Two new dodecahydrate trisodium triphosphates Na3MP3O10
Phosphates containing polyanions
The title compounds Na3M(P3O10)·12H2O (M = Co (
The X-ray diffraction data for (
Crystal data and details of collection and structure refinement for Na3MP3O10·12H2O M = Co (
Structural data | ( |
( |
---|---|---|
Empirical formula | Na3CoP3O10·12H2O | Na3NiP3O10·12H2O |
Formula weight (g/mol) | 597 | 596.8 |
Temperature (K) | 120 | 120 |
Wavelength Mo |
1.54184 | 1.54184 |
Crystal system, space group | Monoclinic, P21/ |
Monoclinic, P21/ |
Unit cell dimensions | ||
|
15.0263(3), 90 | 14,9906(4), 90 |
|
9.1972(2), 90.0492(16) | 9,1628(2), 90.098(2) |
|
14.6654(3), 90 |
14,6660(4), 90 |
Volume (Å3), |
2026.76(7), 4 | 2014.46(9), 4 |
|
1.9559 | 1.967 |
Absorption coefficient (mm−1) | 10.499 | 5.267 |
|
1220 | 1224 |
Crystal size (mm) | 0.3416 * 0.1882 * 0.1274 |
0.5021 * 0.0801 * 0.0527 |
Crystal shape, colour | Prism, pink | Needle, colorless |
Limiting indices |
|
|
Reflections collected | 3534 | 3181 |
Independent reflections | 3456 | 3107 |
Diffractometer | Oxford Diffraction Ltd. | Oxford Diffraction Ltd. |
Data/restraints/parameters | 3534/24/336 | 3181/24/336 |
Goodness-of-fit on |
1.61 | 2.11 |
Final |
|
|
|
|
|
Interatomic distances (Å) and angles (°) in Na3MP3O10·12H2O, M = Co, Ni.
Co(1)O6 in Na3CoP3O10·12H2O | ||||||
---|---|---|---|---|---|---|
Co1 | O2 | O6 | O9 | O11 | O12 | O19 |
O2 |
|
90,35(8) | 94,87(8) | 91,45(8) | 171,96(8) | 91,01(8) |
O6 | 90,35(8) |
|
90,43(8) | 177,32(8) | 85,90(8) | 85,98(8) |
O9 | 94,87(8) | 90,43(8) |
|
91,40(8) | 92,27(8) | 173,13(8) |
O11 | 91,45(8) | 177,32(8) | 91,40(8) |
|
92,07(8) | 91,99(8) |
O12 | 171,96(8) | 85,90(8) | 92,27(8) | 92,07(8) |
|
81,64(8) |
O19 | 91,01(8) | 85,98(8) | 173,13(8) | 91,99(8) | 81,64(8) |
|
P3O10 in Na3CoP3O10·12H2O | ||||
---|---|---|---|---|
P1 | O1 | O2 | O3 | O4 |
O1 |
|
112,1(1) | 114,5(1) | 107,0(1) |
O2 | 112,1(1) |
|
111,7(1) | 107,7(1) |
O3 | 114,5(1) | 111,7(1) |
|
103,0(1) |
O4 | 107,0(1) | 107,7(1) | 103,0(1) |
|
| ||||
P2 | O4 | O5 | O6 | O7 |
| ||||
O4 |
|
109,1(1) | 109,1(1) | 100,9(1) |
O5 | 109,1(1) |
|
120,0(1) | 105,5(1) |
O6 | 109,1(1) | 120,0(1) |
|
110,5(1) |
O7 | 100,9(1) | 105,5(1) | 110,5(1) |
|
| ||||
P3 | O7 | O8 | O9 | O10 |
| ||||
O7 |
|
106,5(1) | 107,8(1) | 102,3(1) |
O8 | 106,5(1) |
|
112,2(1) | 113,4(1) |
O9 | 107,8(1) | 112,2(1) |
|
113,8(1) |
O10 | 102,3(1) | 113,4(1) | 113,8(1) |
|
∠(P1; O4; P2) = 158,3(2)°,
∠(P2; O7; P3) = 70.9(2)°,
Ni(1)O6 in Na3NiP3O10·12H2O | ||||||
---|---|---|---|---|---|---|
Ni1 | O2 | O6 | O9 | O11 | O12 | O19 |
O2 |
|
90,91(9) | 93,51(9) | 90,12(9) | 173,7(1) | 91,51(9) |
O6 | 90,91(9) |
|
91,32(9) | 178,45(9) | 86,63(9) | 86,27(9) |
O9 | 93,51(9) | 91,32(9) |
|
89,76(9) | 92,41(1) | 174,5(1) |
O11 | 90,12(9) | 178,45(9) | 89,76(9) |
|
92,22(9) | 92,55(9) |
O12 | 173,7(1) | 86,63(9) | 92,41(1) | 92,22(9) |
|
82,5(1) |
O19 | 91,51(9) | 86,27(9) | 174,5(1) | 92,55(9) | 82,5(1) |
|
P3O10 in Na3NiP3O10·12H2O | ||||
---|---|---|---|---|
P1 | O1 | O2 | O3 | O4 |
O1 |
|
112,5(1) | 114,3(1) | 106,91(1) |
O2 | 112,5(1) |
|
111,7(1) | 107,7(1) |
O3 | 114,3(1) | 111,7(1) |
|
103,0(1) |
O4 | 106,91(1) | 107,7(1) | 103,0(1) |
|
| ||||
P2 | O4 | O5 | O6 | O7 |
| ||||
O4 |
|
109,2(1) | 108,9(1) | 100,9(1) |
O5 | 109,2(1) |
|
119,5(1) | 106,0(1) |
O6 | 108,9(1) | 119,5(1) |
|
110,7(1) |
O7 | 100,9(1) | 106,0(1) | 110,7(1) |
|
| ||||
P3 | O7 | O8 | O9 | O10 |
| ||||
O7 |
|
106,0(1) | 107,7(1) | 102,4(1) |
O8 | 106,0(1) |
|
112,1(1) | 113,2(1) |
O9 | 107,7(1) | 112,1(1) |
|
114,4(1) |
O10 | 102,4(1) | 113,2(1) | 114,4(1) |
|
∠(P1; O4; P2) = 157.2(2)°,
∠(P2; O7; P3) = 71.3(2)°,
Supplementary tables of crystal structures and refinements, notably atomic positions, full list of bond lengths and angles, and anisotropic thermal parameters, have been deposited with the Inorganic Crystal Structure Database, FIZ, Hermann von Helmholtz Platz 1, 76344 EggensteinLeopoldshafen, Germany; fax: (+49) 7247 808 132; email: crysdata@fiz-karlsruhe.de. CCDC deposition numbers are, respectively, 884535 for Na3Co(P3O10)·12H2O and 884536 for Na3Ni(P3O10)·12H2O.
The infrared measurements were performed in transmission geometry using an FTIR Biorad spectrometer FTS-40A with dynamic alignment and a spectral resolution of 2 cm−1 in the range 400–4000 cm−1. 0.2 mg sample per 200 mg KBr has been pressed into pellets.
Na3MP3O10·12H2O [M = Co (
Hydrogen bonding parameters (Å, °) for (
( |
||||
---|---|---|---|---|
D–H | H |
D–A | D–H |
|
O11–H11A |
0.82(3) | 1.92(3) | 2.741(3) | 174(3) |
O11–H11B |
0.82(3) | 1.90(3) | 2.707(3) | 169(3) |
O12–H12A |
0.82(3) | 1.95(3) | 2.763(3) | 169(3) |
O12–H12B |
0.823(19) | 1.87(2) | 2.685(3) | 171(3) |
O13–H13B |
0.83(3) | 1.95(3) | 2.768(3) | 172(3) |
O14–H14A |
0.82(2) | 1.95(2) | 2.757(3) | 167(3) |
O14–H14B |
0.83(2) | 1.92(2) | 2.735(3) | 169(4) |
O17–H17A |
0.82(3) | 1.95(3) | 2.756(3) | 171(3) |
O17–H17B |
0.82(3) | 1.87(3) | 2.691(3) | 174(4) |
O19–H19A |
0.82(2) | 1.96(2) | 2.773(3) | 171(4) |
O19–H19B |
0.820(19) | 1.91(2) | 2.728(3) | 174(3) |
O20–H20B |
0.822(14) | 1.893(14) | 2.712(3) | 174(4) |
(i)
( |
||||
---|---|---|---|---|
D–H | H |
D–A | D–H | |
O11–H11A |
0.82(3) | 1.91(3) | 2.736(3) | 176(3) |
O12–H12A |
0.82(3) | 1.88(3) | 2.760(3) | 173(4) |
O12–H12B |
0.82(2) | 1.88(3) | 2.694(4) | 173(4) |
O16–H16A |
0.821(16) | 1.965(18) | 2.784(4) | 175(4) |
O18–H18A |
0.82(3) | 1.93(3) | 2.748(4) | 170(3) |
O18–H18B |
0.82(3) | 1.96(3) | 2.775(3) | 177(4) |
O19–H19A |
0.82(3) | 1.96(3) | 2.775(3) | 171(4) |
O19–H19B |
0.82(2) | 1.92(3) | 2.735(4) | 174(4) |
O22–H22B |
0.82(3) | 2.01(3) | 2.835(4) | 180(4) |
(i)
Projection of the crystal structures of Na3MP3O10·12H2O along
A slab in the crystal structures of the title compounds.
Details of the connection between the chains C1 and C2 inside a slab.
Phosphorous (
The Infrared spectra of (
I-R band assignments for (
Frequency |
Assigned vibration mode |
---|---|
3455 |
|
1648 |
|
1241 |
|
1204 |
|
1090 |
|
986 |
|
910 |
|
690 |
|
526 |
|
IR spectrum of Na3CoP3O10·12H2O.
The POP bridge vibrations always occur at lower frequency than the terminal P–O stretching modes. In the IR spectra, the asymmetric mode
Crystals of the title compounds have been synthesized using a wet chemistry route. Na3MP3O10·12H2O (M = Co, Ni) are isostructural and their framework can be described as two kinds of chains connected through O–P–O of P3O10 phosphate groups into slabs parallel with
The authors would like to thank the Grant Agency of the Czech Republic, Grant P204/11/0809.