STUDY OF NEW MOLECULAR AND CRYSTAL STRUCTURES OF 4,4,10,10-TETRAMETHYL-1,3,7,9-TETRAAZOSPIRO[5.5]UNDECANE-2,8-DIONE AND ITS SALTS: MONOCHLORIDE, MONONITRATE, AND TETRAIODOTELLURATE
E.E. Netreba1, E.S. Papayanina2
1V.I. Vernadsky Taurida National University, Simferopol, Russia
2L.M. Litvinenko Institute of Physical Organic Chemistry and Coal Chemistry, National Academy of Sciences of Ukraine, Donetsk, Ukraine
Keywords: спиробисмочевина, спирокарбон, моногидрат, монохлорид, мононитрат, тетраиодотеллурат, ЯМР
Н, ИК, структура, РСА, РФА, spirobisurea, spirocarbone, monohydrate, monochloride, mononitrate, tetraiodotellurate,
Н NMR
, IR, structure, single-crystal XRD, powder XRD
Abstract
This is the first work to synthesize 4,4,10,10-tetramethyl-1,3,7,9-tetraazospiro[5.5]undecane-2,8-dione monohydrate, monochloride, mononitrate, and teteraiodotellurate: C
11H
20N
4O
2×H
2O (
I), C
11H
21N
4O
2
+×Cl
- (
II), C
11H
21N
4O
2
+×NO
3
- (
III), and 2(C
11H
21N
4O
2
+)×TeI
4
2-×C
3H
6O (
IV) and determine their structures. Crystals of I are monoclinic: sp. gr.
P 2
1/
c , at 298 K
a = 5.7118(7),
b = 17.842(2), and
c = 13.5905(16) Å; β = 91.621(11)°;
V = 1384.5(3) Å
3;
d
x = 1.239 g/cm
3,
Z = 4. Crystals of II are tetragonal: sp. gr.
P4
3, at 298 K
a = 6.4134(3) and
c = 34.292(2) Å;
V = 1410.47(14) Å
3;
d
x = 1.303 g/cm
3;
Z = 4. Crystals of
III are triclinic: sp. gr.
P-1, at 298 K
a = 8.7614(14),
b = 9.3904(18), and
c = 10.028(2) Å; α = 63.27(2), β = 78.591(16), and γ = 84.308(15)°;
V = 722.3(2) Å
3;
d
x = 1.40 g/cm
3;
Z = 2. Crystals of
IV are triclinic: sp. gr.
P -1, at 100 K
a = 10.4630(4),
b = 11.9372(6), and
c = 16.4118(5) Å; α = 72.058(3), β = 76.406(3), and γ = 87.029(3)°;
V = 1895.04(12) Å
3;
d
x = 2.06 g/cm
3;
Z = 2. The synthesis of
s- and
p-metals with spirocarbone in acetone medium is found to be impossible due to the protonation by the oxygen atom of the carbonyl group. The main crystalline product of the complexation reaction is a monosalt. Evidence is provided that the recrystallization and drying of the synthesized spirocarbone preparation yields monohydrate (
I); its purity and monophasity is confirmed by a Rietveld refinement of the powder X-ray pattern. The lattice parameters at room temperature are:
a = 5.6885(12),
b = 17.8496(12), and
c = 13.518(3) Å; β = 91.449(15)°;
V = 1372.1(4) Å
3. The sample is monophasic.
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