Identification code | 06F |
Empirical formula | C42H41F3.37N2O6 |
Formula weight | 733.70 |
Temperature/K | 293(2) |
Crystal system | triclinic |
Space group | P-1 |
a/Å | 7.442 |
b/Å | 14.635 |
c/Å | 19.312 |
α/° | 108.27 |
β/° | 98.49 |
γ/° | 93.69 |
Volume/Å3 | 1961.7 |
Z | 2 |
ρcalcg/cm3 | 1.242 |
μ/mm‑1 | 0.088 |
F(000) | 771.0 |
Crystal size/mm3 | 0.5 × 0.06 × 0.02 |
Radiation | Synchrotron Monochromator X-ray (λ = 0.68882) |
2Θ range for data collection/° | 2.86 to 46.64 |
Index ranges | -7 ≤ h ≤ 7, -16 ≤ k ≤ 16, -22 ≤ l ≤ 22 |
Reflections collected | 20424 |
Independent reflections | 5738 [Rint = 0.0902, Rsigma = 0.0574] |
Data/restraints/parameters | 5738/49/509 |
Goodness-of-fit on F2 | 1.367 |
Final R indexes [I>=2σ (I)] | R1 = 0.1133, wR2 = 0.3283 |
Final R indexes [all data] | R1 = 0.1449, wR2 = 0.3671 |
Largest diff. peak/hole / e Å-3 | 0.40/-0.26 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
O0AA | 3097(4) | 5017(2) | 3650.8(14) | 106.6(9) |
O2 | 6631(4) | 4188(3) | 2897.8(16) | 115.7(10) |
O3 | 10204(4) | 3131(2) | 5061.6(16) | 118.2(10) |
O8AA | 4871(5) | 1971(2) | 4455.6(18) | 136.1(12) |
O5 | 1631(4) | 3821(2) | 2606.7(17) | 128.0(11) |
N1 | 6552(5) | 2745(3) | 1909.5(18) | 109.2(11) |
C1AA | 4737(5) | 5938(3) | 4908(2) | 99.8(12) |
C2AA | 1989(6) | 1784(4) | 1868(2) | 112.1(14) |
C3AA | 4316(5) | 4110(3) | 4399(2) | 97.2(11) |
O4AA | 9309(5) | 1617(3) | 4201.3(19) | 141.5(13) |
C5AA | 4105(5) | 5059(3) | 4355(2) | 96.3(11) |
C6AA | 2809(5) | 1677(3) | 2553(2) | 103.2(12) |
C9AA | 10130(5) | 4109(3) | 5065(2) | 102.9(12) |
C0BA | 8756(5) | 3122(3) | 3854(2) | 100.8(12) |
N6 | 4108(5) | 783(3) | 3294.1(19) | 108.0(11) |
C7 | 7032(6) | 3333(4) | 2648(2) | 104.1(13) |
C7AA | 6986(4) | 1771(2) | 1846.7(16) | 105.1(13) |
C20 | 7769(4) | 1698(2) | 2524.0(12) | 103.0(12) |
C14 | 8260(4) | 815(3) | 2567.1(15) | 115.9(14) |
C28 | 7969(5) | 4(2) | 1933(2) | 125.8(15) |
C18 | 7186(5) | 77(2) | 1255.6(15) | 127.6(16) |
C17 | 6695(4) | 961(3) | 1212.5(12) | 125.6(16) |
C8 | 9251(5) | 4150(3) | 4363(2) | 99.8(12) |
C4 | 3465(5) | 3390(3) | 3648(2) | 97.4(12) |
C9 | 3275(6) | 738(3) | 2565(2) | 107.3(13) |
C1BA | 3441(5) | 2372(3) | 3338(2) | 101.7(12) |
C10 | 7955(5) | 2717(3) | 3096(2) | 98.8(12) |
C11 | 9139(5) | 5113(3) | 4308(2) | 102.4(12) |
C12 | 2169(7) | 50(4) | 1227(3) | 124.5(16) |
C13 | 5575(6) | 3094(4) | 1318(3) | 124.7(15) |
F15 | 3520(7) | -961(4) | 1883(2) | 132(2) |
F16 | 910(8) | 1067(4) | 558(2) | 148(2) |
C19 | 2964(7) | -63(4) | 1905(2) | 118.2(15) |
C21 | 1680(7) | 966(4) | 1219(2) | 125.3(16) |
F22 | 1878(8) | -720(4) | 590(2) | 153(2) |
C23 | 4810(6) | -34(3) | 3528(3) | 120.1(14) |
F24 | 5823(10) | 993(4) | 513(3) | 149(3) |
F25 | 8387(9) | -901(4) | 1969(3) | 159(3) |
C26 | 2628(5) | 4034(3) | 3219(2) | 103.3(12) |
C27 | 9393(6) | 2507(4) | 4341(2) | 112.3(13) |
C29 | 4231(6) | 1738(3) | 3789(2) | 105.0(12) |
C30 | 3277(8) | -774(4) | 3604(3) | 144.1(19) |
C31 | 2030(10) | -353(5) | 4137(4) | 135(2) |
C32 | 6849(11) | 3391(7) | 815(4) | 198(3) |
F33 | 6729(11) | -749(5) | 617(3) | 174(4) |
C34 | 4235(10) | -1662(5) | 3749(4) | 172(3) |
C35 | 155(10) | -1010(6) | 4008(5) | 191(3) |
C36 | 5500(14) | 3705(8) | 212(5) | 238(4) |
C37 | 4851(16) | -2340(6) | 3073(5) | 219(4) |
C38 | 8410(10) | 4187(9) | 1224(5) | 267(5) |
C39 | 6040(20) | -3151(8) | 3220(8) | 253(7) |
C40 | 9880(17) | 4137(14) | 732(10) | 400(10) |
C41 | 3920(20) | 2979(10) | -320(7) | 325(7) |
C43 | 2720(20) | 3476(11) | -775(9) | 403(10) |
C47 | 7210(40) | -3628(11) | 2625(10) | 320(11) |
C39A | 3340(40) | -3205(16) | 2719(17) | 253(7) |
C47A | 4040(60) | -4022(16) | 2148(18) | 320(11) |
C31A | 1340(30) | -750(15) | 3371(11) | 135(2) |
C6 | 920(20) | 2937(15) | -1216(14) | 500(16) |
C28A | 7969(5) | 4(2) | 1933(2) | 125.8(15) |
C18A | 7186(5) | 77(2) | 1255.6(15) | 127.6(16) |
C17A | 6695(4) | 961(3) | 1212.5(12) | 125.6(16) |
C19A | 2964(7) | -63(4) | 1905(2) | 118.2(15) |
C12A | 2169(7) | 50(4) | 1227(3) | 124.5(16) |
C21A | 1680(7) | 966(4) | 1219(2) | 125.3(16) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
O0AA | 109.2(19) | 127(2) | 83.7(17) | 44.4(15) | 2.0(13) | 1.5(15) |
O2 | 113(2) | 144(3) | 96.5(19) | 52.9(18) | 8.7(14) | 16.1(18) |
O3 | 131(2) | 126(2) | 105(2) | 56.5(17) | 4.1(16) | 8.5(16) |
O8AA | 174(3) | 126(2) | 98(2) | 44.0(17) | -14.3(19) | -6(2) |
O5 | 125(2) | 147(3) | 103(2) | 49.3(18) | -18.5(17) | -2.6(18) |
N1 | 102(2) | 142(3) | 85(2) | 47(2) | 6.5(16) | -7.3(19) |
C1AA | 91(2) | 128(3) | 86(2) | 50(2) | 9.6(18) | -4(2) |
C2AA | 106(3) | 139(4) | 88(3) | 43(2) | 5(2) | -19(2) |
C3AA | 88(2) | 123(3) | 81(2) | 40(2) | 11.8(17) | -5.6(19) |
O4AA | 175(3) | 127(3) | 118(2) | 55(2) | -11(2) | -1(2) |
C5AA | 88(2) | 124(3) | 79(2) | 44(2) | 6.7(17) | -5(2) |
C6AA | 89(2) | 129(3) | 88(3) | 38(2) | 10.4(18) | -15(2) |
C9AA | 96(3) | 128(3) | 94(3) | 52(2) | 14(2) | 7(2) |
C0BA | 90(2) | 124(3) | 95(3) | 48(2) | 15.1(19) | 3(2) |
N6 | 112(2) | 120(3) | 93(2) | 45(2) | 8.2(17) | -8.9(18) |
C7 | 92(3) | 134(4) | 91(3) | 50(3) | 8.3(19) | -4(2) |
C7AA | 106(3) | 121(3) | 87(3) | 37(2) | 14(2) | -6(2) |
C20 | 95(3) | 117(3) | 102(3) | 46(2) | 18(2) | -4(2) |
C14 | 106(3) | 137(4) | 105(3) | 43(3) | 18(2) | -9(3) |
C28 | 129(4) | 125(4) | 132(4) | 55(3) | 28(3) | 4(3) |
C18 | 142(4) | 125(4) | 107(4) | 28(3) | 26(3) | -6(3) |
C17 | 134(4) | 142(4) | 99(3) | 43(3) | 17(3) | -14(3) |
C8 | 88(2) | 133(3) | 88(2) | 52(2) | 16.8(18) | 6(2) |
C4 | 86(2) | 121(3) | 84(2) | 39(2) | 7.2(17) | -7.7(19) |
C9 | 98(3) | 127(3) | 100(3) | 46(3) | 18(2) | -15(2) |
C1BA | 89(2) | 128(3) | 88(2) | 44(2) | 6.2(18) | -16(2) |
C10 | 86(2) | 128(3) | 92(3) | 51(2) | 16.1(18) | 1.7(19) |
C11 | 93(2) | 134(3) | 90(3) | 56(2) | 8.2(19) | 6(2) |
C12 | 126(3) | 145(4) | 93(3) | 32(3) | 20(2) | -18(3) |
C13 | 114(3) | 164(4) | 94(3) | 54(3) | -4(2) | -6(3) |
F15 | 161(4) | 122(4) | 106(3) | 29(2) | 30(3) | -4(3) |
F16 | 177(5) | 170(5) | 88(3) | 45(3) | 0(3) | -3(3) |
C19 | 125(3) | 129(4) | 92(3) | 34(3) | 13(2) | -21(3) |
C21 | 134(4) | 153(4) | 83(3) | 43(3) | 7(2) | -18(3) |
F22 | 191(5) | 155(4) | 90(3) | 16(3) | 21(3) | -9(3) |
C23 | 116(3) | 118(3) | 121(3) | 45(3) | 6(2) | -9(2) |
F24 | 199(6) | 149(5) | 90(4) | 39(3) | 7(3) | -5(4) |
F25 | 190(6) | 133(5) | 157(5) | 52(3) | 37(4) | 7(3) |
C26 | 96(3) | 131(3) | 84(2) | 47(2) | 3(2) | -8(2) |
C27 | 119(3) | 128(4) | 90(3) | 44(2) | 3(2) | 4(2) |
C29 | 105(3) | 118(3) | 88(3) | 43(2) | -2(2) | -17(2) |
C30 | 148(4) | 163(5) | 154(5) | 90(4) | 44(3) | 7(3) |
C31 | 144(5) | 139(5) | 127(4) | 58(4) | 21(4) | -8(4) |
C32 | 212(6) | 268(8) | 149(5) | 143(5) | -6(4) | -13(5) |
F33 | 259(9) | 142(5) | 112(5) | 26(4) | 42(4) | 3(4) |
C34 | 194(6) | 159(5) | 184(6) | 95(5) | 20(5) | -14(4) |
C35 | 173(6) | 203(7) | 230(8) | 110(6) | 66(5) | -16(5) |
C36 | 260(9) | 294(10) | 185(7) | 158(7) | -25(6) | -49(7) |
C37 | 346(12) | 136(5) | 167(7) | 37(5) | 57(7) | 16(6) |
C38 | 146(5) | 495(15) | 208(7) | 229(9) | -25(5) | -76(7) |
C39 | 430(20) | 116(6) | 228(13) | 72(7) | 82(13) | 23(10) |
C40 | 230(11) | 680(30) | 510(20) | 450(20) | 158(13) | 71(13) |
C41 | 375(14) | 347(15) | 222(10) | 144(9) | -105(9) | -77(11) |
C43 | 429(19) | 420(20) | 343(16) | 236(15) | -156(14) | -101(15) |
C47 | 590(30) | 171(11) | 243(16) | 82(10) | 141(19) | 130(17) |
C39A | 430(20) | 116(6) | 228(13) | 72(7) | 82(13) | 23(10) |
C47A | 590(30) | 171(11) | 243(16) | 82(10) | 141(19) | 130(17) |
C31A | 144(5) | 139(5) | 127(4) | 58(4) | 21(4) | -8(4) |
C6 | 340(20) | 500(30) | 590(40) | 210(30) | -170(20) | -40(17) |
C28A | 129(4) | 125(4) | 132(4) | 55(3) | 28(3) | 4(3) |
C18A | 142(4) | 125(4) | 107(4) | 28(3) | 26(3) | -6(3) |
C17A | 134(4) | 142(4) | 99(3) | 43(3) | 17(3) | -14(3) |
C19A | 125(3) | 129(4) | 92(3) | 34(3) | 13(2) | -21(3) |
C12A | 126(3) | 145(4) | 93(3) | 32(3) | 20(2) | -18(3) |
C21A | 134(4) | 153(4) | 83(3) | 43(3) | 7(2) | -18(3) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
O0AA | C5AA | 1.434(4) | C20 | C10 | 1.535(5) | |
O0AA | C26 | 1.410(5) | C14 | C28 | 1.3900 | |
O2 | C7 | 1.265(5) | C28 | C18 | 1.3900 | |
O3 | C9AA | 1.433(5) | C28 | F25 | 1.401(6) | |
O3 | C27 | 1.421(5) | C18 | F33 | 1.409(6) | |
O8AA | C29 | 1.235(5) | C8 | C11 | 1.453(6) | |
O5 | C26 | 1.235(5) | C4 | C1BA | 1.418(6) | |
N1 | C7 | 1.394(6) | C4 | C26 | 1.541(6) | |
N1 | C7AA | 1.453(5) | C9 | C19 | 1.411(6) | |
N1 | C13 | 1.505(6) | C1BA | C29 | 1.546(6) | |
C1AA | C3AA1 | 1.442(5) | C11 | C9AA2 | 1.386(6) | |
C1AA | C5AA | 1.389(6) | C12 | C19 | 1.419(7) | |
C2AA | C6AA | 1.432(6) | C13 | C32 | 1.586(8) | |
C2AA | C21 | 1.412(7) | F16 | C21 | 1.375(6) | |
C3AA | C1AA1 | 1.442(5) | C23 | C30 | 1.577(7) | |
C3AA | C5AA | 1.435(6) | C30 | C31 | 1.504(9) | |
C3AA | C4 | 1.517(5) | C30 | C34 | 1.601(9) | |
O4AA | C27 | 1.240(6) | C30 | C31A | 1.45(2) | |
C6AA | C9 | 1.446(6) | C31 | C35 | 1.584(9) | |
C6AA | C1BA | 1.523(6) | C32 | C36 | 1.619(10) | |
C9AA | C8 | 1.437(6) | C32 | C38 | 1.520(10) | |
C9AA | C112 | 1.386(6) | C34 | C37 | 1.524(10) | |
C0BA | C8 | 1.503(6) | C35 | C31A | 1.733(19) | |
C0BA | C10 | 1.416(6) | C36 | C41 | 1.538(13) | |
C0BA | C27 | 1.541(7) | C37 | C39 | 1.595(16) | |
N6 | C9 | 1.432(5) | C37 | C39A | 1.546(19) | |
N6 | C23 | 1.502(6) | C38 | C40 | 1.542(14) | |
N6 | C29 | 1.413(6) | C39 | C47 | 1.56(2) | |
C7 | C10 | 1.557(6) | C41 | C43 | 1.533(11) | |
C7AA | C20 | 1.3900 | C43 | C6 | 1.499(14) | |
C7AA | C17 | 1.3900 | C39A | C47A | 1.532(19) | |
C20 | C14 | 1.3900 |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C26 | O0AA | C5AA | 107.9(3) | C1BA | C4 | C26 | 124.0(4) | |
C27 | O3 | C9AA | 107.6(3) | N6 | C9 | C6AA | 111.0(4) | |
C7 | N1 | C7AA | 109.0(3) | C19 | C9 | C6AA | 120.3(4) | |
C7 | N1 | C13 | 122.5(4) | C19 | C9 | N6 | 128.6(5) | |
C7AA | N1 | C13 | 128.2(3) | C6AA | C1BA | C29 | 105.1(4) | |
C5AA | C1AA | C3AA1 | 116.5(4) | C4 | C1BA | C6AA | 131.8(4) | |
C21 | C2AA | C6AA | 118.8(5) | C4 | C1BA | C29 | 123.0(4) | |
C1AA1 | C3AA | C4 | 136.4(4) | C0BA | C10 | C7 | 122.3(4) | |
C5AA | C3AA | C1AA1 | 116.7(4) | C0BA | C10 | C20 | 133.8(4) | |
C5AA | C3AA | C4 | 106.9(3) | C20 | C10 | C7 | 103.9(3) | |
O0AA | C5AA | C3AA | 111.8(3) | C9AA2 | C11 | C8 | 117.0(4) | |
C1AA | C5AA | O0AA | 121.4(4) | N1 | C13 | C32 | 114.8(4) | |
C1AA | C5AA | C3AA | 126.8(4) | C9 | C19 | C12 | 120.0(5) | |
C2AA | C6AA | C9 | 119.5(4) | F16 | C21 | C2AA | 119.1(6) | |
C2AA | C6AA | C1BA | 134.3(4) | N6 | C23 | C30 | 114.6(4) | |
C9 | C6AA | C1BA | 106.2(4) | O0AA | C26 | C4 | 109.7(3) | |
O3 | C9AA | C8 | 112.0(4) | O5 | C26 | O0AA | 119.2(4) | |
C112 | C9AA | O3 | 121.1(4) | O5 | C26 | C4 | 131.1(4) | |
C112 | C9AA | C8 | 126.9(4) | O3 | C27 | C0BA | 109.2(4) | |
C8 | C0BA | C27 | 104.2(3) | O4AA | C27 | O3 | 119.5(4) | |
C10 | C0BA | C8 | 132.5(4) | O4AA | C27 | C0BA | 131.3(4) | |
C10 | C0BA | C27 | 123.2(4) | O8AA | C29 | N6 | 123.2(4) | |
C9 | N6 | C23 | 127.1(4) | O8AA | C29 | C1BA | 129.3(4) | |
C29 | N6 | C9 | 110.1(4) | N6 | C29 | C1BA | 107.5(3) | |
C29 | N6 | C23 | 122.8(4) | C23 | C30 | C34 | 107.9(5) | |
O2 | C7 | N1 | 124.3(4) | C31 | C30 | C23 | 115.9(5) | |
O2 | C7 | C10 | 127.6(4) | C31 | C30 | C34 | 114.1(5) | |
N1 | C7 | C10 | 107.8(4) | C31A | C30 | C23 | 122.9(8) | |
C20 | C7AA | N1 | 112.3(2) | C31A | C30 | C34 | 127.1(9) | |
C20 | C7AA | C17 | 120.0 | C30 | C31 | C35 | 114.2(6) | |
C17 | C7AA | N1 | 127.7(2) | C13 | C32 | C36 | 105.8(6) | |
C7AA | C20 | C10 | 106.7(2) | C38 | C32 | C13 | 115.5(6) | |
C14 | C20 | C7AA | 120.0 | C38 | C32 | C36 | 111.0(7) | |
C14 | C20 | C10 | 133.2(2) | C37 | C34 | C30 | 114.4(6) | |
C20 | C14 | C28 | 120.0 | C41 | C36 | C32 | 120.3(8) | |
C14 | C28 | F25 | 120.9(3) | C34 | C37 | C39 | 115.8(8) | |
C18 | C28 | C14 | 120.0 | C34 | C37 | C39A | 107.2(13) | |
C18 | C28 | F25 | 119.1(3) | C32 | C38 | C40 | 108.9(11) | |
C28 | C18 | F33 | 121.1(4) | C47 | C39 | C37 | 117.0(11) | |
C9AA | C8 | C0BA | 107.0(4) | C43 | C41 | C36 | 110.5(11) | |
C9AA | C8 | C11 | 116.0(4) | C6 | C43 | C41 | 118.0(12) | |
C11 | C8 | C0BA | 136.9(4) | C47A | C39A | C37 | 109.9(18) | |
C3AA | C4 | C26 | 103.5(4) | C30 | C31A | C35 | 108.6(12) | |
C1BA | C4 | C3AA | 132.4(4) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H1AA | 4559 | 6527 | 4834 | 120 |
H2AB | 1666 | 2381 | 1850 | 135 |
H2AA | 1666 | 2381 | 1850 | 135 |
H14 | 8784 | 766 | 3020 | 139 |
H14A | 8784 | 766 | 3020 | 139 |
H17 | 6171 | 1010 | 759 | 151 |
H11 | 8601 | 5203 | 3872 | 123 |
H12 | 1970 | -474 | 790 | 149 |
H13A | 4976 | 3649 | 1553 | 150 |
H13B | 4630 | 2586 | 1002 | 150 |
H19 | 3279 | -664 | 1915 | 142 |
H23A | 5629 | 238 | 4002 | 144 |
H23B | 5520 | -384 | 3170 | 144 |
H30 | 2496 | -1039 | 3114 | 173 |
H30A | 3279 | -430 | 4129 | 173 |
H31A | 1768 | 272 | 4098 | 162 |
H31B | 2666 | -243 | 4637 | 162 |
H32 | 7374 | 2814 | 549 | 238 |
H34A | 5292 | -1405 | 4141 | 207 |
H34B | 3385 | -2034 | 3922 | 207 |
H35A | -519 | -1093 | 3524 | 287 |
H35B | -548 | -705 | 4376 | 287 |
H35C | 397 | -1632 | 4044 | 287 |
H35D | 284 | -1662 | 3999 | 287 |
H35E | -1116 | -945 | 3882 | 287 |
H35F | 643 | -568 | 4494 | 287 |
H36A | 4969 | 4268 | 483 | 286 |
H36B | 6257 | 3917 | -90 | 286 |
H37A | 5560 | -1952 | 2861 | 262 |
H37B | 3772 | -2660 | 2707 | 262 |
H37C | 5999 | -2564 | 3219 | 262 |
H37D | 5024 | -2006 | 2722 | 262 |
H38A | 8934 | 4102 | 1687 | 320 |
H38B | 7958 | 4815 | 1335 | 320 |
H39A | 6857 | -2865 | 3692 | 303 |
H39B | 5217 | -3661 | 3268 | 303 |
H40A | 10278 | 3503 | 605 | 599 |
H40B | 10903 | 4613 | 997 | 599 |
H40C | 9373 | 4262 | 289 | 599 |
H41A | 4412 | 2447 | -650 | 390 |
H41B | 3183 | 2714 | -38 | 390 |
H43A | 2480 | 4085 | -437 | 483 |
H43B | 3430 | 3632 | -1114 | 483 |
H47A | 6426 | -3936 | 2156 | 480 |
H47B | 7863 | -4102 | 2772 | 480 |
H47C | 8073 | -3138 | 2583 | 480 |
H39C | 2969 | -3439 | 3101 | 303 |
H39D | 2274 | -2998 | 2480 | 303 |
H47D | 4204 | -3826 | 1729 | 480 |
H47E | 3174 | -4593 | 1990 | 480 |
H47F | 5193 | -4159 | 2369 | 480 |
H31C | 914 | -1223 | 2883 | 162 |
H31D | 1126 | -113 | 3344 | 162 |
H6A | 1131 | 2426 | -1640 | 750 |
H6B | 193 | 3374 | -1377 | 750 |
H6C | 294 | 2665 | -913 | 750 |
H28A | 8298 | -587 | 1962 | 151 |
H18A | 6992 | -465 | 831 | 153 |
H21A | 1139 | 1032 | 773 | 150 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
H2AB | 0.590(8) | H2AA | 0.410(8) | H14 | 0.410(8) | ||
H14A | 0.590(8) | C28 | 0.410(8) | C18 | 0.410(8) | ||
C17 | 0.590(8) | H17 | 0.590(8) | C12 | 0.410(8) | ||
H12 | 0.410(8) | F15 | 0.590(8) | F16 | 0.590(8) | ||
C19 | 0.410(8) | H19 | 0.410(8) | C21 | 0.590(8) | ||
F22 | 0.590(8) | F24 | 0.520(11) | F25 | 0.566(12) | ||
H30 | 0.730(6) | H30A | 0.270(6) | C31 | 0.730(6) | ||
H31A | 0.730(6) | H31B | 0.730(6) | F33 | 0.537(13) | ||
H35A | 0.730(6) | H35B | 0.730(6) | H35C | 0.730(6) | ||
H35D | 0.270(6) | H35E | 0.270(6) | H35F | 0.270(6) | ||
H37A | 0.410(8) | H37B | 0.410(8) | H37C | 0.590(8) | ||
H37D | 0.590(8) | C39 | 0.730(6) | H39A | 0.730(6) | ||
H39B | 0.730(6) | C47 | 0.730(6) | H47A | 0.24(8) | ||
H47B | 0.24(8) | H47C | 0.24(8) | C39A | 0.270(6) | ||
H39C | 0.270(6) | H39D | 0.270(6) | C47A | 0.270(6) | ||
H47D | 0.76(8) | H47E | 0.76(8) | H47F | 0.76(8) | ||
C31A | 0.270(6) | H31C | 0.270(6) | H31D | 0.270(6) | ||
C28A | 0.590(8) | H28A | 0.590(8) | C18A | 0.590(8) | ||
H18A | 0.590(8) | C17A | 0.410(8) | C19A | 0.590(8) | ||
C12A | 0.590(8) | C21A | 0.410(8) | H21A | 0.410(8) |
Experimental
Single crystals of C42H41F3.37N2O6 [06F] 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 [06F]
Crystal Data for C42H41F3.37N2O6 (M =733.70 g/mol): triclinic, space group P-1 (no. 2), a = 7.442 Å, b = 14.635 Å, c = 19.312 Å, α = 108.27°, β = 98.49°, γ = 93.69°, V = 1961.7 Å3, Z = 2, T = 293(2) K, μ(Synchrotron Monochromator X-ray) = 0.088 mm-1, Dcalc = 1.242 g/cm3, 20424 reflections measured (2.86° ≤ 2Θ ≤ 46.64°), 5738 unique (Rint = 0.0902, Rsigma = 0.0574) which were used in all calculations. The final R1 was 0.1133 (I > 2σ(I)) and wR2 was 0.3671 (all data).
Refinement model description
Number of restraints - 49, 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
{C28A, C28}
{C18A, C18}
{C17, C17A}
{C19, C19A}
{C12, C12A}
{C21A, C21}
3. Restrained distances
C41-C43
1.55 with sigma of 0.02
C37-C39A
1.55 with sigma of 0.02
C39A-C47A
1.55 with sigma of 0.02
C38-C32
1.55 with sigma of 0.02
C7AA-C20
1.395 with sigma of 0.02
C43-C41 = C6-C43
1.55 with sigma of 0.02
C41-C6
2.5 with sigma of 0.02
C20-C10
1.395 with sigma of 0.02
C47A-C37
2.5 with sigma of 0.02
C7-C10
1.4 with sigma of 0.02
4. Rigid bond restraints
C41, C36, C43, C6
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C32, C38, C40
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C36 ≈ C41 ≈ C43 ≈ C6: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C40 ≈ C38 ≈ C32: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C39) = Uanis(C39A)
Uanis(C47) = Uanis(C47A)
Uanis(C31) = Uanis(C31A)
Uanis(C18) = Uanis(C18A)
Uanis(C18A) = Uanis(C18)
Uanis(C17) = Uanis(C17A)
Uanis(C19) = Uanis(C19A)
Uanis(C12) = Uanis(C12A)
Uanis(C21) = Uanis(C21A)
Uanis(C21A) = Uanis(C21)
Uanis(C28) = Uanis(C28A)
Uanis(C28A) = Uanis(C28)
6. Others
Sof(H2AB)=Sof(H14A)=Sof(C17)=Sof(H17)=Sof(F15)=Sof(F16)=Sof(C21)=Sof(F22)=
Sof(H37C)=Sof(H37D)=Sof(C28A)=Sof(H28A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
Sof(C12A)=1-FVAR(1)
Sof(H2AA)=Sof(H14)=Sof(C28)=Sof(C18)=Sof(C12)=Sof(H12)=Sof(C19)=Sof(H19)=
Sof(H37A)=Sof(H37B)=Sof(C17A)=Sof(C21A)=Sof(H21A)=FVAR(1)
Sof(H47D)=Sof(H47E)=Sof(H47F)=1-FVAR(2)
Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(2)
Sof(H30A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C39A)=Sof(H39C)=Sof(H39D)=
Sof(C47A)=Sof(C31A)=Sof(H31C)=Sof(H31D)=1-FVAR(3)
Sof(H30)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C39)=
Sof(H39A)=Sof(H39B)=Sof(C47)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
C30(H30), C30(H30A), C32(H32)
7.b Secondary CH2 refined with riding coordinates:
C13(H13A,H13B), C23(H23A,H23B), C31(H31A,H31B), C34(H34A,H34B), C36(H36A,
H36B), C37(H37A,H37B), C37(H37C,H37D), C38(H38A,H38B), C39(H39A,H39B),
C41(H41A,H41B), C43(H43A,H43B), C39A(H39C,H39D), C31A(H31C,H31D)
7.c Me refined with riding coordinates:
C35(H35A,H35B,H35C), C35(H35D,H35E,H35F), C40(H40A,H40B,H40C), C47(H47A,H47B,
H47C), C47A(H47D,H47E,H47F), C6(H6A,H6B,H6C)
7.d Aromatic/amide H refined with riding coordinates:
C1AA(H1AA), C2AA(H2AB), C2AA(H2AA), C14(H14), C14(H14A), C17(H17), C11(H11),
C12(H12), C19(H19), C28A(H28A), C18A(H18A), C21A(H21A)
7.e Fitted hexagon refined as free rotating group:
C7AA(C20,C14,C28,C18,C17)
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.