Identification code | 3Cl-decomposition |
Empirical formula | C84H78.63Cl9.37N4O12 |
Formula weight | 1668.30 |
Temperature/K | 293(2) |
Crystal system | triclinic |
Space group | P-1 |
a/Å | 7.4241(5) |
b/Å | 12.4935(9) |
c/Å | 20.8699(12) |
α/° | 84.241(6) |
β/° | 83.819(5) |
γ/° | 83.303(6) |
Volume/Å3 | 1903.8(2) |
Z | 1 |
ρcalcg/cm3 | 1.455 |
μ/mm‑1 | 3.698 |
F(000) | 866.0 |
Crystal size/mm3 | 0.15 × 0.1 × 0.1 |
Radiation | CuKα (λ = 1.54178) |
2Θ range for data collection/° | 7.152 to 125.404 |
Index ranges | -6 ≤ h ≤ 8, -14 ≤ k ≤ 14, -23 ≤ l ≤ 23 |
Reflections collected | 10253 |
Independent reflections | 5920 [Rint = 0.0430, Rsigma = 0.0805] |
Data/restraints/parameters | 5920/105/515 |
Goodness-of-fit on F2 | 1.027 |
Final R indexes [I>=2σ (I)] | R1 = 0.0919, wR2 = 0.2285 |
Final R indexes [all data] | R1 = 0.1370, wR2 = 0.2651 |
Largest diff. peak/hole / e Å-3 | 0.46/-0.41 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Cl0A | 4060(2) | 6460.9(13) | 1745.8(8) | 63.1(5) |
Cl2 | 6425(2) | 10245.8(14) | 723.4(7) | 62.7(5) |
Cl1 | 5529(3) | 7963.4(15) | 553.6(8) | 74.0(6) |
Cl6A | 9195(3) | 6497.6(15) | 1602.4(9) | 68.0(5) |
Cl3A | 11300(3) | 10460.0(16) | 844.2(9) | 69.4(6) |
Cl3 | 10541(3) | 8172.5(18) | 527.9(9) | 80.4(6) |
O9AA | 7888(5) | 7812(3) | 4048.7(17) | 57.1(9) |
O1BA | 3082(5) | 7659(3) | 3767.7(18) | 62.6(10) |
O2AA | 10283(5) | 11517(3) | 3979.4(17) | 57.5(9) |
O5AA | 5440(5) | 11543(3) | 3178.3(17) | 65.9(10) |
O7AA | 3827(4) | 8166(3) | 4685.8(16) | 52.8(9) |
O4 | 10021(6) | 11493(3) | 2928.8(19) | 72.2(11) |
N8AA | 5681(5) | 10797(3) | 2215(2) | 51.5(11) |
C0BA | 4299(6) | 8099(4) | 2439(2) | 51.5(13) |
C2BA | 5344(6) | 9815(4) | 2004(2) | 48.3(12) |
C5 | 4751(6) | 9858(4) | 4357(2) | 47.7(12) |
C6 | 4436(6) | 9080(4) | 4875(2) | 47.7(12) |
C7 | 4712(6) | 9121(4) | 2544(2) | 47.4(12) |
C8 | 10127(6) | 10779(4) | 4524(2) | 46.6(12) |
N9 | 8672(5) | 7458(3) | 2993(2) | 50.3(10) |
C10 | 9296(6) | 8056(4) | 2426(2) | 50.3(13) |
C11 | 10297(6) | 9810(4) | 2064(3) | 53.4(14) |
C12 | 9341(6) | 9124(4) | 3264(2) | 48.0(13) |
C13 | 5325(6) | 10829(4) | 4496(2) | 48.7(12) |
C14 | 9713(6) | 9778(4) | 4374(2) | 50.7(13) |
C15 | 9652(6) | 9084(4) | 2566(2) | 47.4(12) |
C16 | 9627(6) | 9861(4) | 3670(2) | 48.7(12) |
C17 | 4406(6) | 9375(4) | 3771(2) | 47.9(12) |
C18 | 4714(6) | 9690(4) | 3132(2) | 46.6(12) |
C19 | 5185(8) | 8441(4) | 1303(3) | 62.6(15) |
C20 | 5583(7) | 9471(4) | 1388(2) | 55.9(14) |
C21 | 4549(7) | 7756(4) | 1831(3) | 60.5(15) |
C22 | 10567(8) | 9532(5) | 1445(3) | 64.3(16) |
C23 | 8562(6) | 8073(4) | 3504(3) | 50.7(13) |
C24 | 5309(7) | 10786(4) | 2874(3) | 52.7(13) |
C25 | 9585(7) | 7752(4) | 1804(3) | 60.7(15) |
C26 | 10211(8) | 8503(5) | 1299(3) | 66.4(16) |
C27 | 9573(6) | 8951(4) | 4880(2) | 52.7(13) |
C28 | 10008(7) | 11011(4) | 3453(3) | 56.4(14) |
C29 | 3729(6) | 8316(4) | 4035(3) | 52.2(13) |
C30 | 7894(7) | 6417(4) | 3083(3) | 58.7(14) |
C31 | 6256(7) | 11769(4) | 1839(3) | 60.3(15) |
C33 | 9158(8) | 5465(5) | 3240(4) | 121(3) |
C34 | 3097(11) | 12800(8) | 1951(5) | 99(3) |
C35 | 4761(9) | 12479(6) | 1516(4) | 105(3) |
C36 | 1461(11) | 13300(7) | 1585(5) | 138(3) |
C37 | 5511(12) | 13536(7) | 1188(6) | 169(4) |
C38 | 7118(12) | 4160(7) | 2913(5) | 152(3) |
C39 | 6919(13) | 13340(7) | 636(5) | 164(4) |
C40 | 8045(10) | 4455(6) | 3416(5) | 166(3) |
C41 | 13753(15) | 3793(7) | 4646(5) | 153(4) |
C42 | 12684(13) | 4748(8) | 4382(6) | 163(4) |
C43 | 10414(12) | 5480(7) | 3737(5) | 91(3) |
C45 | 7470(19) | 14275(8) | 131(6) | 216(5) |
C46 | 11945(9) | 4489(6) | 3757(5) | 141(3) |
C48 | 7600(20) | 15238(9) | 466(9) | 316(9) |
C25A | 9585(7) | 7752(4) | 1804(3) | 60.7(15) |
C26A | 10211(8) | 8503(5) | 1299(3) | 66.4(16) |
C22A | 10567(8) | 9532(5) | 1445(3) | 64.3(16) |
C43A | 11079(17) | 5226(15) | 3182(9) | 91(3) |
C34A | 2850(20) | 12302(16) | 1402(16) | 99(3) |
C20A | 5583(7) | 9471(4) | 1388(2) | 55.9(14) |
C19A | 5185(8) | 8441(4) | 1303(3) | 62.6(15) |
C21A | 4549(7) | 7756(4) | 1831(3) | 60.5(15) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Cl0A | 75.7(10) | 55.0(9) | 63.3(9) | -14.6(7) | -20.1(8) | -6.0(8) |
Cl2 | 73.0(10) | 68.3(10) | 45.1(8) | 0.3(8) | -6.8(7) | -4.6(8) |
Cl1 | 109.4(14) | 68.2(11) | 47.2(9) | -11.0(8) | -19.4(9) | -4.9(10) |
Cl6A | 85.1(12) | 62.6(10) | 59.8(10) | -14.6(8) | -14.6(9) | -7.8(9) |
Cl3A | 72.3(11) | 78.2(12) | 53.1(10) | 12.2(9) | -1.3(8) | -8.6(9) |
Cl3 | 105.2(15) | 87.2(14) | 48.6(10) | -7.9(9) | -7.1(10) | -8.2(11) |
O9AA | 59(2) | 52.6(19) | 60(2) | -2.5(17) | 2.1(17) | -16.2(16) |
O1BA | 65(2) | 55(2) | 72(2) | -12.8(18) | 3.7(18) | -27.0(16) |
O2AA | 68(2) | 45.1(18) | 61(2) | -1.2(16) | -6.4(17) | -18.0(16) |
O5AA | 87(2) | 54(2) | 59(2) | -4.2(18) | 2.6(19) | -23.4(18) |
O7AA | 57.0(19) | 46.9(18) | 55(2) | -9.0(16) | 6.1(16) | -13.6(15) |
O4 | 100(3) | 57(2) | 63(2) | 4.9(19) | -9(2) | -28.6(19) |
N8AA | 47(2) | 56(2) | 52(2) | -4(2) | -2.4(18) | -6.7(19) |
C0BA | 41(3) | 53(3) | 60(3) | -9(2) | -9(2) | 6(2) |
C2BA | 42(2) | 46(3) | 56(3) | -1(2) | -11(2) | 1(2) |
C5 | 48(3) | 45(3) | 49(3) | -4(2) | 4(2) | -8(2) |
C6 | 44(3) | 44(3) | 54(3) | -10(2) | 8(2) | -9(2) |
C7 | 39(2) | 48(3) | 55(3) | -4(2) | -10(2) | 2(2) |
C8 | 39(2) | 44(3) | 57(3) | 0(2) | 1(2) | -13(2) |
N9 | 42(2) | 51(2) | 60(2) | -7(2) | -10.6(18) | -4.9(18) |
C10 | 37(2) | 57(3) | 56(3) | -2(2) | -16(2) | 3(2) |
C11 | 37(2) | 58(3) | 64(3) | -3(3) | -9(2) | 1(2) |
C12 | 34(2) | 51(3) | 57(3) | 0(2) | -3(2) | -1(2) |
C13 | 47(3) | 47(3) | 51(3) | -3(2) | 2(2) | -11(2) |
C14 | 45(3) | 43(3) | 62(3) | -2(2) | 3(2) | -8(2) |
C15 | 35(2) | 44(3) | 63(3) | 1(2) | -12(2) | -2(2) |
C16 | 40(2) | 48(3) | 58(3) | -3(2) | -2(2) | -7(2) |
C17 | 41(2) | 45(3) | 58(3) | -7(2) | 3(2) | -10(2) |
C18 | 36(2) | 48(3) | 55(3) | -9(2) | -1(2) | -2(2) |
C19 | 73(3) | 57(3) | 60(3) | -13(3) | -21(3) | 5(3) |
C20 | 56(3) | 61(3) | 49(3) | -2(2) | -12(2) | 2(3) |
C21 | 60(3) | 60(3) | 63(3) | -11(3) | -14(3) | 0(3) |
C22 | 63(3) | 61(3) | 64(3) | 8(3) | -13(3) | 4(3) |
C23 | 39(2) | 45(3) | 68(3) | -7(2) | -9(2) | -4(2) |
C24 | 52(3) | 49(3) | 58(3) | -10(2) | -3(2) | -6(2) |
C25 | 62(3) | 59(3) | 62(3) | -7(3) | -14(3) | 0(3) |
C26 | 63(3) | 76(4) | 56(3) | -4(3) | -8(3) | 7(3) |
C27 | 49(3) | 46(3) | 63(3) | -4(2) | 5(2) | -14(2) |
C28 | 56(3) | 52(3) | 62(3) | -1(3) | 0(2) | -15(2) |
C29 | 42(3) | 51(3) | 63(3) | -9(2) | 7(2) | -9(2) |
C30 | 48(3) | 59(3) | 73(3) | -9(3) | -15(2) | -12(2) |
C31 | 63(3) | 50(3) | 67(3) | 1(3) | -2(3) | -9(2) |
C33 | 82(4) | 59(4) | 235(8) | 30(4) | -92(4) | -24(3) |
C34 | 82(4) | 97(6) | 107(6) | 25(5) | 1(4) | 3(4) |
C35 | 81(4) | 85(4) | 133(6) | 42(4) | -3(4) | 6(4) |
C36 | 97(5) | 144(7) | 146(7) | 40(6) | 4(5) | 44(5) |
C37 | 96(6) | 116(6) | 268(9) | 76(7) | -15(6) | 20(5) |
C38 | 127(6) | 123(5) | 222(8) | -90(5) | 45(5) | -73(4) |
C39 | 135(7) | 184(7) | 171(8) | 72(6) | -34(5) | -61(6) |
C40 | 117(5) | 81(5) | 314(9) | 51(6) | -121(5) | -40(4) |
C41 | 189(9) | 97(6) | 158(8) | 34(6) | -7(6) | 0(6) |
C42 | 111(6) | 148(8) | 210(7) | 38(6) | -13(5) | 20(6) |
C43 | 60(4) | 62(4) | 147(6) | 6(5) | 12(4) | -23(3) |
C45 | 195(10) | 155(7) | 286(10) | 96(6) | -46(8) | -48(7) |
C46 | 68(4) | 76(4) | 274(7) | 64(5) | -52(4) | -24(3) |
C48 | 330(20) | 169(8) | 460(20) | 36(9) | -122(19) | -40(11) |
C25A | 62(3) | 59(3) | 62(3) | -7(3) | -14(3) | 0(3) |
C26A | 63(3) | 76(4) | 56(3) | -4(3) | -8(3) | 7(3) |
C22A | 63(3) | 61(3) | 64(3) | 8(3) | -13(3) | 4(3) |
C43A | 60(4) | 62(4) | 147(6) | 6(5) | 12(4) | -23(3) |
C34A | 82(4) | 97(6) | 107(6) | 25(5) | 1(4) | 3(4) |
C20A | 56(3) | 61(3) | 49(3) | -2(2) | -12(2) | 2(3) |
C19A | 73(3) | 57(3) | 60(3) | -13(3) | -21(3) | 5(3) |
C21A | 60(3) | 60(3) | 63(3) | -11(3) | -14(3) | 0(3) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Cl6A | C25 | 1.726(6) | C12 | C16 | 1.360(7) | |
Cl3A | C22 | 1.708(6) | C12 | C23 | 1.514(7) | |
Cl3 | C26 | 1.687(6) | C13 | C61 | 1.361(7) | |
O9AA | C23 | 1.221(6) | C14 | C16 | 1.471(7) | |
O1BA | C29 | 1.207(6) | C14 | C27 | 1.404(7) | |
O2AA | C8 | 1.394(6) | C16 | C28 | 1.512(7) | |
O2AA | C28 | 1.366(6) | C17 | C18 | 1.356(7) | |
O5AA | C24 | 1.210(6) | C17 | C29 | 1.502(7) | |
O7AA | C6 | 1.382(6) | C18 | C24 | 1.517(7) | |
O7AA | C29 | 1.362(6) | C19 | C20 | 1.386(8) | |
O4 | C28 | 1.194(6) | C19 | C21 | 1.402(8) | |
N8AA | C2BA | 1.401(6) | C22 | C26 | 1.410(8) | |
N8AA | C24 | 1.373(6) | C25 | C26 | 1.416(8) | |
N8AA | C31 | 1.459(6) | C27 | C82 | 1.368(7) | |
C0BA | C7 | 1.391(7) | C30 | C33 | 1.459(8) | |
C0BA | C21 | 1.367(7) | C31 | C35 | 1.511(8) | |
C2BA | C7 | 1.424(7) | C33 | C40 | 1.580(10) | |
C2BA | C20 | 1.383(7) | C33 | C43 | 1.470(11) | |
C5 | C6 | 1.399(6) | C33 | C43A | 1.417(13) | |
C5 | C13 | 1.398(7) | C34 | C35 | 1.492(10) | |
C5 | C17 | 1.476(7) | C34 | C36 | 1.542(12) | |
C6 | C131 | 1.361(7) | C35 | C37 | 1.559(11) | |
C7 | C18 | 1.478(7) | C35 | C34A | 1.508(16) | |
C8 | C14 | 1.395(7) | C36 | C34A | 1.573(16) | |
C8 | C272 | 1.368(7) | C37 | C39 | 1.490(11) | |
N9 | C10 | 1.398(6) | C38 | C40 | 1.415(11) | |
N9 | C23 | 1.365(6) | C39 | C45 | 1.554(11) | |
N9 | C30 | 1.471(6) | C41 | C42 | 1.448(10) | |
C10 | C15 | 1.405(7) | C42 | C46 | 1.545(15) | |
C10 | C25 | 1.379(7) | C43 | C46 | 1.580(11) | |
C11 | C15 | 1.397(7) | C45 | C48 | 1.469(14) | |
C11 | C22 | 1.360(8) | C46 | C43A | 1.583(15) | |
C12 | C15 | 1.456(7) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C28 | O2AA | C8 | 108.2(4) | C2BA | C20 | C19 | 119.0(5) | |
C29 | O7AA | C6 | 107.7(4) | C0BA | C21 | C19 | 120.3(5) | |
C2BA | N8AA | C31 | 129.6(4) | C11 | C22 | Cl3A | 118.9(5) | |
C24 | N8AA | C2BA | 110.4(4) | C11 | C22 | C26 | 120.5(5) | |
C24 | N8AA | C31 | 119.9(4) | C26 | C22 | Cl3A | 120.6(5) | |
C21 | C0BA | C7 | 120.5(5) | O9AA | C23 | N9 | 124.6(5) | |
N8AA | C2BA | C7 | 109.6(4) | O9AA | C23 | C12 | 127.3(5) | |
C20 | C2BA | N8AA | 129.7(5) | N9 | C23 | C12 | 108.1(4) | |
C20 | C2BA | C7 | 120.7(5) | O5AA | C24 | N8AA | 124.0(5) | |
C6 | C5 | C17 | 106.1(4) | O5AA | C24 | C18 | 127.7(5) | |
C13 | C5 | C6 | 117.5(4) | N8AA | C24 | C18 | 108.3(4) | |
C13 | C5 | C17 | 136.4(4) | C10 | C25 | Cl6A | 123.2(4) | |
O7AA | C6 | C5 | 112.6(4) | C10 | C25 | C26 | 118.9(5) | |
C131 | C6 | O7AA | 121.5(4) | C26 | C25 | Cl6A | 117.9(4) | |
C131 | C6 | C5 | 125.8(5) | C22 | C26 | Cl3 | 120.0(4) | |
C0BA | C7 | C2BA | 118.8(5) | C22 | C26 | C25 | 119.6(5) | |
C0BA | C7 | C18 | 133.5(5) | C25 | C26 | Cl3 | 120.4(5) | |
C2BA | C7 | C18 | 107.7(4) | C82 | C27 | C14 | 115.5(5) | |
O2AA | C8 | C14 | 112.2(4) | O2AA | C28 | C16 | 109.1(4) | |
C272 | C8 | O2AA | 121.1(4) | O4 | C28 | O2AA | 120.6(5) | |
C272 | C8 | C14 | 126.6(4) | O4 | C28 | C16 | 130.2(5) | |
C10 | N9 | C30 | 130.3(4) | O1BA | C29 | O7AA | 119.6(4) | |
C23 | N9 | C10 | 109.5(4) | O1BA | C29 | C17 | 130.4(5) | |
C23 | N9 | C30 | 119.3(4) | O7AA | C29 | C17 | 109.9(4) | |
N9 | C10 | C15 | 110.3(4) | C33 | C30 | N9 | 115.9(4) | |
C25 | C10 | N9 | 128.7(5) | N8AA | C31 | C35 | 115.0(5) | |
C25 | C10 | C15 | 121.0(5) | C30 | C33 | C40 | 108.8(5) | |
C22 | C11 | C15 | 120.6(5) | C30 | C33 | C43 | 120.3(7) | |
C15 | C12 | C23 | 104.1(4) | C43 | C33 | C40 | 108.5(7) | |
C16 | C12 | C15 | 133.3(5) | C43A | C33 | C30 | 135.2(8) | |
C16 | C12 | C23 | 122.7(5) | C43A | C33 | C40 | 115.3(9) | |
C61 | C13 | C5 | 116.7(4) | C35 | C34 | C36 | 113.6(7) | |
C8 | C14 | C16 | 106.6(4) | C31 | C35 | C37 | 109.7(6) | |
C8 | C14 | C27 | 117.9(5) | C34 | C35 | C31 | 115.5(6) | |
C27 | C14 | C16 | 135.4(5) | C34 | C35 | C37 | 107.6(7) | |
C10 | C15 | C12 | 107.6(4) | C34A | C35 | C31 | 132.7(11) | |
C11 | C15 | C10 | 119.4(5) | C34A | C35 | C37 | 117.3(11) | |
C11 | C15 | C12 | 132.9(5) | C39 | C37 | C35 | 113.1(8) | |
C12 | C16 | C14 | 131.8(5) | C37 | C39 | C45 | 121.5(9) | |
C12 | C16 | C28 | 124.4(5) | C38 | C40 | C33 | 115.7(8) | |
C14 | C16 | C28 | 103.8(4) | C41 | C42 | C46 | 108.9(9) | |
C5 | C17 | C29 | 103.3(4) | C33 | C43 | C46 | 114.2(8) | |
C18 | C17 | C5 | 132.4(4) | C48 | C45 | C39 | 109.3(11) | |
C18 | C17 | C29 | 124.1(5) | C42 | C46 | C43 | 95.7(7) | |
C7 | C18 | C24 | 103.9(4) | C42 | C46 | C43A | 132.9(10) | |
C17 | C18 | C7 | 132.6(4) | C33 | C43A | C46 | 117.1(11) | |
C17 | C18 | C24 | 123.4(5) | C35 | C34A | C36 | 110.9(13) | |
C20 | C19 | C21 | 120.7(5) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H0BA | 3850 | 7645 | 2785 | 62 |
H0BB | 3850 | 7645 | 2785 | 62 |
H11 | 10544 | 10489 | 2155 | 64 |
H11A | 10544 | 10489 | 2155 | 64 |
H13 | 5533 | 11385 | 4175 | 58 |
H19 | 5341 | 8203 | 891 | 75 |
H20 | 6005 | 9924 | 1037 | 67 |
H21 | 4296 | 7065 | 1767 | 73 |
H27 | 9294 | 8267 | 4813 | 63 |
H30A | 6905 | 6458 | 3426 | 70 |
H30B | 7375 | 6316 | 2689 | 70 |
H31A | 7213 | 11554 | 1508 | 72 |
H31B | 6773 | 12194 | 2123 | 72 |
H33 | 9925 | 5326 | 2838 | 146 |
H33A | 9116 | 5616 | 3694 | 146 |
H34A | 3385 | 13319 | 2230 | 119 |
H34B | 2754 | 12167 | 2224 | 119 |
H35 | 4394 | 12087 | 1176 | 126 |
H35A | 4332 | 12820 | 1916 | 126 |
H36A | 426 | 13464 | 1890 | 207 |
H36B | 1174 | 12794 | 1303 | 207 |
H36C | 1763 | 13951 | 1333 | 207 |
H36D | 1506 | 13413 | 2031 | 207 |
H36E | 252 | 13161 | 1518 | 207 |
H36F | 1776 | 13933 | 1316 | 207 |
H37A | 4507 | 14027 | 1034 | 203 |
H37B | 6034 | 13884 | 1509 | 203 |
H38A | 6237 | 4747 | 2787 | 228 |
H38B | 6510 | 3531 | 3064 | 228 |
H38C | 7979 | 4002 | 2549 | 228 |
H39A | 6515 | 12798 | 399 | 197 |
H39B | 8022 | 13014 | 819 | 197 |
H40A | 8878 | 3840 | 3555 | 199 |
H40B | 7157 | 4606 | 3781 | 199 |
H41A | 14784 | 3608 | 4344 | 229 |
H41B | 13015 | 3203 | 4723 | 229 |
H41C | 14167 | 3937 | 5046 | 229 |
H42A | 13435 | 5340 | 4287 | 195 |
H42B | 11678 | 4965 | 4696 | 195 |
H43A | 9715 | 5487 | 4157 | 110 |
H43B | 10994 | 6144 | 3659 | 110 |
H45A | 8633 | 14059 | -105 | 259 |
H45B | 6565 | 14439 | -178 | 259 |
H46A | 11449 | 3798 | 3805 | 169 |
H46B | 12846 | 4523 | 3385 | 169 |
H46C | 11038 | 3999 | 3910 | 169 |
H46D | 12952 | 4049 | 3544 | 169 |
H48A | 6444 | 15455 | 692 | 474 |
H48B | 7952 | 15816 | 156 | 474 |
H48C | 8502 | 15072 | 770 | 474 |
H25A | 9372 | 7064 | 1716 | 73 |
H26A | 10387 | 8320 | 874 | 80 |
H22A | 10989 | 10025 | 1115 | 77 |
H43C | 11616 | 5905 | 3132 | 110 |
H43D | 11435 | 4873 | 2788 | 110 |
H34C | 2504 | 11656 | 1661 | 119 |
H34D | 2814 | 12191 | 951 | 119 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
Cl0A | 0.802(2) | Cl2 | 0.802(2) | Cl1 | 0.802(2) | ||
Cl6A | 0.760(3) | Cl3A | 0.760(3) | Cl3 | 0.760(3) | ||
H0BA | 0.198(2) | H0BB | 0.802(2) | H11 | 0.760(3) | ||
H11A | 0.240(3) | C19 | 0.198(2) | H19 | 0.198(2) | ||
C20 | 0.198(2) | H20 | 0.198(2) | C21 | 0.198(2) | ||
H21 | 0.198(2) | C22 | 0.760(3) | C25 | 0.760(3) | ||
C26 | 0.760(3) | H33 | 0.683(9) | H33A | 0.317(9) | ||
C34 | 0.795(10) | H34A | 0.795(10) | H34B | 0.795(10) | ||
H35 | 0.795(10) | H35A | 0.205(10) | H36A | 0.795(10) | ||
H36B | 0.795(10) | H36C | 0.795(10) | H36D | 0.205(10) | ||
H36E | 0.205(10) | H36F | 0.205(10) | C43 | 0.683(9) | ||
H43A | 0.683(9) | H43B | 0.683(9) | H46A | 0.683(9) | ||
H46B | 0.683(9) | H46C | 0.317(9) | H46D | 0.317(9) | ||
C25A | 0.240(3) | H25A | 0.240(3) | C26A | 0.240(3) | ||
H26A | 0.240(3) | C22A | 0.240(3) | H22A | 0.240(3) | ||
C43A | 0.317(9) | H43C | 0.317(9) | H43D | 0.317(9) | ||
C34A | 0.205(10) | H34C | 0.205(10) | H34D | 0.205(10) | ||
C20A | 0.802(2) | C19A | 0.802(2) | C21A | 0.802(2) |
Experimental
Single crystals of C84H78.63Cl9.37N4O12 [3Cl-decomposition] 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 [3Cl-decomposition]
Crystal Data for C84H78.63Cl9.37N4O12 (M =1668.30 g/mol): triclinic, space group P-1 (no. 2), a = 7.4241(5) Å, b = 12.4935(9) Å, c = 20.8699(12) Å, α = 84.241(6)°, β = 83.819(5)°, γ = 83.303(6)°, V = 1903.8(2) Å3, Z = 1, T = 293(2) K, μ(CuKα) = 3.698 mm-1, Dcalc = 1.455 g/cm3, 10253 reflections measured (7.152° ≤ 2Θ ≤ 125.404°), 5920 unique (Rint = 0.0430, Rsigma = 0.0805) which were used in all calculations. The final R1 was 0.0919 (I > 2σ(I)) and wR2 was 0.2651 (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
{C25, C25A}
{C26, C26A}
{C22, C22A}
{C20, C20A}
{C19, C19A}
{C21, C21A}
3. Restrained distances
C42-C41
1.55 with sigma of 0.02
C48-C45
1.55 with sigma of 0.02
C45-C39
1.55 with sigma of 0.02
C39-C48
2.5 with sigma of 0.02
C39-C37
1.55 with sigma of 0.02
C40-C38
1.55 with sigma of 0.02
C43-C33
1.55 with sigma of 0.02
C35-C34A
1.55 with sigma of 0.02
C36-C34A
1.55 with sigma of 0.02
C43A-C33
1.55 with sigma of 0.02
C46-C43A
1.55 with sigma of 0.02
H46c-H40a
2 with sigma of 0.02
C35-C34
1.55 with sigma of 0.02
4. Rigid bond restraints
C37, C39, C45, C48
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C41, C42, C46, C43, C43A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C36, C34, C34A, C35
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C38, C40, C33
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 ≈ C45 ≈ C39 ≈ C37: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C43A ≈ C43 ≈ C46 ≈ C42 ≈ C41: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C35 ≈ C34A ≈ H34a ≈ C36: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C33 ≈ C40 ≈ C38: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C43) = Uanis(C43A)
Uanis(C34) = Uanis(C34A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C22) = Uanis(C22A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
Uanis(C19) = Uanis(C19A)
6. Others
Sof(Cl0A)=Sof(Cl2)=Sof(Cl1)=Sof(H0Bb)=Sof(C20A)=Sof(C19A)=Sof(C21A)=1-FVAR(1)
Sof(H0BA)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(1)
Sof(H33a)=Sof(H46c)=Sof(H46d)=Sof(C43A)=Sof(H43c)=Sof(H43d)=1-FVAR(2)
Sof(H33)=Sof(C43)=Sof(H43a)=Sof(H43b)=Sof(H46a)=Sof(H46b)=FVAR(2)
Sof(H35a)=Sof(H36d)=Sof(H36e)=Sof(H36f)=Sof(C34A)=Sof(H34c)=Sof(H34d)=1-FVAR(3)
Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(H35)=Sof(H36a)=Sof(H36b)=Sof(H36c)=FVAR(3)
Sof(H11a)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C22A)=Sof(H22A)=1-FVAR(4)
Sof(Cl6A)=Sof(Cl3A)=Sof(Cl3)=Sof(H11)=Sof(C22)=Sof(C25)=Sof(C26)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
C33(H33), C33(H33a), C35(H35), C35(H35a)
7.b Secondary CH2 refined with riding coordinates:
C30(H30a,H30b), C31(H31a,H31b), C34(H34a,H34b), C37(H37a,H37b), C39(H39a,
H39b), C40(H40a,H40b), C42(H42a,H42b), C43(H43a,H43b), C45(H45a,H45b),
C46(H46a,H46b), C46(H46c,H46d), C43A(H43c,H43d), C34A(H34c,H34d)
7.c Me refined with riding coordinates:
C36(H36a,H36b,H36c), C36(H36d,H36e,H36f), C38(H38a,H38b,H38c), C41(H41a,H41b,
H41c), C48(H48a,H48b,H48c)
7.d Aromatic/amide H refined with riding coordinates:
C0BA(H0BA), C0BA(H0Bb), C11(H11), C11(H11a), C13(H13), C19(H19), C20(H20),
C21(H21), C27(H27), C25A(H25A), C26A(H26A), C22A(H22A)
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.