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) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
C1' | 9357(12) | 4061(5) | 8123(5) | 22.7(12) |
C2 | 4734(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) |
C4 | 7768(13) | 4564(5) | 10106(5) | 22.8(12) |
C4' | 8704(14) | 3113(5) | 6417(6) | 23.8(14) |
C5 | 8401(14) | 4242(5) | 11250(5) | 25.5(13) |
C5' | 8619(17) | 1988(6) | 6034(7) | 33.6(17) |
C6 | 6998(17) | 4762(7) | 12153(8) | 28.5(17) |
C7 | 10356(13) | 3468(4) | 11117(5) | 24.4(13) |
I1 | 11987.2(8) | 2489.9(3) | 12410.7(3) | 36.28(15) |
N1 | 5210(13) | 5485(5) | 11854(5) | 33.3(13) |
N3 | 5928(11) | 5255(4) | 9768(4) | 26.1(11) |
N4 | 7436(16) | 4552(5) | 13301(5) | 40.8(16) |
N5 | 2838(15) | 6390(5) | 10451(6) | 43.7(17) |
N8 | 10950(11) | 3329(4) | 10013(5) | 27.6(11) |
N9 | 9351(11) | 4022(4) | 9379(5) | 24.1(11) |
O1 | 8072(9) | 3143(4) | 7661(4) | 28.7(11) |
O2 | 13314(11) | 5017(5) | 7580(4) | 32.0(15) |
O3 | 11226(11) | 4504(4) | 5455(4) | 36.1(11) |
O4 | 6067(11) | 1558(4) | 6123(4) | 37.4(12) |
O5 | 6570(10) | 5775(4) | 5832(4) | 36.2(11) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
C1' | 22(3) | 27(3) | 18(3) | -1(2) | 0(2) | 0(2) |
C2 | 35(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) |
C4 | 24(3) | 23(3) | 21(3) | -4(2) | 0(2) | -3(2) |
C4' | 22(3) | 30(3) | 19(3) | 1(3) | 2(2) | 1(3) |
C5 | 31(3) | 25(3) | 20(3) | -1(2) | -3(2) | 1(3) |
C5' | 35(4) | 35(3) | 31(4) | -6(3) | 8(3) | -6(3) |
C6 | 40(5) | 26(4) | 20(3) | -4(3) | -1(3) | 1(3) |
C7 | 36(4) | 22(3) | 15(3) | 7(2) | -5(2) | -2(3) |
I1 | 47.6(3) | 34.6(2) | 26.4(2) | 5.1(2) | -4.91(15) | 10.6(3) |
N1 | 42(3) | 35(3) | 23(3) | -5(2) | 0(2) | 11(3) |
N3 | 32(3) | 27(2) | 19(2) | -1(2) | -2(2) | 5(2) |
N4 | 60(5) | 47(4) | 16(3) | -3(2) | -1(3) | 18(3) |
N5 | 59(5) | 46(4) | 26(3) | -4(3) | 2(3) | 28(3) |
N8 | 30(3) | 29(2) | 24(3) | 2(2) | -1(2) | 5(2) |
N9 | 25(3) | 27(2) | 21(2) | 1(2) | 2(2) | 3(2) |
O1 | 30(3) | 34(3) | 22(2) | -4.6(17) | 8(2) | -6.6(18) |
O2 | 32(3) | 42(4) | 22(3) | 2.0(19) | -4(2) | -15(2) |
O3 | 41(3) | 45(3) | 22(2) | 7(2) | -1(2) | -14(2) |
O4 | 53(3) | 37(3) | 23(2) | -0.7(19) | 2(2) | -20(2) |
O5 | 36(3) | 42(3) | 30(2) | 8(2) | -2(2) | -7(2) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
C1' | C2' | 1.521(8) | C4 | N9 | 1.355(8) | |
C1' | N9 | 1.423(7) | C4' | C5' | 1.499(9) | |
C1' | O1 | 1.433(8) | C4' | O1 | 1.453(7) | |
C2 | N1 | 1.348(9) | C5 | C6 | 1.424(10) | |
C2 | N3 | 1.353(8) | C5 | C7 | 1.412(9) | |
C2 | N5 | 1.335(10) | C5' | O4 | 1.416(10) | |
C2' | C3' | 1.547(8) | C6 | N1 | 1.334(11) | |
C2' | O2 | 1.406(9) | C6 | N4 | 1.341(10) | |
C3' | C4' | 1.537(10) | C7 | I1 | 2.081(6) | |
C3' | O3 | 1.415(8) | C7 | N8 | 1.305(8) | |
C4 | C5 | 1.389(9) | N8 | N9 | 1.389(8) | |
C4 | N3 | 1.335(9) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
N9 | C1' | C2' | 116.2(5) | C4 | C5 | C6 | 115.0(6) | |
N9 | C1' | O1 | 108.9(5) | C4 | C5 | C7 | 104.8(5) | |
O1 | C1' | C2' | 103.8(5) | C7 | C5 | C6 | 140.2(7) | |
N1 | C2 | N3 | 126.8(6) | O4 | C5' | C4' | 111.7(7) | |
N5 | C2 | N1 | 116.7(6) | N1 | C6 | C5 | 119.4(7) | |
N5 | C2 | N3 | 116.5(6) | N1 | C6 | N4 | 118.7(7) | |
C1' | C2' | C3' | 102.1(5) | N4 | C6 | C5 | 121.9(7) | |
O2 | C2' | C1' | 113.2(6) | C5 | C7 | I1 | 127.8(5) | |
O2 | C2' | C3' | 111.8(5) | N8 | C7 | C5 | 112.2(5) | |
C4' | C3' | C2' | 103.3(5) | N8 | C7 | I1 | 119.7(5) | |
O3 | C3' | C2' | 113.9(5) | C6 | N1 | C2 | 119.2(6) | |
O3 | C3' | C4' | 112.8(6) | C4 | N3 | C2 | 112.1(5) | |
N3 | C4 | C5 | 127.4(6) | C7 | N8 | N9 | 105.2(5) | |
N3 | C4 | N9 | 125.9(6) | C4 | N9 | C1' | 127.3(5) | |
N9 | C4 | C5 | 106.7(6) | C4 | N9 | N8 | 111.1(5) | |
C5' | C4' | C3' | 116.0(6) | N8 | N9 | C1' | 121.5(5) | |
O1 | C4' | C3' | 107.2(5) | C1' | O1 | C4' | 105.4(5) | |
O1 | C4' | C5' | 107.4(5) |
D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
---|---|---|---|---|---|---|
N4 | H4B | O41 | 0.86(3) | 2.44(6) | 3.193(8) | 147(8) |
N4 | H4B | O52 | 0.86(3) | 2.64(8) | 3.301(8) | 135(8) |
N5 | H5A | O11 | 0.86 | 2.40 | 3.135(8) | 144.2 |
O2 | H2 | N33 | 0.82 | 1.98 | 2.799(7) | 177.3 |
O3 | H3 | O5 | 0.82 | 2.09 | 2.910(8) | 174.9 |
O4 | H4 | N14 | 0.82 | 1.96 | 2.759(7) | 164.6 |
O5 | H5C | O25 | 0.85 | 2.03 | 2.785(7) | 147.4 |
O5 | H5C | O35 | 0.85 | 2.69 | 3.185(7) | 118.9 |
O5 | H5D | O46 | 0.85 | 1.92 | 2.747(7) | 165.8 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H1' | 8399 | 4685 | 7850 | 27 |
H2' | 13160 | 3511 | 7958 | 28 |
H3' | 12667 | 3167 | 6039 | 31 |
H4' | 7351 | 3502 | 5968 | 29 |
H5'A | 9174 | 1938 | 5223 | 40 |
H5'B | 9841 | 1584 | 6523 | 40 |
H4A | 8930(120) | 4250(80) | 13460(100) | 60(30) |
H4B | 6360(160) | 4920(60) | 13710(70) | 40(30) |
H5A | 1990 | 6678 | 11013 | 52 |
H5B | 2464 | 6549 | 9728 | 52 |
H2 | 14050 | 5104 | 8225 | 48 |
H3 | 9967 | 4882 | 5594 | 54 |
H4 | 5891 | 1313 | 6786 | 56 |
H5C | 5809 | 5316 | 6249 | 54 |
H5D | 5517 | 5988 | 5290 | 54 |
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.
Crystal structure determination of [201804210]
Crystal Data for C10H15IN6O5 (M =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)°, V = 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)
This report has been created with Olex2, compiled on 2018.04.03 svn.r3497 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.