Identification code | 3F-nondecomposition |
Empirical formula | C42H42F3.27N2O6 |
Formula weight | 732.90 |
Temperature/K | 293(2) |
Crystal system | triclinic |
Space group | P-1 |
a/Å | 7.453 |
b/Å | 14.683 |
c/Å | 20.135 |
α/° | 66.42 |
β/° | 79.76 |
γ/° | 93.67 |
Volume/Å3 | 1964.9 |
Z | 2 |
ρcalcg/cm3 | 1.239 |
μ/mm‑1 | 0.090 |
F(000) | 771.0 |
Crystal size/mm3 | 0.05 × 0.01 × 0.01 |
Radiation | Synchrotron (λ = 0.68882) |
2Θ range for data collection/° | 2.856 to 46.636 |
Index ranges | -8 ≤ h ≤ 8, -16 ≤ k ≤ 16, -22 ≤ l ≤ 22 |
Reflections collected | 16866 |
Independent reflections | 5707 [Rint = 0.0826, Rsigma = 0.0628] |
Data/restraints/parameters | 5707/105/523 |
Goodness-of-fit on F2 | 1.618 |
Final R indexes [I>=2σ (I)] | R1 = 0.1392, wR2 = 0.4116 |
Final R indexes [all data] | R1 = 0.1852, wR2 = 0.4455 |
Largest diff. peak/hole / e Å-3 | 0.36/-0.38 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
O1 | 15560(5) | -1359(3) | 6361(2) | 103.1(12) |
O2 | 9839(6) | 1921(3) | 4950(2) | 118.4(14) |
O3 | 11258(6) | -1291(4) | 7115(2) | 117.7(14) |
O4 | 14557(8) | 2475(3) | 5545(2) | 135.3(17) |
O5 | 15977(7) | -1221(3) | 7409(2) | 127.5(15) |
C6 | 15083(7) | 295(4) | 5605(3) | 95.0(16) |
O7 | 9849(9) | 2562(4) | 5796(3) | 145.8(19) |
C8 | 9942(8) | 947(5) | 4920(4) | 107.3(18) |
C9 | 15270(7) | -686(4) | 5649(3) | 97.4(16) |
C10 | 14736(7) | 865(5) | 7452(3) | 102.2(17) |
N11 | 14203(7) | 2497(4) | 6711(3) | 108.5(15) |
C12 | 10082(8) | 732(5) | 6144(3) | 102.8(17) |
C13 | 15162(8) | 260(5) | 6357(3) | 101.8(17) |
C14 | 14282(8) | 1826(5) | 7436(3) | 106.0(18) |
N15 | 10329(7) | -837(4) | 8098(3) | 113.3(16) |
C16 | 14884(8) | 85(5) | 8148(3) | 112.1(19) |
C17 | 10121(7) | 204(5) | 5629(3) | 102.5(17) |
C18 | 15209(7) | -1042(4) | 5089(3) | 95.1(16) |
C19 | 14892(8) | 966(5) | 6665(3) | 103.8(17) |
C20 | 10126(7) | 364(4) | 6910(3) | 103.0(17) |
C21 | 9818(8) | 796(5) | 4300(3) | 105.9(18) |
C22 | 13963(10) | 1976(7) | 8102(4) | 115(2) |
C23 | 9309(9) | 1778(6) | 7416(4) | 118(2) |
C24 | 14092(11) | 1176(7) | 8775(4) | 127(2) |
C25 | 9883(9) | 60(5) | 8175(4) | 114.2(19) |
C26 | 9543(10) | 225(7) | 8818(5) | 126(2) |
F27 | 14687(11) | -583(6) | 9445(3) | 167(5) |
C28 | 10606(8) | -682(5) | 7354(3) | 104.2(18) |
C29 | 9749(8) | 838(5) | 7464(3) | 102.8(17) |
F30 | 13469(11) | 2772(7) | 8112(4) | 143(4) |
C31 | 14571(9) | 2044(5) | 6228(3) | 106.9(18) |
C32 | 9088(11) | 1155(7) | 8777(6) | 138(3) |
F33 | 9708(13) | -445(7) | 9444(4) | 150(5) |
C34 | 9899(9) | 1811(5) | 5673(4) | 113.8(19) |
C35 | 13740(9) | 3551(5) | 6475(4) | 116.2(19) |
C36 | 10763(10) | -1756(6) | 8692(4) | 130(2) |
C37 | 14531(10) | 282(7) | 8807(4) | 127(2) |
C38 | 15569(8) | -793(4) | 6778(4) | 105.4(18) |
F39 | 8598(13) | 2902(7) | 7967(5) | 151(5) |
C40 | 17038(15) | 4469(8) | 5877(5) | 181(4) |
F41 | 13737(12) | 1230(6) | 9413(4) | 153(5) |
C42 | 8969(10) | 1919(7) | 8089(6) | 136(2) |
C43 | 15315(13) | 4373(6) | 6403(5) | 151(3) |
F44 | 8939(17) | 1451(8) | 9322(5) | 159(6) |
C45 | 8954(17) | -2542(7) | 9194(6) | 206(5) |
C46 | 18839(13) | 5022(8) | 5997(7) | 193(4) |
C47 | 14560(15) | 5378(6) | 6251(5) | 169(3) |
C48 | 9680(20) | -3432(8) | 9812(7) | 251(7) |
C49 | 7790(19) | -2931(13) | 8817(9) | 281(8) |
C50 | 10640(50) | 6275(19) | 7341(17) | 299(11) |
C51 | 12320(30) | 6379(10) | 6756(11) | 237(7) |
C52 | 10720(30) | -3302(12) | 10322(10) | 335(9) |
C53 | 5850(20) | -3380(13) | 9265(11) | 331(9) |
C57 | 13220(20) | 5407(8) | 6944(7) | 221(5) |
C1 | 11330(40) | -4321(15) | 10781(15) | 429(14) |
C2 | 13030(40) | -4150(20) | 11078(19) | 479(18) |
C49A | 6880(30) | -2490(50) | 9350(60) | 281(8) |
C51A | 13780(100) | 5960(30) | 7370(30) | 237(7) |
C50A | 13270(70) | 6160(20) | 7930(20) | 299(11) |
C22A | 13963(10) | 1976(7) | 8102(4) | 115(2) |
C24A | 14092(11) | 1176(7) | 8775(4) | 127(2) |
C37A | 14531(10) | 282(7) | 8807(4) | 127(2) |
C42A | 8969(10) | 1919(7) | 8089(6) | 136(2) |
C32A | 9088(11) | 1155(7) | 8777(6) | 138(3) |
C26A | 9543(10) | 225(7) | 8818(5) | 126(2) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
O1 | 102(3) | 106(3) | 80(2) | -19(2) | -21.7(18) | 6(2) |
O2 | 132(3) | 101(3) | 106(3) | -25(2) | -33(2) | 13(2) |
O3 | 118(3) | 124(3) | 90(3) | -26(2) | -17(2) | 25(3) |
O4 | 195(5) | 111(3) | 92(3) | -33(2) | -43(3) | 8(3) |
O5 | 151(4) | 133(3) | 94(3) | -34(2) | -51(3) | 23(3) |
C6 | 81(3) | 103(4) | 82(3) | -24(3) | -16(2) | -6(3) |
O7 | 208(6) | 115(4) | 105(3) | -33(3) | -40(3) | 27(3) |
C8 | 88(4) | 108(5) | 100(4) | -21(3) | -17(3) | 2(3) |
C9 | 87(4) | 106(4) | 78(3) | -20(3) | -17(2) | -2(3) |
C10 | 83(3) | 119(5) | 84(4) | -26(3) | -20(3) | -9(3) |
N11 | 110(3) | 111(4) | 89(3) | -27(3) | -25(2) | -1(3) |
C12 | 88(4) | 105(4) | 94(4) | -26(3) | -11(3) | 3(3) |
C13 | 89(4) | 117(4) | 76(3) | -20(3) | -19(2) | -10(3) |
C14 | 90(4) | 121(5) | 88(4) | -37(3) | -2(3) | -12(3) |
N15 | 102(3) | 128(4) | 89(3) | -23(3) | -28(2) | 1(3) |
C16 | 100(4) | 136(5) | 79(4) | -32(3) | -12(3) | -15(3) |
C17 | 85(4) | 94(4) | 100(4) | -16(3) | -15(3) | 0(3) |
C18 | 77(3) | 111(4) | 80(3) | -28(3) | -9(2) | 0(3) |
C19 | 96(4) | 111(4) | 90(4) | -29(3) | -25(3) | -5(3) |
C20 | 82(3) | 97(4) | 105(4) | -23(3) | -11(3) | 3(3) |
C21 | 101(4) | 106(5) | 86(4) | -17(3) | -21(3) | 4(3) |
C22 | 107(5) | 132(6) | 89(4) | -37(4) | -10(3) | -5(4) |
C23 | 96(4) | 120(5) | 132(6) | -45(4) | -30(4) | 1(3) |
C24 | 131(5) | 148(7) | 81(4) | -35(4) | -11(3) | -14(5) |
C25 | 93(4) | 118(5) | 124(6) | -46(4) | -23(3) | -4(3) |
C26 | 115(5) | 128(6) | 135(7) | -53(6) | -31(4) | 3(4) |
F27 | 188(8) | 187(8) | 93(5) | -33(4) | -20(4) | -3(5) |
C28 | 93(4) | 119(5) | 85(4) | -28(3) | -21(3) | 2(3) |
C29 | 88(4) | 106(4) | 100(4) | -38(3) | -9(3) | -6(3) |
F30 | 152(6) | 159(8) | 110(5) | -62(4) | -6(4) | -2(5) |
C31 | 122(5) | 104(4) | 84(4) | -32(3) | -24(3) | -10(3) |
C32 | 116(5) | 136(7) | 145(7) | -46(6) | -27(5) | -8(4) |
F33 | 192(9) | 140(7) | 87(6) | -23(5) | -23(5) | -4(5) |
C34 | 125(5) | 99(5) | 104(5) | -30(4) | -26(3) | 12(4) |
C35 | 109(4) | 123(5) | 110(4) | -43(4) | -29(3) | 1(4) |
C36 | 120(5) | 146(6) | 96(4) | -20(4) | -29(3) | 13(4) |
C37 | 117(5) | 135(6) | 89(5) | -15(4) | -17(3) | -13(4) |
C38 | 96(4) | 104(4) | 100(4) | -25(4) | -32(3) | -1(3) |
F39 | 150(8) | 140(9) | 166(9) | -78(6) | -18(5) | -3(5) |
C40 | 199(10) | 167(8) | 139(7) | -42(6) | -16(7) | -26(7) |
F41 | 176(8) | 170(7) | 90(6) | -52(4) | 0(4) | -20(5) |
C42 | 112(5) | 135(7) | 168(8) | -75(6) | -26(5) | 2(4) |
C43 | 153(7) | 122(6) | 134(6) | -29(4) | -4(5) | -22(5) |
F44 | 210(11) | 155(9) | 95(7) | -59(6) | 9(6) | -5(7) |
C45 | 219(9) | 122(6) | 180(8) | 38(6) | -72(7) | -17(6) |
C46 | 130(7) | 185(9) | 246(11) | -78(8) | -46(7) | -29(6) |
C47 | 224(10) | 107(5) | 155(6) | -35(5) | -51(6) | 5(5) |
C48 | 336(16) | 175(9) | 165(9) | 13(7) | -103(9) | -56(10) |
C49 | 171(8) | 262(11) | 224(12) | 91(8) | -99(7) | -88(8) |
C50 | 450(20) | 189(13) | 273(19) | -153(15) | 21(16) | 38(16) |
C51 | 371(18) | 114(8) | 204(12) | -77(8) | 0(10) | -1(8) |
C52 | 490(20) | 253(14) | 212(13) | -11(11) | -188(13) | -23(14) |
C53 | 178(10) | 250(13) | 400(20) | 16(12) | -46(10) | -53(10) |
C57 | 313(13) | 147(7) | 197(9) | -83(7) | -22(8) | 2(7) |
C1 | 550(30) | 350(20) | 330(20) | -17(19) | -268(19) | 60(20) |
C2 | 580(40) | 510(40) | 540(40) | -290(30) | -360(30) | 220(30) |
C49A | 171(8) | 262(11) | 224(12) | 91(8) | -99(7) | -88(8) |
C51A | 371(18) | 114(8) | 204(12) | -77(8) | 0(10) | -1(8) |
C50A | 450(20) | 189(13) | 273(19) | -153(15) | 21(16) | 38(16) |
C22A | 107(5) | 132(6) | 89(4) | -37(4) | -10(3) | -5(4) |
C24A | 131(5) | 148(7) | 81(4) | -35(4) | -11(3) | -14(5) |
C37A | 117(5) | 135(6) | 89(5) | -15(4) | -17(3) | -13(4) |
C42A | 112(5) | 135(7) | 168(8) | -75(6) | -26(5) | 2(4) |
C32A | 116(5) | 136(7) | 145(7) | -46(6) | -27(5) | -8(4) |
C26A | 115(5) | 128(6) | 135(7) | -53(6) | -31(4) | 3(4) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O1 | C9 | 1.444(6) | C20 | C28 | 1.541(9) | |
O1 | C38 | 1.399(8) | C20 | C29 | 1.530(9) | |
O2 | C8 | 1.460(8) | C21 | C172 | 1.421(9) | |
O2 | C34 | 1.409(8) | C22 | C24 | 1.418(11) | |
O3 | C28 | 1.259(7) | C22 | F30 | 1.254(10) | |
O4 | C31 | 1.265(7) | C23 | C29 | 1.408(9) | |
O5 | C38 | 1.274(7) | C23 | C42 | 1.434(11) | |
C6 | C9 | 1.425(9) | C24 | F41 | 1.301(9) | |
C6 | C13 | 1.506(8) | C25 | C26 | 1.394(10) | |
C6 | C181 | 1.454(8) | C25 | C29 | 1.457(9) | |
O7 | C34 | 1.224(8) | C26 | C32 | 1.401(12) | |
C8 | C17 | 1.443(8) | C26 | F33 | 1.284(11) | |
C8 | C21 | 1.370(9) | C32 | C42 | 1.414(12) | |
C9 | C18 | 1.425(8) | C32 | F44 | 1.324(12) | |
C10 | C14 | 1.461(9) | C35 | C43 | 1.573(10) | |
C10 | C16 | 1.440(8) | C36 | C45 | 1.598(12) | |
C10 | C19 | 1.513(9) | F39 | C42 | 1.418(12) | |
N11 | C14 | 1.413(8) | C40 | C43 | 1.472(12) | |
N11 | C31 | 1.381(8) | C40 | C46 | 1.630(13) | |
N11 | C35 | 1.509(8) | C43 | C47 | 1.548(12) | |
C12 | C17 | 1.522(9) | C45 | C48 | 1.605(12) | |
C12 | C20 | 1.422(9) | C45 | C49 | 1.473(19) | |
C12 | C34 | 1.517(10) | C45 | C49A | 1.54(2) | |
C13 | C19 | 1.414(9) | C47 | C57 | 1.582(15) | |
C13 | C38 | 1.518(8) | C48 | C52 | 1.457(17) | |
C14 | C22 | 1.426(10) | C49 | C53 | 1.51(2) | |
N15 | C25 | 1.439(9) | C50 | C51 | 1.51(3) | |
N15 | C28 | 1.396(8) | C51 | C57 | 1.55(2) | |
N15 | C36 | 1.502(9) | C52 | C1 | 1.558(16) | |
C16 | C37 | 1.451(10) | C53 | C49A | 1.56(2) | |
C17 | C212 | 1.421(9) | C57 | C51A | 1.49(5) | |
C18 | C61 | 1.454(8) | C1 | C2 | 1.540(17) | |
C19 | C31 | 1.532(9) | C51A | C50A | 1.28(5) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C38 | O1 | C9 | 105.8(4) | C26 | C25 | N15 | 128.4(7) | |
C34 | O2 | C8 | 108.6(5) | C26 | C25 | C29 | 120.8(7) | |
C9 | C6 | C13 | 106.6(5) | C25 | C26 | C32 | 119.5(9) | |
C9 | C6 | C181 | 117.5(5) | F33 | C26 | C25 | 121.2(8) | |
C181 | C6 | C13 | 135.8(6) | F33 | C26 | C32 | 119.2(9) | |
C17 | C8 | O2 | 110.3(6) | O3 | C28 | N15 | 123.5(6) | |
C21 | C8 | O2 | 122.7(6) | O3 | C28 | C20 | 128.4(6) | |
C21 | C8 | C17 | 126.9(6) | N15 | C28 | C20 | 107.9(6) | |
C6 | C9 | O1 | 112.5(5) | C23 | C29 | C20 | 134.6(6) | |
C6 | C9 | C18 | 128.0(5) | C23 | C29 | C25 | 120.1(6) | |
C18 | C9 | O1 | 119.5(5) | C25 | C29 | C20 | 105.3(6) | |
C14 | C10 | C19 | 105.5(5) | O4 | C31 | N11 | 123.2(6) | |
C16 | C10 | C14 | 118.7(6) | O4 | C31 | C19 | 127.9(6) | |
C16 | C10 | C19 | 135.8(7) | N11 | C31 | C19 | 108.8(5) | |
C14 | N11 | C35 | 126.5(5) | C26 | C32 | C42 | 120.3(9) | |
C31 | N11 | C14 | 110.2(5) | F44 | C32 | C26 | 125.6(10) | |
C31 | N11 | C35 | 123.2(5) | F44 | C32 | C42 | 113.7(9) | |
C20 | C12 | C17 | 131.4(6) | O2 | C34 | C12 | 109.4(6) | |
C20 | C12 | C34 | 123.5(6) | O7 | C34 | O2 | 117.5(6) | |
C34 | C12 | C17 | 105.1(5) | O7 | C34 | C12 | 133.1(7) | |
C6 | C13 | C38 | 103.3(6) | N11 | C35 | C43 | 115.8(6) | |
C19 | C13 | C6 | 132.5(6) | N15 | C36 | C45 | 112.3(6) | |
C19 | C13 | C38 | 124.2(6) | O1 | C38 | C13 | 111.4(5) | |
N11 | C14 | C10 | 110.8(5) | O5 | C38 | O1 | 116.3(5) | |
N11 | C14 | C22 | 128.9(7) | O5 | C38 | C13 | 132.2(6) | |
C22 | C14 | C10 | 120.3(6) | C43 | C40 | C46 | 114.0(8) | |
C25 | N15 | C36 | 126.0(6) | C32 | C42 | C23 | 121.8(8) | |
C28 | N15 | C25 | 110.2(6) | C32 | C42 | F39 | 125.8(9) | |
C28 | N15 | C36 | 123.0(7) | F39 | C42 | C23 | 112.3(9) | |
C10 | C16 | C37 | 118.4(7) | C40 | C43 | C35 | 114.1(7) | |
C8 | C17 | C12 | 106.6(6) | C40 | C43 | C47 | 113.6(7) | |
C212 | C17 | C8 | 117.4(6) | C47 | C43 | C35 | 109.6(7) | |
C212 | C17 | C12 | 135.9(5) | C36 | C45 | C48 | 104.9(9) | |
C9 | C18 | C61 | 114.5(5) | C49 | C45 | C36 | 117.7(10) | |
C10 | C19 | C31 | 104.6(6) | C49 | C45 | C48 | 111.7(10) | |
C13 | C19 | C10 | 131.2(6) | C49A | C45 | C36 | 135(3) | |
C13 | C19 | C31 | 124.0(6) | C49A | C45 | C48 | 117(4) | |
C12 | C20 | C28 | 123.2(6) | C43 | C47 | C57 | 114.8(8) | |
C12 | C20 | C29 | 131.5(6) | C52 | C48 | C45 | 124.9(12) | |
C29 | C20 | C28 | 105.4(5) | C45 | C49 | C53 | 114.1(18) | |
C8 | C21 | C172 | 115.7(6) | C50 | C51 | C57 | 113.1(16) | |
C24 | C22 | C14 | 118.6(9) | C48 | C52 | C1 | 109.3(16) | |
F30 | C22 | C14 | 121.6(7) | C51 | C57 | C47 | 113.7(11) | |
F30 | C22 | C24 | 119.7(8) | C51A | C57 | C47 | 123(3) | |
C29 | C23 | C42 | 117.5(7) | C2 | C1 | C52 | 110.9(16) | |
F41 | C24 | C22 | 122.8(10) | C45 | C49A | C53 | 107.8(19) | |
N15 | C25 | C29 | 110.8(6) | C50A | C51A | C57 | 145(5) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H16A | 15198 | -529 | 8174 | 135 |
H16 | 15198 | -529 | 8174 | 135 |
H18A | 14225 | -1607 | 5281 | 114 |
H18B | 16360 | -1285 | 4987 | 114 |
H21 | 9702 | 1314 | 3861 | 127 |
H23A | 9241 | 2287 | 6964 | 142 |
H23 | 9241 | 2287 | 6964 | 142 |
H35A | 12667 | 3540 | 6831 | 139 |
H35B | 13401 | 3751 | 5998 | 139 |
H36A | 11385 | -1555 | 9007 | 157 |
H36B | 11597 | -2080 | 8461 | 157 |
H37 | 14608 | -217 | 9261 | 152 |
H40A | 16887 | 4846 | 5375 | 217 |
H40B | 17258 | 3803 | 5925 | 217 |
H43 | 15615 | 4153 | 6893 | 181 |
H45 | 8183 | -2213 | 9450 | 247 |
H45A | 8910 | -2878 | 8862 | 247 |
H46A | 19913 | 5045 | 5645 | 289 |
H46B | 19003 | 4654 | 6492 | 289 |
H46C | 18662 | 5694 | 5926 | 289 |
H47A | 13908 | 5516 | 5853 | 202 |
H47B | 15595 | 5913 | 6079 | 202 |
H48A | 8599 | -3921 | 10119 | 301 |
H48B | 10426 | -3751 | 9548 | 301 |
H49A | 8369 | -3440 | 8702 | 337 |
H49B | 7734 | -2387 | 8350 | 337 |
H50A | 10232 | 6917 | 7226 | 449 |
H50B | 10954 | 6041 | 7819 | 449 |
H50C | 9675 | 5803 | 7351 | 449 |
H51A | 13225 | 6924 | 6701 | 285 |
H51B | 11967 | 6556 | 6284 | 285 |
H52A | 9967 | -3076 | 10655 | 403 |
H52B | 11802 | -2796 | 10045 | 403 |
H53A | 5889 | -3923 | 9727 | 496 |
H53B | 5183 | -3628 | 8991 | 496 |
H53C | 5245 | -2874 | 9362 | 496 |
H53D | 6102 | -3261 | 8750 | 496 |
H53E | 4547 | -3435 | 9443 | 496 |
H53F | 6270 | -3993 | 9548 | 496 |
H57A | 12250 | 4832 | 7150 | 266 |
H57B | 13904 | 5345 | 7323 | 266 |
H57C | 12142 | 5668 | 6774 | 266 |
H57D | 12806 | 4713 | 7299 | 266 |
H1A | 10323 | -4734 | 11195 | 514 |
H1B | 11621 | -4677 | 10470 | 514 |
H2A | 14015 | -3725 | 10670 | 718 |
H2B | 13414 | -4785 | 11339 | 718 |
H2C | 12719 | -3835 | 11410 | 718 |
H49C | 6623 | -1854 | 9005 | 337 |
H49D | 6463 | -2540 | 9852 | 337 |
H51C | 14923 | 5711 | 7463 | 285 |
H51D | 14161 | 6632 | 6976 | 285 |
H50D | 12601 | 6724 | 7793 | 449 |
H50E | 14331 | 6326 | 8091 | 449 |
H50F | 12483 | 5589 | 8328 | 449 |
H22A | 13675 | 2587 | 8096 | 138 |
H24A | 13867 | 1270 | 9210 | 153 |
H42A | 8661 | 2530 | 8073 | 164 |
H32A | 8863 | 1270 | 9204 | 165 |
H26A | 9618 | -278 | 9272 | 152 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
H16A | 0.10(2) | H16 | 0.90(2) | C22 | 0.90(2) | ||
H23A | 0.10(2) | H23 | 0.90(2) | C24 | 0.90(2) | ||
C26 | 0.10(2) | F27 | 0.649(18) | F30 | 0.604(18) | ||
C32 | 0.10(2) | F33 | 0.525(17) | C37 | 0.10(2) | ||
H37 | 0.10(2) | F39 | 0.491(17) | F41 | 0.555(17) | ||
C42 | 0.10(2) | F44 | 0.447(18) | H45 | 0.90(2) | ||
H45A | 0.10(2) | C49 | 0.90(2) | H49A | 0.90(2) | ||
H49B | 0.90(2) | C50 | 0.570(16) | H50A | 0.570(16) | ||
H50B | 0.570(16) | H50C | 0.570(16) | C51 | 0.742(16) | ||
H51A | 0.742(16) | H51B | 0.742(16) | H53A | 0.90(2) | ||
H53B | 0.90(2) | H53C | 0.90(2) | H53D | 0.10(2) | ||
H53E | 0.10(2) | H53F | 0.10(2) | H57A | 0.742(16) | ||
H57B | 0.742(16) | H57C | 0.258(16) | H57D | 0.258(16) | ||
C49A | 0.10(2) | H49C | 0.10(2) | H49D | 0.10(2) | ||
C51A | 0.258(16) | H51C | 0.258(16) | H51D | 0.258(16) | ||
C50A | 0.430(16) | H50D | 0.430(16) | H50E | 0.430(16) | ||
H50F | 0.430(16) | C22A | 0.10(2) | H22A | 0.10(2) | ||
C24A | 0.10(2) | H24A | 0.10(2) | C37A | 0.90(2) | ||
C42A | 0.90(2) | H42A | 0.90(2) | C32A | 0.90(2) | ||
H32A | 0.90(2) | C26A | 0.90(2) | H26A | 0.90(2) |
Experimental
Single crystals of C42H42F3.27N2O6 [3F-nondecomposition] were []. A suitable crystal was selected and [] on a diffractometer. The crystal was kept at 293(2) K during data collection. Using Olex2 [1], the structure was solved with the XS [2] structure solution program using Direct Methods and refined with the ShelXL [3] refinement package using CGLS minimisation.
Crystal structure determination of [3F-nondecomposition]
Crystal Data for C42H42F3.27N2O6 (M =732.90 g/mol): triclinic, space group P-1 (no. 2), a = 7.453 Å, b = 14.683 Å, c = 20.135 Å, α = 66.42°, β = 79.76°, γ = 93.67°, V = 1964.9 Å3, Z = 2, T = 293(2) K, μ(Synchrotron) = 0.090 mm-1, Dcalc = 1.239 g/cm3, 16866 reflections measured (2.856° ≤ 2Θ ≤ 46.636°), 5707 unique (Rint = 0.0826, Rsigma = 0.0628) which were used in all calculations. The final R1 was 0.1392 (I > 2σ(I)) and wR2 was 0.4455 (all data).
Refinement model description
Number of restraints - 105, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Shared sites
{C22, C22A}
{C24, C24A}
{C37A, C37}
{C42A, C42}
{C32A, C32}
{C26A, C26}
3. Restrained distances
C52-C1 = C2-C1 = C48-C45 = C49A-C45
1.55 with sigma of 0.02
C2-C52
2.5 with sigma of 0.02
C28-C20
1.4 with sigma of 0.02
C13-C38
1.4 with sigma of 0.02
C53-C49A
1.55 with sigma of 0.02
4. Rigid bond restraints
C2, C1, C52, C48
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C47, C57, C51, C51A, C50A, C50
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C45, C49A, C49, C53
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C48 ≈ C52 ≈ C1 ≈ C2: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C47 ≈ C57 ≈ C51 ≈ C51A ≈ C50A ≈ C50: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C53 ≈ C49 ≈ C49A ≈ C45: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C49) = Uanis(C49A)
Uanis(C50) = Uanis(C50A)
Uanis(C51) = Uanis(C51A)
Uanis(C37) = Uanis(C37A)
Uanis(C22) = Uanis(C22A)
Uanis(C24) = Uanis(C24A)
Uanis(C37A) = Uanis(C37)
Uanis(C42) = Uanis(C42A)
Uanis(C32) = Uanis(C32A)
Uanis(C26) = Uanis(C26A)
Uanis(C42A) = Uanis(C42)
Uanis(C32A) = Uanis(C32)
Uanis(C26A) = Uanis(C26)
6. Others
Sof(H16A)=Sof(H23A)=Sof(C26)=Sof(C32)=Sof(C37)=Sof(H37)=Sof(C42)=Sof(H45A)=
Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C22A)=
Sof(H22A)=Sof(C24A)=Sof(H24A)=1-FVAR(1)
Sof(H16)=Sof(C22)=Sof(H23)=Sof(C24)=Sof(H45)=Sof(C49)=Sof(H49A)=Sof(H49B)=
Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C37A)=Sof(C42A)=Sof(H42A)=Sof(C32A)=
Sof(H32A)=Sof(C26A)=Sof(H26A)=FVAR(1)
Sof(H57C)=Sof(H57D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=1-FVAR(2)
Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H57A)=Sof(H57B)=FVAR(2)
Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(3)
Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
C43(H43), C45(H45), C45(H45A)
7.b Secondary CH2 refined with riding coordinates:
C18(H18A,H18B), C35(H35A,H35B), C36(H36A,H36B), C40(H40A,H40B), C47(H47A,
H47B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B), C52(H52A,H52B),
C57(H57A,H57B), C57(H57C,H57D), C1(H1A,H1B), C49A(H49C,H49D), C51A(H51C,H51D)
7.c Me refined with riding coordinates:
C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C), C53(H53D,H53E,
H53F), C2(H2A,H2B,H2C), C50A(H50D,H50E,H50F)
7.d Aromatic/amide H refined with riding coordinates:
C16(H16A), C16(H16), C21(H21), C23(H23A), C23(H23), C37(H37), C22A(H22A),
C24A(H24A), C42A(H42A), C32A(H32A), C26A(H26A)
This report has been created with Olex2, compiled on 2018.04.26 svn.r3504 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.