Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100007769/qa0314sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100007769/qa0314Isup2.hkl |
CCDC reference: 147686
The synthesis of the title compound was carried out by hydrothermal reaction of ethylenediamine, V2O5, H3PO4, CoCl2·6H2O and H2O (molar ratio 5:8:5:1:1000) in a 25 ml acid-digestion bomb at 413 K for 5 d. Blue crystals were isolated from solution after cooling to room temperature.
Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1995); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); software used to prepare material for publication: SHELXTL.
(C2H10N2)4[Co(H2O)2(OH)2(VO)6(HPO4)4(PO4)4]·3H2O | F(000) = 3220 |
Mr = 1596.94 | Dx = 2.213 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 20.709 (4) Å | Cell parameters from 25 reflections |
b = 9.968 (2) Å | θ = 5.0–10.9° |
c = 23.660 (5) Å | µ = 1.86 mm−1 |
β = 101.04 (3)° | T = 293 K |
V = 4793.7 (17) Å3 | Block, blue |
Z = 4 | 0.50 × 0.40 × 0.38 mm |
Siemens P4 diffractometer | 3501 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.024 |
Graphite monochromator | θmax = 25.0°, θmin = 1.8° |
2θ/ω scans | h = −1→24 |
Absorption correction: empirical (using intensity measurements) (North et al., 1968) | k = −1→11 |
Tmin = 0.359, Tmax = 0.494 | l = −28→27 |
5341 measured reflections | 3 standard reflections every 97 reflections |
4207 independent reflections | intensity decay: none |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 1.12 | Calculated w = 1/[σ2(Fo2) + (0.0913P)2] where P = (Fo2 + 2Fc2)/3 |
4207 reflections | (Δ/σ)max = 0.001 |
336 parameters | Δρmax = 1.80 e Å−3 |
0 restraints | Δρmin = −1.69 e Å−3 |
(C2H10N2)4[Co(H2O)2(OH)2(VO)6(HPO4)4(PO4)4]·3H2O | V = 4793.7 (17) Å3 |
Mr = 1596.94 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 20.709 (4) Å | µ = 1.86 mm−1 |
b = 9.968 (2) Å | T = 293 K |
c = 23.660 (5) Å | 0.50 × 0.40 × 0.38 mm |
β = 101.04 (3)° |
Siemens P4 diffractometer | 3501 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) (North et al., 1968) | Rint = 0.024 |
Tmin = 0.359, Tmax = 0.494 | 3 standard reflections every 97 reflections |
5341 measured reflections | intensity decay: none |
4207 independent reflections |
R[F2 > 2σ(F2)] = 0.046 | 0 restraints |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 1.12 | Δρmax = 1.80 e Å−3 |
4207 reflections | Δρmin = −1.69 e Å−3 |
336 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Co | 0.2500 | −0.2500 | 0.5000 | 0.0384 (3) | |
V1 | 0.22125 (3) | 0.09168 (7) | 0.27765 (3) | 0.0160 (2) | |
V2 | 0.17376 (4) | −0.40369 (7) | 0.32715 (3) | 0.0187 (2) | |
V3 | 0.06009 (4) | −0.07764 (7) | 0.43582 (3) | 0.0182 (2) | |
P1 | 0.28549 (5) | 0.37706 (10) | 0.32515 (4) | 0.0167 (3) | |
P2 | 0.18977 (5) | −0.11582 (11) | 0.37636 (5) | 0.0173 (3) | |
P3 | −0.05823 (5) | −0.18513 (11) | 0.49544 (5) | 0.0189 (3) | |
P4 | 0.10602 (6) | −0.37116 (11) | 0.43938 (5) | 0.0197 (3) | |
O1 | 0.15114 (15) | −0.2081 (3) | 0.32945 (13) | 0.0204 (6) | |
O2 | 0.2313 (2) | −0.0123 (3) | 0.35033 (12) | 0.0225 (7) | |
O3 | 0.01460 (15) | −0.1583 (3) | 0.49552 (13) | 0.0223 (7) | |
O4 | 0.2742 (2) | 0.2248 (3) | 0.32873 (13) | 0.0224 (7) | |
O5 | 0.2353 (2) | −0.5501 (3) | 0.35506 (13) | 0.0249 (7) | |
O6 | 0.3551 (2) | 0.4121 (3) | 0.35639 (13) | 0.0242 (7) | |
O7 | 0.2579 (2) | 0.1666 (3) | 0.21342 (13) | 0.0238 (7) | |
O8 | 0.14280 (15) | −0.0382 (3) | 0.40686 (13) | 0.0224 (7) | |
O9 | 0.1405 (2) | −0.4499 (3) | 0.39867 (14) | 0.0265 (7) | |
O10 | −0.0673 (2) | −0.2855 (3) | 0.54122 (14) | 0.0297 (8) | |
O11 | 0.1469 (2) | 0.1401 (4) | 0.26592 (15) | 0.0313 (8) | |
O12 | 0.2244 (2) | −0.0819 (3) | 0.23882 (13) | 0.0219 (7) | |
O13 | 0.1549 (2) | −0.3132 (4) | 0.49062 (15) | 0.0381 (9) | |
O14 | 0.2390 (2) | −0.2028 (4) | 0.41724 (13) | 0.0298 (8) | |
O15 | 0.09492 (15) | 0.0546 (3) | 0.49691 (13) | 0.0229 (7) | |
O16 | 0.1187 (2) | −0.4633 (3) | 0.2776 (2) | 0.0358 (8) | |
O17 | 0.0604 (2) | −0.4661 (3) | 0.4658 (2) | 0.0389 (9) | |
O18 | −0.0925 (2) | −0.2473 (3) | 0.43606 (13) | 0.0240 (7) | |
O19 | 0.0037 (2) | −0.0049 (3) | 0.39172 (14) | 0.0292 (7) | |
O20 | 0.0640 (2) | −0.2602 (3) | 0.40825 (13) | 0.0236 (7) | |
N1 | 0.36370 (10) | −0.0199 (2) | 0.41107 (8) | 0.0300 (9) | |
H1A | 0.37983 (10) | 0.0588 (2) | 0.42487 (8) | 0.045* | |
H1B | 0.35447 (10) | −0.0698 (2) | 0.43971 (8) | 0.045* | |
H1C | 0.32718 (10) | −0.0067 (2) | 0.38496 (8) | 0.045* | |
N2 | 0.38178 (10) | −0.3256 (2) | 0.40340 (8) | 0.0342 (10) | |
H2A | 0.36805 (10) | −0.4030 (2) | 0.38644 (8) | 0.051* | |
H2B | 0.35231 (10) | −0.2961 (2) | 0.42334 (8) | 0.051* | |
H2C | 0.42020 (10) | −0.3381 (2) | 0.42711 (8) | 0.051* | |
N3 | 0.06603 (10) | −0.1107 (2) | 0.22898 (8) | 0.0295 (9) | |
H3A | 0.08493 (10) | −0.1114 (2) | 0.19822 (8) | 0.044* | |
H3B | 0.09652 (10) | −0.1230 (2) | 0.26058 (8) | 0.044* | |
H3C | 0.04629 (10) | −0.0320 (2) | 0.23115 (8) | 0.044* | |
N4 | 0.19249 (10) | 0.2383 (2) | 0.42662 (8) | 0.0356 (10) | |
H4A | 0.19799 (10) | 0.2025 (2) | 0.39342 (8) | 0.053* | |
H4B | 0.18399 (10) | 0.3255 (2) | 0.42174 (8) | 0.053* | |
H4C | 0.15899 (10) | 0.1981 (2) | 0.43834 (8) | 0.053* | |
C1 | 0.4131 (3) | −0.0901 (5) | 0.3839 (3) | 0.0400 (13) | |
H1D | 0.4531 (3) | −0.1022 (5) | 0.4124 (3) | 0.060* | |
H1E | 0.4236 (3) | −0.0342 (5) | 0.3533 (3) | 0.060* | |
C2 | 0.3897 (3) | −0.2256 (5) | 0.3591 (2) | 0.0357 (12) | |
H2D | 0.3479 (3) | −0.2144 (5) | 0.3329 (2) | 0.054* | |
H2E | 0.4211 (3) | −0.2597 (5) | 0.3370 (2) | 0.054* | |
C3 | 0.0163 (2) | −0.2205 (5) | 0.2240 (2) | 0.0304 (11) | |
H3D | 0.0376 (2) | −0.3062 (5) | 0.2211 (2) | 0.046* | |
H3E | −0.0167 (2) | −0.2079 (5) | 0.1893 (2) | 0.046* | |
C4 | 0.2541 (3) | 0.2195 (7) | 0.4711 (2) | 0.0433 (14) | |
H4D | 0.2907 (3) | 0.2622 (7) | 0.4581 (2) | 0.065* | |
H4E | 0.2637 (3) | 0.1245 (7) | 0.4761 (2) | 0.065* | |
OW1 | 0.0471 (3) | 0.3095 (6) | 0.3347 (2) | 0.081 (2) | |
OW2 | 0.0000 | 0.1262 (5) | 0.2500 | 0.0420 (13) | |
OW3 | 0.2777 (2) | −0.4354 (5) | 0.4750 (2) | 0.0500 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co | 0.0348 (6) | 0.0514 (7) | 0.0285 (5) | −0.0088 (5) | 0.0050 (4) | 0.0071 (5) |
V1 | 0.0164 (4) | 0.0159 (4) | 0.0163 (4) | −0.0008 (3) | 0.0045 (3) | 0.0004 (3) |
V2 | 0.0192 (4) | 0.0165 (4) | 0.0210 (4) | 0.0008 (3) | 0.0051 (3) | −0.0005 (3) |
V3 | 0.0172 (4) | 0.0189 (4) | 0.0190 (4) | 0.0007 (3) | 0.0044 (3) | −0.0026 (3) |
P1 | 0.0182 (6) | 0.0150 (5) | 0.0174 (5) | 0.0004 (4) | 0.0045 (4) | 0.0005 (4) |
P2 | 0.0184 (5) | 0.0165 (5) | 0.0179 (5) | −0.0006 (4) | 0.0055 (4) | 0.0020 (4) |
P3 | 0.0197 (6) | 0.0165 (5) | 0.0214 (6) | −0.0023 (4) | 0.0062 (4) | −0.0020 (4) |
P4 | 0.0209 (6) | 0.0175 (5) | 0.0227 (6) | −0.0005 (4) | 0.0094 (5) | 0.0015 (4) |
O1 | 0.0195 (15) | 0.0183 (15) | 0.024 (2) | −0.0005 (12) | 0.0069 (12) | −0.0016 (12) |
O2 | 0.023 (2) | 0.024 (2) | 0.0193 (15) | −0.0068 (13) | 0.0033 (12) | 0.0022 (13) |
O3 | 0.020 (2) | 0.024 (2) | 0.024 (2) | −0.0012 (13) | 0.0069 (13) | −0.0018 (13) |
O4 | 0.029 (2) | 0.0169 (15) | 0.021 (2) | −0.0035 (13) | 0.0034 (13) | 0.0007 (12) |
O5 | 0.027 (2) | 0.026 (2) | 0.024 (2) | 0.0089 (14) | 0.0112 (13) | 0.0048 (13) |
O6 | 0.022 (2) | 0.024 (2) | 0.026 (2) | −0.0048 (13) | 0.0044 (13) | −0.0011 (13) |
O7 | 0.029 (2) | 0.021 (2) | 0.023 (2) | −0.0038 (14) | 0.0118 (13) | −0.0005 (13) |
O8 | 0.020 (2) | 0.0197 (15) | 0.029 (2) | −0.0034 (13) | 0.0081 (13) | −0.0050 (13) |
O9 | 0.033 (2) | 0.0173 (15) | 0.034 (2) | 0.0047 (14) | 0.0183 (15) | 0.0022 (13) |
O10 | 0.039 (2) | 0.024 (2) | 0.029 (2) | −0.005 (2) | 0.013 (2) | 0.0022 (14) |
O11 | 0.023 (2) | 0.038 (2) | 0.034 (2) | 0.0046 (15) | 0.0079 (14) | 0.005 (2) |
O12 | 0.031 (2) | 0.0171 (15) | 0.0184 (15) | −0.0027 (13) | 0.0061 (13) | −0.0009 (12) |
O13 | 0.027 (2) | 0.062 (2) | 0.026 (2) | −0.009 (2) | 0.0077 (15) | 0.001 (2) |
O14 | 0.028 (2) | 0.042 (2) | 0.020 (2) | 0.010 (2) | 0.0076 (14) | 0.0162 (14) |
O15 | 0.021 (2) | 0.0217 (15) | 0.027 (2) | −0.0010 (13) | 0.0061 (13) | −0.0067 (13) |
O16 | 0.035 (2) | 0.027 (2) | 0.041 (2) | −0.003 (2) | −0.006 (2) | −0.004 (2) |
O17 | 0.049 (2) | 0.023 (2) | 0.056 (2) | −0.006 (2) | 0.038 (2) | 0.000 (2) |
O18 | 0.026 (2) | 0.0187 (15) | 0.026 (2) | −0.0026 (13) | 0.0021 (13) | −0.0062 (13) |
O19 | 0.029 (2) | 0.027 (2) | 0.029 (2) | 0.0049 (14) | 0.0023 (14) | −0.0001 (14) |
O20 | 0.029 (2) | 0.020 (2) | 0.022 (2) | 0.0047 (13) | 0.0062 (13) | −0.0019 (13) |
N1 | 0.031 (2) | 0.026 (2) | 0.030 (2) | −0.002 (2) | −0.001 (2) | −0.001 (2) |
N2 | 0.036 (2) | 0.032 (2) | 0.035 (2) | −0.001 (2) | 0.008 (2) | −0.008 (2) |
N3 | 0.022 (2) | 0.043 (2) | 0.025 (2) | 0.004 (2) | 0.008 (2) | 0.002 (2) |
N4 | 0.035 (2) | 0.041 (2) | 0.032 (2) | −0.003 (2) | 0.009 (2) | −0.001 (2) |
C1 | 0.035 (3) | 0.035 (3) | 0.051 (3) | −0.006 (2) | 0.014 (3) | −0.006 (2) |
C2 | 0.039 (3) | 0.037 (3) | 0.032 (3) | −0.001 (2) | 0.011 (2) | −0.005 (2) |
C3 | 0.029 (3) | 0.034 (3) | 0.026 (2) | 0.005 (2) | 0.001 (2) | −0.001 (2) |
C4 | 0.040 (3) | 0.059 (4) | 0.031 (3) | 0.010 (3) | 0.006 (2) | −0.004 (3) |
OW1 | 0.098 (4) | 0.085 (4) | 0.066 (3) | −0.035 (3) | 0.032 (3) | −0.021 (3) |
OW2 | 0.029 (3) | 0.039 (3) | 0.058 (4) | 0.000 | 0.008 (3) | 0.000 |
OW3 | 0.033 (2) | 0.068 (3) | 0.045 (2) | 0.008 (2) | −0.001 (2) | 0.022 (2) |
Co—O14i | 1.984 (3) | P1—O5iv | 1.546 (3) |
Co—O14 | 1.984 (3) | P2—O8 | 1.528 (3) |
Co—O13 | 2.038 (4) | P2—O14 | 1.532 (3) |
Co—O13i | 2.038 (4) | P2—O1 | 1.542 (3) |
Co—OW3i | 2.056 (5) | P2—O2 | 1.544 (3) |
Co—OW3 | 2.056 (5) | P3—O10 | 1.513 (3) |
V1—O11 | 1.586 (3) | P3—O3 | 1.531 (3) |
V1—O12 | 1.966 (3) | P3—O15v | 1.535 (3) |
V1—O7 | 1.971 (3) | P3—O18 | 1.575 (3) |
V1—O4 | 1.979 (3) | P4—O20 | 1.508 (3) |
V1—O2 | 1.985 (3) | P4—O9 | 1.522 (3) |
V2—O16 | 1.586 (3) | P4—O13 | 1.536 (4) |
V2—O5 | 1.966 (3) | P4—O17 | 1.551 (3) |
V2—O7ii | 1.983 (3) | O5—P1vi | 1.546 (3) |
V2—O9 | 1.999 (3) | O7—V2iii | 1.983 (3) |
V2—O1 | 2.009 (3) | O12—P1ii | 1.543 (3) |
V3—O19 | 1.585 (3) | O15—P3v | 1.535 (3) |
V3—O20 | 1.940 (3) | N1—C1 | 1.483 (6) |
V3—O15 | 1.987 (3) | N2—C2 | 1.479 (6) |
V3—O8 | 2.002 (3) | N3—C3 | 1.492 (5) |
V3—O3 | 2.010 (3) | N4—C4 | 1.501 (6) |
P1—O6 | 1.529 (3) | C1—C2 | 1.515 (7) |
P1—O4 | 1.541 (3) | C3—C3vii | 1.515 (9) |
P1—O12iii | 1.543 (3) | C4—C4viii | 1.535 (10) |
O14i—Co—O14 | 180.0 | O15—V3—O3 | 84.72 (13) |
O14i—Co—O13 | 87.73 (14) | O8—V3—O3 | 150.00 (13) |
O14—Co—O13 | 92.27 (14) | O6—P1—O4 | 109.7 (2) |
O14i—Co—O13i | 92.27 (14) | O6—P1—O12iii | 110.4 (2) |
O14—Co—O13i | 87.73 (14) | O4—P1—O12iii | 108.8 (2) |
O13—Co—O13i | 180.0 | O6—P1—O5iv | 109.0 (2) |
O14i—Co—OW3i | 85.14 (15) | O4—P1—O5iv | 108.4 (2) |
O14—Co—OW3i | 94.86 (15) | O12iii—P1—O5iv | 110.5 (2) |
O13—Co—OW3i | 89.5 (2) | O8—P2—O14 | 113.3 (2) |
O13i—Co—OW3i | 90.5 (2) | O8—P2—O1 | 110.6 (2) |
O14i—Co—OW3 | 94.86 (15) | O14—P2—O1 | 107.9 (2) |
O14—Co—OW3 | 85.14 (15) | O8—P2—O2 | 107.7 (2) |
O13—Co—OW3 | 90.5 (2) | O14—P2—O2 | 106.0 (2) |
O13i—Co—OW3 | 89.5 (2) | O1—P2—O2 | 111.3 (2) |
OW3i—Co—OW3 | 180.0 | O10—P3—O3 | 111.9 (2) |
O11—V1—O12 | 107.7 (2) | O10—P3—O15v | 110.1 (2) |
O11—V1—O7 | 104.7 (2) | O3—P3—O15v | 111.2 (2) |
O12—V1—O7 | 85.49 (13) | O10—P3—O18 | 106.4 (2) |
O11—V1—O4 | 108.0 (2) | O3—P3—O18 | 110.2 (2) |
O12—V1—O4 | 144.23 (14) | O15v—P3—O18 | 106.8 (2) |
O7—V1—O4 | 88.07 (13) | O20—P4—O9 | 111.4 (2) |
O11—V1—O2 | 104.3 (2) | O20—P4—O13 | 109.9 (2) |
O12—V1—O2 | 86.42 (12) | O9—P4—O13 | 112.0 (2) |
O7—V1—O2 | 150.92 (14) | O20—P4—O17 | 107.8 (2) |
O4—V1—O2 | 82.37 (12) | O9—P4—O17 | 109.7 (2) |
O16—V2—O5 | 107.3 (2) | O13—P4—O17 | 105.7 (2) |
O16—V2—O7ii | 104.7 (2) | P2—O1—V2 | 120.5 (2) |
O5—V2—O7ii | 87.05 (13) | P2—O2—V1 | 136.1 (2) |
O16—V2—O9 | 102.9 (2) | P3—O3—V3 | 131.5 (2) |
O5—V2—O9 | 81.41 (13) | P1—O4—V1 | 134.3 (2) |
O7ii—V2—O9 | 152.16 (14) | P1vi—O5—V2 | 130.1 (2) |
O16—V2—O1 | 104.2 (2) | V1—O7—V2iii | 130.9 (2) |
O5—V2—O1 | 148.31 (14) | P2—O8—V3 | 136.6 (2) |
O7ii—V2—O1 | 82.06 (12) | P4—O9—V2 | 134.1 (2) |
O9—V2—O1 | 94.64 (12) | P1ii—O12—V1 | 133.0 (2) |
O19—V3—O20 | 106.3 (2) | P4—O13—Co | 132.8 (2) |
O19—V3—O15 | 107.1 (2) | P2—O14—Co | 134.0 (2) |
O20—V3—O15 | 146.51 (13) | P3v—O15—V3 | 122.0 (2) |
O19—V3—O8 | 104.8 (2) | P4—O20—V3 | 125.5 (2) |
O20—V3—O8 | 88.57 (13) | N1—C1—C2 | 113.2 (4) |
O15—V3—O8 | 84.47 (13) | N2—C2—C1 | 113.4 (4) |
O19—V3—O3 | 105.1 (2) | N3—C3—C3vii | 110.1 (3) |
O20—V3—O3 | 85.20 (13) | N4—C4—C4viii | 110.6 (6) |
Symmetry codes: (i) −x+1/2, −y−1/2, −z+1; (ii) −x+1/2, y−1/2, −z+1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x, y+1, z; (v) −x, −y, −z+1; (vi) x, y−1, z; (vii) −x, y, −z+1/2; (viii) −x+1/2, −y+1/2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | (C2H10N2)4[Co(H2O)2(OH)2(VO)6(HPO4)4(PO4)4]·3H2O |
Mr | 1596.94 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 293 |
a, b, c (Å) | 20.709 (4), 9.968 (2), 23.660 (5) |
β (°) | 101.04 (3) |
V (Å3) | 4793.7 (17) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.86 |
Crystal size (mm) | 0.50 × 0.40 × 0.38 |
Data collection | |
Diffractometer | Siemens P4 diffractometer |
Absorption correction | Empirical (using intensity measurements) (North et al., 1968) |
Tmin, Tmax | 0.359, 0.494 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5341, 4207, 3501 |
Rint | 0.024 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.137, 1.12 |
No. of reflections | 4207 |
No. of parameters | 336 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.80, −1.69 |
Computer programs: XSCANS (Siemens, 1994), XSCANS, SHELXTL (Siemens, 1995), SHELXS86 (Sheldrick, 1990), SHELXL93 (Sheldrick, 1993), SHELXTL.
Co—O14 | 1.984 (3) | V3—O8 | 2.002 (3) |
Co—O13 | 2.038 (4) | V3—O3 | 2.010 (3) |
Co—OW3 | 2.056 (5) | P1—O6 | 1.529 (3) |
V1—O11 | 1.586 (3) | P1—O4 | 1.541 (3) |
V1—O12 | 1.966 (3) | P2—O8 | 1.528 (3) |
V1—O7 | 1.971 (3) | P2—O14 | 1.532 (3) |
V1—O4 | 1.979 (3) | P2—O1 | 1.542 (3) |
V1—O2 | 1.985 (3) | P2—O2 | 1.544 (3) |
V2—O16 | 1.586 (3) | P3—O10 | 1.513 (3) |
V2—O5 | 1.966 (3) | P3—O3 | 1.531 (3) |
V2—O9 | 1.999 (3) | P3—O18 | 1.575 (3) |
V2—O1 | 2.009 (3) | P4—O20 | 1.508 (3) |
V3—O19 | 1.585 (3) | P4—O9 | 1.522 (3) |
V3—O20 | 1.940 (3) | P4—O13 | 1.536 (4) |
V3—O15 | 1.987 (3) | P4—O17 | 1.551 (3) |
O14—Co—O13 | 92.27 (14) | O15—V3—O3 | 84.72 (13) |
O14—Co—OW3 | 85.14 (15) | O8—V3—O3 | 150.00 (13) |
O13—Co—OW3 | 90.5 (2) | O6—P1—O4 | 109.7 (2) |
O11—V1—O12 | 107.7 (2) | O8—P2—O14 | 113.3 (2) |
O11—V1—O7 | 104.7 (2) | O8—P2—O1 | 110.6 (2) |
O12—V1—O7 | 85.49 (13) | O14—P2—O1 | 107.9 (2) |
O11—V1—O4 | 108.0 (2) | O8—P2—O2 | 107.7 (2) |
O12—V1—O4 | 144.23 (14) | O14—P2—O2 | 106.0 (2) |
O7—V1—O4 | 88.07 (13) | O1—P2—O2 | 111.3 (2) |
O11—V1—O2 | 104.3 (2) | O10—P3—O3 | 111.9 (2) |
O12—V1—O2 | 86.42 (12) | O10—P3—O18 | 106.4 (2) |
O7—V1—O2 | 150.92 (14) | O3—P3—O18 | 110.2 (2) |
O4—V1—O2 | 82.37 (12) | O20—P4—O9 | 111.4 (2) |
O16—V2—O5 | 107.3 (2) | O20—P4—O13 | 109.9 (2) |
O16—V2—O9 | 102.9 (2) | O9—P4—O13 | 112.0 (2) |
O5—V2—O9 | 81.41 (13) | O20—P4—O17 | 107.8 (2) |
O16—V2—O1 | 104.2 (2) | O9—P4—O17 | 109.7 (2) |
O5—V2—O1 | 148.31 (14) | O13—P4—O17 | 105.7 (2) |
O9—V2—O1 | 94.64 (12) | P2—O1—V2 | 120.5 (2) |
O19—V3—O20 | 106.3 (2) | P2—O2—V1 | 136.1 (2) |
O19—V3—O15 | 107.1 (2) | P3—O3—V3 | 131.5 (2) |
O20—V3—O15 | 146.51 (13) | P1—O4—V1 | 134.3 (2) |
O19—V3—O8 | 104.8 (2) | P2—O8—V3 | 136.6 (2) |
O20—V3—O8 | 88.57 (13) | P4—O9—V2 | 134.1 (2) |
O15—V3—O8 | 84.47 (13) | P4—O13—Co | 132.8 (2) |
O19—V3—O3 | 105.1 (2) | P2—O14—Co | 134.0 (2) |
O20—V3—O3 | 85.20 (13) | P4—O20—V3 | 125.5 (2) |
Structures similar to the title compound that have been reported are as follows: [(VO)3(H2O)2(PO4)2(HPO4)]2− (Lu et al., 1998), [(VO)2(PO4)2]2−, [VO]3(HPO4)2(PO4)2]4− (Soghomonian et al., 1994), [V(OH)(PO4)2(H2)]− (Soghomonian et al., 1998), [VO4(OH)4(PO4)2]2−, [(VO)5(OH)2(PO4)4]2−, [(VO)8(HPO4)3(PO4)4(OH)2]4−,[(VO)3(OH)2(PO4)2]2− (Soghomonian et al., 1995), [(VO)V(HPO4)3(H2O)2]− (Haushalter et al., 1993), [V(H2O)2(VO)8(OH)4(HPO4)4(PO4)4(H2O)2]5− (Soghomonian et al., 1993) and [(VO)3(PO4)(HPO4)]2− (Brircsak et al., 1998). The polyanion structure of the title compound, (I), consists of {V3P4} basic units, which are built up from PO4 tetrahedra and VO5 square pyramids in a corner-sharing linkage mode, leading to a one-dimensional chain. The connection of P2—O8—V3—O20—P4—O9—V2—O1—P2 gives rise to an eight-membered ring in which P2 links P2—O2—V1—O4—P1 and V3 links V3—O3—P3; thus, an infinite one-dimensional chain is formed. The chains are connected by CoO4(H2O)2 octahedra resulting in the formation of layers of the polyanions. Connecting Co with P—V—O also produces two eight-membered rings, namely Co—O13—P4—O20—V3—O8—P2—O14—Co and Co—O13—P4—O9—V2—P2—O14—Co. The PO4 tetrahedra are slightly distorted, with P—O distances ranging from 1.057 to 1.575 Å and angles from 105.7 (2) to 113.3 (2)°. The VO5 square pyramids are also distorted, with V—O distances in the ring of 1.585 (3)–2.010 (3) Å and angles of 104.3 (2)–108.0 (2)°, in addition, the geometry within the CoO4(H2O)2 octahedra are as follows: Co—O13 2.038 (4) Å, Co—O14 1.984 (3) Å and Co—OW3 2.056 (5) Å; O14A—Co—O14, OW3A—Co—OW3 and O13—Co—O13A are all 180°, while the remaining angles are in the range 85.1 (2)–94.9 (2)°; therefore, the title compound exhibits a two-dimensional layered structure constructed from diprotonated ethylenediammonium cations, (H2en)2+, and the polyanion [Co(H2O)2(OH)2(VO)6(HPO4)4(PO4)4]8−, with the organic ammonium cations and water molecules intercalated between the layers.