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Table 1 Crystallographic data for the carbon–bonded anionic sigma complexes 1 – 3

From: Synthesis of a new class of carbon–bonded anionic sigma complexes with 1,3-dimethyl-2,6-dioxo-5-(2,4,6-trinitrophenyl)-1,2,3,6-tetrahydropyrimidin-4-olate moiety as insensitive high energy density materials –– implications from impact sensitivity and thermal testings

Molecule

1

2

3

Empirical formula System, sp. gr ., Z

C 18 H 24 N 6 O 12 Triclinic, P-1, 2

C 17 H 14 N 6 O 9 Triclinic, P-1, 2

C 22 H 24 N 6 O 9 Monoclinic, P2 1 /n, 4

a, b, c Å

8.4411(2), 12.1069(4), 13.3113(6)

8.8720(2), 11.2160(4), 11.5280(4)

14.9093(5), 9.4785(3), 17.7118(6)

α, β, γ deg

111.383(2), 101.163(2), 102.748(10)

75.6030(10), 75.0350(10), 90

90, 100.2370(10), 90

V, Å3

1177.41(8)

1073.40(4)

2463.15(14)

D x, Mg/m3

1.507

1.492

1.393

Radiation, λ, Å

MoKα, 0.71073

MoKα, 0.71073

MoKα, 0.71073

μ, mm−1

0.130

0.127

0.110

T, K

293

293

293

Sample size, mm

0.35 x 0.30 x 0.30

0.20 x 0.15 x 0.15

0.35 x 0.30 x 0.30

Diffractometer

Bruker axs kappa apex2 CCD

Bruker axs kappa apex2 CCD

Bruker axs kappa apex2 CCD

Scan mode

ω and φ

ω and φ

ω and φ

Absorption correction

Semi-empirical from equivalents 0.9432,0.9758

Semi-empirical from equivalents 0.9217,0.9965

Semi-empirical from equivalents 0.9536,0.9765

Tmin, Tmax

θmax, deg

25.00

25.00

25.00

h, k, l ranges

−12 ≤ h ≤ 11,-15 ≤ k ≤ 15,

−9 ≤ h ≤ 9,-19 ≤ k ≤ 19,

−17 ≤ h ≤ 17,-11 ≤ k ≤ 8,

-15 ≤ l ≤ 15

−19 ≤ l ≤ 19

−21 ≤ l ≤ 21

No of reflections: measured/unique (N1), R int

20646/4121, 0.0278

18538/3769, 0.0295

21291/4332, 0.0307

Refinement method

Full-matrix least-squares on F2

Full-matrix least-squares on F2

Full-matrix least-squares on F2

No of refined parameters

345

347

338

R1/wR2 relative to N1

0.0400, 0.1101

0.0386, 0.1041

0.0413, 0.1113

R1/wR2 relative to N2

0.0459, 0.1167

0.0494, 0.1127

0.0596, 0.1293

S

1.041

1.047

1.020

∆ρmax/∆ρmin, e/Å3

0.390, −0.277

0.273, −0.209

0.297,-0.192

Programs

APEX2, SIR92, SHELXL97, ORTEP-3, Mercury

APEX2, SIR92, SHELXL97, ORTEP-3, Mercury

APEX2, SIR92, SHELXL97, ORTEP-3, Mercury