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Both the cation and anion in the title compound, [Mg(H2O)6][Mo2O5(C6H7NO6)2]·6H2O, lie on centers of symmetry, and their metals are both six-coordinate in octahedral environments.
Supporting information
CCDC reference: 180519
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.028
- wR factor = 0.076
- Data-to-parameter ratio = 14.3
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
PLAT_701 Alert C Bond Calc 1.8796(3), Rep 1.8800(10), Dev. 1.33 Sigma
MO1 -O7 1.555 1.555
PLAT_731 Alert C Bond Calc 1.8796(3), Rep 1.8800(10) .... 3.33 s.u-Ratio
MO1 -O7 1.555 1.555
PLAT_731 Alert C Bond Calc 0.84(3), Rep 0.842(10) .... 3.00 s.u-Ratio
O5 -H5 1.555 1.555
PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.840(10) .... 3.00 s.u-Ratio
O5 -H5 1.555 1.555
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
4 Alert Level C = Please check
Magnesium molybdate (10 mmol) dissolved in water (10 ml) was added to
nitrilotriacetic acid (20 mmol) dissolved in water (5 ml) and the mixture was
stirred for several hours. The solution was concentrated to about 10 ml;
colorless crystals of the title hydrate, (I), separated from the solution in
35% yield when it was set aside for several days.
The acid H atom was located and refined. The H atoms of the water molecules were
located in the difference maps, but these were not refined. For the O3w water,
one of its H atoms is disordered over two positions.
Data collection: CAD-4 VAX/PC Fortran System (Enraf-Nonius, 1988); cell refinement: CAD-4 VAX/PC Fortran System; data reduction: XCAD4 (Harms, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Hexaaquamagnesium
bis[
trans[nitrilotriacetato(2-)-O
1,
N,
O2]-µ-oxo-
cis-dioxomolybdate(VI)] hexahydrate
top
Crystal data top
[Mg(H2O)6][Mo2O5(C6H7NO6)2]·6H2O | Z = 1 |
Mr = 890.63 | F(000) = 452 |
Triclinic, P1 | Dx = 1.881 Mg m−3 |
a = 6.4787 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.2555 (6) Å | Cell parameters from 25 reflections |
c = 13.9995 (6) Å | θ = 12.5–13.0° |
α = 91.014 (4)° | µ = 0.93 mm−1 |
β = 101.315 (3)° | T = 293 K |
γ = 106.592 (4)° | Irregular block, colorless |
V = 786.44 (7) Å3 | 0.58 × 0.58 × 0.36 mm |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 2877 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.010 |
Graphite monochromator | θmax = 26.0°, θmin = 1.5° |
ω scans | h = 0→7 |
Absorption correction: empirical (using intensity measurements) via ψ scans (North et al., 1968) | k = −11→10 |
Tmin = 0.618, Tmax = 0.716 | l = −17→16 |
3339 measured reflections | 3 standard reflections every 60 min |
3079 independent reflections | intensity decay: none |
Refinement top
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.076 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0442P)2 + 0.3336P] where P = (Fo2 + 2Fc2)/3 |
3079 reflections | (Δ/σ)max < 0.001 |
215 parameters | Δρmax = 0.38 e Å−3 |
1 restraint | Δρmin = −0.52 e Å−3 |
Crystal data top
[Mg(H2O)6][Mo2O5(C6H7NO6)2]·6H2O | γ = 106.592 (4)° |
Mr = 890.63 | V = 786.44 (7) Å3 |
Triclinic, P1 | Z = 1 |
a = 6.4787 (3) Å | Mo Kα radiation |
b = 9.2555 (6) Å | µ = 0.93 mm−1 |
c = 13.9995 (6) Å | T = 293 K |
α = 91.014 (4)° | 0.58 × 0.58 × 0.36 mm |
β = 101.315 (3)° | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 2877 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) via ψ scans (North et al., 1968) | Rint = 0.010 |
Tmin = 0.618, Tmax = 0.716 | 3 standard reflections every 60 min |
3339 measured reflections | intensity decay: none |
3079 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.028 | 1 restraint |
wR(F2) = 0.076 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | Δρmax = 0.38 e Å−3 |
3079 reflections | Δρmin = −0.52 e Å−3 |
215 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo1 | 0.34964 (4) | 0.47655 (3) | 0.603349 (16) | 0.02808 (9) | |
Mg1 | 1.0000 | 1.0000 | 1.0000 | 0.0343 (3) | |
O1 | 0.3185 (3) | 0.4629 (3) | 0.74794 (15) | 0.0404 (5) | |
O2 | 0.3638 (4) | 0.3656 (3) | 0.89032 (17) | 0.0577 (7) | |
O3 | 0.6482 (3) | 0.6415 (2) | 0.68279 (15) | 0.0389 (5) | |
O4 | 0.9863 (4) | 0.6962 (2) | 0.77156 (18) | 0.0506 (6) | |
O5 | 0.7428 (4) | 0.0227 (3) | 0.57847 (17) | 0.0511 (6) | |
O6 | 0.8650 (4) | 0.1455 (2) | 0.72709 (15) | 0.0459 (5) | |
O7 | 0.5000 | 0.5000 | 0.5000 | 0.0396 (7) | |
O8 | 0.2116 (4) | 0.6077 (2) | 0.58794 (16) | 0.0428 (5) | |
O9 | 0.1564 (3) | 0.3076 (2) | 0.56796 (16) | 0.0444 (5) | |
O1w | 1.0316 (4) | 0.9713 (2) | 0.85900 (14) | 0.0426 (5) | |
O2w | 1.0153 (5) | 1.2215 (3) | 0.9790 (2) | 0.0599 (7) | |
O3w | 0.6571 (4) | 0.9411 (3) | 0.95741 (19) | 0.0623 (7) | |
O4w | 0.7418 (7) | 1.3545 (5) | 1.0429 (3) | 0.1053 (13) | |
O5w | 1.0722 (4) | −0.0913 (3) | 0.60962 (18) | 0.0542 (6) | |
O6w | 0.4555 (5) | 0.8498 (4) | 0.7693 (2) | 0.0842 (10) | |
N1 | 0.5904 (3) | 0.3352 (2) | 0.67952 (15) | 0.0267 (4) | |
C1 | 0.3885 (5) | 0.3731 (3) | 0.8055 (2) | 0.0377 (6) | |
C2 | 0.4974 (6) | 0.2705 (4) | 0.7630 (2) | 0.0452 (7) | |
H2A | 0.6140 | 0.2550 | 0.8131 | 0.054* | |
H2B | 0.3899 | 0.1728 | 0.7415 | 0.054* | |
C3 | 0.8167 (4) | 0.6052 (3) | 0.7247 (2) | 0.0318 (6) | |
C4 | 0.8117 (5) | 0.4423 (3) | 0.7110 (3) | 0.0443 (7) | |
H4A | 0.8978 | 0.4340 | 0.6629 | 0.053* | |
H4B | 0.8824 | 0.4132 | 0.7722 | 0.053* | |
C5 | 0.7485 (5) | 0.1248 (3) | 0.6462 (2) | 0.0354 (6) | |
C6 | 0.5926 (5) | 0.2150 (3) | 0.6092 (2) | 0.0353 (6) | |
H6A | 0.6317 | 0.2610 | 0.5510 | 0.042* | |
H6B | 0.4447 | 0.1461 | 0.5902 | 0.042* | |
H5 | 0.843 (4) | −0.016 (4) | 0.601 (2) | 0.056 (12)* | |
H1w1 | 1.0233 | 0.8858 | 0.8332 | 0.050* | |
H1w2 | 0.9823 | 1.0221 | 0.8143 | 0.050* | |
H2w1 | 0.9293 | 1.2660 | 0.9953 | 0.050* | |
H2w2 | 1.0986 | 1.2772 | 0.9458 | 0.050* | |
H3w1 | 0.5977 | 0.9203 | 0.8990 | 0.050* | |
H3w2 | 0.5856 | 0.9740 | 0.9910 | 0.050* | 0.50 |
H3w3 | 0.6277 | 0.8500 | 0.9751 | 0.050* | 0.50 |
H4w1 | 0.7529 | 1.4325 | 1.0777 | 0.050* | |
H4w2 | 0.6264 | 1.3342 | 0.9983 | 0.050* | |
H5w1 | 1.0742 | −0.1305 | 0.5552 | 0.050* | |
H5w2 | 1.1608 | −0.1149 | 0.6550 | 0.050* | |
H6w1 | 0.3182 | 0.8054 | 0.7596 | 0.050* | |
H6w2 | 0.5152 | 0.8027 | 0.7361 | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo1 | 0.02445 (14) | 0.03280 (14) | 0.02907 (14) | 0.01239 (9) | 0.00459 (9) | 0.00228 (9) |
Mg1 | 0.0404 (7) | 0.0338 (7) | 0.0317 (7) | 0.0143 (6) | 0.0099 (6) | 0.0015 (5) |
O1 | 0.0386 (11) | 0.0567 (13) | 0.0356 (10) | 0.0256 (10) | 0.0126 (9) | 0.0068 (9) |
O2 | 0.0668 (16) | 0.0832 (18) | 0.0387 (12) | 0.0357 (14) | 0.0263 (11) | 0.0157 (12) |
O3 | 0.0335 (11) | 0.0317 (10) | 0.0495 (12) | 0.0123 (8) | 0.0003 (9) | −0.0011 (9) |
O4 | 0.0359 (12) | 0.0375 (12) | 0.0700 (16) | 0.0099 (10) | −0.0053 (11) | −0.0170 (11) |
O5 | 0.0577 (15) | 0.0472 (13) | 0.0512 (13) | 0.0303 (12) | −0.0022 (11) | −0.0151 (10) |
O6 | 0.0641 (15) | 0.0459 (12) | 0.0340 (11) | 0.0319 (11) | 0.0018 (10) | 0.0041 (9) |
O7 | 0.0437 (17) | 0.0493 (17) | 0.0348 (15) | 0.0235 (14) | 0.0143 (13) | 0.0091 (12) |
O8 | 0.0406 (12) | 0.0507 (13) | 0.0446 (12) | 0.0264 (10) | 0.0068 (9) | 0.0067 (10) |
O9 | 0.0345 (11) | 0.0416 (12) | 0.0498 (13) | 0.0059 (9) | −0.0005 (9) | 0.0014 (9) |
O1w | 0.0659 (15) | 0.0377 (11) | 0.0303 (10) | 0.0251 (10) | 0.0101 (10) | 0.0037 (8) |
O2w | 0.0855 (19) | 0.0405 (13) | 0.0723 (17) | 0.0271 (13) | 0.0462 (15) | 0.0181 (11) |
O3w | 0.0448 (14) | 0.0840 (19) | 0.0569 (15) | 0.0208 (13) | 0.0071 (11) | −0.0164 (13) |
O4w | 0.117 (3) | 0.121 (3) | 0.098 (3) | 0.084 (3) | 0.000 (2) | −0.026 (2) |
O5w | 0.0687 (16) | 0.0527 (14) | 0.0516 (14) | 0.0321 (13) | 0.0158 (12) | 0.0029 (11) |
O6w | 0.0652 (19) | 0.094 (2) | 0.090 (2) | 0.0301 (17) | 0.0020 (16) | −0.0411 (18) |
N1 | 0.0254 (11) | 0.0267 (11) | 0.0287 (11) | 0.0093 (9) | 0.0053 (9) | 0.0009 (8) |
C1 | 0.0310 (14) | 0.0463 (17) | 0.0369 (15) | 0.0095 (13) | 0.0122 (12) | 0.0043 (12) |
C2 | 0.059 (2) | 0.0463 (17) | 0.0443 (17) | 0.0270 (16) | 0.0252 (15) | 0.0159 (14) |
C3 | 0.0285 (14) | 0.0309 (14) | 0.0353 (14) | 0.0077 (11) | 0.0067 (11) | −0.0025 (11) |
C4 | 0.0268 (14) | 0.0333 (15) | 0.070 (2) | 0.0113 (12) | 0.0012 (14) | −0.0035 (14) |
C5 | 0.0436 (16) | 0.0276 (13) | 0.0386 (16) | 0.0137 (12) | 0.0127 (13) | 0.0027 (11) |
C6 | 0.0421 (16) | 0.0355 (14) | 0.0308 (13) | 0.0181 (13) | 0.0038 (12) | −0.0008 (11) |
Geometric parameters (Å, º) top
Mo1—O1 | 2.076 (2) | O2w—H2w1 | 0.843 (2) |
Mo1—O3 | 2.172 (2) | O2w—H2w2 | 0.849 (2) |
Mo1—O7 | 1.880 (1) | O3w—H3w1 | 0.827 (2) |
Mo1—O8 | 1.695 (2) | O3w—H3w2 | 0.830 (2) |
Mo1—O9 | 1.694 (2) | O3w—H3w3 | 0.861 (3) |
Mo1—N1 | 2.418 (2) | O4w—H4w1 | 0.841 (3) |
Mg1—O1w | 2.045 (2) | O4w—H4w2 | 0.847 (4) |
Mg1—O1wi | 2.045 (2) | O5w—H5w1 | 0.842 (2) |
Mg1—O2w | 2.053 (2) | O5w—H5w2 | 0.845 (2) |
Mg1—O2wi | 2.053 (2) | O6w—H6w1 | 0.848 (3) |
Mg1—O3w | 2.089 (3) | O6w—H6w2 | 0.845 (3) |
Mg1—O3wi | 2.089 (3) | N1—C4 | 1.469 (4) |
Mg1—H3w3 | 2.3677 (1) | N1—C2 | 1.477 (4) |
O1—C1 | 1.281 (4) | N1—C6 | 1.478 (3) |
O2—C1 | 1.229 (4) | C1—C2 | 1.511 (4) |
O3—C3 | 1.270 (3) | C2—H2A | 0.9700 |
O4—C3 | 1.231 (3) | C2—H2b | 0.9700 |
O5—C5 | 1.314 (3) | C3—C4 | 1.507 (4) |
O5—H5 | 0.842 (10) | C4—H4a | 0.9700 |
O6—C5 | 1.210 (4) | C4—H4b | 0.9700 |
O7—Mo1ii | 1.8796 (2) | C5—C6 | 1.510 (4) |
O1w—H1w1 | 0.847 (2) | C6—H6a | 0.9700 |
O1w—H1w2 | 0.855 (2) | C6—H6b | 0.9700 |
| | | |
O1—Mo1—O3 | 76.6 (1) | Mg1—O2w—H2w2 | 124.1 (2) |
O1—Mo1—O7 | 155.9 (1) | H2w1—O2w—H2w2 | 110.5 (3) |
O1—Mo1—O8 | 91.1 (1) | Mg1—O3w—H3w1 | 119.7 (2) |
O1—Mo1—O9 | 92.5 (1) | Mg1—O3w—H3w2 | 119.8 (2) |
O1—Mo1—N1 | 73.1 (1) | H3w1—O3w—H3w2 | 114.9 (3) |
O3—Mo1—O7 | 83.9 (1) | Mg1—O3w—H3w3 | 98.00 (19) |
O3—Mo1—O8 | 92.1 (1) | H3w1—O3w—H3w3 | 97.5 (3) |
O3—Mo1—O9 | 159.5 (1) | H3w2—O3w—H3w3 | 98.2 (3) |
O3—Mo1—N1 | 73.4 (1) | H4w1—O4w—H4w2 | 110.2 (4) |
O7—Mo1—O8 | 103.8 (1) | H5w1—O5w—H5w2 | 110.7 (3) |
O7—Mo1—O9 | 101.4 (1) | H6w1—O6w—H6w2 | 109.8 (3) |
O7—Mo1—N1 | 88.0 (1) | C4—N1—C2 | 112.2 (3) |
O8—Mo1—O9 | 105.6 (1) | C4—N1—C6 | 110.6 (2) |
O8—Mo1—N1 | 160.5 (1) | C2—N1—C6 | 111.2 (2) |
O9—Mo1—N1 | 86.9 (1) | C4—N1—Mo1 | 107.37 (16) |
O1w—Mg1—O1wi | 180.000 (1) | C2—N1—Mo1 | 105.22 (16) |
O1w—Mg1—O2w | 89.1 (1) | C6—N1—Mo1 | 110.05 (15) |
O1wi—Mg1—O2w | 90.89 (9) | O2—C1—O1 | 122.7 (3) |
O1w—Mg1—O2wi | 90.89 (9) | O2—C1—C2 | 120.7 (3) |
O1wi—Mg1—O2wi | 89.11 (9) | O1—C1—C2 | 116.5 (2) |
O2w—Mg1—O2wi | 180.000 (1) | N1—C2—C1 | 111.4 (2) |
O1w—Mg1—O3wi | 88.28 (10) | N1—C2—H2a | 109.3 |
O1wi—Mg1—O3wi | 91.72 (10) | C1—C2—H2a | 109.3 |
O2w—Mg1—O3wi | 90.73 (12) | N1—C2—H2b | 109.3 |
O2wi—Mg1—O3wi | 89.27 (12) | C1—C2—H2b | 109.3 |
O1w—Mg1—O3w | 91.7 (1) | H2a—C2—H2b | 108.0 |
O1wi—Mg1—O3w | 88.28 (10) | O4—C3—O3 | 123.9 (3) |
O2w—Mg1—O3w | 89.3 (1) | O4—C3—C4 | 118.4 (3) |
O2wi—Mg1—O3w | 90.73 (12) | O3—C3—C4 | 117.5 (2) |
O3wi—Mg1—O3w | 180.000 (1) | N1—C4—C3 | 114.8 (2) |
O1w—Mg1—H3w3 | 96.02 (7) | N1—C4—H4a | 108.6 |
O1wi—Mg1—H3w3 | 83.98 (7) | C3—C4—H4a | 108.6 |
O2w—Mg1—H3w3 | 109.95 (8) | N1—C4—H4b | 108.6 |
O2wi—Mg1—H3w3 | 70.05 (8) | C3—C4—H4b | 108.6 |
O3wi—Mg1—H3w3 | 158.89 (8) | H4a—C4—H4b | 107.6 |
O3w—Mg1—H3w3 | 21.11 (8) | O6—C5—O5 | 124.8 (3) |
C1—O1—Mo1 | 124.28 (18) | O6—C5—C6 | 124.2 (2) |
C3—O3—Mo1 | 122.70 (17) | O5—C5—C6 | 111.0 (2) |
C5—O5—H5 | 106 (2) | N1—C6—C5 | 115.1 (2) |
Mo1—O7—Mo1ii | 180.0 | N1—C6—H6a | 108.5 |
Mg1—O1w—H1w1 | 122.08 (17) | C5—C6—H6a | 108.5 |
Mg1—O1w—H1w2 | 121.22 (17) | N1—C6—H6b | 108.5 |
H1w1—O1w—H1w2 | 108.4 (2) | C5—C6—H6b | 108.5 |
Mg1—O2w—H2w1 | 125.0 (2) | H6a—C6—H6b | 107.5 |
| | | |
O9—Mo1—O1—C1 | 72.2 (2) | O7—Mo1—N1—C6 | −51.03 (17) |
O8—Mo1—O1—C1 | 177.8 (2) | O1—Mo1—N1—C6 | 144.10 (19) |
O7—Mo1—O1—C1 | −53.4 (3) | O3—Mo1—N1—C6 | −135.28 (19) |
O3—Mo1—O1—C1 | −90.2 (2) | Mo1—O1—C1—O2 | −178.6 (2) |
N1—Mo1—O1—C1 | −13.8 (2) | Mo1—O1—C1—C2 | −0.8 (4) |
O9—Mo1—O3—C3 | 22.5 (4) | C4—N1—C2—C1 | 84.4 (3) |
O8—Mo1—O3—C3 | 172.6 (2) | C6—N1—C2—C1 | −151.1 (3) |
O7—Mo1—O3—C3 | −83.8 (2) | Mo1—N1—C2—C1 | −32.0 (3) |
O1—Mo1—O3—C3 | 81.9 (2) | O2—C1—C2—N1 | −157.0 (3) |
N1—Mo1—O3—C3 | 5.9 (2) | O1—C1—C2—N1 | 25.2 (4) |
O9—Mo1—N1—C4 | 170.9 (2) | Mo1—O3—C3—O4 | −178.7 (2) |
O8—Mo1—N1—C4 | −58.4 (3) | Mo1—O3—C3—C4 | 5.0 (4) |
O7—Mo1—N1—C4 | 69.39 (18) | C2—N1—C4—C3 | −92.9 (3) |
O1—Mo1—N1—C4 | −95.48 (19) | C6—N1—C4—C3 | 142.3 (3) |
O3—Mo1—N1—C4 | −14.86 (19) | Mo1—N1—C4—C3 | 22.3 (3) |
O9—Mo1—N1—C2 | −69.4 (2) | O4—C3—C4—N1 | 163.6 (3) |
O8—Mo1—N1—C2 | 61.3 (3) | O3—C3—C4—N1 | −19.9 (4) |
O7—Mo1—N1—C2 | −170.90 (18) | C4—N1—C6—C5 | 57.9 (3) |
O1—Mo1—N1—C2 | 24.23 (19) | C2—N1—C6—C5 | −67.5 (3) |
O3—Mo1—N1—C2 | 104.85 (19) | Mo1—N1—C6—C5 | 176.34 (19) |
O9—Mo1—N1—C6 | 50.49 (19) | O6—C5—C6—N1 | 0.3 (4) |
O8—Mo1—N1—C6 | −178.8 (3) | O5—C5—C6—N1 | −178.8 (3) |
Symmetry codes: (i) −x+2, −y+2, −z+2; (ii) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O5w | 0.84 (1) | 1.80 (2) | 2.607 (3) | 162 (4) |
O1w—H1w1···O4 | 0.85 | 1.87 | 2.718 (3) | 176 |
O1w—H1w2···O6iii | 0.86 | 1.89 | 2.737 (3) | 174 |
O2w—H2w1···O4w | 0.84 | 1.86 | 2.699 (4) | 174 |
O2w—H2w2···O2iv | 0.85 | 2.00 | 2.802 (4) | 160 |
O3w—H3w1···O6w | 0.83 | 1.88 | 2.701 (4) | 174 |
O3w—H3w2···O3wv | 0.83 | 2.18 | 2.989 (5) | 165 |
O4w—H4w2···O2iii | 0.85 | 2.13 | 2.945 (4) | 160 |
O4w—H4w1···O2v | 0.84 | 2.28 | 3.039 (4) | 151 |
O5w—H5w1···O5vi | 0.84 | 2.48 | 3.104 (4) | 131 |
O5w—H5w1···O9vii | 0.84 | 2.32 | 3.011 (3) | 140 |
O5w—H5w2···O6wviii | 0.85 | 2.34 | 3.178 (4) | 170 |
O6w—H6w2···O3 | 0.85 | 2.12 | 2.937 (3) | 164 |
O6w—H6w1···O4ix | 0.85 | 2.14 | 2.972 (4) | 167 |
Symmetry codes: (iii) x, y+1, z; (iv) x+1, y+1, z; (v) −x+1, −y+2, −z+2; (vi) −x+2, −y, −z+1; (vii) −x+1, −y, −z+1; (viii) x+1, y−1, z; (ix) x−1, y, z. |
Experimental details
Crystal data |
Chemical formula | [Mg(H2O)6][Mo2O5(C6H7NO6)2]·6H2O |
Mr | 890.63 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 6.4787 (3), 9.2555 (6), 13.9995 (6) |
α, β, γ (°) | 91.014 (4), 101.315 (3), 106.592 (4) |
V (Å3) | 786.44 (7) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 0.93 |
Crystal size (mm) | 0.58 × 0.58 × 0.36 |
|
Data collection |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | Empirical (using intensity measurements) via ψ scans (North et al., 1968) |
Tmin, Tmax | 0.618, 0.716 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3339, 3079, 2877 |
Rint | 0.010 |
(sin θ/λ)max (Å−1) | 0.616 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.076, 1.11 |
No. of reflections | 3079 |
No. of parameters | 215 |
No. of restraints | 1 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.38, −0.52 |
Selected geometric parameters (Å, º) topMo1—O1 | 2.076 (2) | Mo1—N1 | 2.418 (2) |
Mo1—O3 | 2.172 (2) | Mg1—O1w | 2.045 (2) |
Mo1—O7 | 1.880 (1) | Mg1—O2w | 2.053 (2) |
Mo1—O8 | 1.695 (2) | Mg1—O3w | 2.089 (3) |
Mo1—O9 | 1.694 (2) | | |
| | | |
O1w—Mg1—O2w | 89.1 (1) | O2w—Mg1—O3w | 89.3 (1) |
O1w—Mg1—O3w | 91.7 (1) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O5w | 0.84 (1) | 1.80 (2) | 2.607 (3) | 162 (4) |
O1w—H1w1···O4 | 0.85 | 1.87 | 2.718 (3) | 176 |
O1w—H1w2···O6i | 0.86 | 1.89 | 2.737 (3) | 174 |
O2w—H2w1···O4w | 0.84 | 1.86 | 2.699 (4) | 174 |
O2w—H2w2···O2ii | 0.85 | 2.00 | 2.802 (4) | 160 |
O3w—H3w1···O6w | 0.83 | 1.88 | 2.701 (4) | 174 |
O3w—H3w2···O3wiii | 0.83 | 2.18 | 2.989 (5) | 165 |
O4w—H4w2···O2i | 0.85 | 2.13 | 2.945 (4) | 160 |
O4w—H4w1···O2iii | 0.84 | 2.28 | 3.039 (4) | 151 |
O5w—H5w1···O5iv | 0.84 | 2.48 | 3.104 (4) | 131 |
O5w—H5w1···O9v | 0.84 | 2.32 | 3.011 (3) | 140 |
O5w—H5w2···O6wvi | 0.85 | 2.34 | 3.178 (4) | 170 |
O6w—H6w2···O3 | 0.85 | 2.12 | 2.937 (3) | 164 |
O6w—H6w1···O4vii | 0.85 | 2.14 | 2.972 (4) | 167 |
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+1, z; (iii) −x+1, −y+2, −z+2; (iv) −x+2, −y, −z+1; (v) −x+1, −y, −z+1; (vi) x+1, y−1, z; (vii) x−1, y, z. |
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Oxomolybdate(VI) complexes are of interest as possible models for molybdenum sites in metalloenzymes (Chan et al., 1993; Hille, 1996; Stiefel, 1977). Among the complexes, those chelated by tridentate ligands derive their stability through the binding of the ligand to the vacant coordination sites (Gebreyes et al., 1985). The deprotonated nitrilotriacetato ligand, which functions as a tetradentate entity in a number of metal complexes, is only tridentate in the dipyridinium (Matsumoto et al., 1984), monohydrated bis(tetrabutylammonium) (Liu et al., 1990) and octahydrated disodium (Knobler et al., 1980, 1983) µ-oxobis(hydrogennitrilotriacetatodioxomolybdates). In the peroxo complex, potassium nitrilotriacetato(oxo)(peroxo)molybdenate monohydate, the ligand behaves as a tetradentate chelate (Won et al., 1994). On the other hand, as the hexaaquamagnesium(II) cation has been used to balance the charges of a number of organic (Arranz Mascarós et al., 2000; Castellari et al., 1999, Kariuki et al., 1994; Solans, Font-Altaba, Aguilo et al., 1983) and inorganic (Coiro & Mazza, 1991; Kariuki & Jones, 1989; Maslen et al., 1988; Solans, Font-Altaba, Oliva & Herrera, 1983) derivatives, we have used this dication as counter-ion in the title compound, (I).
Both the cation and anion lies at the center of symmetry; for the anion, this symmetry requires the Mo—O—Mo unit to be linear. The Mo—O bond distance is similar to that [Mo—O = 1.880 (1) Å] found in the sodium salt (Knobler et al., 1983), which is also centrosymmetric. In the related dipotassium tetrasodium oxobis(citratodioxomolybdate), the Mo—O—Mo unit is bent [Mo—O—Mo = 144.7 (2)°; Zhou et al., 1997]. In the title compound, the anions and the water-coordinated cations are linked by hydrogen bonds into a three-dimensional network motif.