Identification code | 06Cl |
Empirical formula | C42H39Cl5.6N2O6 |
Formula weight | 866.09 |
Temperature/K | 293(2) |
Crystal system | triclinic |
Space group | P-1 |
a/Å | 7.464 |
b/Å | 12.493 |
c/Å | 21.027 |
α/° | 83.96 |
β/° | 83.58 |
γ/° | 83.25 |
Volume/Å3 | 1926.5 |
Z | 2 |
ρcalcg/cm3 | 1.493 |
μ/mm‑1 | 0.435 |
F(000) | 896.0 |
Crystal size/mm3 | 0.5 × 0.06 × 0.02 |
Radiation | Synchrotron Monochromator X-ray (λ = 0.68882) |
2Θ range for data collection/° | 5.184 to 46.636 |
Index ranges | -8 ≤ h ≤ 8, -14 ≤ k ≤ 14, -24 ≤ l ≤ 24 |
Reflections collected | 15946 |
Independent reflections | 5405 [Rint = 0.0597, Rsigma = 0.0448] |
Data/restraints/parameters | 5405/46/535 |
Goodness-of-fit on F2 | 1.104 |
Final R indexes [I>=2σ (I)] | R1 = 0.0934, wR2 = 0.2194 |
Final R indexes [all data] | R1 = 0.0947, wR2 = 0.2203 |
Largest diff. peak/hole / e Å-3 | 0.66/-0.43 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Cl0A | 1489(2) | 5275.7(11) | 739.6(6) | 41.1(6) |
Cl3A | -947(2) | 1498.8(11) | 1750.0(7) | 42.1(6) |
Cl1 | 6407(2) | 5486.7(12) | 867.3(6) | 42.8(6) |
Cl3 | 4175(2) | 1545.3(11) | 1603.4(7) | 41.5(6) |
Cl4A | 544(3) | 3006.0(12) | 565.9(7) | 49.3(7) |
Cl6A | 5581(3) | 3225.1(13) | 541.5(7) | 52.5(7) |
O9AA | 2890(6) | 2825(3) | 4052.4(17) | 40.0(10) |
O1AA | 5228(6) | 6535(3) | 3988.0(16) | 41.4(10) |
O1BA | -1177(5) | 3177(3) | 4683.4(16) | 38.1(9) |
N2 | 730(6) | 5810(3) | 2233(2) | 34.9(11) |
O2AA | 486(7) | 6557(3) | 3187.6(18) | 56.4(13) |
O7AA | 4982(7) | 6520(3) | 2946.3(18) | 57.3(13) |
N4 | 3670(6) | 2474(3) | 3004.9(19) | 32.5(10) |
C5AA | 4365(7) | 4128(4) | 3276(2) | 30.4(11) |
O2BA | -1917(6) | 2679(3) | 3769.2(18) | 50.4(12) |
C8AA | 3596(7) | 3095(4) | 3517(2) | 31.6(12) |
C0BA | -1279(8) | 3324(4) | 4038(2) | 37.4(13) |
C0AA | 4631(7) | 4880(4) | 3685(2) | 32.6(12) |
C1AA | -258(8) | 4707(4) | 3129(2) | 33.8(12) |
C2AA | -239(7) | 4142(4) | 2556(2) | 32.1(11) |
C3AA | 4721(8) | 4787(4) | 4374(2) | 33.7(12) |
C9 | -573(8) | 4083(4) | 4877(2) | 35.4(13) |
C10 | -250(8) | 4867(4) | 4355(2) | 33.2(12) |
C11 | 407(7) | 4833(4) | 2020(2) | 32.1(12) |
C12 | 4303(7) | 3069(4) | 2435(2) | 30.5(11) |
C13 | 4599(8) | 2784(4) | 1814(3) | 35.6(12) |
C14 | 5605(8) | 4554(4) | 1468(2) | 36.4(13) |
C15 | -668(7) | 3117(4) | 2460(2) | 33.5(12) |
C16 | 349(8) | 5801(4) | 2884(2) | 38.5(13) |
C17 | -585(8) | 4388(4) | 3780(2) | 34.4(12) |
C18 | 5114(8) | 5794(4) | 4529(2) | 35.0(13) |
C19 | 1324(9) | 6805(4) | 1860(3) | 42.3(14) |
C20 | 4706(7) | 4096(4) | 2580(2) | 29.1(11) |
C21 | 4586(8) | 3948(4) | 4882(2) | 35.3(13) |
C22 | 2866(8) | 1445(4) | 3094(3) | 39.6(13) |
C23 | 5352(7) | 4832(4) | 2091(2) | 33.4(12) |
C24 | -429(8) | 2790(4) | 1845(2) | 35.4(12) |
C25 | 630(8) | 4491(4) | 1414(2) | 37.0(13) |
C26 | 4977(9) | 6018(4) | 3468(3) | 42.6(14) |
C27 | 5252(8) | 3545(4) | 1326(2) | 38.5(13) |
C28 | 222(8) | 3454(4) | 1327(2) | 38.5(13) |
C29 | -350(8) | 4164(4) | 5503(2) | 37.2(13) |
C30 | -222(14) | 7505(7) | 1511(6) | 45(3) |
C31 | 4131(14) | 472(6) | 3262(6) | 103(4) |
C32 | -1835(14) | 7815(7) | 1984(5) | 66(3) |
C33 | 575(14) | 8567(7) | 1210(6) | 115(4) |
C1 | 1904(17) | 8390(8) | 650(4) | 107(4) |
C2 | 5386(17) | 532(8) | 3733(6) | 74(3) |
C3 | 3008(16) | -530(7) | 3432(7) | 144(5) |
C4 | 2390(20) | 9209(9) | 101(6) | 68(3) |
C5 | 2056(16) | -770(8) | 2902(6) | 128(4) |
C6 | -3466(13) | 8335(8) | 1648(6) | 104(4) |
C7 | 6878(14) | -474(7) | 3777(7) | 137(5) |
C8 | 2680(20) | 10234(11) | 381(7) | 87(4) |
C6AA | 8829(18) | -1203(8) | 4625(7) | 137(5) |
C4AA | 7746(19) | -196(9) | 4366(7) | 144(5) |
C2A | 6090(30) | 242(18) | 3188(10) | 74(3) |
C4A | 2190(30) | 9652(15) | 501(10) | 68(3) |
C8A | 3070(40) | 9673(18) | -198(12) | 87(4) |
C32A | -1730(50) | 7370(30) | 1518(18) | 66(3) |
C30A | -30(40) | 7680(20) | 1809(18) | 45(3) |
C13A | 4599(8) | 2784(4) | 1814(3) | 35.6(12) |
C27A | 5252(8) | 3545(4) | 1326(2) | 38.5(13) |
C14A | 5605(8) | 4554(4) | 1468(2) | 36.4(13) |
C24A | -429(8) | 2790(4) | 1845(2) | 35.4(12) |
C28A | 222(8) | 3454(4) | 1327(2) | 38.5(13) |
C25A | 630(8) | 4491(4) | 1414(2) | 37.0(13) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Cl0A | 62.4(12) | 35.8(9) | 22.8(8) | 7.8(5) | -3.0(6) | -6.7(6) |
Cl3A | 62.0(12) | 27.8(8) | 39.5(9) | -4.5(6) | -11.4(7) | -10.1(6) |
Cl1 | 58.6(12) | 43.4(9) | 22.6(8) | 12.3(6) | 1.4(6) | -8.4(7) |
Cl3 | 61.0(12) | 33.4(9) | 32.5(9) | -7.6(6) | -8.2(7) | -8.4(6) |
Cl4A | 87.6(15) | 37.5(9) | 24.6(8) | -1.7(6) | -12.9(7) | -8.3(8) |
Cl6A | 85.1(15) | 51.4(10) | 21.0(8) | -4.2(6) | -1.0(7) | -10.5(8) |
O9AA | 56(3) | 32.7(19) | 32(2) | 1.1(15) | 2.8(17) | -17.9(17) |
O1AA | 71(3) | 26.7(18) | 27.7(19) | 6.5(14) | -4.4(17) | -20.0(17) |
O1BA | 54(3) | 27.8(18) | 32.1(19) | -0.4(14) | 6.3(17) | -17.4(16) |
N2 | 45(3) | 28(2) | 32(2) | 7.1(17) | -1.5(19) | -11.8(19) |
O2AA | 104(4) | 34(2) | 33(2) | 0.0(17) | 3(2) | -26(2) |
O7AA | 109(4) | 36(2) | 29(2) | 7.6(17) | -8(2) | -27(2) |
N4 | 43(3) | 26(2) | 28(2) | 4.3(16) | -3.3(19) | -10.9(18) |
C5AA | 34(3) | 26(2) | 30(3) | 5.6(19) | -3(2) | -8(2) |
O2BA | 76(3) | 39(2) | 39(2) | -3.2(17) | 9(2) | -31(2) |
C8AA | 41(3) | 24(2) | 30(3) | 7(2) | -6(2) | -8(2) |
C0BA | 51(4) | 27(3) | 33(3) | -1(2) | 10(2) | -11(2) |
C0AA | 43(3) | 26(2) | 27(3) | 4.5(19) | 1(2) | -10(2) |
C1AA | 43(3) | 25(2) | 32(3) | 4(2) | 2(2) | -11(2) |
C2AA | 32(3) | 30(3) | 33(3) | 2(2) | -5(2) | -3(2) |
C3AA | 45(3) | 28(3) | 27(3) | 5(2) | 2(2) | -12(2) |
C9 | 48(4) | 22(2) | 34(3) | -3(2) | 11(2) | -10(2) |
C10 | 42(3) | 26(2) | 28(3) | 1(2) | 7(2) | -5(2) |
C11 | 35(3) | 28(3) | 31(3) | 3(2) | -3(2) | -2(2) |
C12 | 32(3) | 33(3) | 27(3) | 3(2) | -10(2) | -3(2) |
C13 | 42(3) | 31(3) | 35(3) | 1(2) | -11(2) | -5(2) |
C14 | 42(3) | 36(3) | 28(3) | 6(2) | -1(2) | -2(2) |
C15 | 37(3) | 27(2) | 36(3) | 4(2) | -6(2) | -4(2) |
C16 | 56(4) | 27(3) | 33(3) | 1(2) | 2(2) | -14(2) |
C17 | 45(3) | 24(2) | 32(3) | -1(2) | 8(2) | -10(2) |
C18 | 54(4) | 22(2) | 27(3) | 7(2) | 4(2) | -13(2) |
C19 | 57(4) | 37(3) | 32(3) | 10(2) | -1(3) | -19(3) |
C20 | 34(3) | 27(2) | 27(2) | 4.1(19) | -7(2) | -6(2) |
C21 | 57(4) | 21(2) | 28(3) | 4.8(19) | 3(2) | -15(2) |
C22 | 57(4) | 26(3) | 39(3) | 0(2) | -8(3) | -19(2) |
C23 | 38(3) | 32(3) | 29(3) | 7(2) | -6(2) | -5(2) |
C24 | 45(3) | 25(2) | 38(3) | 0(2) | -11(2) | -3(2) |
C25 | 42(3) | 34(3) | 33(3) | 8(2) | -5(2) | -6(2) |
C26 | 63(4) | 36(3) | 28(3) | 5(2) | 2(3) | -16(3) |
C27 | 49(4) | 45(3) | 20(2) | 1(2) | -5(2) | 2(2) |
C28 | 53(4) | 37(3) | 25(3) | -3(2) | -13(2) | 2(2) |
C29 | 50(4) | 27(3) | 33(3) | 1(2) | 8(2) | -12(2) |
C30 | 60(5) | 33(4) | 39(7) | 10(4) | -3(5) | -3(3) |
C31 | 112(8) | 32(4) | 178(10) | 31(5) | -89(7) | -25(4) |
C32 | 70(6) | 48(5) | 71(6) | 9(4) | 5(5) | 7(4) |
C33 | 85(7) | 59(5) | 181(11) | 62(6) | 2(7) | 4(4) |
C1 | 154(10) | 105(7) | 71(6) | 42(5) | -28(6) | -80(7) |
C2 | 93(8) | 41(5) | 87(7) | 7(5) | 4(5) | -25(5) |
C3 | 112(9) | 54(5) | 278(15) | 57(7) | -124(10) | -30(5) |
C4 | 95(9) | 37(6) | 71(7) | -5(4) | 13(6) | -20(5) |
C5 | 111(9) | 82(7) | 205(12) | -63(8) | 9(8) | -52(6) |
C6 | 73(6) | 84(6) | 136(9) | 26(6) | 7(6) | 21(5) |
C7 | 83(7) | 54(5) | 270(13) | 77(7) | -69(8) | -23(4) |
C8 | 116(11) | 59(7) | 86(9) | -9(6) | 16(8) | -26(7) |
C6AA | 156(11) | 75(6) | 162(11) | 63(7) | -15(8) | -3(6) |
C4AA | 136(11) | 93(8) | 184(12) | 51(8) | -31(8) | 24(7) |
C2A | 93(8) | 41(5) | 87(7) | 7(5) | 4(5) | -25(5) |
C4A | 95(9) | 37(6) | 71(7) | -5(4) | 13(6) | -20(5) |
C8A | 116(11) | 59(7) | 86(9) | -9(6) | 16(8) | -26(7) |
C32A | 70(6) | 48(5) | 71(6) | 9(4) | 5(5) | 7(4) |
C30A | 60(5) | 33(4) | 39(7) | 10(4) | -3(5) | -3(3) |
C13A | 42(3) | 31(3) | 35(3) | 1(2) | -11(2) | -5(2) |
C27A | 49(4) | 45(3) | 20(2) | 1(2) | -5(2) | 2(2) |
C14A | 42(3) | 36(3) | 28(3) | 6(2) | -1(2) | -2(2) |
C24A | 45(3) | 25(2) | 38(3) | 0(2) | -11(2) | -3(2) |
C28A | 53(4) | 37(3) | 25(3) | -3(2) | -13(2) | 2(2) |
C25A | 42(3) | 34(3) | 33(3) | 8(2) | -5(2) | -6(2) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Cl0A | C25 | 1.743(5) | C10 | C291 | 1.410(7) | |
Cl1 | C14 | 1.731(5) | C11 | C25 | 1.372(7) | |
Cl3 | C13 | 1.727(5) | C12 | C13 | 1.378(7) | |
Cl4A | C28 | 1.733(5) | C12 | C20 | 1.423(7) | |
Cl6A | C27 | 1.722(5) | C13 | C27 | 1.409(7) | |
O9AA | C8AA | 1.221(6) | C14 | C23 | 1.376(7) | |
O1AA | C18 | 1.390(6) | C14 | C27 | 1.387(8) | |
O1AA | C26 | 1.368(7) | C15 | C24 | 1.382(7) | |
O1BA | C0BA | 1.360(6) | C18 | C212 | 1.361(7) | |
O1BA | C9 | 1.382(6) | C19 | C30 | 1.567(12) | |
N2 | C11 | 1.400(7) | C19 | C30A | 1.41(3) | |
N2 | C16 | 1.366(7) | C20 | C23 | 1.390(7) | |
N2 | C19 | 1.484(6) | C21 | C182 | 1.361(7) | |
O2AA | C16 | 1.215(6) | C22 | C31 | 1.486(10) | |
O7AA | C26 | 1.204(6) | C25 | C28 | 1.399(8) | |
N4 | C8AA | 1.383(7) | C29 | C101 | 1.410(7) | |
N4 | C12 | 1.406(6) | C30 | C32 | 1.514(14) | |
N4 | C22 | 1.467(6) | C30 | C33 | 1.562(11) | |
C5AA | C8AA | 1.490(6) | C31 | C2 | 1.450(15) | |
C5AA | C0AA | 1.383(7) | C31 | C3 | 1.575(11) | |
C5AA | C20 | 1.461(7) | C31 | C2A | 1.450(17) | |
O2BA | C0BA | 1.201(7) | C32 | C6 | 1.520(13) | |
C0BA | C17 | 1.508(7) | C33 | C1 | 1.471(15) | |
C0AA | C3AA | 1.450(7) | C33 | C30A | 1.64(3) | |
C0AA | C26 | 1.490(7) | C1 | C4 | 1.502(14) | |
C1AA | C2AA | 1.457(7) | C1 | C4A | 1.61(2) | |
C1AA | C16 | 1.510(7) | C2 | C7 | 1.580(15) | |
C1AA | C17 | 1.389(7) | C3 | C5 | 1.461(13) | |
C2AA | C11 | 1.421(7) | C4 | C8 | 1.512(14) | |
C2AA | C15 | 1.395(7) | C6 | C32A | 1.68(3) | |
C3AA | C18 | 1.404(7) | C7 | C4AA | 1.549(18) | |
C3AA | C21 | 1.419(7) | C7 | C2A | 1.576(13) | |
C9 | C10 | 1.411(7) | C6AA | C4AA | 1.498(10) | |
C9 | C29 | 1.360(8) | C4A | C8A | 1.54(3) | |
C10 | C17 | 1.462(7) | C32A | C30A | 1.57(6) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C26 | O1AA | C18 | 108.0(4) | C1AA | C17 | C0BA | 123.4(5) | |
C0BA | O1BA | C9 | 108.7(4) | C1AA | C17 | C10 | 132.3(4) | |
C11 | N2 | C19 | 129.9(4) | C10 | C17 | C0BA | 104.1(4) | |
C16 | N2 | C11 | 111.0(4) | O1AA | C18 | C3AA | 111.4(4) | |
C16 | N2 | C19 | 119.0(4) | C212 | C18 | O1AA | 121.9(4) | |
C8AA | N4 | C12 | 109.5(4) | C212 | C18 | C3AA | 126.8(4) | |
C8AA | N4 | C22 | 119.8(4) | N2 | C19 | C30 | 113.4(5) | |
C12 | N4 | C22 | 129.8(4) | C30A | C19 | N2 | 115.2(13) | |
C0AA | C5AA | C8AA | 122.1(4) | C12 | C20 | C5AA | 107.4(4) | |
C0AA | C5AA | C20 | 132.8(4) | C23 | C20 | C5AA | 132.5(5) | |
C20 | C5AA | C8AA | 105.1(4) | C23 | C20 | C12 | 120.0(4) | |
O9AA | C8AA | N4 | 122.9(4) | C182 | C21 | C3AA | 115.9(4) | |
O9AA | C8AA | C5AA | 128.7(5) | N4 | C22 | C31 | 115.3(5) | |
N4 | C8AA | C5AA | 108.2(4) | C14 | C23 | C20 | 119.4(5) | |
O1BA | C0BA | C17 | 108.9(4) | C11 | C25 | Cl0A | 122.8(4) | |
O2BA | C0BA | O1BA | 120.6(4) | C11 | C25 | C28 | 119.6(5) | |
O2BA | C0BA | C17 | 130.4(5) | C28 | C25 | Cl0A | 117.5(4) | |
C5AA | C0AA | C3AA | 131.3(4) | O1AA | C26 | C0AA | 109.2(4) | |
C5AA | C0AA | C26 | 124.1(4) | O7AA | C26 | O1AA | 119.3(5) | |
C3AA | C0AA | C26 | 104.5(4) | O7AA | C26 | C0AA | 131.4(5) | |
C2AA | C1AA | C16 | 105.0(4) | C13 | C27 | Cl6A | 119.5(4) | |
C17 | C1AA | C2AA | 132.5(4) | C14 | C27 | Cl6A | 119.6(4) | |
C17 | C1AA | C16 | 122.3(5) | C14 | C27 | C13 | 120.8(5) | |
C11 | C2AA | C1AA | 107.5(4) | C25 | C28 | Cl4A | 119.9(4) | |
C15 | C2AA | C1AA | 133.0(5) | C9 | C29 | C101 | 116.7(5) | |
C15 | C2AA | C11 | 119.4(5) | C32 | C30 | C19 | 111.1(8) | |
C18 | C3AA | C0AA | 106.8(4) | C32 | C30 | C33 | 107.9(8) | |
C18 | C3AA | C21 | 117.3(5) | C33 | C30 | C19 | 106.4(8) | |
C21 | C3AA | C0AA | 135.8(5) | C22 | C31 | C3 | 108.7(8) | |
O1BA | C9 | C10 | 111.8(4) | C2 | C31 | C22 | 118.7(8) | |
C29 | C9 | O1BA | 121.7(4) | C2 | C31 | C3 | 111.9(8) | |
C29 | C9 | C10 | 126.6(5) | C2A | C31 | C22 | 133.5(10) | |
C9 | C10 | C17 | 106.2(4) | C2A | C31 | C3 | 116.6(11) | |
C291 | C10 | C9 | 116.8(5) | C30 | C32 | C6 | 112.1(9) | |
C291 | C10 | C17 | 137.0(4) | C1 | C33 | C30 | 112.6(9) | |
N2 | C11 | C2AA | 109.1(4) | C1 | C33 | C30A | 128.2(14) | |
C25 | C11 | N2 | 130.6(4) | C33 | C1 | C4 | 126.9(10) | |
C25 | C11 | C2AA | 120.3(5) | C33 | C1 | C4A | 93.8(11) | |
N4 | C12 | C20 | 109.4(4) | C31 | C2 | C7 | 113.5(9) | |
C13 | C12 | N4 | 130.1(5) | C5 | C3 | C31 | 113.5(9) | |
C13 | C12 | C20 | 120.4(4) | C1 | C4 | C8 | 107.8(11) | |
C12 | C13 | Cl3 | 123.0(4) | C4AA | C7 | C2 | 98.2(10) | |
C12 | C13 | C27 | 118.5(5) | C4AA | C7 | C2A | 132.9(12) | |
C27 | C13 | Cl3 | 118.5(4) | C6AA | C4AA | C7 | 107.7(11) | |
C23 | C14 | Cl1 | 118.5(4) | C31 | C2A | C7 | 113.8(13) | |
C23 | C14 | C27 | 120.8(5) | C8A | C4A | C1 | 100.7(15) | |
C27 | C14 | Cl1 | 120.7(4) | C30A | C32A | C6 | 109(2) | |
C24 | C15 | C2AA | 119.1(5) | C19 | C30A | C33 | 110(2) | |
N2 | C16 | C1AA | 107.3(4) | C19 | C30A | C32A | 112(3) | |
O2AA | C16 | N2 | 124.2(4) | C32A | C30A | C33 | 97(2) | |
O2AA | C16 | C1AA | 128.5(5) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H15 | -1108 | 2659 | 2805 | 40 |
H15A | -1108 | 2659 | 2805 | 40 |
H19A | 2316 | 6601 | 1542 | 51 |
H19B | 1779 | 7242 | 2149 | 51 |
H19C | 2312 | 7029 | 2060 | 51 |
H19D | 1796 | 6629 | 1431 | 51 |
H21 | 4309 | 3264 | 4816 | 42 |
H22A | 2363 | 1347 | 2701 | 48 |
H22B | 1870 | 1495 | 3432 | 48 |
H23 | 5610 | 5506 | 2183 | 40 |
H23A | 5610 | 5506 | 2183 | 40 |
H24 | -714 | 2108 | 1780 | 42 |
H29 | -581 | 3608 | 5821 | 45 |
H30 | -592 | 7115 | 1175 | 54 |
H31 | 4890 | 329 | 2862 | 124 |
H31A | 4093 | 622 | 3712 | 124 |
H32A | -1500 | 8317 | 2261 | 79 |
H32B | -2163 | 7173 | 2252 | 79 |
H33A | -408 | 9096 | 1081 | 138 |
H33B | 1153 | 8863 | 1534 | 138 |
H33C | -544 | 8864 | 1033 | 138 |
H33D | 976 | 9150 | 1410 | 138 |
H1AA | 1528 | 7793 | 455 | 129 |
H1AB | 3037 | 8118 | 824 | 129 |
H1BC | 1399 | 8103 | 306 | 129 |
H1BD | 2998 | 7943 | 760 | 129 |
H2A | 4708 | 585 | 4152 | 89 |
H2B | 5984 | 1185 | 3624 | 89 |
H3A | 3824 | -1161 | 3558 | 172 |
H3B | 2129 | -391 | 3798 | 172 |
H4A | 1418 | 9354 | -177 | 82 |
H4B | 3485 | 8937 | -151 | 82 |
H5A | 2878 | -785 | 2517 | 191 |
H5B | 1063 | -221 | 2838 | 191 |
H5C | 1602 | -1462 | 3003 | 191 |
H6AA | -3167 | 8363 | 1191 | 156 |
H6AB | -3793 | 9056 | 1771 | 156 |
H6AC | -4468 | 7915 | 1770 | 156 |
H6BD | -3811 | 8679 | 1243 | 156 |
H6BE | -3099 | 8864 | 1893 | 156 |
H6BF | -4478 | 8013 | 1882 | 156 |
H7AB | 6348 | -1154 | 3858 | 164 |
H7AA | 7734 | -489 | 3394 | 164 |
H7BD | 5889 | -882 | 3963 | 164 |
H7BC | 7778 | -996 | 3579 | 164 |
H8A | 2870 | 10795 | 39 | 131 |
H8B | 3729 | 10101 | 616 | 131 |
H8C | 1637 | 10455 | 664 | 131 |
H6AD | 9872 | -1371 | 4327 | 206 |
H6AE | 8094 | -1793 | 4683 | 206 |
H6AF | 9217 | -1089 | 5030 | 206 |
H4AC | 8526 | 374 | 4240 | 173 |
H4AD | 6810 | 51 | 4693 | 173 |
H2AA | 6623 | 922 | 3129 | 89 |
H2AB | 6444 | -127 | 2803 | 89 |
H4AA | 1042 | 10108 | 533 | 82 |
H4AB | 2984 | 9874 | 786 | 82 |
H8AA | 4271 | 9294 | -205 | 131 |
H8AB | 3147 | 10410 | -373 | 131 |
H8AC | 2355 | 9328 | -450 | 131 |
H32C | -2055 | 6676 | 1721 | 79 |
H32D | -1452 | 7311 | 1061 | 79 |
H30A | -356 | 8014 | 2214 | 54 |
H13A | 4374 | 2105 | 1718 | 43 |
H27A | 5448 | 3368 | 903 | 46 |
H14A | 6018 | 5050 | 1139 | 44 |
H28A | 390 | 3213 | 919 | 46 |
H25A | 1049 | 4945 | 1064 | 44 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
Cl0A | 0.929(8) | Cl3A | 0.930(8) | Cl1 | 0.919(8) | ||
Cl3 | 0.904(8) | Cl4A | 0.912(8) | Cl6A | 0.919(8) | ||
C13 | 0.707(12) | C14 | 0.707(12) | H15 | 0.707(12) | ||
H15A | 0.293(12) | H19A | 0.74(2) | H19B | 0.74(2) | ||
H19C | 0.26(2) | H19D | 0.26(2) | H23 | 0.707(12) | ||
H23A | 0.293(12) | C24 | 0.707(12) | H24 | 0.707(12) | ||
C25 | 0.293(12) | C27 | 0.707(12) | C28 | 0.293(12) | ||
C30 | 0.74(2) | H30 | 0.74(2) | H31 | 0.707(12) | ||
H31A | 0.293(12) | C32 | 0.774(13) | H32A | 0.774(13) | ||
H32B | 0.774(13) | H33A | 0.74(2) | H33B | 0.74(2) | ||
H33C | 0.26(2) | H33D | 0.26(2) | H1AA | 0.608(12) | ||
H1AB | 0.608(12) | H1BC | 0.392(12) | H1BD | 0.392(12) | ||
C2 | 0.707(12) | H2A | 0.707(12) | H2B | 0.707(12) | ||
C4 | 0.608(12) | H4A | 0.608(12) | H4B | 0.608(12) | ||
H6AA | 0.774(13) | H6AB | 0.774(13) | H6AC | 0.774(13) | ||
H6BD | 0.226(13) | H6BE | 0.226(13) | H6BF | 0.226(13) | ||
H7AB | 0.707(12) | H7AA | 0.707(12) | H7BD | 0.293(12) | ||
H7BC | 0.293(12) | C8 | 0.610(12) | H8A | 0.610(12) | ||
H8B | 0.610(12) | H8C | 0.610(12) | C2A | 0.293(12) | ||
H2AA | 0.293(12) | H2AB | 0.293(12) | C4A | 0.392(12) | ||
H4AA | 0.392(12) | H4AB | 0.392(12) | C8A | 0.390(12) | ||
H8AA | 0.390(12) | H8AB | 0.390(12) | H8AC | 0.390(12) | ||
C32A | 0.226(13) | H32C | 0.226(13) | H32D | 0.226(13) | ||
C30A | 0.26(2) | H30A | 0.26(2) | C13A | 0.293(12) | ||
H13A | 0.293(12) | C27A | 0.293(12) | H27A | 0.293(12) | ||
C14A | 0.293(12) | H14A | 0.293(12) | C24A | 0.293(12) | ||
C28A | 0.707(12) | H28A | 0.707(12) | C25A | 0.707(12) | ||
H25A | 0.707(12) |
Experimental
Single crystals of C42H39Cl5.6N2O6 [06Cl] 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 [06Cl]
Crystal Data for C42H39Cl5.6N2O6 (M =866.09 g/mol): triclinic, space group P-1 (no. 2), a = 7.464 Å, b = 12.493 Å, c = 21.027 Å, α = 83.96°, β = 83.58°, γ = 83.25°, V = 1926.5 Å3, Z = 2, T = 293(2) K, μ(Synchrotron Monochromator X-ray) = 0.435 mm-1, Dcalc = 1.493 g/cm3, 15946 reflections measured (5.184° ≤ 2Θ ≤ 46.636°), 5405 unique (Rint = 0.0597, Rsigma = 0.0448) which were used in all calculations. The final R1 was 0.0934 (I > 2σ(I)) and wR2 was 0.2203 (all data).
Refinement model description
Number of restraints - 46, 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
{C13, C13A}
{C27, C27A}
{C14, C14A}
{C24A, C24}
{C28, C28A}
{C25A, C25}
3. Restrained distances
C7-C2A
1.55 with sigma of 0.02
C6AA-C4AA
1.55 with sigma of 0.02
C7_$1-C2A_$1
1.55 with sigma of 0.02
C6AA_$1-C4AA_$1
1.55 with sigma of 0.02
C8-C4
1.55 with sigma of 0.02
C5-C3
1.55 with sigma of 0.02
C31-C2A
1.55 with sigma of 0.02
H3A-H7BD
2 with sigma of 0.02
4. Rigid bond restraints
C7, C2A, C4AA, C6AA
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C5, C3, C31
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2A ≈ C7 ≈ C4AA ≈ C6AA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C5 ≈ C3 ≈ C31: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C4) = Uanis(C4A)
Uanis(C8) = Uanis(C8A)
Uanis(C32) = Uanis(C32A)
Uanis(C30) = Uanis(C30A)
Uanis(C13) = Uanis(C13A)
Uanis(C27) = Uanis(C27A)
Uanis(C14) = Uanis(C14A)
Uanis(C2) = Uanis(C2A)
Uanis(C24) = Uanis(C24A)
Uanis(C24A) = Uanis(C24)
Uanis(C28) = Uanis(C28A)
Uanis(C25) = Uanis(C25A)
Uanis(C25A) = Uanis(C25)
6. Others
Sof(H15A)=Sof(H23A)=Sof(C25)=Sof(C28)=Sof(H31A)=Sof(H7BD)=Sof(H7BC)=Sof(C2A)=
Sof(H2AA)=Sof(H2AB)=Sof(C13A)=Sof(H13A)=Sof(C27A)=Sof(H27A)=Sof(C14A)=
Sof(H14A)=Sof(C24A)=1-FVAR(1)
Sof(C13)=Sof(C14)=Sof(H15)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C27)=Sof(H31)=
Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H7AB)=Sof(H7AA)=Sof(C28A)=Sof(H28A)=Sof(C25A)=
Sof(H25A)=FVAR(1)
Sof(H1BC)=Sof(H1BD)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(2)
Sof(H1AA)=Sof(H1AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(2)
Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(3)
Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(3)
Sof(H6BD)=Sof(H6BE)=Sof(H6BF)=Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(4)
Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=FVAR(4)
Sof(H19C)=Sof(H19D)=Sof(H33C)=Sof(H33D)=Sof(C30A)=Sof(H30A)=1-FVAR(5)
Sof(H19A)=Sof(H19B)=Sof(C30)=Sof(H30)=Sof(H33A)=Sof(H33B)=FVAR(5)
7.a Ternary CH refined with riding coordinates:
C30(H30), C31(H31), C31(H31A), C30A(H30A)
7.b Secondary CH2 refined with riding coordinates:
C19(H19A,H19B), C19(H19C,H19D), C22(H22A,H22B), C32(H32A,H32B), C33(H33A,
H33B), C33(H33C,H33D), C1(H1AA,H1AB), C1(H1BC,H1BD), C2(H2A,H2B), C3(H3A,H3B),
C4(H4A,H4B), C7(H7AB,H7AA), C7(H7BD,H7BC), C4AA(H4AC,H4AD), C2A(H2AA,H2AB),
C4A(H4AA,H4AB), C32A(H32C,H32D)
7.c Me refined with riding coordinates:
C6(H6AA,H6AB,H6AC), C6(H6BD,H6BE,H6BF)
7.d Aromatic/amide H refined with riding coordinates:
C15(H15), C15(H15A), C21(H21), C23(H23), C23(H23A), C24(H24), C29(H29),
C13A(H13A), C27A(H27A), C14A(H14A), C28A(H28A), C25A(H25A)
7.e Idealised Me refined as rotating group:
C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C6AA(H6AD,H6AE,H6AF), C8A(H8AA,H8AB,H8AC)
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.