | 96 |
H10F | 1646 | 7378 | 3196 | 96 |
H2AA | 2826 | 7868 | 910 | 96 |
H2AB | 3120 | 6339 | 844 | 96 |
H2AC | 4332 | 6827 | 905 | 96 |
H1AA | 4181 | 7791 | 1347 | 93 |
H1AB | 2710 | 8141 | 1094 | 93 |
H1AC | 3873 | 6738 | 819 | 93 |
H0AA | 1829 | 8478 | 5135 | 50 |
H0AB | 979 | 9584 | 5907 | 50 |
H10G | 1170 | 8046 | 7633 | 81 |
H10H | -237 | 7816 | 7720 | 81 |
H10I | -154 | 9205 | 7412 | 81 |
H3AA | -921 | 8768 | 5790 | 74 |
H3AB | -904 | 7398 | 6221 | 74 |
H3AC | 5 | 7436 | 5234 | 74 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
H8AA | 0.626(6) | H8AB | 0.626(6) | H8BC | 0.374(6) | ||
H8BD | 0.374(6) | H12A | 0.928(3) | H12B | 0.928(3) | ||
H12C | 0.072(3) | H12D | 0.072(3) | C13 | 0.928(3) | ||
H13A | 0.928(3) | H13B | 0.928(3) | C14 | 0.928(3) | ||
H14A | 0.928(3) | H14B | 0.928(3) | H14C | 0.928(3) | ||
C15 | 0.928(3) | H15A | 0.928(3) | H15B | 0.928(3) | ||
H15C | 0.928(3) | C9A | 0.626(6) | H9AA | 0.626(6) | ||
H9AB | 0.626(6) | C10A | 0.626(6) | H10A | 0.626(6) | ||
H10B | 0.626(6) | H10C | 0.626(6) | C9B | 0.374(6) | ||
H9BA | 0.374(6) | H9BB | 0.374(6) | C10B | 0.374(6) | ||
H10D | 0.374(6) | H10E | 0.374(6) | H10F | 0.374(6) | ||
C2AA | 0.374(6) | H2AA | 0.374(6) | H2AB | 0.374(6) | ||
H2AC | 0.374(6) | C1AA | 0.626(6) | H1AA | 0.626(6) | ||
H1AB | 0.626(6) | H1AC | 0.626(6) | C0AA | 0.072(3) | ||
H0AA | 0.072(3) | H0AB | 0.072(3) | C10 | 0.072(3) | ||
H10G | 0.072(3) | H10H | 0.072(3) | H10I | 0.072(3) | ||
C3AA | 0.072(3) | H3AA | 0.072(3) | H3AB | 0.072(3) | ||
H3AC | 0.072(3) |
Number | X | Y | Z | Volume | Electron count | Content |
---|---|---|---|---|---|---|
1 | 0.000 | 0.000 | 0.000 | 180.4 | 32.3 | ? |
Experimental
Single crystals of C19H47KLi3N3O5Si [mo_B0747_0m_4] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 100.03 K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program using Intrinsic Phasing and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0747_0m_4]
Crystal Data for C19H47KLi3N3O5Si (M =485.60 g/mol): triclinic, space group P-1 (no. 2), a = 10.740(3) Å, b = 11.012(3) Å, c = 14.879(4) Å, α = 86.695(9)°, β = 78.411(9)°, γ = 68.404(9)°, V = 1602.5(7) Å3, Z = 2, T = 100.03 K, μ(MoKα) = 0.229 mm-1, Dcalc = 1.006 g/cm3, 6289 reflections measured (4.538° ≤ 2Θ ≤ 51.998°), 6289 unique (Rint = 0.0000, Rsigma = 0.0474) which were used in all calculations. The final R1 was 0.0645 (I > 2σ(I)) and wR2 was 0.1728 (all data).
Refinement model description
Number of restraints - 1, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups, All C(H,H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
N3-C3AA
1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2AA) = Uanis(C10B)
Uanis(C10A) = Uanis(C1AA)
Uanis(C3AA) = Uanis(C14)
Uanis(C15) = Uanis(C10)
Uanis(C13) = Uanis(C0AA)
4. Others
Sof(H8BC)=Sof(H8BD)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10D)=
Sof(H10E)=Sof(H10F)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=1-FVAR(1)
Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=
Sof(H10B)=Sof(H10C)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
Sof(H12C)=Sof(H12D)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C10)=Sof(H10G)=
Sof(H10H)=Sof(H10I)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(2)
Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=
Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
C4(H4A,H4B), C5(H5A,H5B), C8(H8AA,H8AB), C8(H8BC,H8BD), C12(H12A,H12B),
C12(H12C,H12D), C13(H13A,H13B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
C19(H19A,H19B), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C0AA(H0AA,H0AB)
5.b Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C7(H7A,
H7B,H7C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C10A(H10A,H10B,H10C),
C10B(H10D,H10E,H10F), C2AA(H2AA,H2AB,H2AC), C1AA(H1AA,H1AB,H1AC), C10(H10G,
H10H,H10I), C3AA(H3AA,H3AB,H3AC)
This report has been created with Olex2, compiled on 2017.03.28 svn.r3405 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.