3Cl-decomposition

Table 1 Crystal data and structure refinement for 3Cl-decomposition.
Identification code 3Cl-decomposition
Empirical formula C84H78.63Cl9.37N4O12
Formula weight 1668.30
Temperature/K 293(2)
Crystal system triclinic
Space group P-1
a/Å 7.4241(5)
b/Å 12.4935(9)
c/Å 20.8699(12)
α/° 84.241(6)
β/° 83.819(5)
γ/° 83.303(6)
Volume/Å3 1903.8(2)
Z 1
ρcalcg/cm3 1.455
μ/mm‑1 3.698
F(000) 866.0
Crystal size/mm3 0.15 × 0.1 × 0.1
Radiation CuKα (λ = 1.54178)
2Θ range for data collection/° 7.152 to 125.404
Index ranges -6 ≤ h ≤ 8, -14 ≤ k ≤ 14, -23 ≤ l ≤ 23
Reflections collected 10253
Independent reflections 5920 [Rint = 0.0430, Rsigma = 0.0805]
Data/restraints/parameters 5920/105/515
Goodness-of-fit on F2 1.027
Final R indexes [I>=2σ (I)] R1 = 0.0919, wR2 = 0.2285
Final R indexes [all data] R1 = 0.1370, wR2 = 0.2651
Largest diff. peak/hole / e Å-3 0.46/-0.41

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3Cl-decomposition. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Cl0A4060(2)6460.9(13)1745.8(8)63.1(5)
Cl26425(2)10245.8(14)723.4(7)62.7(5)
Cl15529(3)7963.4(15)553.6(8)74.0(6)
Cl6A9195(3)6497.6(15)1602.4(9)68.0(5)
Cl3A11300(3)10460.0(16)844.2(9)69.4(6)
Cl310541(3)8172.5(18)527.9(9)80.4(6)
O9AA7888(5)7812(3)4048.7(17)57.1(9)
O1BA3082(5)7659(3)3767.7(18)62.6(10)
O2AA10283(5)11517(3)3979.4(17)57.5(9)
O5AA5440(5)11543(3)3178.3(17)65.9(10)
O7AA3827(4)8166(3)4685.8(16)52.8(9)
O410021(6)11493(3)2928.8(19)72.2(11)
N8AA5681(5)10797(3)2215(2)51.5(11)
C0BA4299(6)8099(4)2439(2)51.5(13)
C2BA5344(6)9815(4)2004(2)48.3(12)
C54751(6)9858(4)4357(2)47.7(12)
C64436(6)9080(4)4875(2)47.7(12)
C74712(6)9121(4)2544(2)47.4(12)
C810127(6)10779(4)4524(2)46.6(12)
N98672(5)7458(3)2993(2)50.3(10)
C109296(6)8056(4)2426(2)50.3(13)
C1110297(6)9810(4)2064(3)53.4(14)
C129341(6)9124(4)3264(2)48.0(13)
C135325(6)10829(4)4496(2)48.7(12)
C149713(6)9778(4)4374(2)50.7(13)
C159652(6)9084(4)2566(2)47.4(12)
C169627(6)9861(4)3670(2)48.7(12)
C174406(6)9375(4)3771(2)47.9(12)
C184714(6)9690(4)3132(2)46.6(12)
C195185(8)8441(4)1303(3)62.6(15)
C205583(7)9471(4)1388(2)55.9(14)
C214549(7)7756(4)1831(3)60.5(15)
C2210567(8)9532(5)1445(3)64.3(16)
C238562(6)8073(4)3504(3)50.7(13)
C245309(7)10786(4)2874(3)52.7(13)
C259585(7)7752(4)1804(3)60.7(15)
C2610211(8)8503(5)1299(3)66.4(16)
C279573(6)8951(4)4880(2)52.7(13)
C2810008(7)11011(4)3453(3)56.4(14)
C293729(6)8316(4)4035(3)52.2(13)
C307894(7)6417(4)3083(3)58.7(14)
C316256(7)11769(4)1839(3)60.3(15)
C339158(8)5465(5)3240(4)121(3)
C343097(11)12800(8)1951(5)99(3)
C354761(9)12479(6)1516(4)105(3)
C361461(11)13300(7)1585(5)138(3)
C375511(12)13536(7)1188(6)169(4)
C387118(12)4160(7)2913(5)152(3)
C396919(13)13340(7)636(5)164(4)
C408045(10)4455(6)3416(5)166(3)
C4113753(15)3793(7)4646(5)153(4)
C4212684(13)4748(8)4382(6)163(4)
C4310414(12)5480(7)3737(5)91(3)
C457470(19)14275(8)131(6)216(5)
C4611945(9)4489(6)3757(5)141(3)
C487600(20)15238(9)466(9)316(9)
C25A9585(7)7752(4)1804(3)60.7(15)
C26A10211(8)8503(5)1299(3)66.4(16)
C22A10567(8)9532(5)1445(3)64.3(16)
C43A11079(17)5226(15)3182(9)91(3)
C34A2850(20)12302(16)1402(16)99(3)
C20A5583(7)9471(4)1388(2)55.9(14)
C19A5185(8)8441(4)1303(3)62.6(15)
C21A4549(7)7756(4)1831(3)60.5(15)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3Cl-decomposition. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Cl0A75.7(10)55.0(9)63.3(9)-14.6(7)-20.1(8)-6.0(8)
Cl273.0(10)68.3(10)45.1(8)0.3(8)-6.8(7)-4.6(8)
Cl1109.4(14)68.2(11)47.2(9)-11.0(8)-19.4(9)-4.9(10)
Cl6A85.1(12)62.6(10)59.8(10)-14.6(8)-14.6(9)-7.8(9)
Cl3A72.3(11)78.2(12)53.1(10)12.2(9)-1.3(8)-8.6(9)
Cl3105.2(15)87.2(14)48.6(10)-7.9(9)-7.1(10)-8.2(11)
O9AA59(2)52.6(19)60(2)-2.5(17)2.1(17)-16.2(16)
O1BA65(2)55(2)72(2)-12.8(18)3.7(18)-27.0(16)
O2AA68(2)45.1(18)61(2)-1.2(16)-6.4(17)-18.0(16)
O5AA87(2)54(2)59(2)-4.2(18)2.6(19)-23.4(18)
O7AA57.0(19)46.9(18)55(2)-9.0(16)6.1(16)-13.6(15)
O4100(3)57(2)63(2)4.9(19)-9(2)-28.6(19)
N8AA47(2)56(2)52(2)-4(2)-2.4(18)-6.7(19)
C0BA41(3)53(3)60(3)-9(2)-9(2)6(2)
C2BA42(2)46(3)56(3)-1(2)-11(2)1(2)
C548(3)45(3)49(3)-4(2)4(2)-8(2)
C644(3)44(3)54(3)-10(2)8(2)-9(2)
C739(2)48(3)55(3)-4(2)-10(2)2(2)
C839(2)44(3)57(3)0(2)1(2)-13(2)
N942(2)51(2)60(2)-7(2)-10.6(18)-4.9(18)
C1037(2)57(3)56(3)-2(2)-16(2)3(2)
C1137(2)58(3)64(3)-3(3)-9(2)1(2)
C1234(2)51(3)57(3)0(2)-3(2)-1(2)
C1347(3)47(3)51(3)-3(2)2(2)-11(2)
C1445(3)43(3)62(3)-2(2)3(2)-8(2)
C1535(2)44(3)63(3)1(2)-12(2)-2(2)
C1640(2)48(3)58(3)-3(2)-2(2)-7(2)
C1741(2)45(3)58(3)-7(2)3(2)-10(2)
C1836(2)48(3)55(3)-9(2)-1(2)-2(2)
C1973(3)57(3)60(3)-13(3)-21(3)5(3)
C2056(3)61(3)49(3)-2(2)-12(2)2(3)
C2160(3)60(3)63(3)-11(3)-14(3)0(3)
C2263(3)61(3)64(3)8(3)-13(3)4(3)
C2339(2)45(3)68(3)-7(2)-9(2)-4(2)
C2452(3)49(3)58(3)-10(2)-3(2)-6(2)
C2562(3)59(3)62(3)-7(3)-14(3)0(3)
C2663(3)76(4)56(3)-4(3)-8(3)7(3)
C2749(3)46(3)63(3)-4(2)5(2)-14(2)
C2856(3)52(3)62(3)-1(3)0(2)-15(2)
C2942(3)51(3)63(3)-9(2)7(2)-9(2)
C3048(3)59(3)73(3)-9(3)-15(2)-12(2)
C3163(3)50(3)67(3)1(3)-2(3)-9(2)
C3382(4)59(4)235(8)30(4)-92(4)-24(3)
C3482(4)97(6)107(6)25(5)1(4)3(4)
C3581(4)85(4)133(6)42(4)-3(4)6(4)
C3697(5)144(7)146(7)40(6)4(5)44(5)
C3796(6)116(6)268(9)76(7)-15(6)20(5)
C38127(6)123(5)222(8)-90(5)45(5)-73(4)
C39135(7)184(7)171(8)72(6)-34(5)-61(6)
C40117(5)81(5)314(9)51(6)-121(5)-40(4)
C41189(9)97(6)158(8)34(6)-7(6)0(6)
C42111(6)148(8)210(7)38(6)-13(5)20(6)
C4360(4)62(4)147(6)6(5)12(4)-23(3)
C45195(10)155(7)286(10)96(6)-46(8)-48(7)
C4668(4)76(4)274(7)64(5)-52(4)-24(3)
C48330(20)169(8)460(20)36(9)-122(19)-40(11)
C25A62(3)59(3)62(3)-7(3)-14(3)0(3)
C26A63(3)76(4)56(3)-4(3)-8(3)7(3)
C22A63(3)61(3)64(3)8(3)-13(3)4(3)
C43A60(4)62(4)147(6)6(5)12(4)-23(3)
C34A82(4)97(6)107(6)25(5)1(4)3(4)
C20A56(3)61(3)49(3)-2(2)-12(2)2(3)
C19A73(3)57(3)60(3)-13(3)-21(3)5(3)
C21A60(3)60(3)63(3)-11(3)-14(3)0(3)

 

Table 4 Bond Lengths for 3Cl-decomposition.
AtomAtomLength/Å AtomAtomLength/Å
Cl6AC251.726(6) C12C161.360(7)
Cl3AC221.708(6) C12C231.514(7)
Cl3C261.687(6) C13C611.361(7)
O9AAC231.221(6) C14C161.471(7)
O1BAC291.207(6) C14C271.404(7)
O2AAC81.394(6) C16C281.512(7)
O2AAC281.366(6) C17C181.356(7)
O5AAC241.210(6) C17C291.502(7)
O7AAC61.382(6) C18C241.517(7)
O7AAC291.362(6) C19C201.386(8)
O4C281.194(6) C19C211.402(8)
N8AAC2BA1.401(6) C22C261.410(8)
N8AAC241.373(6) C25C261.416(8)
N8AAC311.459(6) C27C821.368(7)
C0BAC71.391(7) C30C331.459(8)
C0BAC211.367(7) C31C351.511(8)
C2BAC71.424(7) C33C401.580(10)
C2BAC201.383(7) C33C431.470(11)
C5C61.399(6) C33C43A1.417(13)
C5C131.398(7) C34C351.492(10)
C5C171.476(7) C34C361.542(12)
C6C1311.361(7) C35C371.559(11)
C7C181.478(7) C35C34A1.508(16)
C8C141.395(7) C36C34A1.573(16)
C8C2721.368(7) C37C391.490(11)
N9C101.398(6) C38C401.415(11)
N9C231.365(6) C39C451.554(11)
N9C301.471(6) C41C421.448(10)
C10C151.405(7) C42C461.545(15)
C10C251.379(7) C43C461.580(11)
C11C151.397(7) C45C481.469(14)
C11C221.360(8) C46C43A1.583(15)
C12C151.456(7)    

11-X,2-Y,1-Z; 22-X,2-Y,1-Z

 

Table 5 Bond Angles for 3Cl-decomposition.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C28O2AAC8108.2(4) C2BAC20C19119.0(5)
C29O7AAC6107.7(4) C0BAC21C19120.3(5)
C2BAN8AAC31129.6(4) C11C22Cl3A118.9(5)
C24N8AAC2BA110.4(4) C11C22C26120.5(5)
C24N8AAC31119.9(4) C26C22Cl3A120.6(5)
C21C0BAC7120.5(5) O9AAC23N9124.6(5)
N8AAC2BAC7109.6(4) O9AAC23C12127.3(5)
C20C2BAN8AA129.7(5) N9C23C12108.1(4)
C20C2BAC7120.7(5) O5AAC24N8AA124.0(5)
C6C5C17106.1(4) O5AAC24C18127.7(5)
C13C5C6117.5(4) N8AAC24C18108.3(4)
C13C5C17136.4(4) C10C25Cl6A123.2(4)
O7AAC6C5112.6(4) C10C25C26118.9(5)
C131C6O7AA121.5(4) C26C25Cl6A117.9(4)
C131C6C5125.8(5) C22C26Cl3120.0(4)
C0BAC7C2BA118.8(5) C22C26C25119.6(5)
C0BAC7C18133.5(5) C25C26Cl3120.4(5)
C2BAC7C18107.7(4) C82C27C14115.5(5)
O2AAC8C14112.2(4) O2AAC28C16109.1(4)
C272C8O2AA121.1(4) O4C28O2AA120.6(5)
C272C8C14126.6(4) O4C28C16130.2(5)
C10N9C30130.3(4) O1BAC29O7AA119.6(4)
C23N9C10109.5(4) O1BAC29C17130.4(5)
C23N9C30119.3(4) O7AAC29C17109.9(4)
N9C10C15110.3(4) C33C30N9115.9(4)
C25C10N9128.7(5) N8AAC31C35115.0(5)
C25C10C15121.0(5) C30C33C40108.8(5)
C22C11C15120.6(5) C30C33C43120.3(7)
C15C12C23104.1(4) C43C33C40108.5(7)
C16C12C15133.3(5) C43AC33C30135.2(8)
C16C12C23122.7(5) C43AC33C40115.3(9)
C61C13C5116.7(4) C35C34C36113.6(7)
C8C14C16106.6(4) C31C35C37109.7(6)
C8C14C27117.9(5) C34C35C31115.5(6)
C27C14C16135.4(5) C34C35C37107.6(7)
C10C15C12107.6(4) C34AC35C31132.7(11)
C11C15C10119.4(5) C34AC35C37117.3(11)
C11C15C12132.9(5) C39C37C35113.1(8)
C12C16C14131.8(5) C37C39C45121.5(9)
C12C16C28124.4(5) C38C40C33115.7(8)
C14C16C28103.8(4) C41C42C46108.9(9)
C5C17C29103.3(4) C33C43C46114.2(8)
C18C17C5132.4(4) C48C45C39109.3(11)
C18C17C29124.1(5) C42C46C4395.7(7)
C7C18C24103.9(4) C42C46C43A132.9(10)
C17C18C7132.6(4) C33C43AC46117.1(11)
C17C18C24123.4(5) C35C34AC36110.9(13)
C20C19C21120.7(5)     

11-X,2-Y,1-Z; 22-X,2-Y,1-Z

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3Cl-decomposition.
AtomxyzU(eq)
H0BA38507645278562
H0BB38507645278562
H111054410489215564
H11A1054410489215564
H13553311385417558
H195341820389175
H2060059924103767
H2142967065176773
H2792948267481363
H30A69056458342670
H30B73756316268970
H31A721311554150872
H31B677312194212372
H33992553262838146
H33A911656163694146
H34A3385133192230119
H34B2754121672224119
H354394120871176126
H35A4332128201916126
H36A426134641890207
H36B1174127941303207
H36C1763139511333207
H36D1506134132031207
H36E252131611518207
H36F1776139331316207
H37A4507140271034203
H37B6034138841509203
H38A623747472787228
H38B651035313064228
H38C797940022549228
H39A651512798399197
H39B802213014819197
H40A887838403555199
H40B715746063781199
H41A1478436084344229
H41B1301532034723229
H41C1416739375046229
H42A1343553404287195
H42B1167849654696195
H43A971554874157110
H43B1099461443659110
H45A863314059-105259
H45B656514439-178259
H46A1144937983805169
H46B1284645233385169
H46C1103839993910169
H46D1295240493544169
H48A644415455692474
H48B795215816156474
H48C850215072770474
H25A93727064171673
H26A10387832087480
H22A1098910025111577
H43C1161659053132110
H43D1143548732788110
H34C2504116561661119
H34D281412191951119

 

Table 7 Atomic Occupancy for 3Cl-decomposition.
AtomOccupancy AtomOccupancy AtomOccupancy
Cl0A0.802(2) Cl20.802(2) Cl10.802(2)
Cl6A0.760(3) Cl3A0.760(3) Cl30.760(3)
H0BA0.198(2) H0BB0.802(2) H110.760(3)
H11A0.240(3) C190.198(2) H190.198(2)
C200.198(2) H200.198(2) C210.198(2)
H210.198(2) C220.760(3) C250.760(3)
C260.760(3) H330.683(9) H33A0.317(9)
C340.795(10) H34A0.795(10) H34B0.795(10)
H350.795(10) H35A0.205(10) H36A0.795(10)
H36B0.795(10) H36C0.795(10) H36D0.205(10)
H36E0.205(10) H36F0.205(10) C430.683(9)
H43A0.683(9) H43B0.683(9) H46A0.683(9)
H46B0.683(9) H46C0.317(9) H46D0.317(9)
C25A0.240(3) H25A0.240(3) C26A0.240(3)
H26A0.240(3) C22A0.240(3) H22A0.240(3)
C43A0.317(9) H43C0.317(9) H43D0.317(9)
C34A0.205(10) H34C0.205(10) H34D0.205(10)
C20A0.802(2) C19A0.802(2) C21A0.802(2)

Experimental

Single crystals of C84H78.63Cl9.37N4O12 [3Cl-decomposition] 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.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.

Crystal structure determination of [3Cl-decomposition]

Crystal Data for C84H78.63Cl9.37N4O12 (=1668.30 g/mol): triclinic, space group P-1 (no. 2), a = 7.4241(5) Å, b = 12.4935(9) Å, c = 20.8699(12) Å, α = 84.241(6)°, β = 83.819(5)°, γ = 83.303(6)°, = 1903.8(2) Å3, Z = 1, T = 293(2) K, μ(CuKα) = 3.698 mm-1, Dcalc = 1.455 g/cm3, 10253 reflections measured (7.152° ≤ 2Θ ≤ 125.404°), 5920 unique (Rint = 0.0430, Rsigma = 0.0805) which were used in all calculations. The final R1 was 0.0919 (I > 2σ(I)) and wR2 was 0.2651 (all data).

Refinement model description

Number of restraints - 105, 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
{C25, C25A}
{C26, C26A}
{C22, C22A}
{C20, C20A}
{C19, C19A}
{C21, C21A}
3. Restrained distances
C42-C41
1.55 with sigma of 0.02
C48-C45
1.55 with sigma of 0.02
C45-C39
1.55 with sigma of 0.02
C39-C48
2.5 with sigma of 0.02
C39-C37
1.55 with sigma of 0.02
C40-C38
1.55 with sigma of 0.02
C43-C33
1.55 with sigma of 0.02
C35-C34A
1.55 with sigma of 0.02
C36-C34A
1.55 with sigma of 0.02
C43A-C33
1.55 with sigma of 0.02
C46-C43A
1.55 with sigma of 0.02
H46c-H40a
2 with sigma of 0.02
C35-C34
1.55 with sigma of 0.02
4. Rigid bond restraints
C37, C39, C45, C48
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C41, C42, C46, C43, C43A
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C36, C34, C34A, C35
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C38, C40, C33
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C48 ≈ C45 ≈ C39 ≈ C37: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C43A ≈ C43 ≈ C46 ≈ C42 ≈ C41: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C35 ≈ C34A ≈ H34a ≈ C36: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C33 ≈ C40 ≈ C38: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C43) = Uanis(C43A)
Uanis(C34) = Uanis(C34A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C22) = Uanis(C22A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
Uanis(C19) = Uanis(C19A)
6. Others
Sof(Cl0A)=Sof(Cl2)=Sof(Cl1)=Sof(H0Bb)=Sof(C20A)=Sof(C19A)=Sof(C21A)=1-FVAR(1)
Sof(H0BA)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(1)
Sof(H33a)=Sof(H46c)=Sof(H46d)=Sof(C43A)=Sof(H43c)=Sof(H43d)=1-FVAR(2)
Sof(H33)=Sof(C43)=Sof(H43a)=Sof(H43b)=Sof(H46a)=Sof(H46b)=FVAR(2)
Sof(H35a)=Sof(H36d)=Sof(H36e)=Sof(H36f)=Sof(C34A)=Sof(H34c)=Sof(H34d)=1-FVAR(3)
Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(H35)=Sof(H36a)=Sof(H36b)=Sof(H36c)=FVAR(3)
Sof(H11a)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C22A)=Sof(H22A)=1-FVAR(4)
Sof(Cl6A)=Sof(Cl3A)=Sof(Cl3)=Sof(H11)=Sof(C22)=Sof(C25)=Sof(C26)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
C33(H33), C33(H33a), C35(H35), C35(H35a)
7.b Secondary CH2 refined with riding coordinates:
C30(H30a,H30b), C31(H31a,H31b), C34(H34a,H34b), C37(H37a,H37b), C39(H39a,
H39b), C40(H40a,H40b), C42(H42a,H42b), C43(H43a,H43b), C45(H45a,H45b),
C46(H46a,H46b), C46(H46c,H46d), C43A(H43c,H43d), C34A(H34c,H34d)
7.c Me refined with riding coordinates:
C36(H36a,H36b,H36c), C36(H36d,H36e,H36f), C38(H38a,H38b,H38c), C41(H41a,H41b,
H41c), C48(H48a,H48b,H48c)
7.d Aromatic/amide H refined with riding coordinates:
C0BA(H0BA), C0BA(H0Bb), C11(H11), C11(H11a), C13(H13), C19(H19), C20(H20),
C21(H21), C27(H27), C25A(H25A), C26A(H26A), C22A(H22A)

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.