201804211

Table 1 Crystal data and structure refinement for 201804211.
Identification code 201804211
Empirical formula C10H13N5O5
Formula weight 283.25
Temperature/K 293(2)
Crystal system orthorhombic
Space group P212121
a/Å 4.7669(2)
b/Å 11.0409(5)
c/Å 21.6334(9)
α/° 90
β/° 90
γ/° 90
Volume/Å3 1138.59(8)
Z 4
ρcalcg/cm3 1.652
μ/mm‑1 1.157
F(000) 592.0
Crystal size/mm3 0.15 × 0.11 × 0.1
Radiation CuKα (λ = 1.54184)
2Θ range for data collection/° 8.174 to 134.138
Index ranges -3 ≤ h ≤ 5, -13 ≤ k ≤ 13, -25 ≤ l ≤ 25
Reflections collected 4100
Independent reflections 2032 [Rint = 0.0304, Rsigma = 0.0405]
Data/restraints/parameters 2032/0/184
Goodness-of-fit on F2 1.036
Final R indexes [I>=2σ (I)] R1 = 0.0366, wR2 = 0.0880
Final R indexes [all data] R1 = 0.0408, wR2 = 0.0924
Largest diff. peak/hole / e Å-3 0.14/-0.21
Flack parameter0.2(2)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 201804211. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C1'4663(6)2481(2)3422.2(13)21.7(6)
C2832(6)5821(3)4035.5(14)22.7(6)
C2'7547(6)2355(3)3124.7(13)22.4(6)
C3'6988(7)1333(3)2674.1(13)25.2(6)
C43543(6)4186(2)4141.0(13)20.0(6)
C4'5133(7)498(3)3059.4(14)25.5(6)
C54812(6)4588(3)4682.5(13)22.6(6)
C5'6688(8)-481(3)3405.0(17)35.6(8)
C64144(6)5762(3)4902.0(13)23.5(6)
C76793(7)3686(3)4838.0(14)26.0(6)
N12061(6)6311(2)4554.1(12)26.0(6)
N31519(5)4751(2)3805.2(11)22.0(5)
N4-1135(6)6508(2)3770.3(13)31.8(6)
N86804(6)2803(2)4434.6(11)26.7(6)
N94761(5)3109(2)4004.7(11)22.5(5)
O13700(5)1267.1(18)3504.8(11)28.8(5)
O28443(5)3436(2)2836.4(10)29.5(5)
O35381(5)1733(2)2162.3(10)32.2(5)
O44822(6)-1309(2)3702.3(11)40.6(6)
O55239(5)6310(2)5342.1(10)32.2(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 201804211. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
C1'20.1(14)18.8(13)26.2(13)-1.5(11)-3.2(12)-0.2(11)
C222.9(14)19.0(13)26.1(13)1.8(11)1.8(12)0.8(11)
C2'20.5(15)21.9(14)24.7(13)0.2(12)-0.9(12)0.0(11)
C3'24.4(15)24.2(15)27.0(14)-4.3(12)-0.9(12)5.4(13)
C420.3(13)17.1(12)22.7(13)0.8(10)3.3(12)-1.3(11)
C4'26.5(16)21.5(14)28.4(14)-5.9(11)-3.5(12)2.3(13)
C525.2(15)20.0(13)22.8(13)2.4(11)0.2(12)-2.0(12)
C5'38.1(19)26.2(16)42.4(18)5.4(14)2.6(16)7.6(15)
C627.5(15)19.7(14)23.2(14)-1.0(11)2.5(12)-4.8(12)
C728.3(15)26.2(15)23.6(13)2.6(12)-6.5(12)0.1(13)
N132.9(14)16.6(11)28.4(13)-4.3(10)1.0(11)3.8(10)
N321.3(12)19.6(12)25.1(12)-0.6(9)-0.7(10)-0.1(10)
N434.0(15)26.0(13)35.4(14)-5.7(11)-6.7(12)9.9(11)
N828.8(13)24.6(12)26.7(12)3.3(10)-3.7(11)4.5(11)
N922.7(12)19.2(12)25.7(11)-0.8(9)-0.6(10)4.7(10)
O126.0(11)19.2(10)41.4(12)-5.0(9)7.7(9)-2.6(9)
O229.9(11)28.8(12)29.8(11)2.4(9)-4.3(9)-7.3(9)
O340.0(13)30.5(13)26.0(10)2.2(9)-6.9(10)-5.0(11)
O452.3(16)24.8(11)44.7(13)1.1(10)13.3(13)6.0(12)
O544.1(13)24.2(10)28.4(10)-4.4(9)-7.2(10)-4.5(10)

 

Table 4 Bond Lengths for 201804211.
AtomAtomLength/Å AtomAtomLength/Å
C1'C2'1.524(4) C4N31.360(4)
C1'N91.439(4) C4N91.356(4)
C1'O11.428(3) C4'C5'1.510(4)
C2N11.377(4) C4'O11.454(4)
C2N31.323(4) C5C61.416(4)
C2N41.335(4) C5C71.413(4)
C2'C3'1.515(4) C5'O41.428(4)
C2'O21.413(3) C6N11.386(4)
C3'C4'1.525(4) C6O51.243(4)
C3'O31.417(4) C7N81.308(4)
C4C51.391(4) N8N91.388(3)

 

Table 5 Bond Angles for 201804211.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
N9C1'C2'112.6(2) O1C4'C5'108.7(3)
O1C1'C2'104.9(2) C4C5C6118.4(3)
O1C1'N9110.7(2) C4C5C7105.4(3)
N3C2N1123.6(3) C7C5C6135.7(3)
N3C2N4121.3(3) O4C5'C4'112.1(3)
N4C2N1115.2(3) N1C6C5112.3(3)
C3'C2'C1'100.4(2) O5C6C5127.4(3)
O2C2'C1'112.5(2) O5C6N1120.2(3)
O2C2'C3'113.5(2) N8C7C5111.7(3)
C2'C3'C4'101.6(2) C2N1C6125.1(2)
O3C3'C2'111.4(2) C2N3C4112.6(3)
O3C3'C4'107.6(3) C7N8N9105.2(2)
N3C4C5127.8(3) C4N9C1'126.8(2)
N9C4C5106.1(3) C4N9N8111.6(2)
N9C4N3126.2(3) N8N9C1'119.5(2)
C5'C4'C3'114.8(3) C1'O1C4'108.3(2)
O1C4'C3'106.4(2)     

 

Table 6 Hydrogen Bonds for 201804211.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1O510.861.942.775(3)161.9
N4H4AO320.862.152.869(3)140.9
N4H4BO430.862.433.090(4)133.5
N4H4BO510.862.443.150(3)140.7
O2H2N340.822.132.941(3)172.9
O3H3O450.822.212.860(3)135.7
O4H4O560.822.343.008(3)139.3

1-1/2+X,3/2-Y,1-Z; 2-X,1/2+Y,1/2-Z; 3-1+X,1+Y,+Z; 41+X,+Y,+Z; 51-X,1/2+Y,1/2-Z; 6-1/2+X,1/2-Y,1-Z

 

Table 7 Torsion Angles for 201804211.
ABCDAngle/˚ ABCDAngle/˚
C1'C2'C3'C4'-40.3(3) N3C2N1C6-0.2(5)
C1'C2'C3'O374.0(3) N3C4C5C6-5.5(5)
C2'C1'N9C4116.3(3) N3C4C5C7-179.0(3)
C2'C1'N9N8-45.7(3) N3C4N9C1'15.3(5)
C2'C1'O1C4'-24.2(3) N3C4N9N8178.5(3)
C2'C3'C4'C5'-92.9(3) N4C2N1C6-179.9(3)
C2'C3'C4'O127.3(3) N4C2N3C4-179.6(3)
C3'C4'C5'O4-173.7(2) N9C1'C2'C3'161.0(2)
C3'C4'O1C1'-2.1(3) N9C1'C2'O2-78.0(3)
C4C5C6N15.2(4) N9C1'O1C4'-145.9(2)
C4C5C6O5-173.2(3) N9C4C5C6173.7(3)
C4C5C7N80.5(4) N9C4C5C70.2(3)
C5C4N3C22.2(4) N9C4N3C2-176.9(3)
C5C4N9C1'-164.0(3) O1C1'C2'C3'40.6(3)
C5C4N9N8-0.8(3) O1C1'C2'O2161.5(2)
C5C6N1C2-2.8(4) O1C1'N9C4-126.6(3)
C5C7N8N9-0.9(3) O1C1'N9N871.3(3)
C5'C4'O1C1'122.0(3) O1C4'C5'O467.4(3)
C6C5C7N8-171.4(3) O2C2'C3'C4'-160.5(2)
C7C5C6N1176.3(3) O2C2'C3'O3-46.2(3)
C7C5C6O5-2.1(6) O3C3'C4'C5'150.0(3)
C7N8N9C1'165.6(3) O3C3'C4'O1-89.8(3)
C7N8N9C41.0(3) O5C6N1C2175.7(3)
N1C2N3C40.7(4)      

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 201804211.
AtomxyzU(eq)
H1'34012909313926
H2'89262099343427
H3'8724931254430
H4'3735121278931
H5'A7871-923311843
H5'B7892-111371343
H779463716518431
H114927014467131
H4A-19816257344338
H4B-15547201392638
H292773859308844
H362482261197648
H43933-952397161

Experimental

Single crystals of C10H13N5O5 [201804211] 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 Direct Methods 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 [201804211]

Crystal Data for C10H13N5O5 (=283.25 g/mol): orthorhombic, space group P212121 (no. 19), a = 4.7669(2) Å, b = 11.0409(5) Å, c = 21.6334(9) Å, = 1138.59(8) Å3, Z = 4, T = 293(2) K, μ(CuKα) = 1.157 mm-1, Dcalc = 1.652 g/cm3, 4100 reflections measured (8.174° ≤ 2Θ ≤ 134.138°), 2032 unique (Rint = 0.0304, Rsigma = 0.0405) which were used in all calculations. The final R1 was 0.0366 (I > 2σ(I)) and wR2 was 0.0924 (all data).

Refinement model description

Number of restraints - 0, 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) groups, All N(H,H) groups
At 1.5 times of:
All O(H) groups
2.a Ternary CH refined with riding coordinates:
C1'(H1'), C2'(H2'), C3'(H3'), C4'(H4')
2.b Secondary CH2 refined with riding coordinates:
C5'(H5'A,H5'B)
2.c Aromatic/amide H refined with riding coordinates:
C7(H7), N1(H1)
2.d X=CH2 refined with riding coordinates:
N4(H4A,H4B)
2.e Idealised tetrahedral OH refined as rotating group:
O2(H2), O3(H3), O4(H4)

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