201804210

Table 1 Crystal data and structure refinement for 201804210.
Identification code 201804210
Empirical formula C10H15IN6O5
Formula weight 426.18
Temperature/K 293(2)
Crystal system monoclinic
Space group P21
a/Å 5.08845(13)
b/Å 12.7514(2)
c/Å 11.3200(2)
α/° 90
β/° 91.4146(19)
γ/° 90
Volume/Å3 734.28(3)
Z 2
ρcalcg/cm3 1.928
μ/mm‑1 17.478
F(000) 420.0
Crystal size/mm3 0.15 × 0.13 × 0.11
Radiation CuKα (λ = 1.54184)
2Θ range for data collection/° 7.812 to 134.094
Index ranges -3 ≤ h ≤ 6, -15 ≤ k ≤ 15, -13 ≤ l ≤ 12
Reflections collected 5309
Independent reflections 2616 [Rint = 0.0300, Rsigma = 0.0391]
Data/restraints/parameters 2616/3/213
Goodness-of-fit on F2 1.062
Final R indexes [I>=2σ (I)] R1 = 0.0286, wR2 = 0.0701
Final R indexes [all data] R1 = 0.0296, wR2 = 0.0711
Largest diff. peak/hole / e Å-3 0.56/-0.62
Flack parameter-0.021(5)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 201804210. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C1'9357(12)4061(5)8123(5)22.7(12)
C24734(14)5695(5)10701(6)29.6(14)
C2'12043(12)4037(5)7562(5)23.3(12)
C3'11351(13)3677(5)6287(5)25.6(13)
C47768(13)4564(5)10106(5)22.8(12)
C4'8704(14)3113(5)6417(6)23.8(14)
C58401(14)4242(5)11250(5)25.5(13)
C5'8619(17)1988(6)6034(7)33.6(17)
C66998(17)4762(7)12153(8)28.5(17)
C710356(13)3468(4)11117(5)24.4(13)
I111987.2(8)2489.9(3)12410.7(3)36.28(15)
N15210(13)5485(5)11854(5)33.3(13)
N35928(11)5255(4)9768(4)26.1(11)
N47436(16)4552(5)13301(5)40.8(16)
N52838(15)6390(5)10451(6)43.7(17)
N810950(11)3329(4)10013(5)27.6(11)
N99351(11)4022(4)9379(5)24.1(11)
O18072(9)3143(4)7661(4)28.7(11)
O213314(11)5017(5)7580(4)32.0(15)
O311226(11)4504(4)5455(4)36.1(11)
O46067(11)1558(4)6123(4)37.4(12)
O56570(10)5775(4)5832(4)36.2(11)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 201804210. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
C1'22(3)27(3)18(3)-1(2)0(2)0(2)
C235(4)29(3)24(3)-5(2)-2(3)3(3)
C2'21(3)30(3)19(3)5(2)1(2)-2(2)
C3'23(3)33(3)20(3)-4(2)5(2)-1(3)
C424(3)23(3)21(3)-4(2)0(2)-3(2)
C4'22(3)30(3)19(3)1(3)2(2)1(3)
C531(3)25(3)20(3)-1(2)-3(2)1(3)
C5'35(4)35(3)31(4)-6(3)8(3)-6(3)
C640(5)26(4)20(3)-4(3)-1(3)1(3)
C736(4)22(3)15(3)7(2)-5(2)-2(3)
I147.6(3)34.6(2)26.4(2)5.1(2)-4.91(15)10.6(3)
N142(3)35(3)23(3)-5(2)0(2)11(3)
N332(3)27(2)19(2)-1(2)-2(2)5(2)
N460(5)47(4)16(3)-3(2)-1(3)18(3)
N559(5)46(4)26(3)-4(3)2(3)28(3)
N830(3)29(2)24(3)2(2)-1(2)5(2)
N925(3)27(2)21(2)1(2)2(2)3(2)
O130(3)34(3)22(2)-4.6(17)8(2)-6.6(18)
O232(3)42(4)22(3)2.0(19)-4(2)-15(2)
O341(3)45(3)22(2)7(2)-1(2)-14(2)
O453(3)37(3)23(2)-0.7(19)2(2)-20(2)
O536(3)42(3)30(2)8(2)-2(2)-7(2)

 

Table 4 Bond Lengths for 201804210.
AtomAtomLength/Å AtomAtomLength/Å
C1'C2'1.521(8) C4N91.355(8)
C1'N91.423(7) C4'C5'1.499(9)
C1'O11.433(8) C4'O11.453(7)
C2N11.348(9) C5C61.424(10)
C2N31.353(8) C5C71.412(9)
C2N51.335(10) C5'O41.416(10)
C2'C3'1.547(8) C6N11.334(11)
C2'O21.406(9) C6N41.341(10)
C3'C4'1.537(10) C7I12.081(6)
C3'O31.415(8) C7N81.305(8)
C4C51.389(9) N8N91.389(8)
C4N31.335(9)    

 

Table 5 Bond Angles for 201804210.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
N9C1'C2'116.2(5) C4C5C6115.0(6)
N9C1'O1108.9(5) C4C5C7104.8(5)
O1C1'C2'103.8(5) C7C5C6140.2(7)
N1C2N3126.8(6) O4C5'C4'111.7(7)
N5C2N1116.7(6) N1C6C5119.4(7)
N5C2N3116.5(6) N1C6N4118.7(7)
C1'C2'C3'102.1(5) N4C6C5121.9(7)
O2C2'C1'113.2(6) C5C7I1127.8(5)
O2C2'C3'111.8(5) N8C7C5112.2(5)
C4'C3'C2'103.3(5) N8C7I1119.7(5)
O3C3'C2'113.9(5) C6N1C2119.2(6)
O3C3'C4'112.8(6) C4N3C2112.1(5)
N3C4C5127.4(6) C7N8N9105.2(5)
N3C4N9125.9(6) C4N9C1'127.3(5)
N9C4C5106.7(6) C4N9N8111.1(5)
C5'C4'C3'116.0(6) N8N9C1'121.5(5)
O1C4'C3'107.2(5) C1'O1C4'105.4(5)
O1C4'C5'107.4(5)     

 

Table 6 Hydrogen Bonds for 201804210.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N4H4BO410.86(3)2.44(6)3.193(8)147(8)
N4H4BO520.86(3)2.64(8)3.301(8)135(8)
N5H5AO110.862.403.135(8)144.2
O2H2N330.821.982.799(7)177.3
O3H3O50.822.092.910(8)174.9
O4H4N140.821.962.759(7)164.6
O5H5CO250.852.032.785(7)147.4
O5H5CO350.852.693.185(7)118.9
O5H5DO460.851.922.747(7)165.8

11-X,1/2+Y,2-Z; 2+X,+Y,1+Z; 31+X,+Y,+Z; 41-X,-1/2+Y,2-Z; 5-1+X,+Y,+Z; 61-X,1/2+Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 201804210.
AtomxyzU(eq)
H1'83994685785027
H2'131603511795828
H3'126673167603931
H4'73513502596829
H5'A91741938522340
H5'B98411584652340
H4A8930(120)4250(80)13460(100)60(30)
H4B6360(160)4920(60)13710(70)40(30)
H5A199066781101352
H5B24646549972852
H2140505104822548
H399674882559454
H458911313678656
H5C58095316624954
H5D55175988529054

Experimental

Single crystals of C10H15IN6O5 [201804210] were []. A suitable crystal was selected and [] on a Xcalibur, Eos, Gemini diffractometer. The crystal was kept at 293(2) K during data collection. Using Olex2 [1], the structure was solved with the ShelXS [2] structure solution program using Patterson Method and refined with the ShelXL [3] refinement package using Least Squares 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. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [201804210]

Crystal Data for C10H15IN6O5 (=426.18 g/mol): monoclinic, space group P21 (no. 4), a = 5.08845(13) Å, b = 12.7514(2) Å, c = 11.3200(2) Å, β = 91.4146(19)°, = 734.28(3) Å3, Z = 2, T = 293(2) K, μ(CuKα) = 17.478 mm-1, Dcalc = 1.928 g/cm3, 5309 reflections measured (7.812° ≤ 2Θ ≤ 134.094°), 2616 unique (Rint = 0.0300, Rsigma = 0.0391) which were used in all calculations. The final R1 was 0.0286 (I > 2σ(I)) and wR2 was 0.0711 (all data).

Refinement model description

Number of restraints - 3, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H,H) groups
At 1.5 times of:
All O(H) groups, All O(H,H) groups
2. Restrained distances
N4-H4B
0.87 with sigma of 0.02
N4-H4A
0.87 with sigma of 0.02
3.a Free rotating group:
O5(H5C,H5D)
3.b Ternary CH refined with riding coordinates:
C1'(H1'), C2'(H2'), C3'(H3'), C4'(H4')
3.c Secondary CH2 refined with riding coordinates:
C5'(H5'A,H5'B)
3.d X=CH2 refined with riding coordinates:
N5(H5A,H5B)
3.e Idealised tetrahedral OH refined as rotating group:
O2(H2), O3(H3), O4(H4)

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