| Identification code | 287c |
| Empirical formula | C15H21MnO6 |
| Formula weight | 352.26 |
| Temperature/K | 293(2) |
| Crystal system | monoclinic |
| Space group | P21 |
| a/Å | 19.8840(19) |
| b/Å | 7.6471(6) |
| c/Å | 23.415(2) |
| α/° | 90 |
| β/° | 98.946(9) |
| γ/° | 90 |
| Volume/Å3 | 3517.1(6) |
| Z | 8 |
| ρcalcg/cm3 | 1.330 |
| μ/mm‑1 | 0.773 |
| F(000) | 1472.0 |
| Crystal size/mm3 | 0.399 × 0.12 × 0.083 |
| Radiation | Mo Kα (λ = 0.71073) |
| 2Θ range for data collection/° | 3.522 to 50.244 |
| Index ranges | -23 ≤ h ≤ 23, -9 ≤ k ≤ 9, -27 ≤ l ≤ 27 |
| Reflections collected | 50406 |
| Independent reflections | 12441 [Rint = 0.2978, Rsigma = 0.2468] |
| Data/restraints/parameters | 12441/1/817 |
| Goodness-of-fit on F2 | 0.893 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0961, wR2 = 0.2069 |
| Final R indexes [all data] | R1 = 0.2576, wR2 = 0.2820 |
| Largest diff. peak/hole / e Å-3 | 0.74/-0.50 |
| Flack parameter | 0.56(9) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Mn1 | 7673.0(17) | 2794(4) | 4897.9(15) | 62.4(13) |
| O1 | 6770(7) | 2070(20) | 4568(6) | 67(5) |
| O2 | 7310(9) | 5230(20) | 5033(7) | 81(6) |
| O3 | 7542(8) | 2170(20) | 5726(6) | 78(5) |
| O4 | 8554(8) | 3560(20) | 5177(6) | 85(6) |
| O5 | 8038(8) | 360(20) | 4792(6) | 76(5) |
| O6 | 7855(8) | 3470(20) | 4103(7) | 76(5) |
| C1 | 5626(11) | 2030(40) | 4073(10) | 113(11) |
| C2 | 6252(12) | 2950(40) | 4408(10) | 92(10) |
| C3 | 6221(14) | 4770(40) | 4511(11) | 96(10) |
| C4 | 6710(16) | 5810(40) | 4841(12) | 80(9) |
| C5 | 6573(15) | 7680(30) | 5000(13) | 126(11) |
| C6 | 7723(10) | 1960(30) | 6714(10) | 122(9) |
| C7 | 7975(10) | 2470(30) | 6165(9) | 63(6) |
| C8 | 8621(10) | 3150(30) | 6184(9) | 84(7) |
| C9 | 8866(10) | 3700(30) | 5653(13) | 80(8) |
| C10 | 9580(11) | 4430(30) | 5782(10) | 117(9) |
| C11 | 8561(11) | -2050(30) | 4397(11) | 100(9) |
| C12 | 8326(10) | -120(30) | 4345(11) | 64(8) |
| C13 | 8420(12) | 940(40) | 3887(10) | 71(7) |
| C14 | 8181(9) | 2610(30) | 3752(8) | 56(6) |
| C15 | 8296(12) | 3480(40) | 3197(9) | 102(10) |
| Mn2 | 9718.5(19) | 7422(4) | 7543.6(16) | 72.0(12) |
| O7 | 8789(7) | 6870(20) | 7149(7) | 84(5) |
| O8 | 9949(8) | 8300(20) | 6813(6) | 70(5) |
| O9 | 10078(8) | 5040(20) | 7388(7) | 79(5) |
| O10 | 10642(9) | 8020(20) | 7937(7) | 81(6) |
| O11 | 9514(9) | 6590(30) | 8292(8) | 108(7) |
| O12 | 9401(8) | 9840(20) | 7730(7) | 93(6) |
| C16 | 7733(10) | 7080(30) | 6493(12) | 151(12) |
| C17 | 8482(11) | 7390(40) | 6654(11) | 95(9) |
| C18 | 8859(12) | 8360(30) | 6258(10) | 89(8) |
| C19 | 9565(11) | 8710(30) | 6368(12) | 80(8) |
| C20 | 9857(12) | 9530(30) | 5883(9) | 112(9) |
| C21 | 10753(13) | 2500(40) | 7400(11) | 109(9) |
| C22 | 10645(14) | 4420(30) | 7583(11) | 76(9) |
| C23 | 11184(13) | 5260(40) | 7920(10) | 102(10) |
| C24 | 11143(13) | 6980(30) | 8081(9) | 71(7) |
| C25 | 11773(13) | 7750(40) | 8437(10) | 117(11) |
| C26 | 9229(12) | 6510(40) | 9230(9) | 96(9) |
| C27 | 9266(10) | 7500(40) | 8664(10) | 86(9) |
| C28 | 9123(12) | 9310(40) | 8617(11) | 77(8) |
| C29 | 9169(11) | 10380(40) | 8152(12) | 81(9) |
| C30 | 8950(13) | 12210(30) | 8198(11) | 95(9) |
| Mn3 | 5149.4(17) | 2314(4) | 7426.3(15) | 67.2(12) |
| O13 | 5299(7) | 1710(20) | 6610(7) | 84(5) |
| O14 | 5493(7) | 4750(20) | 7302(6) | 77(5) |
| O15 | 6049(8) | 1500(20) | 7690(6) | 83(6) |
| O16 | 5031(8) | 2960(30) | 8244(7) | 80(5) |
| O17 | 4764(7) | -120(20) | 7546(7) | 74(5) |
| O18 | 4230(7) | 3050(20) | 7098(6) | 65(5) |
| C31 | 5791(12) | 1730(40) | 5767(9) | 108(11) |
| C32 | 5672(11) | 2620(40) | 6308(10) | 91(10) |
| C33 | 5874(12) | 4340(40) | 6435(10) | 74(8) |
| C34 | 5788(11) | 5300(40) | 6912(11) | 72(8) |
| C35 | 6037(11) | 7140(30) | 6946(10) | 86(8) |
| C36 | 7081(10) | 620(30) | 8267(10) | 123(10) |
| C37 | 6374(12) | 1420(30) | 8200(14) | 91(9) |
| C38 | 6104(13) | 1890(40) | 8698(11) | 105(9) |
| C39 | 5462(14) | 2550(40) | 8705(11) | 102(9) |
| C40 | 5193(11) | 2990(40) | 9266(8) | 132(10) |
| C41 | 4025(12) | -2490(40) | 7479(12) | 111(10) |
| C42 | 4174(13) | -580(40) | 7332(11) | 74(8) |
| C43 | 3663(11) | 380(40) | 7038(9) | 84(8) |
| C44 | 3691(12) | 2150(40) | 6914(9) | 78(8) |
| C45 | 3105(12) | 3120(40) | 6601(10) | 111(10) |
| Mn4 | 7246.1(19) | 7441(4) | 10028.7(16) | 70.0(12) |
| O19 | 6317(8) | 7980(30) | 9638(8) | 93(6) |
| O20 | 7455(8) | 6580(20) | 9270(7) | 79(5) |
| O21 | 7575(9) | 9870(20) | 9855(7) | 78(5) |
| O22 | 8159(9) | 6830(20) | 10407(7) | 82(6) |
| O23 | 7016(8) | 8290(20) | 10769(7) | 83(5) |
| O24 | 6910(8) | 5020(20) | 10198(7) | 86(6) |
| C46 | 5265(11) | 7820(30) | 8982(10) | 124(10) |
| C47 | 6037(11) | 7530(30) | 9154(12) | 81(7) |
| C48 | 6354(10) | 6640(30) | 8732(9) | 84(7) |
| C49 | 7038(11) | 6330(30) | 8807(11) | 79(7) |
| C50 | 7367(11) | 5480(30) | 8346(9) | 105(9) |
| C51 | 8257(13) | 12420(30) | 9871(11) | 98(8) |
| C52 | 8147(13) | 10540(40) | 10050(10) | 67(8) |
| C53 | 8669(11) | 9620(40) | 10410(10) | 80(9) |
| C54 | 8654(14) | 7750(40) | 10562(10) | 91(10) |
| C55 | 9289(13) | 7100(50) | 10930(11) | 130(12) |
| C56 | 6740(14) | 8430(40) | 11719(10) | 113(11) |
| C57 | 6814(10) | 7430(30) | 11169(11) | 78(9) |
| C58 | 6645(14) | 5740(40) | 11141(11) | 103(11) |
| C59 | 6712(11) | 4580(30) | 10678(12) | 78(10) |
| C60 | 6527(12) | 2600(40) | 10683(11) | 98(9) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Mn1 | 61(2) | 61(3) | 66(2) | -2.9(19) | 13.8(17) | 4(2) |
| O1 | 70(10) | 73(13) | 55(9) | -3(8) | 3(8) | 22(10) |
| O2 | 88(13) | 55(12) | 112(14) | -17(9) | 49(11) | 1(10) |
| O3 | 79(11) | 84(12) | 71(11) | 0(10) | 15(8) | -12(10) |
| O4 | 67(10) | 127(16) | 57(9) | -10(10) | 0(8) | 19(10) |
| O5 | 100(12) | 41(10) | 81(12) | 3(8) | -5(9) | 7(9) |
| O6 | 83(11) | 69(11) | 81(11) | 1(9) | 27(8) | 8(9) |
| C1 | 77(17) | 160(30) | 95(19) | 10(20) | -17(14) | -10(20) |
| C2 | 60(15) | 120(20) | 89(18) | 83(17) | -27(12) | -10(16) |
| C3 | 100(20) | 90(20) | 110(20) | 69(18) | 40(17) | 22(18) |
| C4 | 100(20) | 50(16) | 110(20) | 1(14) | 70(17) | 3(15) |
| C5 | 150(20) | 50(20) | 190(30) | 23(18) | 90(20) | 32(19) |
| C6 | 96(17) | 140(20) | 130(20) | 0(20) | 21(15) | 24(19) |
| C7 | 62(14) | 70(16) | 59(14) | 0(12) | 14(11) | 15(14) |
| C8 | 54(14) | 110(20) | 82(18) | -17(16) | -5(12) | 9(15) |
| C9 | 31(13) | 66(16) | 140(20) | -23(16) | -12(14) | 5(11) |
| C10 | 90(20) | 100(20) | 160(20) | 6(17) | 19(16) | 24(17) |
| C11 | 62(15) | 90(20) | 150(20) | 7(19) | 27(15) | 10(16) |
| C12 | 48(13) | 38(13) | 100(20) | -46(13) | -13(13) | 11(11) |
| C13 | 86(17) | 60(16) | 77(16) | 18(13) | 40(13) | -7(14) |
| C14 | 44(11) | 62(15) | 57(13) | -41(11) | -5(9) | 4(10) |
| C15 | 110(20) | 110(20) | 91(19) | 18(17) | 43(16) | 10(20) |
| Mn2 | 79(3) | 64(3) | 80(2) | -14(2) | 34(2) | -8(3) |
| O7 | 61(10) | 86(13) | 108(13) | -33(11) | 22(9) | -22(10) |
| O8 | 57(10) | 84(12) | 65(10) | -1(9) | -6(8) | 4(9) |
| O9 | 73(11) | 63(12) | 102(13) | -23(9) | 17(9) | -6(10) |
| O10 | 100(13) | 59(12) | 84(12) | -2(9) | 17(10) | 5(11) |
| O11 | 137(15) | 87(14) | 120(14) | -2(11) | 89(12) | -3(12) |
| O12 | 100(13) | 90(13) | 108(14) | -27(10) | 81(11) | -4(11) |
| C16 | 59(15) | 130(20) | 270(40) | -60(20) | 30(18) | 3(18) |
| C17 | 64(15) | 120(20) | 97(19) | -46(18) | -9(14) | 37(17) |
| C18 | 90(20) | 67(17) | 100(20) | 1(14) | 7(16) | 5(15) |
| C19 | 52(15) | 54(15) | 140(20) | -15(15) | 31(15) | 7(12) |
| C20 | 140(20) | 110(20) | 92(18) | 15(15) | 32(16) | -17(19) |
| C21 | 111(19) | 90(20) | 130(20) | -8(18) | 50(17) | -4(19) |
| C22 | 100(20) | 51(16) | 88(19) | 15(14) | 42(17) | 27(17) |
| C23 | 83(18) | 100(20) | 110(20) | -58(16) | -29(14) | -16(16) |
| C24 | 95(19) | 69(18) | 55(14) | -21(12) | 29(13) | -23(15) |
| C25 | 130(20) | 100(30) | 110(20) | -13(18) | 8(18) | -30(20) |
| C26 | 120(20) | 80(20) | 100(20) | 4(16) | 48(17) | -3(19) |
| C27 | 47(13) | 140(30) | 81(17) | 52(17) | 33(12) | -30(16) |
| C28 | 78(17) | 65(19) | 87(19) | -34(15) | 8(14) | 19(14) |
| C29 | 56(15) | 90(20) | 100(20) | 20(16) | 37(14) | -18(15) |
| C30 | 100(18) | 45(14) | 140(20) | -21(15) | 28(16) | 19(15) |
| Mn3 | 59(2) | 72(3) | 72(2) | 9(2) | 16.2(17) | -2(2) |
| O13 | 70(10) | 100(14) | 91(11) | 2(10) | 41(9) | 0(9) |
| O14 | 71(10) | 91(13) | 84(12) | 9(10) | 54(9) | -3(10) |
| O15 | 65(10) | 112(14) | 67(10) | 8(10) | -4(8) | 7(9) |
| O16 | 71(10) | 98(14) | 73(11) | 7(10) | 17(8) | 6(10) |
| O17 | 44(9) | 71(13) | 102(13) | 17(9) | -4(9) | 4(10) |
| O18 | 49(9) | 76(13) | 68(11) | 5(9) | 1(8) | 14(10) |
| C31 | 100(20) | 160(30) | 77(18) | -51(19) | 44(15) | -20(20) |
| C32 | 58(14) | 120(30) | 101(19) | -54(17) | 40(13) | 26(16) |
| C33 | 78(17) | 73(19) | 64(16) | 26(14) | -12(13) | -5(15) |
| C34 | 41(13) | 79(19) | 98(19) | -23(15) | 13(13) | 11(13) |
| C35 | 68(15) | 74(18) | 120(20) | 15(16) | 25(14) | 16(15) |
| C36 | 61(16) | 100(20) | 200(30) | 63(19) | -11(16) | -12(15) |
| C37 | 65(18) | 63(17) | 150(30) | 31(18) | 30(18) | -17(13) |
| C38 | 83(19) | 130(30) | 90(20) | 31(18) | 6(15) | -21(19) |
| C39 | 110(20) | 110(20) | 90(20) | 25(17) | 29(17) | -40(20) |
| C40 | 160(20) | 200(30) | 52(14) | -6(17) | 46(14) | -30(20) |
| C41 | 91(17) | 90(20) | 160(30) | -18(19) | 42(16) | -12(18) |
| C42 | 56(15) | 78(19) | 86(18) | -41(15) | 3(13) | -4(14) |
| C43 | 47(14) | 110(20) | 88(17) | 24(15) | -21(11) | -26(14) |
| C44 | 65(15) | 100(20) | 76(15) | 53(14) | 36(13) | 6(15) |
| C45 | 84(18) | 110(20) | 130(20) | 19(19) | -6(16) | 29(18) |
| Mn4 | 83(2) | 56(3) | 77(2) | 5(2) | 32.6(19) | 3(2) |
| O19 | 93(13) | 89(14) | 99(14) | -13(12) | 26(10) | -16(11) |
| O20 | 66(11) | 74(12) | 97(13) | -1(9) | 11(9) | 8(9) |
| O21 | 88(12) | 64(13) | 88(12) | 5(9) | 30(10) | -4(10) |
| O22 | 105(13) | 72(14) | 70(11) | -1(9) | 16(10) | -19(11) |
| O23 | 121(13) | 42(9) | 97(12) | 23(8) | 54(10) | 0(9) |
| O24 | 93(13) | 62(13) | 100(13) | 8(10) | 5(10) | -7(10) |
| C46 | 98(18) | 130(20) | 150(20) | 36(18) | 33(16) | 7(19) |
| C47 | 65(15) | 59(17) | 120(20) | 11(16) | 8(14) | 4(14) |
| C48 | 56(15) | 87(19) | 103(19) | 9(14) | -5(13) | -1(13) |
| C49 | 54(15) | 79(18) | 98(19) | 3(15) | -5(13) | -2(13) |
| C50 | 109(19) | 100(20) | 109(19) | -15(15) | 14(15) | 23(17) |
| C51 | 130(20) | 48(16) | 130(20) | 16(15) | 42(16) | -8(16) |
| C52 | 67(18) | 90(20) | 51(14) | 5(13) | 24(13) | 21(17) |
| C53 | 57(15) | 100(20) | 90(19) | -64(17) | 26(13) | -33(15) |
| C54 | 96(19) | 90(20) | 69(16) | -63(15) | -31(14) | 15(17) |
| C55 | 120(20) | 140(30) | 110(20) | -20(20) | -35(18) | 10(20) |
| C56 | 150(30) | 90(20) | 110(20) | 0(19) | 50(20) | 10(20) |
| C57 | 43(12) | 69(16) | 110(20) | 85(15) | -15(12) | -4(11) |
| C58 | 130(20) | 100(20) | 110(20) | -12(17) | 97(19) | 12(19) |
| C59 | 44(13) | 64(17) | 110(20) | 77(16) | -24(13) | -14(12) |
| C60 | 67(14) | 100(20) | 130(20) | 34(17) | 20(14) | 3(16) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Mn1 | O1 | 1.922(16) | Mn3 | O13 | 2.033(16) | |
| Mn1 | O2 | 2.037(19) | Mn3 | O14 | 2.022(17) | |
| Mn1 | O3 | 2.052(15) | Mn3 | O15 | 1.905(15) | |
| Mn1 | O4 | 1.867(17) | Mn3 | O16 | 2.026(16) | |
| Mn1 | O5 | 2.026(16) | Mn3 | O17 | 2.047(19) | |
| Mn1 | O6 | 2.018(15) | Mn3 | O18 | 1.954(14) | |
| O1 | C2 | 1.24(2) | O13 | C32 | 1.30(3) | |
| O2 | C4 | 1.29(3) | O14 | C34 | 1.24(3) | |
| O3 | C7 | 1.26(2) | O15 | C37 | 1.27(3) | |
| O4 | C9 | 1.19(2) | O16 | C39 | 1.31(3) | |
| O5 | C12 | 1.32(2) | O17 | C42 | 1.25(3) | |
| O6 | C14 | 1.30(2) | O18 | C44 | 1.29(3) | |
| C1 | C2 | 1.54(3) | C31 | C32 | 1.49(3) | |
| C2 | C3 | 1.41(4) | C32 | C33 | 1.39(4) | |
| C3 | C4 | 1.39(4) | C33 | C34 | 1.37(3) | |
| C4 | C5 | 1.52(3) | C34 | C35 | 1.49(3) | |
| C6 | C7 | 1.50(3) | C36 | C37 | 1.52(3) | |
| C7 | C8 | 1.38(2) | C37 | C38 | 1.40(3) | |
| C8 | C9 | 1.47(3) | C38 | C39 | 1.37(3) | |
| C9 | C10 | 1.51(3) | C39 | C40 | 1.53(3) | |
| C11 | C12 | 1.55(3) | C41 | C42 | 1.54(3) | |
| C12 | C13 | 1.38(3) | C42 | C43 | 1.35(3) | |
| C13 | C14 | 1.38(3) | C43 | C44 | 1.38(4) | |
| C14 | C15 | 1.51(3) | C44 | C45 | 1.48(3) | |
| Mn2 | O7 | 1.978(16) | Mn4 | O19 | 1.973(18) | |
| Mn2 | O8 | 1.957(16) | Mn4 | O20 | 1.999(16) | |
| Mn2 | O9 | 2.014(19) | Mn4 | O21 | 2.033(19) | |
| Mn2 | O10 | 1.976(17) | Mn4 | O22 | 1.948(18) | |
| Mn2 | O11 | 1.964(17) | Mn4 | O23 | 1.971(16) | |
| Mn2 | O12 | 2.023(17) | Mn4 | O24 | 2.025(18) | |
| O7 | C17 | 1.29(3) | O19 | C47 | 1.23(2) | |
| O8 | C19 | 1.23(3) | O20 | C49 | 1.27(2) | |
| O9 | C22 | 1.24(3) | O21 | C52 | 1.27(3) | |
| O10 | C24 | 1.28(3) | O22 | C54 | 1.22(3) | |
| O11 | C27 | 1.27(3) | O23 | C57 | 1.26(2) | |
| O12 | C29 | 1.22(3) | O24 | C59 | 1.29(3) | |
| C16 | C17 | 1.50(3) | C46 | C47 | 1.54(3) | |
| C17 | C18 | 1.48(3) | C47 | C48 | 1.43(3) | |
| C18 | C19 | 1.41(3) | C48 | C49 | 1.36(3) | |
| C19 | C20 | 1.49(3) | C49 | C50 | 1.50(3) | |
| C21 | C22 | 1.55(3) | C51 | C52 | 1.52(3) | |
| C22 | C23 | 1.39(3) | C52 | C53 | 1.42(3) | |
| C23 | C24 | 1.38(4) | C53 | C54 | 1.47(4) | |
| C24 | C25 | 1.51(3) | C54 | C55 | 1.50(3) | |
| C26 | C27 | 1.54(3) | C56 | C57 | 1.53(3) | |
| C27 | C28 | 1.41(4) | C57 | C58 | 1.33(4) | |
| C28 | C29 | 1.37(3) | C58 | C59 | 1.42(3) | |
| C29 | C30 | 1.48(3) | C59 | C60 | 1.56(3) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| O1 | Mn1 | O2 | 89.6(7) | O13 | Mn3 | O17 | 92.1(7) | |
| O1 | Mn1 | O3 | 93.7(6) | O14 | Mn3 | O13 | 88.4(7) | |
| O1 | Mn1 | O5 | 90.9(7) | O14 | Mn3 | O16 | 90.2(7) | |
| O1 | Mn1 | O6 | 89.6(6) | O14 | Mn3 | O17 | 177.8(7) | |
| O2 | Mn1 | O3 | 88.1(7) | O15 | Mn3 | O13 | 87.9(7) | |
| O4 | Mn1 | O1 | 176.6(7) | O15 | Mn3 | O14 | 91.6(7) | |
| O4 | Mn1 | O2 | 89.7(8) | O15 | Mn3 | O16 | 90.8(7) | |
| O4 | Mn1 | O3 | 89.6(6) | O15 | Mn3 | O17 | 90.6(7) | |
| O4 | Mn1 | O5 | 89.9(7) | O15 | Mn3 | O18 | 175.4(7) | |
| O4 | Mn1 | O6 | 87.1(7) | O16 | Mn3 | O13 | 178.0(7) | |
| O5 | Mn1 | O2 | 178.1(7) | O16 | Mn3 | O17 | 89.4(7) | |
| O5 | Mn1 | O3 | 90.0(7) | O18 | Mn3 | O13 | 87.7(6) | |
| O6 | Mn1 | O2 | 91.7(7) | O18 | Mn3 | O14 | 89.6(7) | |
| O6 | Mn1 | O3 | 176.7(7) | O18 | Mn3 | O16 | 93.6(6) | |
| O6 | Mn1 | O5 | 90.2(7) | O18 | Mn3 | O17 | 88.3(7) | |
| C2 | O1 | Mn1 | 130.3(19) | C32 | O13 | Mn3 | 124.6(17) | |
| C4 | O2 | Mn1 | 126.3(18) | C34 | O14 | Mn3 | 129.1(17) | |
| C7 | O3 | Mn1 | 124.0(14) | C37 | O15 | Mn3 | 129.6(17) | |
| C9 | O4 | Mn1 | 132.7(18) | C39 | O16 | Mn3 | 124.4(17) | |
| C12 | O5 | Mn1 | 123.9(15) | C42 | O17 | Mn3 | 123.2(19) | |
| C14 | O6 | Mn1 | 129.2(16) | C44 | O18 | Mn3 | 130.7(17) | |
| O1 | C2 | C1 | 118(3) | O13 | C32 | C31 | 113(3) | |
| O1 | C2 | C3 | 123(3) | O13 | C32 | C33 | 124(2) | |
| C3 | C2 | C1 | 119(3) | C33 | C32 | C31 | 122(3) | |
| C4 | C3 | C2 | 128(3) | C34 | C33 | C32 | 128(2) | |
| O2 | C4 | C3 | 122(3) | O14 | C34 | C33 | 124(3) | |
| O2 | C4 | C5 | 116(3) | O14 | C34 | C35 | 118(2) | |
| C3 | C4 | C5 | 123(3) | C33 | C34 | C35 | 118(3) | |
| O3 | C7 | C6 | 112.1(19) | O15 | C37 | C36 | 116(3) | |
| O3 | C7 | C8 | 127.7(19) | O15 | C37 | C38 | 124(2) | |
| C8 | C7 | C6 | 120(2) | C38 | C37 | C36 | 119(3) | |
| C7 | C8 | C9 | 120.8(19) | C39 | C38 | C37 | 125(2) | |
| O4 | C9 | C8 | 125(2) | O16 | C39 | C38 | 125(2) | |
| O4 | C9 | C10 | 124(3) | O16 | C39 | C40 | 113(2) | |
| C8 | C9 | C10 | 111(2) | C38 | C39 | C40 | 123(2) | |
| O5 | C12 | C11 | 111(2) | O17 | C42 | C41 | 112(3) | |
| O5 | C12 | C13 | 126(2) | O17 | C42 | C43 | 129(3) | |
| C13 | C12 | C11 | 123(2) | C43 | C42 | C41 | 118(2) | |
| C12 | C13 | C14 | 130(2) | C42 | C43 | C44 | 126(2) | |
| O6 | C14 | C13 | 121(2) | O18 | C44 | C43 | 121(2) | |
| O6 | C14 | C15 | 118(2) | O18 | C44 | C45 | 116(2) | |
| C13 | C14 | C15 | 121.0(19) | C43 | C44 | C45 | 123(2) | |
| O7 | Mn2 | O9 | 93.2(7) | O19 | Mn4 | O20 | 88.0(7) | |
| O7 | Mn2 | O12 | 89.7(7) | O19 | Mn4 | O21 | 91.4(8) | |
| O8 | Mn2 | O7 | 89.6(7) | O19 | Mn4 | O24 | 88.1(7) | |
| O8 | Mn2 | O9 | 90.9(7) | O20 | Mn4 | O21 | 90.4(7) | |
| O8 | Mn2 | O10 | 90.1(7) | O20 | Mn4 | O24 | 89.6(7) | |
| O8 | Mn2 | O11 | 178.0(8) | O22 | Mn4 | O19 | 178.1(9) | |
| O8 | Mn2 | O12 | 89.9(7) | O22 | Mn4 | O20 | 91.0(7) | |
| O9 | Mn2 | O12 | 177.0(8) | O22 | Mn4 | O21 | 90.2(8) | |
| O10 | Mn2 | O7 | 178.9(8) | O22 | Mn4 | O23 | 90.3(7) | |
| O10 | Mn2 | O9 | 87.9(7) | O22 | Mn4 | O24 | 90.3(7) | |
| O10 | Mn2 | O12 | 89.3(7) | O23 | Mn4 | O19 | 90.6(7) | |
| O11 | Mn2 | O7 | 92.3(8) | O23 | Mn4 | O20 | 178.6(7) | |
| O11 | Mn2 | O9 | 89.8(8) | O23 | Mn4 | O21 | 90.0(7) | |
| O11 | Mn2 | O10 | 88.0(7) | O23 | Mn4 | O24 | 90.0(7) | |
| O11 | Mn2 | O12 | 89.3(7) | O24 | Mn4 | O21 | 179.5(8) | |
| C17 | O7 | Mn2 | 129.4(17) | C47 | O19 | Mn4 | 128.8(17) | |
| C19 | O8 | Mn2 | 128.9(16) | C49 | O20 | Mn4 | 127.4(16) | |
| C22 | O9 | Mn2 | 127.4(18) | C52 | O21 | Mn4 | 126.6(18) | |
| C24 | O10 | Mn2 | 127.6(17) | C54 | O22 | Mn4 | 130.5(19) | |
| C27 | O11 | Mn2 | 126.2(19) | C57 | O23 | Mn4 | 128.6(19) | |
| C29 | O12 | Mn2 | 130.5(19) | C59 | O24 | Mn4 | 124.4(17) | |
| O7 | C17 | C16 | 120(3) | O19 | C47 | C46 | 119(2) | |
| O7 | C17 | C18 | 120(2) | O19 | C47 | C48 | 126(2) | |
| C18 | C17 | C16 | 120(2) | C48 | C47 | C46 | 115(2) | |
| C19 | C18 | C17 | 125(2) | C49 | C48 | C47 | 122(2) | |
| O8 | C19 | C18 | 125(2) | O20 | C49 | C48 | 126(2) | |
| O8 | C19 | C20 | 119(2) | O20 | C49 | C50 | 112(2) | |
| C18 | C19 | C20 | 116(2) | C48 | C49 | C50 | 121(2) | |
| O9 | C22 | C21 | 115(3) | O21 | C52 | C51 | 116(2) | |
| O9 | C22 | C23 | 127(3) | O21 | C52 | C53 | 123(3) | |
| C23 | C22 | C21 | 118(2) | C53 | C52 | C51 | 121(3) | |
| C24 | C23 | C22 | 122(3) | C52 | C53 | C54 | 126(2) | |
| O10 | C24 | C23 | 127(3) | O22 | C54 | C53 | 122(2) | |
| O10 | C24 | C25 | 117(2) | O22 | C54 | C55 | 123(3) | |
| C23 | C24 | C25 | 116(3) | C53 | C54 | C55 | 115(3) | |
| O11 | C27 | C26 | 113(3) | O23 | C57 | C56 | 117(2) | |
| O11 | C27 | C28 | 125(2) | O23 | C57 | C58 | 125(3) | |
| C28 | C27 | C26 | 121(3) | C58 | C57 | C56 | 118(2) | |
| C29 | C28 | C27 | 127(2) | C57 | C58 | C59 | 126(3) | |
| O12 | C29 | C28 | 121(3) | O24 | C59 | C58 | 125(2) | |
| O12 | C29 | C30 | 122(2) | O24 | C59 | C60 | 111(3) | |
| C28 | C29 | C30 | 117(3) | C58 | C59 | C60 | 123(3) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H | 5743.98 | 1506.53 | 3729.3 | 169 |
| HA | 5267.63 | 2864.58 | 3969.48 | 169 |
| HB | 5473.44 | 1134.52 | 4311.61 | 169 |
| HC | 5827.42 | 5333.56 | 4338.65 | 115 |
| HD | 6686.52 | 7827.46 | 5410.79 | 188 |
| HE | 6100.17 | 7945.83 | 4880.8 | 188 |
| HF | 6846.03 | 8455.31 | 4808.73 | 188 |
| HG | 7271.62 | 2413.03 | 6709.6 | 183 |
| HH | 8020.94 | 2439.51 | 7038.9 | 183 |
| HI | 7715.91 | 711.49 | 6745.08 | 183 |
| HJ | 8904.47 | 3265.88 | 6537.54 | 101 |
| HK | 9902.52 | 3492.33 | 5797.18 | 175 |
| HL | 9639.08 | 5028.09 | 6146.9 | 175 |
| HM | 9652.4 | 5238.04 | 5482.76 | 175 |
| HN | 8775.52 | -2276.66 | 4786.37 | 150 |
| HO | 8878.6 | -2263.14 | 4136.09 | 150 |
| HP | 8173.33 | -2801.91 | 4302.33 | 150 |
| HQ | 8684.33 | 458.52 | 3632.41 | 86 |
| HR | 7999.4 | 2972.46 | 2877.25 | 153 |
| HS | 8760.75 | 3323.3 | 3142.77 | 153 |
| HT | 8199.98 | 4709.78 | 3216.79 | 153 |
| HU | 7611.11 | 6013.72 | 6667.81 | 227 |
| HV | 7619.38 | 6989.85 | 6080.2 | 227 |
| HW | 7487.38 | 8037.63 | 6627.47 | 227 |
| HX | 8615.25 | 8759.86 | 5912.45 | 107 |
| HY | 10100.21 | 10572.53 | 6018.6 | 168 |
| HZ | 9496.46 | 9822.74 | 5575.86 | 168 |
| H1 | 10163.73 | 8723.98 | 5742.5 | 168 |
| H2 | 10437.43 | 1751.82 | 7554.04 | 164 |
| H3 | 11210.04 | 2143.33 | 7547.21 | 164 |
| H4 | 10678.31 | 2418.79 | 6985.88 | 164 |
| H5 | 11584.85 | 4643.86 | 8039.37 | 123 |
| H6 | 11959.1 | 8637.43 | 8216.23 | 175 |
| H7 | 12104.67 | 6849.09 | 8539.12 | 175 |
| H8 | 11654.79 | 8265.18 | 8782.92 | 175 |
| H9 | 8787.83 | 5987.33 | 9211.62 | 144 |
| H10 | 9304.96 | 7315.18 | 9548.24 | 144 |
| H11 | 9571.87 | 5617.38 | 9282.37 | 144 |
| H12 | 8981.26 | 9837.06 | 8935.82 | 92 |
| H13 | 9279.58 | 12976 | 8069.63 | 142 |
| H14 | 8913.01 | 12470.02 | 8592.51 | 142 |
| H15 | 8516.22 | 12378.19 | 7959.99 | 142 |
| H31A | 6230.46 | 1183.36 | 5828.73 | 162 |
| H31B | 5774.94 | 2581.05 | 5462.21 | 162 |
| H31C | 5445.67 | 866.8 | 5660.63 | 162 |
| H33 | 6094.72 | 4894.68 | 6163.43 | 89 |
| H35A | 5723.72 | 7860.82 | 7113.35 | 129 |
| H35B | 6069.72 | 7554.8 | 6564.05 | 129 |
| H35C | 6476.77 | 7188.66 | 7181.14 | 129 |
| H36A | 7045.33 | -618.22 | 8212.41 | 185 |
| H36B | 7320.12 | 871.7 | 8646.62 | 185 |
| H36C | 7326.44 | 1117.93 | 7982.82 | 185 |
| H38 | 6382.49 | 1739.02 | 9051.92 | 126 |
| H40A | 5456.49 | 3929.42 | 9459.91 | 199 |
| H40B | 5229.15 | 1980.72 | 9512.64 | 199 |
| H40C | 4724.66 | 3340.56 | 9177.85 | 199 |
| H41A | 4440.1 | -3053.06 | 7647.22 | 167 |
| H41B | 3833.15 | -3095.41 | 7132.54 | 167 |
| H41C | 3707.5 | -2513.13 | 7749.17 | 167 |
| H43 | 3256.03 | -195.31 | 6908.78 | 100 |
| H45A | 2763.23 | 2314.42 | 6430.36 | 167 |
| H45B | 3253.41 | 3821.94 | 6303.33 | 167 |
| H45C | 2919.14 | 3869.97 | 6866.95 | 167 |
| H16 | 5103.62 | 8567.81 | 9262.36 | 186 |
| H17 | 5032.92 | 6721.03 | 8968.5 | 186 |
| H18 | 5177.71 | 8369.64 | 8608.68 | 186 |
| H19 | 6086.31 | 6250.4 | 8394.26 | 100 |
| H20 | 7739.68 | 6182.61 | 8265.21 | 158 |
| H21 | 7039.18 | 5351.18 | 8001.78 | 158 |
| H22 | 7533.14 | 4342.63 | 8476.95 | 158 |
| H23 | 8209.09 | 12494.2 | 9457.49 | 148 |
| H24 | 8706.11 | 12798.08 | 10037.47 | 148 |
| H25 | 7925.72 | 13167.51 | 10006.05 | 148 |
| H26 | 9054.6 | 10250.6 | 10564.52 | 95 |
| H27 | 9567.02 | 8070.48 | 11078.45 | 195 |
| H28 | 9538.22 | 6372.36 | 10700.35 | 195 |
| H29 | 9169.65 | 6424.31 | 11245.28 | 195 |
| H30 | 7170.57 | 8458.61 | 11970.02 | 169 |
| H31 | 6409.13 | 7858.97 | 11913.08 | 169 |
| H32 | 6593.51 | 9602.97 | 11621.34 | 169 |
| H34 | 6466.79 | 5276.47 | 11452.59 | 124 |
| H35 | 6292.78 | 2267.24 | 10308.72 | 146 |
| H36 | 6237.99 | 2393.11 | 10968.14 | 146 |
| H37 | 6935.75 | 1922.26 | 10773.94 | 146 |
Experimental
Single crystals of C15H21MnO6 [287c] were []. A suitable crystal was selected and [] on a XtaLAB Mini II diffractometer. The crystal was kept at 293(2) K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program using Intrinsic Phasing and refined with the ShelXL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [287c]
Crystal Data for C15H21MnO6 (M =352.26 g/mol): monoclinic, space group P21 (no. 4), a = 19.8840(19) Å, b = 7.6471(6) Å, c = 23.415(2) Å, β = 98.946(9)°, V = 3517.1(6) Å3, Z = 8, T = 293(2) K, μ(Mo Kα) = 0.773 mm-1, Dcalc = 1.330 g/cm3, 50406 reflections measured (3.522° ≤ 2Θ ≤ 50.244°), 12441 unique (Rint = 0.2978, Rsigma = 0.2468) which were used in all calculations. The final R1 was 0.0961 (I > 2σ(I)) and wR2 was 0.2820 (all data).
Refinement model description
Number of restraints - 1, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
C3(HC), C8(HJ), C13(HQ), C18(HX), C23(H5), C28(H12), C33(H33), C38(H38),
C43(H43), C48(H19), C53(H26), C58(H34)
2.b Idealised Me refined as rotating group:
C1(H,HA,HB), C5(HD,HE,HF), C6(HG,HH,HI), C10(HK,HL,HM), C11(HN,HO,HP), C15(HR,
HS,HT), C16(HU,HV,HW), C20(HY,HZ,H1), C21(H2,H3,H4), C25(H6,H7,H8), C26(H9,H10,
H11), C30(H13,H14,H15), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,
H36B,H36C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C45(H45A,H45B,H45C),
C46(H16,H17,H18), C50(H20,H21,H22), C51(H23,H24,H25), C55(H27,H28,H29),
C56(H30,H31,H32), C60(H35,H36,H37)
This report has been created with Olex2, compiled on 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction. Please let us know if there are any errors or if you would like to have additional features.