Identification code | 3Cl-nondecomposition |
Empirical formula | C42H41Cl3N2O6 |
Formula weight | 776.12 |
Temperature/K | 293(2) |
Crystal system | triclinic |
Space group | P-1 |
a/Å | 7.722 |
b/Å | 12.874 |
c/Å | 21.477 |
α/° | 84.25 |
β/° | 84.18 |
γ/° | 83.73 |
Volume/Å3 | 2102.8 |
Z | 2 |
ρcalcg/cm3 | 1.226 |
μ/mm‑1 | 0.245 |
F(000) | 812.0 |
Crystal size/mm3 | 0.15 × 0.1 × 0.1 |
Radiation | Synchrotron Monochromator X-ray (λ = 0.68882) |
2Θ range for data collection/° | 1.854 to 46.64 |
Index ranges | -8 ≤ h ≤ 8, -14 ≤ k ≤ 14, -24 ≤ l ≤ 24 |
Reflections collected | 24179 |
Independent reflections | 6278 [Rint = 0.1829, Rsigma = 0.1087] |
Data/restraints/parameters | 6278/154/489 |
Goodness-of-fit on F2 | 1.840 |
Final R indexes [I>=2σ (I)] | R1 = 0.1561, wR2 = 0.4454 |
Final R indexes [all data] | R1 = 0.1757, wR2 = 0.4645 |
Largest diff. peak/hole / e Å-3 | 0.53/-0.44 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Cl0A | 1383(4) | 5187(2) | 5720.2(11) | 66.0(9) |
Cl3A | -1001(4) | 1427(2) | 6766.2(14) | 69.2(9) |
Cl1A | 414(5) | 2920(3) | 5560.4(13) | 81.5(11) |
Cl6A | 4143(5) | 1473(3) | 6598.5(16) | 79.7(11) |
Cl2 | 6263(4) | 5429(3) | 5840.7(14) | 80.3(11) |
Cl7A | 5460(5) | 3156(3) | 5525.2(15) | 91.3(12) |
O9AA | 2950(7) | 2778(4) | 9046(3) | 86.6(14) |
O2AA | -1160(6) | 3171(3) | 9695(2) | 76.0(12) |
O4AA | -1855(7) | 2633(4) | 8777(3) | 95.0(15) |
O1BA | 564(9) | 6486(4) | 8171(2) | 102.2(18) |
O3 | 5344(7) | 6490(4) | 8971(2) | 92.5(15) |
O4 | 5176(9) | 6448(4) | 7926(3) | 111.8(19) |
N5 | 708(7) | 5743(4) | 7209(3) | 77.6(15) |
C0AA | 368(8) | 5818(5) | 9501(3) | 67.9(15) |
C5AA | -240(8) | 4834(5) | 9349(3) | 68.3(15) |
C8AA | -546(8) | 4069(4) | 9878(3) | 67.0(15) |
C0BA | 5178(9) | 5764(5) | 9525(3) | 74.2(17) |
C2BA | -698(8) | 3050(5) | 7457(4) | 75.6(17) |
C6 | 4393(8) | 4090(5) | 8260(3) | 73.4(17) |
C7 | -527(8) | 4349(5) | 8781(3) | 68.4(15) |
C8 | -270(8) | 4081(5) | 7552(3) | 70.0(15) |
C9 | 4687(8) | 4827(5) | 8685(3) | 74.7(17) |
N10 | 3693(7) | 2427(4) | 8009(3) | 79.5(15) |
C11 | 4700(8) | 4763(5) | 9370(3) | 70.8(16) |
C12 | 336(8) | 4773(5) | 7015(3) | 73.5(16) |
C13 | -227(8) | 4653(5) | 8121(3) | 71.7(16) |
C14 | 4305(8) | 3032(5) | 7427(4) | 78.1(18) |
C15 | 148(11) | 3386(7) | 6311(4) | 95(2) |
C16 | 559(9) | 4434(6) | 6391(3) | 78.7(17) |
C17 | 5310(9) | 4780(6) | 7066(4) | 87(2) |
C18 | 4680(8) | 4063(5) | 7568(4) | 77.1(17) |
C19 | -498(10) | 2723(6) | 6846(4) | 86.7(19) |
C20 | 1317(11) | 6705(6) | 6828(4) | 93(2) |
C21 | 4566(8) | 3947(5) | 9878(3) | 78.8(19) |
C22 | 4535(10) | 2726(7) | 6804(4) | 89(2) |
C23 | 2964(9) | 1393(6) | 8083(4) | 85.5(19) |
C24 | -1257(9) | 3291(5) | 9045(3) | 76.6(17) |
C25 | 392(9) | 5722(6) | 7870(3) | 80.1(18) |
C26 | 5555(10) | 4488(6) | 6439(4) | 86.6(19) |
C27 | 3626(8) | 3049(5) | 8512(4) | 76.7(17) |
C28 | 5129(10) | 5967(5) | 8449(4) | 82.7(19) |
C29 | 5153(12) | 3491(7) | 6294(4) | 102(2) |
C30 | -205(14) | 7443(9) | 6516(6) | 147(4) |
C31 | 4193(14) | 421(7) | 8236(7) | 163(5) |
C32 | -1776(19) | 7776(12) | 6924(7) | 130(4) |
C33 | 5445(18) | 424(11) | 8717(9) | 156(6) |
C1 | 6969(18) | -485(9) | 8729(9) | 198(6) |
C2 | -3409(18) | 8232(13) | 6586(8) | 194(7) |
C3 | 540(30) | 8492(16) | 6237(15) | 397(18) |
C4 | 2990(20) | -497(12) | 8478(10) | 157(5) |
C2AA | 1900(30) | 8400(20) | 5670(14) | 418(17) |
C4AA | 8520(30) | -1209(17) | 9573(11) | 258(10) |
C1AA | 2310(20) | -898(12) | 7902(10) | 160(6) |
C3AA | 7740(30) | -353(17) | 9370(11) | 262(9) |
C6AA | 2690(40) | 9060(30) | 5080(16) | 454(19) |
C7AA | 2540(40) | 10120(30) | 5336(19) | 470(20) |
C4A | 3800(50) | -660(20) | 8020(20) | 157(5) |
C1AB | 2250(60) | -1040(30) | 8460(30) | 160(6) |
C32A | -1810(50) | 7220(30) | 6450(20) | 130(4) |
C33A | 6140(30) | 210(30) | 8180(18) | 156(6) |
C16A | 559(9) | 4434(6) | 6391(3) | 78.7(17) |
C15A | 148(11) | 3386(7) | 6311(4) | 95(2) |
C19A | -498(10) | 2723(6) | 6846(4) | 86.7(19) |
C26A | 5555(10) | 4488(6) | 6439(4) | 86.6(19) |
C29A | 5153(12) | 3491(7) | 6294(4) | 102(2) |
C22A | 4535(10) | 2726(7) | 6804(4) | 89(2) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Cl0A | 82.4(18) | 68.4(17) | 44.7(13) | 0.7(11) | -3.4(11) | -2.8(13) |
Cl3A | 88(2) | 50.0(15) | 75.1(18) | -19.6(12) | -22.7(14) | -6.3(12) |
Cl1A | 123(3) | 72.8(19) | 51.4(15) | -16.9(13) | -19.9(15) | 0.8(17) |
Cl6A | 102(2) | 64.8(19) | 76(2) | -23.0(15) | -15.0(16) | -4.9(15) |
Cl2 | 81(2) | 92(2) | 61.3(17) | 13.4(15) | 5.3(13) | -6.1(16) |
Cl7A | 110(3) | 105(3) | 58.1(18) | -13.1(16) | -1.8(16) | -4(2) |
O9AA | 95(3) | 68(3) | 99(3) | -9(2) | 3(3) | -28(2) |
O2AA | 86(3) | 63(2) | 80(3) | -8(2) | 3(2) | -22(2) |
O4AA | 114(4) | 74(3) | 103(4) | -15(3) | -1(3) | -40(3) |
O1BA | 158(5) | 70(3) | 84(3) | -5(2) | -5(3) | -46(3) |
O3 | 124(4) | 61(3) | 94(3) | 3(2) | 2(3) | -31(2) |
O4 | 165(6) | 81(3) | 93(4) | 1(3) | -4(3) | -46(4) |
N5 | 85(4) | 73(3) | 75(3) | -1(3) | -8(3) | -12(3) |
C0AA | 66(3) | 60(3) | 76(4) | 3(3) | 0(3) | -15(3) |
C5AA | 66(3) | 55(3) | 83(4) | -8(3) | 4(3) | -10(3) |
C8AA | 70(4) | 52(3) | 78(4) | -1(3) | 3(3) | -13(3) |
C0BA | 74(4) | 57(3) | 89(4) | 7(3) | -1(3) | -17(3) |
C2BA | 68(4) | 66(4) | 95(5) | -8(3) | -13(3) | -9(3) |
C6 | 64(4) | 60(4) | 95(5) | 4(3) | -13(3) | -7(3) |
C7 | 65(3) | 57(3) | 80(4) | -1(3) | 1(3) | -8(3) |
C8 | 59(3) | 66(4) | 84(4) | -5(3) | -8(3) | 3(3) |
C9 | 66(4) | 60(4) | 96(5) | -1(3) | 0(3) | -9(3) |
N10 | 82(3) | 63(3) | 93(4) | -7(3) | -13(3) | -3(2) |
C11 | 63(3) | 53(3) | 94(4) | -3(3) | 4(3) | -11(3) |
C12 | 68(4) | 68(4) | 82(4) | 0(3) | -8(3) | 0(3) |
C13 | 67(3) | 68(4) | 80(4) | -5(3) | -5(3) | -6(3) |
C14 | 63(4) | 73(4) | 100(5) | -14(4) | -18(3) | 0(3) |
C17 | 78(4) | 84(5) | 95(5) | 4(4) | -10(3) | 2(3) |
C18 | 62(4) | 67(4) | 99(5) | 5(3) | -7(3) | -4(3) |
C20 | 108(5) | 73(4) | 92(5) | 10(4) | -4(4) | -8(4) |
C21 | 75(4) | 56(3) | 106(5) | -3(3) | 0(3) | -19(3) |
C23 | 80(4) | 76(4) | 105(5) | -13(4) | -17(3) | -15(3) |
C24 | 77(4) | 65(4) | 86(4) | -5(3) | 7(3) | -14(3) |
C25 | 78(4) | 73(4) | 86(4) | 5(3) | -4(3) | -7(3) |
C27 | 61(4) | 61(4) | 107(5) | -7(3) | -1(3) | -9(3) |
C28 | 97(5) | 65(4) | 86(5) | 8(3) | -19(4) | -12(3) |
C30 | 117(6) | 124(8) | 176(10) | 51(7) | 17(6) | 9(5) |
C31 | 116(7) | 90(6) | 295(15) | 23(7) | -100(8) | -29(5) |
C32 | 132(7) | 121(9) | 120(9) | 28(7) | 0(6) | 15(6) |
C33 | 84(7) | 96(7) | 284(16) | 26(10) | -29(9) | -22(5) |
C1 | 126(8) | 92(7) | 359(17) | 71(9) | -45(10) | -3(6) |
C2 | 139(8) | 203(13) | 199(13) | 79(10) | 14(8) | 55(9) |
C3 | 162(13) | 256(19) | 710(40) | 320(30) | -98(18) | -37(13) |
C4 | 115(10) | 106(8) | 257(15) | 17(9) | -57(9) | -42(8) |
C2AA | 186(16) | 315(19) | 700(40) | 350(20) | -94(18) | -84(15) |
C4AA | 240(18) | 225(18) | 270(20) | 141(17) | 2(13) | -17(13) |
C1AA | 159(11) | 86(8) | 242(17) | -51(12) | 15(12) | -43(7) |
C3AA | 186(14) | 236(17) | 340(20) | 106(16) | -73(13) | 2(13) |
C6AA | 290(20) | 330(20) | 700(40) | 340(30) | -90(20) | -120(20) |
C7AA | 300(30) | 310(20) | 760(50) | 340(30) | -140(30) | -90(30) |
C4A | 115(10) | 106(8) | 257(15) | 17(9) | -57(9) | -42(8) |
C1AB | 159(11) | 86(8) | 242(17) | -51(12) | 15(12) | -43(7) |
C32A | 132(7) | 121(9) | 120(9) | 28(7) | 0(6) | 15(6) |
C33A | 84(7) | 96(7) | 284(16) | 26(10) | -29(9) | -22(5) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Cl0A | C16 | 1.758(7) | N10 | C23 | 1.489(9) | |
Cl3A | C19 | 1.781(8) | N10 | C27 | 1.402(9) | |
Cl1A | C15 | 1.760(9) | C11 | C21 | 1.441(9) | |
Cl2 | C26 | 1.763(8) | C12 | C16 | 1.438(10) | |
O9AA | C27 | 1.245(9) | C13 | C25 | 1.535(10) | |
O2AA | C8AA | 1.402(7) | C14 | C18 | 1.455(10) | |
O2AA | C24 | 1.397(8) | C14 | C22 | 1.421(11) | |
O4AA | C24 | 1.224(8) | C15 | C16 | 1.449(11) | |
O1BA | C25 | 1.256(9) | C15 | C19 | 1.443(12) | |
O3 | C0BA | 1.441(8) | C17 | C18 | 1.431(10) | |
O3 | C28 | 1.396(9) | C17 | C26 | 1.424(11) | |
O4 | C28 | 1.226(8) | C20 | C30 | 1.588(13) | |
N5 | C12 | 1.423(9) | C21 | C0BA2 | 1.409(10) | |
N5 | C20 | 1.506(9) | C22 | C29 | 1.477(12) | |
N5 | C25 | 1.414(9) | C23 | C31 | 1.516(12) | |
C0AA | C5AA | 1.475(9) | C30 | C32 | 1.473(17) | |
C0AA | C8AA1 | 1.377(9) | C30 | C3 | 1.57(2) | |
C5AA | C8AA | 1.446(9) | C30 | C32A | 1.33(4) | |
C5AA | C7 | 1.471(10) | C31 | C33 | 1.485(15) | |
C8AA | C0AA1 | 1.377(9) | C31 | C4 | 1.596(14) | |
C0BA | C11 | 1.457(9) | C31 | C4A | 1.574(19) | |
C0BA | C212 | 1.409(10) | C31 | C33A | 1.496(19) | |
C2BA | C8 | 1.441(9) | C32 | C2 | 1.550(18) | |
C2BA | C19 | 1.405(11) | C33 | C1 | 1.567(19) | |
C6 | C9 | 1.432(10) | C1 | C3AA | 1.585(17) | |
C6 | C18 | 1.484(10) | C1 | C33A | 1.555(19) | |
C6 | C27 | 1.550(9) | C2 | C32A | 1.72(4) | |
C7 | C13 | 1.434(9) | C3 | C2AA | 1.528(19) | |
C7 | C24 | 1.563(9) | C4 | C1AA | 1.545(17) | |
C8 | C12 | 1.456(9) | C2AA | C6AA | 1.561(18) | |
C8 | C13 | 1.494(10) | C4AA | C3AA | 1.26(2) | |
C9 | C11 | 1.466(10) | C6AA | C7AA | 1.51(2) | |
C9 | C28 | 1.566(9) | C4A | C1AB | 1.54(2) | |
N10 | C14 | 1.469(9) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C24 | O2AA | C8AA | 108.9(5) | C15 | C16 | Cl0A | 117.5(5) | |
C28 | O3 | C0BA | 108.5(5) | C26 | C17 | C18 | 120.2(8) | |
C12 | N5 | C20 | 130.3(6) | C14 | C18 | C6 | 107.2(6) | |
C25 | N5 | C12 | 109.2(5) | C17 | C18 | C6 | 133.7(7) | |
C25 | N5 | C20 | 120.5(6) | C17 | C18 | C14 | 119.0(7) | |
C8AA1 | C0AA | C5AA | 118.0(5) | C2BA | C19 | Cl3A | 116.9(6) | |
C8AA | C5AA | C0AA | 115.4(6) | C2BA | C19 | C15 | 121.8(7) | |
C8AA | C5AA | C7 | 107.1(5) | C15 | C19 | Cl3A | 121.2(6) | |
C7 | C5AA | C0AA | 137.4(6) | N5 | C20 | C30 | 113.8(7) | |
O2AA | C8AA | C5AA | 111.6(5) | C0BA2 | C21 | C11 | 115.5(6) | |
C0AA1 | C8AA | O2AA | 121.7(5) | C14 | C22 | C29 | 118.1(7) | |
C0AA1 | C8AA | C5AA | 126.7(6) | N10 | C23 | C31 | 117.9(6) | |
O3 | C0BA | C11 | 110.9(6) | O2AA | C24 | C7 | 108.2(5) | |
C212 | C0BA | O3 | 121.4(5) | O4AA | C24 | O2AA | 121.2(6) | |
C212 | C0BA | C11 | 127.7(6) | O4AA | C24 | C7 | 130.6(7) | |
C19 | C2BA | C8 | 119.4(7) | O1BA | C25 | N5 | 123.2(6) | |
C9 | C6 | C18 | 134.0(6) | O1BA | C25 | C13 | 128.5(6) | |
C9 | C6 | C27 | 120.3(6) | N5 | C25 | C13 | 108.2(6) | |
C18 | C6 | C27 | 105.6(6) | C17 | C26 | Cl2 | 117.7(6) | |
C5AA | C7 | C24 | 103.7(5) | O9AA | C27 | C6 | 129.5(6) | |
C13 | C7 | C5AA | 133.5(6) | O9AA | C27 | N10 | 122.4(6) | |
C13 | C7 | C24 | 122.8(6) | N10 | C27 | C6 | 108.0(6) | |
C2BA | C8 | C12 | 119.6(6) | O3 | C28 | C9 | 108.3(6) | |
C2BA | C8 | C13 | 133.8(6) | O4 | C28 | O3 | 119.5(6) | |
C12 | C8 | C13 | 106.6(6) | O4 | C28 | C9 | 131.9(7) | |
C6 | C9 | C11 | 133.0(6) | C32 | C30 | C20 | 118.0(10) | |
C6 | C9 | C28 | 121.9(6) | C32 | C30 | C3 | 104.6(14) | |
C11 | C9 | C28 | 105.0(6) | C3 | C30 | C20 | 108.2(11) | |
C14 | N10 | C23 | 128.5(6) | C32A | C30 | C20 | 127.6(18) | |
C27 | N10 | C14 | 109.0(5) | C32A | C30 | C3 | 124.0(19) | |
C27 | N10 | C23 | 121.9(6) | C23 | C31 | C4 | 106.5(9) | |
C0BA | C11 | C9 | 107.0(5) | C23 | C31 | C4A | 118.8(19) | |
C21 | C11 | C0BA | 116.7(6) | C33 | C31 | C23 | 120.0(10) | |
C21 | C11 | C9 | 135.8(6) | C33 | C31 | C4 | 106.2(11) | |
N5 | C12 | C8 | 110.8(6) | C33A | C31 | C23 | 132.6(15) | |
N5 | C12 | C16 | 128.1(6) | C33A | C31 | C4A | 97(2) | |
C16 | C12 | C8 | 121.0(6) | C30 | C32 | C2 | 116.2(13) | |
C7 | C13 | C8 | 132.6(6) | C31 | C33 | C1 | 116.5(14) | |
C7 | C13 | C25 | 122.1(6) | C33 | C1 | C3AA | 101.2(14) | |
C8 | C13 | C25 | 105.2(6) | C33A | C1 | C3AA | 139(2) | |
C18 | C14 | N10 | 109.7(6) | C2AA | C3 | C30 | 115.6(18) | |
C22 | C14 | N10 | 128.6(6) | C1AA | C4 | C31 | 108.5(13) | |
C22 | C14 | C18 | 121.7(7) | C3 | C2AA | C6AA | 142(2) | |
C16 | C15 | Cl1A | 120.4(6) | C4AA | C3AA | C1 | 110(2) | |
C19 | C15 | Cl1A | 119.7(7) | C7AA | C6AA | C2AA | 100(2) | |
C19 | C15 | C16 | 120.0(7) | C1AB | C4A | C31 | 108(3) | |
C12 | C16 | Cl0A | 124.3(5) | C30 | C32A | C2 | 114(3) | |
C12 | C16 | C15 | 118.2(6) | C31 | C33A | C1 | 116.6(18) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H0AA | 623 | 6346 | 9188 | 81 |
H2BA | -1102 | 2605 | 7796 | 91 |
H2BB | -1102 | 2605 | 7796 | 91 |
H17A | 5561 | 5440 | 7149 | 104 |
H17 | 5561 | 5440 | 7149 | 104 |
H20A | 2196 | 6485 | 6499 | 111 |
H20B | 1867 | 7106 | 7098 | 111 |
H21 | 4326 | 3274 | 9816 | 95 |
H22 | 4304 | 2062 | 6720 | 106 |
H23A | 2470 | 1307 | 7696 | 103 |
H23B | 2006 | 1419 | 8412 | 103 |
H29 | 5278 | 3323 | 5879 | 122 |
H30 | -566 | 7097 | 6172 | 176 |
H30A | -595 | 7738 | 6916 | 176 |
H31A | 3926 | 307 | 8693 | 195 |
H31 | 4865 | 233 | 7845 | 195 |
H32A | -1479 | 8301 | 7179 | 156 |
H32B | -2086 | 7176 | 7208 | 156 |
H33A | 4790 | 399 | 9128 | 187 |
H33B | 5957 | 1086 | 8653 | 187 |
H1AA | 7835 | -392 | 8373 | 237 |
H1AB | 6534 | -1166 | 8733 | 237 |
H1A | 7922 | -899 | 8510 | 237 |
H1B | 6094 | -969 | 8860 | 237 |
H2AA | -3144 | 8848 | 6318 | 291 |
H2AB | -4359 | 8414 | 6893 | 291 |
H2AC | -3738 | 7718 | 6338 | 291 |
H2A | -3415 | 8414 | 7009 | 291 |
H2B | -4530 | 8019 | 6527 | 291 |
H2C | -3175 | 8830 | 6297 | 291 |
H3A | -424 | 8991 | 6116 | 476 |
H3B | 1071 | 8776 | 6566 | 476 |
H4A | 3660 | -1064 | 8706 | 188 |
H4B | 2011 | -235 | 8758 | 188 |
H2AD | 1547 | 7814 | 5483 | 501 |
H2AE | 2944 | 8124 | 5870 | 501 |
H4AA | 9083 | -1569 | 9226 | 387 |
H4AB | 7687 | -1635 | 9808 | 387 |
H4AC | 9375 | -1076 | 9841 | 387 |
H1AC | 1608 | -340 | 7689 | 240 |
H1AD | 1624 | -1470 | 8039 | 240 |
H1AE | 3290 | -1135 | 7620 | 240 |
H3AA | 8542 | 182 | 9304 | 314 |
H3AB | 6792 | -133 | 9677 | 314 |
H6AA | 3893 | 8811 | 4961 | 545 |
H6AB | 2003 | 9071 | 4724 | 545 |
H7AA | 1338 | 10318 | 5482 | 711 |
H7AB | 2918 | 10637 | 5010 | 711 |
H7AC | 3253 | 10089 | 5679 | 711 |
H4AD | 3501 | -567 | 7592 | 188 |
H4AE | 4815 | -1165 | 8052 | 188 |
H1AF | 2591 | -1195 | 8881 | 240 |
H1AG | 1910 | -1667 | 8318 | 240 |
H1AH | 1280 | -508 | 8459 | 240 |
H32C | -2068 | 6615 | 6745 | 156 |
H32D | -1851 | 7019 | 6031 | 156 |
H33C | 6631 | 884 | 8139 | 187 |
H33D | 6504 | -115 | 7794 | 187 |
H16A | 957 | 4874 | 6049 | 94 |
H15A | 300 | 3142 | 5914 | 115 |
H19A | -791 | 2060 | 6786 | 104 |
H26A | 5987 | 4956 | 6117 | 104 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
Cl0A | 0.506(3) | Cl3A | 0.506(3) | Cl1A | 0.506(3) | ||
Cl6A | 0.494(3) | Cl2 | 0.494(3) | Cl7A | 0.494(3) | ||
H2BA | 0.506(3) | H2BB | 0.494(3) | C15 | 0.506(3) | ||
C16 | 0.506(3) | H17A | 0.494(3) | H17 | 0.506(3) | ||
C19 | 0.506(3) | C22 | 0.506(3) | H22 | 0.506(3) | ||
C26 | 0.494(3) | C29 | 0.506(3) | H29 | 0.506(3) | ||
H30 | 0.722(9) | H30A | 0.278(9) | H31A | 0.278(9) | ||
H31 | 0.722(9) | C32 | 0.722(9) | H32A | 0.722(9) | ||
H32B | 0.722(9) | C33 | 0.722(9) | H33A | 0.722(9) | ||
H33B | 0.722(9) | H1AA | 0.722(9) | H1AB | 0.722(9) | ||
H1A | 0.278(9) | H1B | 0.278(9) | H2AA | 0.722(9) | ||
H2AB | 0.722(9) | H2AC | 0.722(9) | H2A | 0.278(9) | ||
H2B | 0.278(9) | H2C | 0.278(9) | C4 | 0.722(9) | ||
H4A | 0.722(9) | H4B | 0.722(9) | C1AA | 0.722(9) | ||
H1AC | 0.722(9) | H1AD | 0.722(9) | H1AE | 0.722(9) | ||
C4A | 0.278(9) | H4AD | 0.278(9) | H4AE | 0.278(9) | ||
C1AB | 0.278(9) | H1AF | 0.278(9) | H1AG | 0.278(9) | ||
H1AH | 0.278(9) | C32A | 0.278(9) | H32C | 0.278(9) | ||
H32D | 0.278(9) | C33A | 0.278(9) | H33C | 0.278(9) | ||
H33D | 0.278(9) | C16A | 0.494(3) | H16A | 0.494(3) | ||
C15A | 0.494(3) | H15A | 0.494(3) | C19A | 0.494(3) | ||
H19A | 0.494(3) | C26A | 0.506(3) | H26A | 0.506(3) | ||
C29A | 0.494(3) | C22A | 0.494(3) |
Experimental
Single crystals of C42H41Cl3N2O6 [3Cl-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 [3Cl-nondecomposition]
Crystal Data for C42H41Cl3N2O6 (M =776.12 g/mol): triclinic, space group P-1 (no. 2), a = 7.722 Å, b = 12.874 Å, c = 21.477 Å, α = 84.25°, β = 84.18°, γ = 83.73°, V = 2102.8 Å3, Z = 2, T = 293(2) K, μ(Synchrotron Monochromator X-ray) = 0.245 mm-1, Dcalc = 1.226 g/cm3, 24179 reflections measured (1.854° ≤ 2Θ ≤ 46.64°), 6278 unique (Rint = 0.1829, Rsigma = 0.1087) which were used in all calculations. The final R1 was 0.1561 (I > 2σ(I)) and wR2 was 0.4645 (all data).
Refinement model description
Number of restraints - 154, 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
{C16, C16A}
{C15, C15A}
{C19A, C19}
{C26A, C26}
{C29, C29A}
{C22, C22A}
3. Restrained distances
C7AA-C6AA
1.55 with sigma of 0.02
C4-C1AA = C4-C31 = C33-C31 = C3AA-C1
1.55 with sigma of 0.02
C4A-C31 = C4A-C1AB
1.55 with sigma of 0.02
C33A-C1 = C33A-C31
1.55 with sigma of 0.02
C6AA-C2AA
1.55 with sigma of 0.02
C3-C2AA
1.55 with sigma of 0.02
4. Rigid bond restraints
C30, C32, C2, C32A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C31, C4, C1AA, C4A, C1AB
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C33, C1, C4AA, C3AA, C33A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C3, C2AA, C6AA, C7AA
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C30 ≈ C32 ≈ C2 ≈ C32A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C31 ≈ C4 ≈ C1AA ≈ C4A ≈ C1AB: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C33 ≈ C1 ≈ C4AA ≈ C3AA ≈ C33A: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C3 ≈ C2AA ≈ C6AA ≈ C7AA: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C4) = Uanis(C4A)
Uanis(C1AA) = Uanis(C1AB)
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
Uiso(C16) = Uiso(C16A)
Uiso(C15) = Uiso(C15A)
Uiso(C26) = Uiso(C26A)
Uiso(C26A) = Uiso(C26)
Uiso(C29) = Uiso(C29A)
Uiso(C22) = Uiso(C22A)
Uiso(C19) = Uiso(C19A)
Uiso(C19A) = Uiso(C19)
6. Others
Sof(Cl6A)=Sof(Cl2)=Sof(Cl7A)=Sof(H2BB)=Sof(H17A)=Sof(C26)=Sof(C16A)=Sof(H16A)=
Sof(C15A)=Sof(H15A)=Sof(C19A)=Sof(H19A)=Sof(C29A)=Sof(C22A)=1-FVAR(1)
Sof(Cl0A)=Sof(Cl3A)=Sof(Cl1A)=Sof(H2BA)=Sof(C15)=Sof(C16)=Sof(H17)=Sof(C19)=
Sof(C22)=Sof(H22)=Sof(C29)=Sof(H29)=Sof(C26A)=Sof(H26A)=FVAR(1)
Sof(H30A)=Sof(H31A)=Sof(H1A)=Sof(H1B)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C4A)=
Sof(H4AD)=Sof(H4AE)=Sof(C1AB)=Sof(H1AF)=Sof(H1AG)=Sof(H1AH)=Sof(C32A)=
Sof(H32C)=Sof(H32D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(2)
Sof(H30)=Sof(H31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=
Sof(H1AA)=Sof(H1AB)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C4)=Sof(H4A)=Sof(H4B)=
Sof(C1AA)=Sof(H1AC)=Sof(H1AD)=Sof(H1AE)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
C30(H30), C30(H30A), C31(H31A), C31(H31)
7.b Secondary CH2 refined with riding coordinates:
C20(H20A,H20B), C23(H23A,H23B), C32(H32A,H32B), C33(H33A,H33B), C1(H1AA,H1AB),
C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C2AA(H2AD,H2AE), C3AA(H3AA,H3AB),
C6AA(H6AA,H6AB), C4A(H4AD,H4AE), C32A(H32C,H32D), C33A(H33C,H33D)
7.c Me refined with riding coordinates:
C2(H2AA,H2AB,H2AC), C2(H2A,H2B,H2C), C4AA(H4AA,H4AB,H4AC), C1AA(H1AC,H1AD,
H1AE), C7AA(H7AA,H7AB,H7AC), C1AB(H1AF,H1AG,H1AH)
7.d Aromatic/amide H refined with riding coordinates:
C0AA(H0AA), C2BA(H2BA), C2BA(H2BB), C17(H17A), C17(H17), C21(H21), C22(H22),
C29(H29), C16A(H16A), C15A(H15A), C19A(H19A), 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.