Identification code | 6Cl |
Empirical formula | C42H38Cl6N2O6 |
Formula weight | 879.44 |
Temperature/K | 113.15 |
Crystal system | triclinic |
Space group | P-1 |
a/Å | 7.4787(6) |
b/Å | 12.4743(8) |
c/Å | 21.0321(14) |
α/° | 83.940(6) |
β/° | 82.931(6) |
γ/° | 82.882(6) |
Volume/Å3 | 1924.1(2) |
Z | 2 |
ρcalcg/cm3 | 1.518 |
μ/mm‑1 | 4.512 |
F(000) | 908.0 |
Crystal size/mm3 | 0.5 × 0.06 × 0.02 |
Radiation | CuKα (λ = 1.54178) |
2Θ range for data collection/° | 7.172 to 125.124 |
Index ranges | -8 ≤ h ≤ 7, -14 ≤ k ≤ 13, -19 ≤ l ≤ 23 |
Reflections collected | 10560 |
Independent reflections | 5943 [Rint = 0.0453, Rsigma = 0.0698] |
Data/restraints/parameters | 5943/136/483 |
Goodness-of-fit on F2 | 1.081 |
Final R indexes [I>=2σ (I)] | R1 = 0.0793, wR2 = 0.1926 |
Final R indexes [all data] | R1 = 0.1060, wR2 = 0.2132 |
Largest diff. peak/hole / e Å-3 | 0.72/-0.56 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Cl1 | 4019.3(17) | -3483.6(10) | 1755.6(6) | 43.6(3) |
Cl2 | 5519(2) | -1983.5(10) | 570.0(6) | 51.8(4) |
Cl3 | 6466.7(18) | 283.7(10) | 739.6(6) | 44.4(3) |
O1 | 5434(5) | 1568(3) | 3188.9(17) | 48.7(10) |
O2 | 6954(5) | 2300(3) | 6212.7(16) | 44.3(9) |
O3 | 6180(4) | 1824(2) | 5310.1(15) | 37.8(8) |
N1 | 5684(5) | 829(3) | 2234.5(18) | 30.8(9) |
C1 | 4518(6) | -2204(4) | 1859(2) | 37.6(11) |
C2 | 5194(6) | -1533(4) | 1320(2) | 37.0(11) |
C3 | 5606(6) | -497(4) | 1414(2) | 33.7(11) |
C4 | 5352(6) | -138(4) | 2020(2) | 30.5(10) |
C5 | 4697(6) | -843(4) | 2563(2) | 30.0(10) |
C6 | 4275(6) | -1859(4) | 2463(2) | 33.1(11) |
C7 | 5316(6) | 806(4) | 2891(2) | 33.5(11) |
C8 | 4713(6) | -280(4) | 3138(2) | 33.8(11) |
C9 | 4406(6) | -597(4) | 3783(2) | 37.6(12) |
C10 | 6301(6) | 1665(4) | 5958(2) | 35.8(12) |
C11 | 5583(6) | 906(4) | 5120(2) | 36.2(12) |
C12 | 4728(6) | -128(4) | 4358(2) | 36.7(11) |
C13 | 5328(6) | 845(4) | 4495(2) | 36.5(12) |
C14 | 6224(11) | 1836(7) | 1862(5) | 50.6(9) |
C15 | 4719(9) | 2508(5) | 1504(3) | 50.6(9) |
C16 | 3105(8) | 2824(7) | 2007(3) | 50.6(9) |
C17 | 1428(10) | 3398(7) | 1723(4) | 50.6(9) |
C18 | 5470(10) | 3524(6) | 1145(4) | 50.6(9) |
C19 | 7022(10) | 3291(6) | 609(3) | 50.6(9) |
C20 | 7399(12) | 4208(5) | 83(3) | 50.6(9) |
C21 | 7714(11) | 5214(6) | 392(4) | 50.6(9) |
C14' | 6349(17) | 1773(10) | 1860(10) | 50.1(17) |
C15' | 4811(11) | 2683(7) | 1758(6) | 50.1(17) |
C16' | 3139(11) | 2378(9) | 1505(7) | 50.1(17) |
C17' | 1411(15) | 3187(10) | 1522(9) | 50.1(17) |
C18' | 5540(18) | 3736(8) | 1456(5) | 50.1(17) |
C19' | 6405(19) | 3620(8) | 763(5) | 50.1(17) |
C20' | 7103(18) | 4692(8) | 479(5) | 50.1(17) |
C21' | 8040(20) | 4711(12) | -216(5) | 50.1(17) |
Cl4 | 852.8(17) | 3448.5(10) | 8383.5(6) | 43.1(3) |
Cl5 | -557(2) | 1778.7(11) | 9454.3(6) | 53.5(4) |
Cl6 | -1379.0(18) | -484.9(11) | 9138.8(6) | 47.1(3) |
O4 | 2142(4) | 2151(3) | 5934.7(15) | 38.4(8) |
O5 | 226(5) | 1535(3) | 3990.7(16) | 42.1(9) |
O6 | -41(5) | 1531(3) | 2949.1(17) | 51.0(10) |
N2 | 1375(5) | 2506(3) | 6985.2(18) | 31.8(9) |
C22 | 459(6) | 2199(4) | 8178(2) | 34.8(11) |
C23 | -213(7) | 1443(4) | 8677(2) | 38.6(12) |
C24 | -574(6) | 437(4) | 8525(2) | 33.9(11) |
C25 | -295(6) | 146(4) | 7910(2) | 32.9(11) |
C26 | 362(6) | 879(4) | 7408(2) | 31.4(10) |
C27 | 742(6) | 1913(4) | 7556(2) | 30.8(10) |
C28 | 1450(6) | 1893(4) | 6474(2) | 31.6(11) |
C29 | 670(6) | 854(4) | 6720(2) | 33.0(11) |
C30 | 393(6) | 103(4) | 6312(2) | 31.5(10) |
C31 | 297(6) | 207(4) | 5622(2) | 34.1(11) |
C32 | 421(6) | 1046(4) | 5122(2) | 34.4(11) |
C33 | 117(6) | 797(4) | 4530(2) | 32.5(11) |
C34 | -48(7) | 1036(4) | 3469(2) | 37.2(12) |
C35 | 2165(12) | 3548(6) | 6878(5) | 55.7(9) |
C36 | 776(9) | 4561(5) | 6804(4) | 55.7(9) |
C37 | 1867(10) | 5547(6) | 6644(4) | 55.7(9) |
C38 | 3090(10) | 5711(7) | 7145(4) | 55.7(9) |
C39 | -341(9) | 4451(6) | 6252(4) | 55.7(9) |
C40 | -1720(9) | 5423(6) | 6102(4) | 55.7(9) |
C41 | -2877(10) | 5150(6) | 5598(4) | 55.7(9) |
C42 | -3990(11) | 6161(6) | 5329(4) | 55.7(9) |
C35' | 2242(19) | 3521(10) | 6898(7) | 36.1(15) |
C36' | 1142(10) | 4424(7) | 6510(6) | 36.1(15) |
C37' | 2240(15) | 5391(7) | 6306(5) | 36.1(15) |
C38' | 2637(19) | 5944(10) | 6882(5) | 36.1(15) |
C39' | -753(11) | 4730(9) | 6850(5) | 36.1(15) |
C40' | -1953(15) | 5608(9) | 6475(4) | 36.1(15) |
C41' | -2210(16) | 5325(8) | 5801(4) | 36.1(15) |
C42' | -3384(16) | 6291(9) | 5490(7) | 36.1(15) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Cl1 | 52.6(7) | 33.5(6) | 48.2(7) | -6.9(5) | -13.7(5) | -7.3(5) |
Cl2 | 81.4(9) | 42.4(7) | 34.8(6) | -5.4(5) | -14.5(6) | -10.0(6) |
Cl3 | 60.1(8) | 40.4(7) | 32.2(6) | 2.2(5) | -6.8(5) | -6.5(6) |
O1 | 75(2) | 31.9(18) | 41.2(19) | -5.5(15) | -1.3(17) | -16.9(16) |
O2 | 57(2) | 36.9(18) | 41.5(19) | -7.8(15) | 2.6(16) | -18.9(16) |
O3 | 41.4(18) | 33.3(17) | 38.9(18) | -3.6(14) | 5.1(14) | -13.7(14) |
N1 | 30.8(19) | 26.8(19) | 36(2) | -0.4(16) | -5.6(16) | -6.6(15) |
C1 | 37(3) | 32(2) | 45(3) | -4(2) | -15(2) | 0(2) |
C2 | 41(3) | 31(2) | 40(2) | 1(2) | -15(2) | -1(2) |
C3 | 34(2) | 33(2) | 33(2) | 2.3(19) | -8.9(19) | 1.6(19) |
C4 | 22(2) | 29(2) | 39(2) | 1.9(18) | -7.2(18) | 1.1(18) |
C5 | 25(2) | 28(2) | 37(2) | -1.2(18) | -7.8(18) | 0.5(18) |
C6 | 28(2) | 33(2) | 38(2) | -1.0(19) | -7.6(19) | -2.0(19) |
C7 | 34(2) | 30(2) | 37(3) | -1(2) | -6(2) | -6.1(19) |
C8 | 29(2) | 32(2) | 41(2) | -4.2(19) | -2(2) | -4.9(19) |
C9 | 37(3) | 31(2) | 43(2) | -6(2) | 1(2) | -3(2) |
C10 | 41(3) | 31(2) | 35(3) | -6(2) | 6(2) | -7(2) |
C11 | 38(3) | 32(3) | 38(3) | -8(2) | 6(2) | -9(2) |
C12 | 33(2) | 35(3) | 40(2) | -6(2) | 1(2) | 1(2) |
C13 | 35(2) | 32(2) | 41(3) | -5(2) | 5(2) | -5(2) |
C14 | 51.0(18) | 44.7(17) | 53.9(19) | -0.6(14) | -4.2(14) | -1.5(14) |
C15 | 51.0(18) | 44.7(17) | 53.9(19) | -0.6(14) | -4.2(14) | -1.5(14) |
C16 | 51.0(18) | 44.7(17) | 53.9(19) | -0.6(14) | -4.2(14) | -1.5(14) |
C17 | 51.0(18) | 44.7(17) | 53.9(19) | -0.6(14) | -4.2(14) | -1.5(14) |
C18 | 51.0(18) | 44.7(17) | 53.9(19) | -0.6(14) | -4.2(14) | -1.5(14) |
C19 | 51.0(18) | 44.7(17) | 53.9(19) | -0.6(14) | -4.2(14) | -1.5(14) |
C20 | 51.0(18) | 44.7(17) | 53.9(19) | -0.6(14) | -4.2(14) | -1.5(14) |
C21 | 51.0(18) | 44.7(17) | 53.9(19) | -0.6(14) | -4.2(14) | -1.5(14) |
C14' | 55(3) | 32(3) | 63(4) | 1(3) | -5(3) | -11(2) |
C15' | 55(3) | 32(3) | 63(4) | 1(3) | -5(3) | -11(2) |
C16' | 55(3) | 32(3) | 63(4) | 1(3) | -5(3) | -11(2) |
C17' | 55(3) | 32(3) | 63(4) | 1(3) | -5(3) | -11(2) |
C18' | 55(3) | 32(3) | 63(4) | 1(3) | -5(3) | -11(2) |
C19' | 55(3) | 32(3) | 63(4) | 1(3) | -5(3) | -11(2) |
C20' | 55(3) | 32(3) | 63(4) | 1(3) | -5(3) | -11(2) |
C21' | 55(3) | 32(3) | 63(4) | 1(3) | -5(3) | -11(2) |
Cl4 | 52.9(7) | 39.2(6) | 40.2(6) | -9.9(5) | -9.4(5) | -7.5(5) |
Cl5 | 77.9(9) | 54.0(8) | 29.2(6) | -5.1(5) | -4.7(6) | -10.0(7) |
Cl6 | 56.0(7) | 47.6(7) | 35.5(6) | 6.6(5) | -3.1(5) | -8.4(6) |
O4 | 42.0(18) | 39.6(18) | 34.7(18) | -2.3(14) | 1.3(14) | -15.3(14) |
O5 | 54(2) | 37.6(18) | 36.5(18) | 0.1(15) | -5.6(15) | -13.0(15) |
O6 | 81(3) | 37.9(19) | 38.1(19) | 0.6(16) | -11.0(17) | -22.3(17) |
N2 | 31.2(19) | 29(2) | 36(2) | -0.8(16) | -7.9(16) | -3.8(16) |
C22 | 29(2) | 38(2) | 38(2) | -5.2(19) | -10.6(19) | 1.7(19) |
C23 | 42(3) | 46(3) | 29(2) | -2(2) | -10(2) | -1(2) |
C24 | 33(2) | 31(2) | 36(2) | 4.1(19) | -7.7(19) | -0.1(19) |
C25 | 29(2) | 35(2) | 35(2) | -1.3(19) | -9.9(19) | -2.4(19) |
C26 | 27(2) | 32(2) | 35(2) | -1.0(18) | -10.2(18) | -1.9(18) |
C27 | 24(2) | 35(2) | 33(2) | 0.1(19) | -9.3(18) | -0.1(18) |
C28 | 28(2) | 30(2) | 38(2) | -3.6(19) | -6.5(19) | -4.7(18) |
C29 | 31(2) | 30(2) | 38(2) | 2.5(18) | -10.1(19) | -4.0(19) |
C30 | 30(2) | 30(2) | 33(2) | -1.5(18) | -0.7(19) | -6.7(19) |
C31 | 28(2) | 35(3) | 39(2) | 0(2) | -3.2(19) | -5.7(19) |
C32 | 34(2) | 33(2) | 37(2) | -0.9(19) | -2(2) | -11(2) |
C33 | 33(2) | 30(2) | 33(2) | 3(2) | -1.0(19) | -5.8(19) |
C34 | 43(3) | 34(3) | 36(3) | -5(2) | -5(2) | -9(2) |
C35 | 58.6(18) | 43.6(17) | 70(2) | 1.0(14) | -26.3(15) | -11.7(13) |
C36 | 58.6(18) | 43.6(17) | 70(2) | 1.0(14) | -26.3(15) | -11.7(13) |
C37 | 58.6(18) | 43.6(17) | 70(2) | 1.0(14) | -26.3(15) | -11.7(13) |
C38 | 58.6(18) | 43.6(17) | 70(2) | 1.0(14) | -26.3(15) | -11.7(13) |
C39 | 58.6(18) | 43.6(17) | 70(2) | 1.0(14) | -26.3(15) | -11.7(13) |
C40 | 58.6(18) | 43.6(17) | 70(2) | 1.0(14) | -26.3(15) | -11.7(13) |
C41 | 58.6(18) | 43.6(17) | 70(2) | 1.0(14) | -26.3(15) | -11.7(13) |
C42 | 58.6(18) | 43.6(17) | 70(2) | 1.0(14) | -26.3(15) | -11.7(13) |
C35' | 32(3) | 38(3) | 43(3) | -4(2) | -11(2) | -14(2) |
C36' | 32(3) | 38(3) | 43(3) | -4(2) | -11(2) | -14(2) |
C37' | 32(3) | 38(3) | 43(3) | -4(2) | -11(2) | -14(2) |
C38' | 32(3) | 38(3) | 43(3) | -4(2) | -11(2) | -14(2) |
C39' | 32(3) | 38(3) | 43(3) | -4(2) | -11(2) | -14(2) |
C40' | 32(3) | 38(3) | 43(3) | -4(2) | -11(2) | -14(2) |
C41' | 32(3) | 38(3) | 43(3) | -4(2) | -11(2) | -14(2) |
C42' | 32(3) | 38(3) | 43(3) | -4(2) | -11(2) | -14(2) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Cl1 | C1 | 1.725(5) | Cl4 | C22 | 1.729(5) | |
Cl2 | C2 | 1.710(5) | Cl5 | C23 | 1.712(5) | |
Cl3 | C3 | 1.737(5) | Cl6 | C24 | 1.738(5) | |
O1 | C7 | 1.211(6) | O4 | C28 | 1.215(5) | |
O2 | C10 | 1.185(6) | O5 | C33 | 1.385(5) | |
O3 | C10 | 1.368(6) | O5 | C34 | 1.365(6) | |
O3 | C11 | 1.391(6) | O6 | C34 | 1.198(6) | |
N1 | C4 | 1.392(6) | N2 | C27 | 1.403(6) | |
N1 | C7 | 1.372(6) | N2 | C28 | 1.376(6) | |
N1 | C14 | 1.482(10) | N2 | C35 | 1.479(10) | |
N1 | C14' | 1.452(15) | N2 | C35' | 1.478(15) | |
C1 | C2 | 1.415(7) | C22 | C23 | 1.421(7) | |
C1 | C6 | 1.369(7) | C22 | C27 | 1.378(6) | |
C2 | C3 | 1.404(7) | C23 | C24 | 1.394(7) | |
C3 | C4 | 1.378(7) | C24 | C25 | 1.363(7) | |
C4 | C5 | 1.440(6) | C25 | C26 | 1.404(6) | |
C5 | C6 | 1.386(6) | C26 | C27 | 1.428(7) | |
C5 | C8 | 1.463(7) | C26 | C29 | 1.441(6) | |
C7 | C8 | 1.502(6) | C28 | C29 | 1.504(6) | |
C8 | C9 | 1.372(7) | C29 | C30 | 1.385(7) | |
C9 | C101 | 1.517(7) | C30 | C31 | 1.451(7) | |
C9 | C12 | 1.456(7) | C30 | C342 | 1.491(6) | |
C10 | C91 | 1.517(7) | C31 | C32 | 1.406(6) | |
C11 | C121 | 1.403(7) | C31 | C332 | 1.405(7) | |
C11 | C13 | 1.362(7) | C32 | C33 | 1.366(7) | |
C12 | C111 | 1.403(7) | C33 | C312 | 1.405(7) | |
C12 | C13 | 1.413(7) | C34 | C302 | 1.491(6) | |
C14 | C15 | 1.542(8) | C35 | C36 | 1.540(7) | |
C15 | C16 | 1.545(7) | C36 | C37 | 1.545(7) | |
C15 | C18 | 1.536(7) | C36 | C39 | 1.539(7) | |
C16 | C17 | 1.520(8) | C37 | C38 | 1.522(8) | |
C18 | C19 | 1.538(7) | C39 | C40 | 1.524(7) | |
C19 | C20 | 1.533(7) | C40 | C41 | 1.536(8) | |
C20 | C21 | 1.528(8) | C41 | C42 | 1.520(7) | |
C14' | C15' | 1.531(9) | C35' | C36' | 1.535(9) | |
C15' | C16' | 1.521(9) | C36' | C37' | 1.538(8) | |
C15' | C18' | 1.531(9) | C36' | C39' | 1.530(8) | |
C16' | C17' | 1.537(9) | C37' | C38' | 1.533(9) | |
C18' | C19' | 1.534(9) | C39' | C40' | 1.542(9) | |
C19' | C20' | 1.531(9) | C40' | C41' | 1.536(9) | |
C20' | C21' | 1.541(9) | C41' | C42' | 1.537(9) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C10 | O3 | C11 | 108.2(3) | C34 | O5 | C33 | 108.9(4) | |
C4 | N1 | C14 | 129.8(5) | C27 | N2 | C35 | 130.9(5) | |
C4 | N1 | C14' | 128.5(9) | C27 | N2 | C35' | 129.4(7) | |
C7 | N1 | C4 | 110.8(4) | C28 | N2 | C27 | 109.8(4) | |
C7 | N1 | C14 | 119.2(5) | C28 | N2 | C35 | 118.6(5) | |
C7 | N1 | C14' | 120.6(9) | C28 | N2 | C35' | 119.6(7) | |
C2 | C1 | Cl1 | 119.6(4) | C23 | C22 | Cl4 | 118.1(4) | |
C6 | C1 | Cl1 | 119.4(4) | C27 | C22 | Cl4 | 123.0(4) | |
C6 | C1 | C2 | 121.1(4) | C27 | C22 | C23 | 118.9(4) | |
C1 | C2 | Cl2 | 120.5(4) | C22 | C23 | Cl5 | 119.6(4) | |
C3 | C2 | Cl2 | 120.7(4) | C24 | C23 | Cl5 | 121.0(4) | |
C3 | C2 | C1 | 118.8(4) | C24 | C23 | C22 | 119.4(4) | |
C2 | C3 | Cl3 | 116.9(4) | C23 | C24 | Cl6 | 119.0(4) | |
C4 | C3 | Cl3 | 122.4(4) | C25 | C24 | Cl6 | 118.9(4) | |
C4 | C3 | C2 | 120.7(4) | C25 | C24 | C23 | 122.1(4) | |
N1 | C4 | C5 | 109.1(4) | C24 | C25 | C26 | 119.7(4) | |
C3 | C4 | N1 | 131.3(4) | C25 | C26 | C27 | 119.0(4) | |
C3 | C4 | C5 | 119.6(4) | C25 | C26 | C29 | 133.1(4) | |
C4 | C5 | C8 | 107.0(4) | C27 | C26 | C29 | 107.8(4) | |
C6 | C5 | C4 | 119.3(4) | N2 | C27 | C26 | 109.1(4) | |
C6 | C5 | C8 | 133.7(4) | C22 | C27 | N2 | 130.0(4) | |
C1 | C6 | C5 | 120.6(4) | C22 | C27 | C26 | 120.9(4) | |
O1 | C7 | N1 | 123.3(4) | O4 | C28 | N2 | 124.0(4) | |
O1 | C7 | C8 | 128.7(4) | O4 | C28 | C29 | 128.0(4) | |
N1 | C7 | C8 | 108.0(4) | N2 | C28 | C29 | 107.8(4) | |
C5 | C8 | C7 | 105.0(4) | C26 | C29 | C28 | 105.1(4) | |
C9 | C8 | C5 | 132.6(4) | C30 | C29 | C26 | 132.9(4) | |
C9 | C8 | C7 | 122.3(4) | C30 | C29 | C28 | 122.1(4) | |
C8 | C9 | C101 | 123.0(4) | C29 | C30 | C31 | 131.1(4) | |
C8 | C9 | C12 | 133.1(5) | C29 | C30 | C342 | 124.0(4) | |
C12 | C9 | C101 | 103.8(4) | C31 | C30 | C342 | 104.9(4) | |
O2 | C10 | O3 | 119.8(4) | C32 | C31 | C30 | 135.8(4) | |
O2 | C10 | C91 | 131.3(5) | C332 | C31 | C30 | 106.5(4) | |
O3 | C10 | C91 | 108.9(4) | C332 | C31 | C32 | 117.6(4) | |
O3 | C11 | C121 | 111.7(4) | C33 | C32 | C31 | 116.0(4) | |
C13 | C11 | O3 | 120.9(4) | O5 | C33 | C312 | 111.2(4) | |
C13 | C11 | C121 | 127.4(4) | C32 | C33 | O5 | 122.5(4) | |
C111 | C12 | C9 | 107.0(4) | C32 | C33 | C312 | 126.3(4) | |
C111 | C12 | C13 | 116.7(4) | O5 | C34 | C302 | 108.5(4) | |
C13 | C12 | C9 | 136.2(5) | O6 | C34 | O5 | 120.4(4) | |
C11 | C13 | C12 | 115.9(4) | O6 | C34 | C302 | 131.1(5) | |
N1 | C14 | C15 | 114.8(6) | N2 | C35 | C36 | 114.8(6) | |
C14 | C15 | C16 | 108.1(6) | C35 | C36 | C37 | 106.9(6) | |
C18 | C15 | C14 | 108.9(6) | C39 | C36 | C35 | 109.1(6) | |
C18 | C15 | C16 | 110.9(6) | C39 | C36 | C37 | 110.4(6) | |
C17 | C16 | C15 | 114.6(6) | C38 | C37 | C36 | 115.2(6) | |
C15 | C18 | C19 | 114.6(6) | C40 | C39 | C36 | 115.0(6) | |
C20 | C19 | C18 | 117.8(6) | C39 | C40 | C41 | 109.2(6) | |
C21 | C20 | C19 | 109.5(6) | C42 | C41 | C40 | 111.0(6) | |
N1 | C14' | C15' | 111.5(9) | N2 | C35' | C36' | 111.4(10) | |
C14' | C15' | C18' | 111.5(9) | C35' | C36' | C37' | 110.6(9) | |
C16' | C15' | C14' | 116.9(9) | C39' | C36' | C35' | 112.5(9) | |
C16' | C15' | C18' | 117.0(10) | C39' | C36' | C37' | 114.1(8) | |
C15' | C16' | C17' | 119.2(10) | C38' | C37' | C36' | 112.4(9) | |
C15' | C18' | C19' | 111.0(9) | C36' | C39' | C40' | 115.1(9) | |
C20' | C19' | C18' | 109.2(8) | C41' | C40' | C39' | 113.9(9) | |
C19' | C20' | C21' | 116.1(9) | C40' | C41' | C42' | 107.1(9) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H6 | 3812 | -2320 | 2818 | 40 |
H13 | 5540 | 1421 | 4172 | 44 |
H14A | 7272 | 1641 | 1544 | 61 |
H14B | 6631 | 2296 | 2160 | 61 |
H15 | 4322 | 2064 | 1189 | 61 |
H16A | 2772 | 2158 | 2271 | 61 |
H16B | 3500 | 3302 | 2297 | 61 |
H17A | 485 | 3588 | 2072 | 76 |
H17B | 981 | 2917 | 1455 | 76 |
H17C | 1739 | 4060 | 1461 | 76 |
H18A | 5910 | 3936 | 1460 | 61 |
H18B | 4468 | 3991 | 954 | 61 |
H19A | 8149 | 3067 | 814 | 61 |
H19B | 6763 | 2663 | 398 | 61 |
H20A | 8484 | 3976 | -211 | 61 |
H20B | 6355 | 4381 | -172 | 61 |
H21A | 7915 | 5807 | 56 | 76 |
H21B | 8781 | 5048 | 627 | 76 |
H21C | 6649 | 5431 | 690 | 76 |
H14C | 6942 | 1564 | 1437 | 60 |
H14D | 7269 | 2041 | 2086 | 60 |
H15' | 4349 | 2855 | 2207 | 60 |
H16C | 2820 | 1694 | 1752 | 60 |
H16D | 3488 | 2217 | 1053 | 60 |
H17D | 582 | 2994 | 1904 | 75 |
H17E | 818 | 3161 | 1135 | 75 |
H17F | 1730 | 3921 | 1539 | 75 |
H18C | 6455 | 3924 | 1715 | 60 |
H18D | 4536 | 4333 | 1457 | 60 |
H19C | 7422 | 3030 | 759 | 60 |
H19D | 5497 | 3432 | 500 | 60 |
H20C | 7970 | 4876 | 759 | 60 |
H20D | 6066 | 5268 | 493 | 60 |
H21D | 8377 | 5440 | -359 | 75 |
H21E | 7211 | 4517 | -500 | 75 |
H21F | 9135 | 4189 | -232 | 75 |
H25 | -544 | -549 | 7822 | 40 |
H32 | 699 | 1744 | 5192 | 41 |
H35A | 3043 | 3535 | 6485 | 67 |
H35B | 2847 | 3613 | 7244 | 67 |
H36 | -41 | 4639 | 7214 | 67 |
H37A | 2625 | 5464 | 6228 | 67 |
H37B | 1004 | 6210 | 6588 | 67 |
H38A | 3709 | 6358 | 7008 | 84 |
H38B | 3992 | 5075 | 7192 | 84 |
H38C | 2356 | 5804 | 7559 | 84 |
H39A | 503 | 4331 | 5858 | 67 |
H39B | -991 | 3800 | 6361 | 67 |
H40A | -1085 | 6063 | 5934 | 67 |
H40B | -2508 | 5601 | 6499 | 67 |
H41A | -2076 | 4819 | 5244 | 67 |
H41B | -3699 | 4615 | 5799 | 67 |
H42A | -4733 | 5964 | 5016 | 84 |
H42B | -3175 | 6681 | 5117 | 84 |
H42C | -4780 | 6491 | 5680 | 84 |
H35C | 3479 | 3385 | 6672 | 43 |
H35D | 2351 | 3759 | 7325 | 43 |
H36' | 962 | 4119 | 6104 | 43 |
H37C | 3401 | 5136 | 6059 | 43 |
H37D | 1557 | 5928 | 6019 | 43 |
H38D | 3369 | 6539 | 6730 | 54 |
H38E | 3304 | 5414 | 7170 | 54 |
H38F | 1493 | 6232 | 7116 | 54 |
H39C | -624 | 4988 | 7270 | 43 |
H39D | -1383 | 4069 | 6939 | 43 |
H40C | -3158 | 5726 | 6727 | 43 |
H40D | -1402 | 6298 | 6432 | 43 |
H41C | -2820 | 4658 | 5833 | 43 |
H41D | -1021 | 5202 | 5540 | 43 |
H42D | -3553 | 6147 | 5053 | 54 |
H42E | -2779 | 6949 | 5471 | 54 |
H42F | -4567 | 6392 | 5747 | 54 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
C14 | 0.652(5) | H14A | 0.652(5) | H14B | 0.652(5) | ||
C15 | 0.652(5) | H15 | 0.652(5) | C16 | 0.652(5) | ||
H16A | 0.652(5) | H16B | 0.652(5) | C17 | 0.652(5) | ||
H17A | 0.652(5) | H17B | 0.652(5) | H17C | 0.652(5) | ||
C18 | 0.652(5) | H18A | 0.652(5) | H18B | 0.652(5) | ||
C19 | 0.652(5) | H19A | 0.652(5) | H19B | 0.652(5) | ||
C20 | 0.652(5) | H20A | 0.652(5) | H20B | 0.652(5) | ||
C21 | 0.652(5) | H21A | 0.652(5) | H21B | 0.652(5) | ||
H21C | 0.652(5) | C14' | 0.348(5) | H14C | 0.348(5) | ||
H14D | 0.348(5) | C15' | 0.348(5) | H15' | 0.348(5) | ||
C16' | 0.348(5) | H16C | 0.348(5) | H16D | 0.348(5) | ||
C17' | 0.348(5) | H17D | 0.348(5) | H17E | 0.348(5) | ||
H17F | 0.348(5) | C18' | 0.348(5) | H18C | 0.348(5) | ||
H18D | 0.348(5) | C19' | 0.348(5) | H19C | 0.348(5) | ||
H19D | 0.348(5) | C20' | 0.348(5) | H20C | 0.348(5) | ||
H20D | 0.348(5) | C21' | 0.348(5) | H21D | 0.348(5) | ||
H21E | 0.348(5) | H21F | 0.348(5) | C35 | 0.682(5) | ||
H35A | 0.682(5) | H35B | 0.682(5) | C36 | 0.682(5) | ||
H36 | 0.682(5) | C37 | 0.682(5) | H37A | 0.682(5) | ||
H37B | 0.682(5) | C38 | 0.682(5) | H38A | 0.682(5) | ||
H38B | 0.682(5) | H38C | 0.682(5) | C39 | 0.682(5) | ||
H39A | 0.682(5) | H39B | 0.682(5) | C40 | 0.682(5) | ||
H40A | 0.682(5) | H40B | 0.682(5) | C41 | 0.682(5) | ||
H41A | 0.682(5) | H41B | 0.682(5) | C42 | 0.682(5) | ||
H42A | 0.682(5) | H42B | 0.682(5) | H42C | 0.682(5) | ||
C35' | 0.318(5) | H35C | 0.318(5) | H35D | 0.318(5) | ||
C36' | 0.318(5) | H36' | 0.318(5) | C37' | 0.318(5) | ||
H37C | 0.318(5) | H37D | 0.318(5) | C38' | 0.318(5) | ||
H38D | 0.318(5) | H38E | 0.318(5) | H38F | 0.318(5) | ||
C39' | 0.318(5) | H39C | 0.318(5) | H39D | 0.318(5) | ||
C40' | 0.318(5) | H40C | 0.318(5) | H40D | 0.318(5) | ||
C41' | 0.318(5) | H41C | 0.318(5) | H41D | 0.318(5) | ||
C42' | 0.318(5) | H42D | 0.318(5) | H42E | 0.318(5) | ||
H42F | 0.318(5) |
Experimental
Single crystals of C42H38Cl6N2O6 [6Cl] were []. A suitable crystal was selected and [] on a diffractometer. The crystal was kept at 113.15 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 [6Cl]
Crystal Data for C42H38Cl6N2O6 (M =879.44 g/mol): triclinic, space group P-1 (no. 2), a = 7.4787(6) Å, b = 12.4743(8) Å, c = 21.0321(14) Å, α = 83.940(6)°, β = 82.931(6)°, γ = 82.882(6)°, V = 1924.1(2) Å3, Z = 2, T = 113.15 K, μ(CuKα) = 4.512 mm-1, Dcalc = 1.518 g/cm3, 10560 reflections measured (7.172° ≤ 2Θ ≤ 125.124°), 5943 unique (Rint = 0.0453, Rsigma = 0.0698) which were used in all calculations. The final R1 was 0.0793 (I > 2σ(I)) and wR2 was 0.2132 (all data).
Refinement model description
Number of restraints - 136, 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. Restrained distances
C14-C15 = C15-C16 = C16-C17 = C15-C18 = C18-C19 = C19-C20 = C20-C21
1.54 with sigma of 0.01
C14'-C15' = C15'-C16' = C16'-C17'
1.54 with sigma of 0.01
C15'-C18' = C18'-C19' = C19'-C20' = C20'-C21'
1.54 with sigma of 0.01
C35'-C36' = C36'-C37' = C37'-C38'
1.54 with sigma of 0.01
C36'-C39' = C39'-C40' = C40'-C41' = C41'-C42'
1.54 with sigma of 0.01
C35-C36 = C36-C37 = C37-C38 = C36-C39 = C39-C40 = C40-C41 = C41-C42
1.54 with sigma of 0.01
3. Rigid bond restraints
C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
C18, C19, C20, C21, C14', C15', C16', C17', C18', C19', C20', C21', C22, C23,
C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39,
C40, C41, C42, C35', C36', C37', C38', C39', C40', C41', C42'
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) =
Uanis(C20) = Uanis(C21)
Uanis(C14') = Uanis(C15') = Uanis(C16') = Uanis(C17') = Uanis(C18') =
Uanis(C19') = Uanis(C20') = Uanis(C21')
Uanis(C35') = Uanis(C36') = Uanis(C37') = Uanis(C38') = Uanis(C39') =
Uanis(C40') = Uanis(C41') = Uanis(C42')
Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C40) =
Uanis(C41) = Uanis(C42)
5. Others
Sof(C35')=Sof(H35C)=Sof(H35D)=Sof(C36')=Sof(H36')=Sof(C37')=Sof(H37C)=
Sof(H37D)=Sof(C38')=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39')=Sof(H39C)=
Sof(H39D)=Sof(C40')=Sof(H40C)=Sof(H40D)=Sof(C41')=Sof(H41C)=Sof(H41D)=
Sof(C42')=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(1)
Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=
Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=
Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=
Sof(H42C)=FVAR(1)
Sof(C14')=Sof(H14C)=Sof(H14D)=Sof(C15')=Sof(H15')=Sof(C16')=Sof(H16C)=
Sof(H16D)=Sof(C17')=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18')=Sof(H18C)=
Sof(H18D)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20C)=Sof(H20D)=
Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(2)
Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=
Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=
Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=
Sof(H21C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
C15(H15), C15'(H15'), C36(H36), C36'(H36')
6.b Secondary CH2 refined with riding coordinates:
C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,
H20B), C14'(H14C,H14D), C16'(H16C,H16D), C18'(H18C,H18D), C19'(H19C,H19D),
C20'(H20C,H20D), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,
H40B), C41(H41A,H41B), C35'(H35C,H35D), C37'(H37C,H37D), C39'(H39C,H39D),
C40'(H40C,H40D), C41'(H41C,H41D)
6.c Me refined with riding coordinates:
C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C17'(H17D,H17E,H17F), C21'(H21D,
H21E,H21F), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C38'(H38D,H38E,H38F),
C42'(H42D,H42E,H42F)
6.d Aromatic/amide H refined with riding coordinates:
C6(H6), C13(H13), C25(H25), C32(H32)
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.