DC152

Table 1 Crystal data and structure refinement for DC152
Identification code DC152
Empirical formula C20H40O8Ti
Formula weight 360.18
Temperature/K N/A
Crystal system triclinic
Space group P-1
a/Å 17.125(5)
b/Å 24.491(6)
c/Å 28.844(8)
α/° 89.890(7)
β/° 80.815(6)
γ/° 89.601(8)
Volume/Å3 11942(5)
Z 21
ρcalcmg/mm3 1.0517
m/mm‑1 0.257
F(000) 3939.7
Crystal size/mm3 N/A × N/A × N/A
Radiation Mo Kα (λ = 0.71073)
2Θ range for data collection 2.2 to 41.88°
Index ranges -15 ≤ h ≤ 17, -21 ≤ k ≤ 23, -28 ≤ l ≤ 28
Reflections collected 46548
Independent reflections 15614 [Rint = 0.0824, Rsigma = 0.0991]
Data/restraints/parameters 15614/0/1079
Goodness-of-fit on F2 2.582
Final R indexes [I>=2σ (I)] R1 = 0.2463, wR2 = 0.5804
Final R indexes [all data] R1 = 0.3080, wR2 = 0.6206
Largest diff. peak/hole / e Å-3 3.71/-1.57

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for DC152. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Ti1368(3)8039(3)4114.1(17)21.4(15)
Ti2-4659(3)6949(3)9109.4(17)18.1(15)
Ti3-3632(3)8065(3)9404.7(16)14.7(14)
Ti41411(3)6912(3)4403.6(17)21.5(15)
Ti51843(3)7483(3)3306.0(16)15.5(14)
Ti6-3197(3)7509(3)8297.9(16)13.9(14)
O11870(11)7821(10)2638(6)18(5)
O2-2194(11)7881(10)7924(6)20(5)
O3-3163(11)7159(9)7630(6)16(5)
O5-102(11)8724(10)3859(6)21(5)
O6-176(12)6105(10)7207(6)24(5)
O72619(11)8034(10)3448(6)21(5)
O8-5092(12)6244(11)8851(6)29(5)
O94602(12)10015(10)4016(6)26(5)
O101188(11)6955(10)3031(6)20(5)
O113641(11)8491(10)624(6)21(5)
O12544(11)6448(12)4273(6)22(5)
O13-1369(11)6504(10)5613(6)21(5)
O14-867(12)4979(10)2486(6)26(5)
O15-3170(10)7945(9)8802(5)8(4)
O16722(11)7497(10)4450(6)25(5)
O18-488(11)7662(10)3857(6)18(5)
O192861(11)7122(10)2922(6)16(5)
O20-3932(11)8216(10)10117(6)20(5)
O21-2726(11)7665(10)9608(6)20(5)
O222307(12)7269(11)4608(6)29(5)
O24-2428(11)6948(9)8443(5)13(5)
O26-5149(11)8865(10)12219(6)21(5)
O27-340(12)4975(11)8982(7)35(6)
O28968(11)8578(10)4401(6)21(5)
O29-5503(11)7338(9)8851(5)12(4)
O305059(11)6422(10)1049(6)24(5)
O31-526(12)8235(10)4646(6)25(5)
O32-5867(12)10041(10)7477(6)27(5)
O33400(12)6449(10)9888(6)25(5)
O34-4291(11)7495(10)9450(6)19(5)
C35999(16)6630(14)5937(8)5(6)
O36-3890(10)8036(9)8035(6)14(5)
C37-2747(15)7173(14)6818(8)5(6)
O38-3103(12)9039(11)6326(6)30(5)
O39-7595(13)9786(12)8906(7)41(6)
O40-7349(13)4407(11)8315(7)36(6)
O411848(11)7008(10)3807(6)18(5)
O4229(13)8580(12)6072(7)42(6)
C433877(16)7094(14)2299(8)11(7)
O44-8087(13)5953(12)11336(7)40(6)
C463219(17)8253(17)980(9)19(7)
O472001(13)6173(13)4434(7)33(6)
O485386(14)8570(13)4923(7)45(6)
O49-4519(10)8560(9)9282(5)13(5)
C50572(17)6338(15)2562(9)14(7)
C51-335(17)8333(16)6465(9)15(7)
C522285(16)7798(15)1815(8)7(7)
C53-6380(19)6299(16)10413(10)26(8)
C542928(19)8635(19)1362(10)36(9)
O55-3084(12)8810(11)9432(6)29(5)
O56-5562(12)6775(10)9651(6)25(5)
C57-4685(17)9073(15)9378(9)15(7)
O58-2588(14)6521(13)2568(8)47(7)
C59-58(17)5709(16)2126(9)17(7)
C604200(17)9577(15)3852(9)14(7)
C613463(18)9432(16)3983(9)17(7)
O633176(12)9891(10)5538(6)26(5)
C644702(16)7239(14)1521(9)13(7)
C654685(16)6697(15)1462(8)10(7)
C661463(15)7087(14)2226(8)8(7)
O67-7636(14)8488(13)7597(8)51(7)
O68-1274(16)10873(14)10079(9)61(8)
C69-1960(16)7341(14)6014(9)15(7)
C70-6373(17)9969(16)9155(9)19(7)
C71-1853(16)6755(14)5988(8)10(7)
O721101(11)6773(10)5103(6)25(5)
C734435(18)8812(17)3315(10)24(8)
C74235(18)6033(17)2992(10)24(8)
C753300(20)7689(19)4988(11)38(9)
C76-1152(17)7883(16)7293(9)17(7)
C77-6671(18)7641(16)8594(9)19(7)
C78-6313(16)6822(14)9669(8)7(7)
C79-1691(18)7373(16)9953(9)23(8)
C80-705(18)8674(18)6801(10)33(9)
C81-1688(18)6831(16)8233(9)19(8)
O82-2311(13)10611(12)3287(7)45(6)
C83-3936(15)8176(14)7604(8)7(7)
C84-6222(19)7906(16)8247(9)21(8)
C853016(17)7710(17)1032(9)19(8)
C86888(17)9123(15)4483(9)16(7)
C871492(16)9344(14)4778(8)10(7)
C892590(18)9682(16)5304(9)21(8)
C90-5698(18)4817(17)8865(9)23(8)
C913659(17)8646(15)3441(9)14(7)
C923564(18)7952(17)4587(10)24(8)
C932533(17)7487(16)1441(9)22(8)
C94-382(17)5431(15)2525(9)16(7)
C95207(17)6274(15)6776(9)14(7)
C964686(19)8314(17)4930(10)25(8)
C97-691(18)9600(16)3818(9)24(8)
C983316(18)8176(15)3256(9)15(7)
C993937(17)6559(16)2214(10)22(8)
C1001417(18)6882(16)5469(10)23(8)
C101-2620(18)8840(16)5911(9)22(8)
C102-5954(16)8855(16)9155(9)17(7)
C103859(18)6586(17)6774(10)24(8)
C104-221(19)5721(16)8485(9)24(8)
C107-317(19)7769(18)6516(10)29(8)
C108-7623(19)6161(17)10920(10)27(8)
C1095445(18)6798(17)684(10)28(9)
C110-258(17)5626(15)2985(9)19(7)
C1111982(16)8964(16)4955(9)20(7)
C1124161(19)10268(17)4435(10)33(9)
C113-2539(18)6624(16)6777(10)24(8)
C114-5737(17)5363(16)8848(9)16(7)
C115-1416(17)7029(15)9569(9)16(7)
C116-2399(18)10670(18)9777(10)31(8)
C117-2140(20)9500(20)9838(11)46(10)
C118-5088(18)9349(16)7128(10)28(9)
C119-1190(20)10520(20)3651(11)46(10)
C1204752(19)9265(15)3503(9)21(8)
C1212562(17)7360(15)5018(9)18(7)
C1221270(19)6791(16)6349(9)25(8)
C123-3560(19)8126(16)10460(10)26(8)
C1243140(20)8977(16)3795(10)26(8)
C1251521(17)9866(15)4877(9)16(7)
C127-6639(19)7065(16)9317(9)20(8)
C128-2950(18)10265(16)9659(9)21(8)
C129-6868(19)4769(17)8488(10)26(8)
C130-135(17)9237(15)4000(9)15(7)
C1311121(16)6805(15)2608(9)15(7)
C132-3581(17)7907(16)7212(10)24(8)
C133-780(20)5767(19)7205(11)39(9)
C134-1643(18)7974(15)4328(9)21(8)
C135-4983(17)8896(16)11341(9)19(8)
C136-3000(20)8563(16)5628(10)28(8)
C138-2770(20)7146(19)3246(11)44(10)
C1393465(17)7367(15)2716(9)10(7)
C140-781(19)5428(16)8835(9)22(8)
C141-1280(16)8166(13)4660(8)6(7)
C142-6346(19)10224(19)7886(11)35(9)
C144-1147(18)8438(17)7224(10)23(8)
C145-1340(20)8730(16)5403(10)27(8)
C146-4120(17)9417(16)9517(9)23(8)
C147-1000(20)6848(19)5235(11)45(10)
C148-1831(19)6023(17)8764(10)25(8)
C1491884(15)7591(14)2236(8)7(7)
C150-6813(16)6585(14)10115(8)10(7)
C151-2398(17)7537(16)6426(9)22(8)
C1534319(17)7487(16)1932(9)24(8)
C154-3976(18)8350(15)10917(9)18(7)
C155-6277(17)7287(15)8936(8)12(7)
C156-2103(16)6385(16)6363(9)19(7)
C157-55(18)6089(16)6358(9)24(8)
C1592152(19)7138(17)5441(10)29(9)
C160-4450(17)8648(15)7567(9)14(7)
C162426(17)6141(15)2147(9)18(7)
C163-1372(17)6343(15)8414(9)15(7)
C164-2849(18)7886(16)10408(10)22(8)
C165-2702(17)9365(16)6638(9)21(8)
C167-2583(18)8347(16)5206(10)25(8)
C168365(18)9414(17)4324(10)31(9)
C1694331(16)6355(16)1810(9)18(7)
C170726(19)6203(18)9464(10)30(8)
C171-6799(18)6096(16)10838(10)24(8)
C172-640(17)10174(15)3839(9)20(8)
C173-1170(18)7068(15)3229(9)20(8)
C174-1808(18)8410(15)5096(9)20(8)
C175-5700(20)9815(18)9268(10)35(9)
C176-7510(20)7577(17)8601(11)34(9)
C177-2828(18)9663(17)9682(10)24(8)
C178-6332(16)5667(16)8636(9)19(7)
C179-790(20)4710(20)9374(13)60(12)
C1802101(19)10071(18)5135(10)37(9)
C182-6260(20)4489(19)8689(11)41(9)
C1832470(18)8358(18)1791(10)27(8)
C184-5803(18)9246(17)12235(10)23(8)
C1854450(20)8018(19)5329(11)35(9)
C186-6896(19)5327(17)8475(9)25(8)
C187-554(19)6210(17)8288(10)30(8)
C188-8020(20)6404(18)10640(10)35(9)
C189381(18)6334(16)5942(9)20(8)
C190-1580(20)9870(20)9978(12)50(11)
C191-5432(18)9272(16)9274(9)19(7)
C192-7600(19)6638(17)10225(10)27(8)
C193-3151(16)7386(14)7235(8)11(7)
C194-1648(19)7385(17)3599(10)30(9)
C195-6874(19)9581(17)9029(10)30(8)
C196-1313(19)4794(17)2897(10)33(9)
C198-4806(18)8913(16)7989(10)26(8)
C199-1220(18)7681(15)3916(9)17(7)
C200-1770(20)10230(20)3455(11)40(10)
C202-1730(20)10430(20)9945(12)49(10)
C204-1477(19)5551(15)8956(10)20(8)
C205-2458(17)7625(15)10001(9)16(7)
C207-1579(17)7627(15)7713(8)13(7)
C208-559(18)6981(16)10306(9)20(8)
C209-7850(20)7854(19)8272(11)45(10)
C210-1250(20)7272(18)10351(11)35(9)
C211-1316(19)7126(16)7887(9)23(8)
C214-3708(19)8201(17)11347(10)30(9)
C2153769(18)7882(16)2878(10)24(8)
C216-5275(18)9373(16)7969(10)25(8)
C217-3337(17)9299(15)9537(9)14(7)
C218-1782(18)8929(16)5837(10)24(8)
C2192540(20)9116(18)5195(10)34(9)
C221-4634(16)8664(14)10956(9)11(7)
C222-4745(17)8720(15)11772(9)14(7)
C2243690(20)7730(20)5398(13)53(11)
C227-7690(20)5639(19)11648(11)44(10)
C229-6720(20)8987(18)9023(10)38(9)
C231-4568(18)8877(17)7137(10)26(8)
C234-5404(16)9532(14)7540(8)11(7)
C235-740(20)7540(20)6935(13)60(12)
C239-2900(20)10320(20)3046(13)56(11)
C244-2320(20)6816(18)2930(11)33(9)
C246-2458(19)7401(17)3592(10)31(9)
C248-1520(20)6790(18)2915(11)36(9)
C251-298(19)6698(17)9889(10)27(8)
C253-6570(20)8218(17)7917(10)31(9)
C254-7880(20)4700(20)8038(12)55(11)
C255460(20)8270(20)5696(12)45(10)
C2565720(20)8820(20)4475(12)58(11)
C257-728(17)6739(15)9538(9)19(8)
C258-4123(17)8402(15)11763(9)20(8)
C259-1334(19)9338(18)3620(10)33(9)
C262-8160(20)9370(20)8747(12)52(11)
C2633700(30)9560(20)5708(15)77(14)
C264-1850(20)9678(19)3450(11)37(9)
C2664270(20)8255(18)4567(12)40(10)
C267-7310(20)8222(19)7910(11)39(10)
O2691029(11)7926(10)3574(6)19(5)
C291-500(30)10680(30)10162(17)91(15)
C3074000(20)8157(16)234(10)33(9)
O238194(12)5084(11)502(7)32(6)
O4-4006(11)6387(11)9384(6)18(5)
O17-4039(10)7043(9)8564(5)14(4)
C2-4638(17)5571(17)9328(9)25(8)
C1-2969(16)6035(16)9924(9)18(7)
O1a-2589(14)5255(13)3926(8)49(7)
C8-3510(17)5671(16)9771(9)15(7)
C16-2393(18)5828(16)10163(9)23(8)
C4-2858(17)4914(17)10138(9)25(8)
C10890(18)5541(16)4527(10)27(8)
O1b3762(17)4100(16)5086(9)72(9)
C11-4097(16)5880(16)9480(8)8(7)
C6-2350(20)5285(19)10267(11)36(9)
C5-3461(18)5128(16)9862(9)23(8)
C13-1390(20)5060(20)4152(11)44(10)
C322950(30)5450(20)4864(14)73(13)
C21375(17)5961(18)4364(9)17(7)
C17-649(18)5217(17)4277(10)26(8)
C32080(20)4737(19)4648(11)39(9)
C33-3220(30)5590(30)3790(19)102(19)
C443290(30)4520(30)4952(15)77(14)
C7-5159(18)5764(17)9022(10)23(8)
C42-3470(30)6590(30)2530(19)105(18)
C92210(20)5280(20)4666(12)46(10)
C493450(20)5060(20)4997(13)58(12)
C72-8470(30)8420(30)7536(16)86(15)
C12-900(16)6128(15)4150(8)14(7)
C142620(20)4320(20)4793(12)51(11)
C15-1836(19)5447(18)4020(10)31(9)
C18-432(19)5752(18)4273(10)27(8)
C624520(30)4310(30)5213(16)89(15)
C191692(19)5707(18)4534(10)23(8)
C1a-1670(20)5990(20)4027(11)42(10)
C1c-1260(30)5450(20)10664(15)76(14)

 

Table 3 Bond Lengths for DC152.
AtomAtomLength/Å AtomAtomLength/Å
Ti1Ti43.450(9) C77C841.33(5)
Ti1Ti53.429(7) C77C1551.54(4)
Ti1O52.04(2) C77C1761.45(4)
Ti1O161.80(2) C78C1271.37(4)
Ti1O181.98(2) C78C1501.54(4)
Ti1O281.94(2) C79C1151.41(4)
Ti1O312.041(19) C79C2051.44(4)
Ti1O2691.794(18) C79C2101.49(4)
Ti2Ti33.442(9) C80C1441.45(5)
Ti2Ti63.435(9) C81C1631.44(5)
Ti2O82.07(3) C81C2111.31(5)
Ti2O291.967(17) O82C2001.45(4)
Ti2O341.83(2) O82C2391.51(5)
Ti2O562.06(2) C83C1321.36(4)
Ti2O42.01(2) C83C1601.46(4)
Ti2O171.768(19) C84C2531.42(5)
Ti3Ti63.441(6) C85C931.44(5)
Ti3O151.814(16) C86C871.54(4)
Ti3O202.068(17) C86C1681.28(4)
Ti3O211.995(18) C87C1111.40(4)
Ti3O341.79(2) C87C1251.31(5)
Ti3O492.011(18) C89C1801.40(5)
Ti3O552.07(3) C89C2191.43(5)
Ti4Ti53.431(8) C90C1141.34(5)
Ti4O121.96(3) C90C1821.41(5)
Ti4O161.84(2) C91C981.44(5)
Ti4O221.94(2) C91C1241.48(4)
Ti4O411.780(19) C92C2661.42(5)
Ti4O472.08(3) C94C1101.46(4)
Ti4O722.03(2) C95C1031.36(5)
Ti5O12.09(2) C95C1571.43(4)
Ti5O71.99(2) C96C1851.37(6)
Ti5O101.97(2) C96C2661.36(4)
Ti5O192.100(18) C97C1301.46(4)
Ti5O411.85(2) C97C1721.41(5)
Ti5O2691.832(19) C97C2591.47(5)
Ti6O22.09(2) C98C2151.43(4)
Ti6O32.103(16) C99C1691.34(4)
Ti6O151.813(16) C100C1591.40(5)
Ti6O241.987(19) C101C1361.31(4)
Ti6O361.977(18) C101C2181.43(4)
Ti6O171.91(2) C102C1911.44(5)
O1C1491.29(3) C102C2291.46(4)
O2C2071.29(3) C103C1221.41(5)
O3C1931.26(3) C104C1401.47(5)
O5C1301.32(4) C104C1871.47(5)
O6C951.37(4) C107C2351.42(6)
O6C1331.32(5) C108C1711.40(4)
O7C981.28(4) C108C1881.28(4)
O8C71.27(4) C111C2191.33(4)
O9C601.40(4) C113C1561.43(4)
O9C1121.46(3) C114C1781.47(4)
O10C1311.30(3) C114C71.54(5)
O11C461.30(4) C115C2571.36(4)
O11C3071.44(3) C116C1281.45(5)
O12C211.25(4) C116C2021.43(5)
O13C711.39(3) C117C1771.38(4)
O13C1471.44(5) C117C1901.44(6)
O14C941.41(4) C118C2311.46(5)
O14C1961.38(4) C118C2341.30(4)
O18C1991.24(3) C119C1721.43(5)
O19C1391.26(4) C119C2001.41(6)
O20C1231.28(3) C121C1591.42(5)
O21C2051.29(3) C123C1541.50(4)
O22C1211.34(3) C123C1641.34(4)
O24C811.34(3) C125C1801.43(4)
O26C1841.45(3) C127C1551.29(5)
O26C2221.41(3) C128C1771.49(5)
O27C1401.44(4) C129C1821.44(5)
O27C1791.42(5) C129C1861.37(5)
O28C861.36(4) C130C1681.44(4)
O29C1551.32(3) C132C1931.48(5)
O30C651.43(3) C134C1411.31(4)
O30C1091.48(4) C134C1991.47(4)
O31C1411.30(3) C135C2211.30(3)
O32C1421.40(3) C135C2221.44(4)
O32C2341.50(4) C136C1671.41(4)
O33C1701.40(3) C138C2441.36(4)
O33C2511.34(3) C138C2461.36(5)
C35C1001.55(5) C139C2151.47(5)
C35C1221.40(4) C140C2041.22(3)
C35C1891.29(5) C141C1741.54(4)
O36C831.30(3) C145C1741.50(5)
C37C1131.39(5) C145C2181.44(4)
C37C1511.49(5) C146C2171.38(4)
C37C1931.39(3) C148C1631.42(5)
O38C1011.43(3) C148C2041.45(5)
O38C1651.46(4) C150C1921.34(4)
O39C1951.43(4) C154C2141.43(4)
O39C2621.53(5) C154C2211.35(4)
O40C1291.36(4) C157C1891.44(5)
O40C2541.49(4) C160C1981.43(4)
O42C511.35(4) C160C2311.40(4)
O42C2551.42(4) C163C1871.42(4)
C43C991.33(5) C164C2051.41(4)
C43C1391.46(4) C167C1741.32(4)
C43C1531.54(5) C173C1941.46(4)
O44C1081.42(4) C173C2481.35(5)
O44C2271.43(4) C175C1911.40(5)
C46C541.47(4) C176C2091.36(5)
C46C851.38(5) C177C2171.36(5)
O47C191.27(4) C178C1861.41(5)
O48C961.35(4) C185C2241.47(6)
O48C2561.46(5) C188C1921.42(5)
O49C571.31(4) C190C2021.39(6)
C50C741.48(5) C194C1991.46(5)
C50C1311.51(5) C194C2461.39(4)
C50C1621.35(4) C195C2291.48(6)
C51C801.36(4) C198C2161.38(5)
C51C1071.39(5) C200C2641.37(6)
C52C931.33(4) C207C2111.42(5)
C52C1491.40(4) C208C2101.36(4)
C52C1831.41(5) C208C2511.40(4)
C53C1501.41(4) C209C2671.57(6)
C53C1711.41(5) C214C2581.38(4)
C54C1831.52(5) C216C2341.35(4)
O55C2171.29(4) C222C2581.31(4)
O56C781.28(3) C244C2481.37(4)
C57C1461.40(5) C251C2571.35(4)
C57C1911.44(4) C253C2671.28(4)
O58C2441.41(4) C259C2641.36(5)
O58C421.55(5) O23C611.33(4)
C59C941.38(5) O23C1c11.44(5)
C59C1621.36(5) O4C111.28(4)
C60C611.31(4) C2C111.33(5)
C60C1201.48(4) C2C71.43(4)
C61C1241.40(5) C1C81.41(5)
O63C891.40(4) C1C161.38(4)
O63C2631.35(4) O1aC331.45(5)
C64C651.34(4) O1aC151.44(4)
C64C1531.40(4) C8C111.49(4)
C65C1691.37(5) C8C51.36(5)
C66C1311.35(5) C16C61.37(5)
C66C1491.44(4) C4C61.35(5)
O67C2671.30(4) C4C51.49(4)
O67C721.47(5) C10C211.47(5)
O68C2021.44(6) C10C191.44(5)
O68C2911.46(5) O1bC441.39(6)
C69C711.45(5) O1bC621.50(6)
C69C1511.39(4) C13C171.43(5)
C70C1751.31(4) C13C151.31(5)
C70C1951.37(5) C32C91.52(6)
C71C1561.42(5) C32C491.38(6)
O72C1001.29(3) C21C181.54(5)
C73C911.38(5) C17C181.36(5)
C73C1201.39(5) C3C91.36(6)
C74C1101.31(5) C3C141.47(5)
C75C921.34(5) C44C491.36(7)
C75C1211.49(5) C44C141.40(6)
C75C2241.46(5) C9C191.45(5)
C76C1441.37(5) C12C181.30(4)
C76C2071.45(5) C12C1a1.47(5)
C76C2351.42(5) C15C1a1.36(6)

11+X,+Y,-1+Z

 

Table 4 Bond Angles for DC152.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Ti5Ti1Ti459.84(16) C144C80C51119(4)
O5Ti1Ti4170.9(6) C163C81O24113(3)
O5Ti1Ti5111.5(6) C211C81O24122(3)
O16Ti1Ti418.8(6) C211C81C163125(3)
O16Ti1Ti578.6(6) C239O82C200111(3)
O16Ti1O5168.7(8) C132C83O36125(3)
O18Ti1Ti499.1(7) C160C83O36114(2)
O18Ti1Ti594.0(5) C160C83C132121(2)
O18Ti1O583.9(9) C253C84C77121(3)
O18Ti1O16100.8(10) C93C85C46124(3)
O28Ti1Ti496.4(6) C87C86O28113(2)
O28Ti1Ti5100.2(6) C168C86O28122(3)
O28Ti1O581.9(9) C168C86C87125(3)
O28Ti1O1691.5(9) C111C87C86117(3)
O28Ti1O18162.9(8) C125C87C86121(2)
O31Ti1Ti4110.9(7) C125C87C111121(3)
O31Ti1Ti5169.8(8) C180C89O63116(3)
O31Ti1O577.9(9) C219C89O63123(3)
O31Ti1O1692.4(9) C219C89C180121(3)
O31Ti1O1883.1(8) C182C90C114121(3)
O31Ti1O2884.6(8) C98C91C73125(3)
O269Ti1Ti479.1(7) C124C91C73118(3)
O269Ti1Ti519.2(7) C124C91C98117(3)
O269Ti1O592.4(9) C266C92C75118(3)
O269Ti1O1697.8(9) C85C93C52121(4)
O269Ti1O1890.3(8) C59C94O14119(2)
O269Ti1O2899.8(9) C110C94O14121(3)
O269Ti1O31168.7(8) C110C94C59120(4)
Ti6Ti2Ti360.06(17) C103C95O6117(2)
O8Ti2Ti3169.7(6) C157C95O6120(3)
O8Ti2Ti6110.9(6) C157C95C103123(3)
O29Ti2Ti398.4(7) C185C96O48114(3)
O29Ti2Ti692.8(6) C266C96O48128(3)
O29Ti2O886.4(8) C266C96C185118(4)
O34Ti2Ti318.2(7) C172C97C130123(3)
O34Ti2Ti678.1(7) C259C97C130116(3)
O34Ti2O8168.3(10) C259C97C172121(3)
O34Ti2O29100.8(9) C91C98O7118(2)
O56Ti2Ti3109.3(6) C215C98O7123(3)
O56Ti2Ti6168.1(7) C215C98C91119(3)
O56Ti2O880.1(9) C169C99C43122(4)
O56Ti2O2983.1(8) O72C100C35116(3)
O56Ti2O3491.6(9) C159C100C35121(2)
O4Ti2Ti396.2(7) C159C100O72123(3)
O4Ti2Ti698.7(6) C136C101O38115(3)
O4Ti2O880.0(9) C218C101O38120(2)
O4Ti2O29164.6(10) C218C101C136125(3)
O4Ti2O3491.5(9) C229C102C191122(3)
O4Ti2O5687.5(8) C122C103C95120(3)
O17Ti2Ti381.7(7) C187C104C140114(3)
O17Ti2Ti621.7(7) C235C107C51118(3)
O17Ti2O889.4(9) C171C108O44121(3)
O17Ti2O2988.4(8) C188C108O44115(3)
O17Ti2O3499.8(10) C188C108C171124(3)
O17Ti2O56166.9(8) C94C110C74117(3)
O17Ti2O498.5(8) C219C111C87122(4)
Ti6Ti3Ti259.87(16) C156C113C37124(3)
O15Ti3Ti278.3(7) C178C114C90124(3)
O15Ti3Ti618.4(7) C7C114C90126(3)
O20Ti3Ti2109.4(7) C7C114C178110(3)
O20Ti3Ti6166.9(8) C257C115C79122(2)
O20Ti3O15168.7(8) C202C116C128112(4)
O21Ti3Ti297.9(7) C190C117C177124(4)
O21Ti3Ti691.0(5) C234C118C231115(3)
O21Ti3O1587.8(7) C200C119C172113(4)
O21Ti3O2082.9(7) C73C120C60115(3)
O34Ti3Ti218.6(5) C75C121O22116(3)
O34Ti3Ti678.4(6) C159C121O22120(3)
O34Ti3O1596.7(9) C159C121C75124(3)
O34Ti3O2090.8(9) C103C122C35117(3)
O34Ti3O2196.2(9) C154C123O20113(2)
O49Ti3Ti290.2(6) C164C123O20123(3)
O49Ti3Ti697.5(5) C164C123C154124(2)
O49Ti3O1598.8(7) C91C124C61118(3)
O49Ti3O2089.7(7) C180C125C87121(3)
O49Ti3O21170.5(8) C155C127C78128(3)
O49Ti3O3489.8(9) C177C128C116125(3)
O55Ti3Ti2166.1(5) C182C129O40111(4)
O55Ti3Ti6110.7(6) C186C129O40128(3)
O55Ti3O1592.7(9) C186C129C182121(3)
O55Ti3O2081.2(9) C97C130O5118(2)
O55Ti3O2192.3(9) C168C130O5120(3)
O55Ti3O34167.5(8) C168C130C97123(3)
O55Ti3O4980.7(9) C50C131O10117(3)
Ti5Ti4Ti159.77(16) C66C131O10122(3)
O12Ti4Ti189.0(7) C66C131C50121(2)
O12Ti4Ti596.9(6) C193C132C83122(3)
O16Ti4Ti118.4(6) C199C134C141122(3)
O16Ti4Ti578.0(7) C222C135C221117(3)
O16Ti4O1288.3(10) C167C136C101120(3)
O22Ti4Ti1100.1(8) C246C138C244121(3)
O22Ti4Ti591.7(7) C43C139O19115(3)
O22Ti4O12169.8(11) C215C139O19125(2)
O22Ti4O1698.8(10) C215C139C43120(3)
O41Ti4Ti179.2(6) C104C140O27105(2)
O41Ti4Ti519.6(7) C204C140O27129(4)
O41Ti4O1296.1(9) C204C140C104125(3)
O41Ti4O1697.6(9) C134C141O31128(2)
O41Ti4O2290.1(9) C174C141O31115(2)
O47Ti4Ti1167.4(5) C174C141C134117(2)
O47Ti4Ti5111.0(6) C80C144C76121(3)
O47Ti4O1283.6(11) C218C145C174116(3)
O47Ti4O16168.5(12) C217C146C57128(3)
O47Ti4O2288.3(10) C204C148C163120(3)
O47Ti4O4191.5(9) C52C149O1124(3)
O72Ti4Ti1108.1(6) C66C149O1118(2)
O72Ti4Ti5165.5(7) C66C149C52118(2)
O72Ti4O1290.4(9) C78C150C53115(2)
O72Ti4O1689.7(8) C192C150C53121(3)
O72Ti4O2282.4(9) C192C150C78125(2)
O72Ti4O41170.3(8) C69C151C37123(3)
O72Ti4O4782.2(9) C64C153C43115(3)
Ti4Ti5Ti160.40(16) C214C154C123120(3)
O1Ti5Ti1112.2(5) C221C154C123123(2)
O1Ti5Ti4168.9(6) C221C154C214117(2)
O7Ti5Ti192.0(5) C77C155O29111(3)
O7Ti5Ti498.1(6) C127C155O29122(2)
O7Ti5O190.2(9) C127C155C77125(3)
O10Ti5Ti197.4(5) C113C156C71115(3)
O10Ti5Ti492.8(7) C189C157C95112(3)
O10Ti5O179.6(9) C121C159C100123(3)
O10Ti5O7168.2(8) C198C160C83118(2)
O19Ti5Ti1169.0(5) C231C160C83123(2)
O19Ti5Ti4110.9(6) C231C160C198118(3)
O19Ti5O177.5(7) C59C162C50121(3)
O19Ti5O782.4(8) C148C163C81121(3)
O19Ti5O1089.5(8) C187C163C81120(3)
O41Ti5Ti179.1(6) C187C163C148118(3)
O41Ti5Ti418.8(5) C205C164C123126(2)
O41Ti5O1164.5(9) C174C167C136121(3)
O41Ti5O7100.4(9) C130C168C86126(4)
O41Ti5O1088.5(10) C99C169C65121(4)
O41Ti5O1992.6(8) C108C171C53118(3)
O269Ti5Ti118.8(6) C119C172C97122(3)
O269Ti5Ti479.2(7) C248C173C194120(3)
O269Ti5O193.5(8) C145C174C141113(3)
O269Ti5O790.0(9) C167C174C141126(3)
O269Ti5O1096.6(8) C167C174C145122(3)
O269Ti5O19168.1(11) C191C175C70125(4)
O269Ti5O4197.8(9) C209C176C77118(4)
Ti3Ti6Ti260.07(17) C128C177C117115(3)
O2Ti6Ti2168.2(5) C217C177C117122(4)
O2Ti6Ti3110.1(5) C217C177C128122(3)
O3Ti6Ti2111.7(7) C186C178C114113(4)
O3Ti6Ti3169.2(5) C125C180C89116(4)
O3Ti6O278.9(8) C129C182C90117(4)
O15Ti6Ti278.5(7) C54C183C52124(3)
O15Ti6Ti318.4(7) C224C185C96121(3)
O15Ti6O291.7(8) C178C186C129124(3)
O15Ti6O3167.6(10) C163C187C104120(4)
O24Ti6Ti290.8(6) C192C188C108118(3)
O24Ti6Ti397.4(5) C157C189C35124(3)
O24Ti6O283.9(8) C202C190C117117(4)
O24Ti6O389.4(7) C102C191C57115(3)
O24Ti6O1597.7(7) C175C191C57128(3)
O36Ti6Ti296.1(6) C175C191C102117(3)
O36Ti6Ti392.6(5) C188C192C150121(3)
O36Ti6O290.6(9) C37C193O3123(3)
O36Ti6O381.0(7) C132C193O3119(2)
O36Ti6O1591.1(7) C132C193C37118(3)
O36Ti6O24169.7(7) C199C194C173117(3)
O17Ti6Ti220.1(5) C246C194C173116(3)
O17Ti6Ti380.1(5) C246C194C199127(3)
O17Ti6O2168.3(8) C70C195O39115(3)
O17Ti6O391.7(8) C229C195O39120(3)
O17Ti6O1598.5(8) C229C195C70125(3)
O17Ti6O2489.1(9) C216C198C160120(3)
O17Ti6O3694.8(8) C134C199O18119(2)
C149O1Ti5131(2) C194C199O18120(2)
C207O2Ti6125(2) C194C199C134121(3)
C193O3Ti6130(2) C119C200O82110(4)
C130O5Ti1132.0(15) C264C200O82124(3)
C133O6C95116(2) C264C200C119126(3)
C98O7Ti5135.0(18) C116C202O68106(4)
C7O8Ti2130.4(17) C190C202O68128(3)
C112O9C60113(2) C190C202C116126(4)
C131O10Ti5135(2) C148C204C140122(4)
C307O11C46118(3) C79C205O21113(2)
C21O12Ti4132.7(17) C164C205O21121(2)
C147O13C71118(3) C164C205C79125(2)
C196O14C94117(2) C76C207O2117(3)
Ti6O15Ti3143.2(13) C211C207O2122(3)
Ti4O16Ti1142.8(11) C211C207C76121(3)
C199O18Ti1136.7(18) C251C208C210119(2)
C139O19Ti5127(2) C267C209C176119(3)
C123O20Ti3131.6(18) C208C210C79123(3)
C205O21Ti3133.9(17) C207C211C81127(3)
C121O22Ti4137(2) C258C214C154118(3)
C81O24Ti6131.0(19) C139C215C98120(3)
C222O26C184117(2) C234C216C198117(3)
C179O27C140110(2) C146C217O55118(3)
C86O28Ti1134.4(16) C177C217O55118(3)
C155O29Ti2131(2) C177C217C146123(3)
C109O30C65113(3) C145C218C101116(3)
C141O31Ti1128.0(15) C111C219C89118(3)
C234O32C142114(2) C154C221C135125(2)
C251O33C170115(2) C135C222O26124(2)
Ti3O34Ti2143.2(11) C258C222O26116(2)
C122C35C100117(3) C258C222C135120(2)
C189C35C100120(2) C185C224C75116(4)
C189C35C122122(3) C195C229C102112(3)
C83O36Ti6131.8(16) C160C231C118120(3)
C151C37C113117(3) C118C234O32109(2)
C193C37C113121(3) C216C234O32121(2)
C193C37C151121(3) C216C234C118129(3)
C165O38C101116(2) C107C235C76121(5)
C262O39C195117(3) C138C244O58126(3)
C254O40C129110(3) C248C244O58113(3)
Ti5O41Ti4141.7(11) C248C244C138120(3)
C255O42C51121(3) C194C246C138121(3)
C139C43C99128(3) C244C248C173121(3)
C153C43C99118(3) C208C251O33113(2)
C153C43C139114(3) C257C251O33129(3)
C227O44C108118(2) C257C251C208118(3)
C54C46O11113(4) C267C253C84122(4)
C85C46O11128(3) C251C257C115124(3)
C85C46C54119(3) C222C258C214122(3)
C19O47Ti4127.0(19) C264C259C97116(4)
C256O48C96115(3) C259C264C200122(4)
C57O49Ti3133.0(17) C96C266C92125(4)
C131C50C74118(2) C209C267O67119(3)
C162C50C74117(4) C253C267O67123(4)
C162C50C131124(3) C253C267C209118(3)
C80C51O42115(4) Ti5O269Ti1142.0(12)
C107C51O42121(3) C1c1O23C61119(4)
C107C51C80123(3) C11O4Ti2133.8(17)
C149C52C93123(4) Ti6O17Ti2138.2(11)
C183C52C93118(3) C7C2C11124(4)
C183C52C149118(3) C16C1C8119(4)
C171C53C150118(3) C15O1aC33126(4)
C183C54C46113(4) C11C8C1120(4)
C217O55Ti3134(2) C5C8C1120(3)
C78O56Ti2129.7(16) C5C8C11120(3)
C146C57O49121(3) C6C16C1122(3)
C191C57O49116(3) C5C4C6116(4)
C191C57C146122(3) C19C10C21115(4)
C42O58C244116(3) C62O1bC44111(5)
C162C59C94121(3) C2C11O4124(3)
C61C60O9128(3) C8C11O4112(3)
C120C60O9109(3) C8C11C2124(4)
C120C60C61123(3) C16C6O232122(3)
C124C61C60122(3) C4C6O232115(4)
C263O63C89122(3) C4C6C16123(3)
C153C64C65121(3) C4C5C8121(3)
C64C65O30124(3) C15C13C17117(4)
C169C65O30114(3) C49C32C9120(5)
C169C65C64122(3) C10C21O12127(3)
C149C66C131125(3) C18C21O12118(3)
C72O67C267123(4) C18C21C10115(4)
C291O68C202110(4) C18C17C13121(3)
C151C69C71116(3) C14C3C9123(3)
C195C70C175119(4) C49C44O1b124(4)
C69C71O13122(3) C14C44O1b112(5)
C156C71O13112(3) C14C44C49124(5)
C156C71C69125(3) C114C7O8119(3)
C100O72Ti4135(2) C2C7O8121(3)
C120C73C91124(3) C2C7C114119(4)
C110C74C50123(3) C3C9C32116(4)
C121C75C92119(3) C19C9C32119(4)
C224C75C92122(4) C19C9C3125(3)
C224C75C121119(4) C44C49C32121(4)
C207C76C144123(3) C1aC12C18121(4)
C235C76C144119(3) C44C14C3116(5)
C235C76C207118(4) C13C15O1a113(4)
C155C77C84120(3) C1aC15O1a121(3)
C176C77C84121(3) C1aC15C13125(4)
C176C77C155118(3) C17C18C21125(3)
C127C78O56122(3) C12C18C21115(4)
C150C78O56115(2) C12C18C17120(3)
C150C78C127123(2) C10C19O47128(3)
C205C79C115121(2) C9C19O47117(3)
C210C79C115111(3) C9C19C10115(4)
C210C79C205124(2) C15C1aC12115(3)

11+X,+Y,-1+Z; 2-1+X,+Y,1+Z

 

Table 5 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for DC152.
AtomxyzU(eq)
H259-1385(19)8961(18)3613(10)40(10)
H264-2270(20)9530(19)3325(11)44(11)
H119-1170(20)10900(20)3658(11)55(12)
H172-240(17)10329(15)3977(9)24(9)
H246-2789(19)7588(17)3827(10)37(11)
H138-3300(20)7199(19)3226(11)52(12)
H248-1210(20)6580(18)2686(11)43(11)
H173-623(18)7056(15)3209(9)24(9)
H1251158(17)10106(15)4778(9)19(9)
H1802152(19)10443(18)5188(10)45(11)
H2192900(20)8862(18)5288(10)40(11)
H1111911(16)8594(16)4904(9)24(9)
H167-2855(18)8158(16)5003(10)30(10)
H136-3540(20)8509(16)5706(10)33(10)
H218-1535(18)9106(16)6058(10)29(10)
H145-810(20)8796(16)5317(10)32(10)
H12-741(16)6490(15)4141(8)17(8)
H1a-2030(20)6260(20)3958(11)51(12)
H13-1540(20)4700(20)4164(11)53(12)
H17-309(18)4951(17)4363(10)31(10)
H2243480(20)7580(20)5687(13)64(13)
H1854770(20)7999(19)5559(11)42(11)
H2664460(20)8428(18)4285(12)48(11)
H923296(18)7936(17)4331(10)28(10)
H31620(20)4620(19)4540(11)47(11)
H142510(20)3950(20)4779(12)61(13)
H493900(20)5160(20)5119(13)69(14)
H323060(30)5820(20)4896(14)87(16)
H189203(18)6274(16)5659(9)24(9)
H157-461(18)5840(16)6354(9)29(9)
H1031034(18)6665(17)7056(10)29(10)
H1221701(19)7022(16)6342(9)30(10)
H1832301(18)8571(18)2055(10)33(10)
H543016(19)9010(19)1343(10)44(11)
H853202(17)7473(17)787(9)23(9)
H932393(17)7121(16)1445(9)27(9)
H1242610(20)8885(16)3889(10)31(10)
H613145(18)9639(16)4210(9)20(9)
H1205277(19)9366(15)3415(9)26(9)
H734763(18)8607(17)3092(10)29(10)
H162663(17)6305(15)1870(9)21(9)
H59-173(17)5598(16)1837(9)20(9)
H110-516(17)5470(15)3261(9)23(9)
H74378(18)6135(17)3277(10)29(10)
H1534331(17)7862(16)1981(9)29(9)
H644974(16)7454(14)1284(9)16(8)
H1694365(16)5979(16)1766(9)22(9)
H993698(17)6319(16)2443(10)26(9)
H178-6337(16)6045(16)8610(9)23(9)
H186-7309(19)5492(17)8353(9)30(10)
H182-6240(20)4110(19)8703(11)49(11)
H90-5294(18)4651(17)8996(9)28(10)
H176-7810(20)7354(17)8821(11)40(11)
H209-8390(20)7824(19)8264(11)54(12)
H253-6240(20)8428(17)7698(10)38(10)
H84-5674(19)7885(16)8220(9)25(9)
H192-7876(19)6832(17)10025(10)32(10)
H188-8570(20)6427(18)10706(10)42(11)
H171-6537(18)5924(16)11058(10)29(10)
H53-5837(19)6246(16)10333(10)31(10)
H5-3806(18)4887(16)9751(9)28(9)
H4-2831(17)4547(17)10216(9)30(10)
H16-2025(18)6066(16)10255(9)27(9)
H1-2998(16)6407(16)9864(9)22(9)
H221-4857(16)8719(14)10686(9)13(9)
H135-5370(17)9164(16)11336(9)23(9)
H258-3957(17)8309(15)12045(9)24(9)
H214-3268(19)7976(17)11346(10)36(10)
H210-1460(20)7414(18)10644(11)42(11)
H208-266(18)6971(16)10551(9)24(9)
H257-545(17)6557(15)9258(9)22(9)
H115-1715(17)7000(15)9327(9)19(9)
H175-5370(20)10085(18)9352(10)42(11)
H70-6514(17)10336(16)9159(9)22(9)
H229-7070(20)8728(18)8945(10)46(11)
H102-5797(16)8491(16)9162(9)20(9)
H128-3412(18)10390(16)9562(9)25(9)
H116-2470(18)11044(18)9747(10)37(10)
H190-1130(20)9750(20)10086(12)60(13)
H117-2040(20)9130(20)9853(11)55(12)
H235-750(20)7160(20)6976(13)73(14)
H107-37(19)7548(18)6284(10)35(10)
H80-676(18)9050(18)6761(10)40(10)
H144-1428(18)8665(17)7451(10)28(9)
H151-2477(17)7912(16)6460(9)27(9)
H69-1748(16)7571(14)5769(9)18(8)
H156-1990(16)6013(16)6340(9)23(9)
H113-2693(18)6398(16)7034(10)28(9)
H187-228(19)6433(17)8080(10)36(10)
H104300(19)5608(16)8395(9)29(10)
H204-1789(19)5336(15)9177(10)24(9)
H148-2357(19)6115(17)8871(10)30(10)
H231-4313(18)8728(17)6856(10)32(10)
H118-5188(18)9508(16)6850(10)33(10)
H216-5492(18)9562(16)8239(10)30(10)
H198-4722(18)8777(16)8278(10)31(10)
H661421(15)6943(14)1932(8)9(8)
H10a5560(80)6610(20)390(16)42(13)
H10b5100(40)7100(40)650(40)42(13)
H10c5930(50)6930(50)770(30)42(13)
H11a3800(100)10530(60)4345(10)50(13)
H11b3870(100)9990(20)4630(40)50(13)
H11c4520(20)10440(80)4610(40)50(13)
H127-7189(19)7072(16)9357(9)24(9)
H132-3611(17)8057(16)6919(10)29(10)
H134-2187(18)8025(15)4353(9)25(9)
H14a-6630(100)10550(50)7820(20)52(14)
H14b-6720(90)9940(30)8000(40)52(14)
H14c-6020(20)10310(100)8120(30)52(14)
H146-4291(17)9768(16)9606(9)27(9)
H14d-840(100)6630(20)4960(20)67(15)
H14e-1380(40)7120(50)5170(50)67(15)
H14f-550(70)7020(60)5330(30)67(15)
H1592380(19)7164(17)5712(10)34(10)
H164-2586(18)7892(16)10666(10)26(10)
H16a-2460(80)9680(40)6470(19)32(12)
H16b-3080(20)9490(60)6900(30)32(12)
H16c-2300(70)9150(20)6750(50)32(12)
H168303(18)9773(17)4429(10)37(10)
H17a700(110)6450(30)9210(14)45(13)
H17b1270(40)6110(90)9470(30)45(13)
H17c430(80)5880(40)9420(30)45(13)
H17d-1140(100)4450(70)9266(13)90(18)
H17e-440(30)4520(80)9550(50)90(18)
H17f-1100(110)4980(20)9570(40)90(18)
H18a-5630(30)9560(30)12050(50)34(12)
H18b-6230(40)9070(20)12110(60)34(12)
H18c-5980(80)9350(70)12555(12)34(12)
H19a-1710(70)4550(60)2823(10)49(13)
H19b-980(30)4600(70)3080(30)49(13)
H19c-1560(80)5099(17)3070(30)49(13)
H211-829(19)6993(16)7741(9)27(10)
H21a3861(18)8126(16)2610(10)29(10)
H21b4281(18)7803(16)2967(10)29(10)
H22a-7580(120)5280(30)11520(40)66(15)
H22b-7200(70)5810(50)11680(60)66(15)
H22c-8020(60)5610(80)11950(30)66(15)
H23a-2730(80)10320(90)2713(13)85(17)
H23b-2960(100)9950(40)3160(60)85(17)
H23c-3410(40)10500(60)3110(70)85(17)
H25d-7610(60)4770(100)7730(30)82(17)
H25e-8350(70)4490(50)8020(80)82(17)
H25f-8040(120)5050(50)8190(50)82(17)
H25g510(120)8480(30)5410(20)67(15)
H25h970(60)8180(100)5770(40)67(15)
H25i180(80)7940(40)5660(50)67(15)
H25a5830(130)8540(20)4240(20)86(17)
H25b5350(60)9080(70)4380(40)86(17)
H25c6200(80)9000(80)4510(20)86(17)
H26d-8010(80)9300(70)8417(19)78(16)
H26e-8130(90)9030(40)8920(50)78(16)
H26f-8690(30)9510(40)8810(70)78(16)
H26a3940(150)9320(100)5470(40)120(20)
H26b4100(100)9780(30)5810(100)120(20)
H26c3430(40)9360(90)5970(80)120(20)
H29a-340(110)10370(100)9960(90)140(20)
H29b-120(60)10960(50)10100(140)140(20)
H29c-540(60)10560(150)10480(40)140(20)
H30a4300(100)8380(20)0(30)49(13)
H30b4340(100)7890(60)342(16)49(13)
H30c3590(20)7980(70)100(50)49(13)
H2-4680(17)5209(17)9425(9)30(10)
H10d658(18)5430(16)4842(10)32(10)
H10e899(18)5224(16)4325(10)32(10)
H33a-3010(50)5810(130)3530(110)150(30)
H33b-3620(120)5360(30)3700(150)150(30)
H33c-3440(190)5820(150)4050(60)150(30)
H42a-3640(80)6290(120)2350(140)160(30)
H42b-3780(40)6590(170)2840(20)160(30)
H42c-3550(50)6930(110)2380(140)160(30)
H72a-8590(70)8660(90)7290(90)130(20)
H72b-8550(50)8050(30)7450(120)130(20)
H72c-8810(30)8500(150)7820(40)130(20)
H62a4610(100)4680(50)5090(100)130(20)
H62b4480(80)4320(130)5548(16)130(20)
H62c4950(40)4080(80)5080(100)130(20)
H1ca-1080(130)5720(70)10420(40)110(20)
H1cb-1510(60)5630(90)10940(60)110(20)
H1cc-810(80)5250(30)10730(90)110(20)

Experimental

Single crystals of C20H40O8Ti [DC152] were [. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at N/A K during data collection. Using Olex2 [1], the structure was solved with the ShelXS [2] structure solution program using Direct Methods and refined with the olex2.refine [3] refinement package using Gauss-Newton minimisation.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
  2. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
  3. Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H. (2013). in preparation

Crystal structure determination of [DC152]

Crystal Data for C20H40O8Ti (=360.18): triclinic, space group P-1 (no. 2), a = 17.125(5) Å, b = 24.491(6) Å, c = 28.844(8) Å, α = 89.890(7)°, β = 80.815(6)°, γ = 89.601(8)°, = 11942(5) Å3, Z = 21, T = N/A K, μ(Mo Kα) = 0.257 mm-1, Dcalc = 1.0517 g/mm3, 46548 reflections measured (2.2 ≤ 2Θ ≤ 41.88), 15614 unique (Rint = 0.0824, Rsigma = 0.0991) which were used in all calculations. The final R1 was 0.2463 (I>=2u(I)) and wR2 was 0.6206 (all data).

Refinement model description

Number of restraints - 0, number of constraints - 310.

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
3.a Secondary CH2 refined with riding coordinates:
C215(H21a,H21b), C10(H10d,H10e)
3.b Aromatic/amide H refined with riding coordinates:
C259(H259), C264(H264), C119(H119), C172(H172), C246(H246), C138(H138),
C248(H248), C173(H173), C125(H125), C180(H180), C219(H219), C111(H111),
C167(H167), C136(H136), C218(H218), C145(H145), C12(H12), C1a(H1a), C13(H13),
C17(H17), C224(H224), C185(H185), C266(H266), C92(H92), C3(H3), C14(H14),
C49(H49), C32(H32), C189(H189), C157(H157), C103(H103), C122(H122), C183(H183),
C54(H54), C85(H85), C93(H93), C124(H124), C61(H61), C120(H120), C73(H73),
C162(H162), C59(H59), C110(H110), C74(H74), C153(H153), C64(H64), C169(H169),
C99(H99), C178(H178), C186(H186), C182(H182), C90(H90), C176(H176), C209(H209),
C253(H253), C84(H84), C192(H192), C188(H188), C171(H171), C53(H53), C5(H5),
C4(H4), C16(H16), C1(H1), C221(H221), C135(H135), C258(H258), C214(H214),
C210(H210), C208(H208), C257(H257), C115(H115), C175(H175), C70(H70),
C229(H229), C102(H102), C128(H128), C116(H116), C190(H190), C117(H117),
C235(H235), C107(H107), C80(H80), C144(H144), C151(H151), C69(H69), C156(H156),
C113(H113), C187(H187), C104(H104), C204(H204), C148(H148), C231(H231),
C118(H118), C216(H216), C198(H198), C66(H66), C127(H127), C132(H132),
C134(H134), C146(H146), C159(H159), C164(H164), C168(H168), C211(H211), C2(H2)
3.c Idealised Me refined as rotating group:
C109(H10a,H10b,H10c), C112(H11a,H11b,H11c), C142(H14a,H14b,H14c), C147(H14d,
H14e,H14f), C165(H16a,H16b,H16c), C170(H17a,H17b,H17c), C179(H17d,H17e,H17f),
C184(H18a,H18b,H18c), C196(H19a,H19b,H19c), C227(H22a,H22b,H22c), C239(H23a,
H23b,H23c), C254(H25d,H25e,H25f), C255(H25g,H25h,H25i), C256(H25a,H25b,H25c),
C262(H26d,H26e,H26f), C263(H26a,H26b,H26c), C291(H29a,H29b,H29c), C307(H30a,
H30b,H30c), C33(H33a,H33b,H33c), C42(H42a,H42b,H42c), C72(H72a,H72b,H72c),
C62(H62a,H62b,H62c), C1c(H1ca,H1cb,H1cc)

This report has been created with Olex2, compiled on 2013.11.15 svn.r2834 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.