The crystal structures of dimagnesium disodium decavanadate icosahydrate, Mg
2Na
2V
10O
28·20H
2O, (I), and trimagnesium decavanadate octacosahydrate, Mg
3V
10O
28·28H
2O, (II), have been determined by single-crystal X-ray diffraction. They crystallize with monoclinic (
C2/
c) and triclinic (
) symmetry, respectively. All the Mg
2+ cations in (I) and (II) are octahedrally coordinated by six water molecules. The Na
+ cations in (I) are coordinated by three water molecules and three O atoms of the decavanadate anions, and link the latter into a three-dimensional network. The decavanadate anions in (II) are not linked to one another.
Supporting information
NaVO3 (1.22 g) was dissolved in hot water (100 ml) and the pH was adjusted to 3.70 by adding CH3COOH. An aqueous solution of Mg(CH3COO)2·4H2O (0.65 g in 10 ml of water) was then added. The crude product, (I) (1.12 g), was obtained by adding acetone (100 ml) dropwise to the reaction mixture. Diffraction-quality crystals of (I) were obtained by vapor-phase diffusion of acetone into an aqueous solution (15 ml) containing the dissolved crude product (0.1 g). A solution of decavanadic acid was prepared according to Jahr & Preuss (1965): V2O5 (3.64 g) was dissolved in aqueous H2O2 (50 ml of 30% aqueous H2O2 diluted with 400 ml of water). An aqueous solution of Mg(CH3COO)2·4H2O (2.68 g in 10 ml of water) was added to the decavanadic acid solution. After the volume of the resulting solution was reduced to 100 ml by heating, acetone (100 ml) was added dropwise to obtain the crude product, (II) (4.50 g). Diffraction-quality crystals of (II) were obtained by vapor-phase diffusion of acetone into an aqueous solution (15 ml) containing the crude product (0.1 g).
All H atoms were located from difference Fourier syntheses. For (I), the positional and displacement parameters of the H atoms were fully refined. For (II), the positional parameters of the H atoms were fixed and their Uiso parameters were fixed at 1.5Ueq of the O atom of the corresponding H2O molecule. Thus the geometrical parameters involving the H atoms in (II) are less reliable and show some discrepancies with normal values. They are nevertheless included in the current structure analysis because they provide sufficient information on the hydrogen-bond networks. Two H2O molecules in (II) are disordered, viz. O55A/O55B, with site occupancies of 0.685 (12) and 0.315 (12), and O56A/O56B, with occupancies of 0.657 (6) and 0.343 (6). The H atoms bonded to the minor O-atom positions could not be located from Fourier maps. A short contact between atoms O12 and O55B (2.86 Å) may be attributed to the hydrogen bond via the undetermined H atom.
For both compounds, data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 1999) and ORTEPIII (Burnett & Johnson, 1996).
(I) dimagnesium disodium decavanadate icosahydrate
top
Crystal data top
Mg2Na2V10O28·20H2O | F(000) = 2800 |
Mr = 1412.32 | Dx = 2.387 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 8192 reflections |
a = 23.8384 (6) Å | θ = 1.9–30.0° |
b = 11.0248 (2) Å | µ = 2.46 mm−1 |
c = 16.9332 (4) Å | T = 93 K |
β = 118.005 (1)° | Plate, yellow-orange |
V = 3929.18 (15) Å3 | 0.20 × 0.18 × 0.08 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector system diffractometer | 5746 independent reflections |
Radiation source: Rigaku UltraX-18 rotating anode | 4522 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
Detector resolution: 10 pixels mm-1 | θmax = 30.0°, θmin = 1.9° |
ω scans | h = −32→33 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −15→15 |
Tmin = 0.640, Tmax = 0.821 | l = −23→18 |
18758 measured reflections | |
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)] = 0.029 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.075 | All H-atom parameters refined |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0404P)2] where P = (Fo2 + 2Fc2)/3 |
5746 reflections | (Δ/σ)max = 0.001 |
360 parameters | Δρmax = 0.72 e Å−3 |
0 restraints | Δρmin = −1.24 e Å−3 |
Crystal data top
Mg2Na2V10O28·20H2O | V = 3929.18 (15) Å3 |
Mr = 1412.32 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 23.8384 (6) Å | µ = 2.46 mm−1 |
b = 11.0248 (2) Å | T = 93 K |
c = 16.9332 (4) Å | 0.20 × 0.18 × 0.08 mm |
β = 118.005 (1)° | |
Data collection top
Bruker SMART CCD area-detector system diffractometer | 5746 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 4522 reflections with I > 2σ(I) |
Tmin = 0.640, Tmax = 0.821 | Rint = 0.034 |
18758 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.029 | 0 restraints |
wR(F2) = 0.075 | All H-atom parameters refined |
S = 1.01 | Δρmax = 0.72 e Å−3 |
5746 reflections | Δρmin = −1.24 e Å−3 |
360 parameters | |
Special details top
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 of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
V1 | 0.071893 (13) | 0.21033 (3) | 0.283133 (19) | 0.00579 (7) | |
V2 | 0.073321 (13) | 0.61761 (3) | 0.286072 (19) | 0.00558 (7) | |
V3 | 0.133464 (14) | 0.41597 (3) | 0.218853 (19) | 0.00599 (7) | |
V4 | 0.155828 (14) | 0.41074 (3) | 0.412962 (19) | 0.00636 (7) | |
V5 | 0.011514 (13) | 0.41638 (3) | 0.352932 (19) | 0.00489 (7) | |
O1 | 0.07166 (6) | 0.06513 (12) | 0.28211 (9) | 0.0104 (3) | |
O2 | 0.07392 (6) | 0.76400 (12) | 0.28697 (8) | 0.0094 (3) | |
O3 | 0.17340 (6) | 0.41393 (12) | 0.16419 (9) | 0.0097 (2) | |
O4 | 0.21439 (6) | 0.41404 (12) | 0.51254 (9) | 0.0111 (3) | |
O5 | 0.04407 (6) | 0.41401 (11) | 0.11155 (8) | 0.0074 (2) | |
O6 | 0.08335 (6) | 0.41632 (11) | 0.44589 (8) | 0.0070 (2) | |
O7 | 0.19249 (6) | 0.41349 (11) | 0.33890 (8) | 0.0076 (2) | |
O8 | 0.11699 (6) | 0.24886 (12) | 0.22362 (8) | 0.0074 (2) | |
O9 | 0.13695 (6) | 0.24692 (12) | 0.39493 (8) | 0.0075 (2) | |
O10 | 0.11717 (6) | 0.57965 (11) | 0.22367 (8) | 0.0075 (2) | |
O11 | 0.13780 (6) | 0.58033 (11) | 0.39391 (8) | 0.0076 (2) | |
O12 | 0.00939 (6) | 0.24470 (11) | 0.32797 (8) | 0.0065 (2) | |
O13 | 0.00925 (6) | 0.58639 (11) | 0.32791 (8) | 0.0061 (2) | |
O14 | 0.06284 (6) | 0.41564 (11) | 0.27887 (8) | 0.0060 (2) | |
Mg | 0.11263 (3) | 0.09300 (6) | 0.59027 (4) | 0.00735 (12) | |
O15 | 0.11310 (7) | −0.09275 (13) | 0.59606 (10) | 0.0111 (3) | |
H15A | 0.1137 (12) | −0.127 (3) | 0.6325 (19) | 0.021 (7)* | |
H15B | 0.0996 (12) | −0.132 (2) | 0.5571 (19) | 0.019 (7)* | |
O16 | 0.04096 (7) | 0.09098 (14) | 0.46271 (9) | 0.0112 (3) | |
H16A | 0.0321 (15) | 0.132 (3) | 0.430 (2) | 0.036 (10)* | |
H16B | 0.0197 (13) | 0.038 (3) | 0.4394 (18) | 0.023 (7)* | |
O17 | 0.17754 (7) | 0.08550 (13) | 0.53848 (10) | 0.0094 (3) | |
H17A | 0.1732 (11) | 0.128 (2) | 0.5001 (16) | 0.009 (6)* | |
H17B | 0.2098 (15) | 0.087 (3) | 0.572 (2) | 0.032 (9)* | |
O18 | 0.17799 (7) | 0.08937 (15) | 0.72108 (10) | 0.0130 (3) | |
H18A | 0.1941 (13) | 0.031 (3) | 0.7421 (18) | 0.021 (7)* | |
H18B | 0.1913 (13) | 0.140 (3) | 0.7475 (19) | 0.024 (8)* | |
O19 | 0.03705 (7) | 0.10426 (13) | 0.62451 (10) | 0.0105 (3) | |
H19A | 0.0447 (13) | 0.106 (2) | 0.6715 (19) | 0.020 (7)* | |
H19B | 0.0158 (13) | 0.154 (3) | 0.6036 (18) | 0.021 (7)* | |
O20 | 0.11855 (7) | 0.27880 (13) | 0.59552 (11) | 0.0127 (3) | |
H20A | 0.1091 (12) | 0.315 (2) | 0.5590 (19) | 0.016 (7)* | |
H20B | 0.1190 (14) | 0.311 (3) | 0.633 (2) | 0.032 (9)* | |
Na | 0.19887 (4) | 0.67605 (8) | 0.53862 (5) | 0.01792 (18) | |
O21 | 0.19082 (8) | 0.85630 (15) | 0.45240 (11) | 0.0181 (3) | |
H21A | 0.1870 (17) | 0.913 (3) | 0.471 (2) | 0.048 (11)* | |
H21B | 0.1597 (15) | 0.861 (3) | 0.405 (2) | 0.036 (9)* | |
O22 | 0.26327 (7) | 0.78830 (14) | 0.66768 (10) | 0.0148 (3) | |
H22A | 0.2529 (15) | 0.810 (3) | 0.697 (2) | 0.036 (10)* | |
H22B | 0.2906 (14) | 0.830 (3) | 0.6721 (18) | 0.025 (7)* | |
O23 | 0.23146 (7) | 0.12755 (14) | 0.29653 (10) | 0.0134 (3) | |
H23A | 0.2055 (13) | 0.160 (3) | 0.2934 (18) | 0.020 (7)* | |
H23B | 0.2555 (15) | 0.141 (3) | 0.349 (2) | 0.038 (9)* | |
O24 | 0.05511 (8) | 0.72088 (14) | 0.47750 (11) | 0.0186 (3) | |
H24A | 0.0444 (15) | 0.687 (3) | 0.435 (2) | 0.042 (10)* | |
H24B | 0.0472 (12) | 0.692 (2) | 0.5060 (18) | 0.015 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.00634 (14) | 0.00436 (14) | 0.00689 (14) | 0.00063 (10) | 0.00328 (11) | 0.00035 (10) |
V2 | 0.00648 (14) | 0.00398 (14) | 0.00618 (13) | −0.00068 (10) | 0.00290 (11) | −0.00018 (10) |
V3 | 0.00583 (13) | 0.00621 (14) | 0.00645 (13) | −0.00001 (10) | 0.00330 (11) | 0.00013 (10) |
V4 | 0.00517 (13) | 0.00764 (14) | 0.00530 (13) | −0.00022 (10) | 0.00166 (10) | 0.00039 (11) |
V5 | 0.00573 (13) | 0.00466 (14) | 0.00435 (13) | −0.00004 (10) | 0.00243 (11) | 0.00021 (10) |
O1 | 0.0114 (6) | 0.0068 (6) | 0.0135 (6) | 0.0014 (5) | 0.0061 (5) | 0.0010 (5) |
O2 | 0.0116 (6) | 0.0066 (6) | 0.0107 (6) | −0.0012 (5) | 0.0057 (5) | 0.0002 (5) |
O3 | 0.0089 (6) | 0.0115 (6) | 0.0105 (6) | −0.0001 (5) | 0.0061 (5) | 0.0004 (5) |
O4 | 0.0084 (6) | 0.0151 (7) | 0.0077 (6) | −0.0008 (5) | 0.0021 (5) | 0.0008 (5) |
O5 | 0.0078 (6) | 0.0077 (6) | 0.0071 (6) | −0.0001 (5) | 0.0038 (5) | −0.0002 (5) |
O6 | 0.0071 (6) | 0.0081 (6) | 0.0050 (5) | 0.0006 (5) | 0.0022 (4) | 0.0008 (4) |
O7 | 0.0072 (6) | 0.0083 (6) | 0.0070 (6) | 0.0005 (5) | 0.0030 (5) | 0.0012 (5) |
O8 | 0.0086 (6) | 0.0059 (6) | 0.0084 (5) | 0.0005 (5) | 0.0045 (5) | 0.0003 (5) |
O9 | 0.0073 (6) | 0.0067 (6) | 0.0076 (5) | 0.0011 (5) | 0.0028 (4) | 0.0013 (5) |
O10 | 0.0086 (6) | 0.0066 (6) | 0.0082 (6) | −0.0010 (5) | 0.0048 (5) | −0.0002 (5) |
O11 | 0.0072 (6) | 0.0073 (6) | 0.0071 (5) | −0.0008 (5) | 0.0024 (5) | −0.0002 (5) |
O12 | 0.0074 (6) | 0.0055 (6) | 0.0064 (5) | −0.0003 (4) | 0.0031 (4) | 0.0004 (5) |
O13 | 0.0072 (6) | 0.0053 (6) | 0.0055 (5) | 0.0004 (4) | 0.0027 (4) | 0.0004 (4) |
O14 | 0.0072 (5) | 0.0050 (6) | 0.0057 (5) | 0.0002 (4) | 0.0028 (4) | 0.0005 (4) |
Mg | 0.0082 (3) | 0.0069 (3) | 0.0064 (3) | −0.0005 (2) | 0.0030 (2) | 0.0003 (2) |
O15 | 0.0170 (7) | 0.0077 (6) | 0.0078 (6) | −0.0031 (5) | 0.0053 (5) | 0.0002 (6) |
O16 | 0.0117 (6) | 0.0100 (7) | 0.0076 (6) | −0.0028 (5) | 0.0010 (5) | 0.0030 (6) |
O17 | 0.0071 (6) | 0.0119 (6) | 0.0089 (6) | −0.0006 (5) | 0.0036 (5) | 0.0025 (5) |
O18 | 0.0152 (7) | 0.0082 (7) | 0.0085 (6) | −0.0005 (6) | −0.0002 (5) | −0.0003 (6) |
O19 | 0.0115 (7) | 0.0127 (7) | 0.0069 (6) | −0.0001 (5) | 0.0040 (5) | −0.0002 (5) |
O20 | 0.0246 (8) | 0.0074 (7) | 0.0077 (6) | 0.0019 (5) | 0.0089 (6) | 0.0008 (6) |
Na | 0.0257 (4) | 0.0151 (4) | 0.0096 (4) | −0.0090 (3) | 0.0056 (3) | −0.0037 (3) |
O21 | 0.0197 (8) | 0.0139 (8) | 0.0156 (7) | 0.0000 (6) | 0.0041 (6) | −0.0049 (6) |
O22 | 0.0126 (7) | 0.0136 (7) | 0.0186 (7) | −0.0033 (6) | 0.0076 (6) | −0.0018 (6) |
O23 | 0.0115 (7) | 0.0127 (7) | 0.0111 (7) | 0.0046 (5) | 0.0012 (6) | −0.0006 (5) |
O24 | 0.0381 (10) | 0.0113 (7) | 0.0108 (7) | −0.0090 (6) | 0.0152 (7) | −0.0042 (6) |
Geometric parameters (Å, º) top
V1—O1 | 1.6008 (13) | O5—V5i | 1.6931 (13) |
V1—O8 | 1.8356 (12) | O12—V1i | 2.0036 (12) |
V1—O9 | 1.8425 (12) | O13—V2i | 2.0373 (12) |
V1—O12 | 2.0005 (12) | O14—V5i | 2.0995 (12) |
V1—O12i | 2.0036 (12) | Mg—O18 | 2.0234 (15) |
V1—O14 | 2.2717 (13) | Mg—O16 | 2.0298 (15) |
V1—V1i | 3.0652 (6) | Mg—O15 | 2.0500 (16) |
V1—V4 | 3.0964 (4) | Mg—O20 | 2.0523 (16) |
V2—O2 | 1.6140 (14) | Mg—O17 | 2.1082 (15) |
V2—O11 | 1.7973 (13) | Mg—O19 | 2.1398 (15) |
V2—O10 | 1.8496 (13) | O15—H15A | 0.72 (3) |
V2—O13 | 1.9923 (13) | O15—H15B | 0.72 (3) |
V2—O13i | 2.0373 (12) | O16—H16A | 0.67 (3) |
V2—O14 | 2.2376 (13) | O16—H16B | 0.75 (3) |
V2—V2i | 3.1148 (6) | O17—H17A | 0.77 (3) |
V2—V4 | 3.1174 (4) | O17—H17B | 0.71 (3) |
V3—O3 | 1.6097 (13) | O18—H18A | 0.74 (3) |
V3—O7 | 1.8512 (13) | O18—H18B | 0.69 (3) |
V3—O10 | 1.8557 (13) | O19—H19A | 0.73 (3) |
V3—O8 | 1.8933 (13) | O19—H19B | 0.72 (3) |
V3—O5 | 2.0510 (13) | O20—H20A | 0.68 (3) |
V3—O14 | 2.3396 (12) | O20—H20B | 0.72 (3) |
V3—V4 | 3.0734 (4) | Na—O22 | 2.3481 (17) |
V3—V5i | 3.0784 (4) | Na—O21 | 2.4195 (19) |
V4—O4 | 1.6071 (13) | Na—O11 | 2.4264 (15) |
V4—O7 | 1.8349 (13) | Na—O21ii | 2.5864 (19) |
V4—O9 | 1.8516 (13) | Na—O3iii | 2.6620 (15) |
V4—O11 | 1.9117 (13) | Na—O4 | 2.9714 (16) |
V4—O6 | 2.0506 (13) | Na—Naii | 3.6476 (17) |
V4—O14 | 2.3120 (12) | O21—Naii | 2.5863 (19) |
V4—V5 | 3.0965 (4) | O21—H21A | 0.72 (3) |
V4—Na | 3.4764 (9) | O21—H21B | 0.80 (3) |
V5—O5i | 1.6932 (13) | O22—H22A | 0.69 (3) |
V5—O6 | 1.6967 (13) | O22—H22B | 0.77 (3) |
V5—O13 | 1.9168 (13) | O23—H23A | 0.69 (3) |
V5—O12 | 1.9349 (13) | O23—H23B | 0.82 (3) |
V5—O14i | 2.0995 (12) | O24—H24A | 0.74 (3) |
V5—O14 | 2.1239 (12) | O24—H24B | 0.67 (3) |
V5—V3i | 3.0784 (4) | | |
| | | |
O1—V1—O8 | 103.03 (6) | V1—V4—Na | 160.316 (19) |
O1—V1—O9 | 103.12 (6) | V5—V4—Na | 98.462 (18) |
O8—V1—O9 | 94.93 (6) | V2—V4—Na | 73.482 (17) |
O1—V1—O12 | 101.19 (6) | O5i—V5—O6 | 106.72 (6) |
O8—V1—O12 | 153.78 (6) | O5i—V5—O13 | 98.52 (6) |
O9—V1—O12 | 89.21 (5) | O6—V5—O13 | 96.71 (6) |
O1—V1—O12i | 100.49 (6) | O5i—V5—O12 | 96.77 (6) |
O8—V1—O12i | 89.90 (5) | O6—V5—O12 | 96.53 (6) |
O9—V1—O12i | 154.13 (6) | O13—V5—O12 | 155.94 (6) |
O12—V1—O12i | 75.89 (6) | O5i—V5—O14i | 88.09 (5) |
O1—V1—O14 | 175.01 (6) | O6—V5—O14i | 165.19 (6) |
O8—V1—O14 | 79.82 (5) | O13—V5—O14i | 81.19 (5) |
O9—V1—O14 | 80.56 (5) | O12—V5—O14i | 80.88 (5) |
O12—V1—O14 | 75.33 (5) | O5i—V5—O14 | 166.81 (6) |
O12i—V1—O14 | 75.30 (5) | O6—V5—O14 | 86.42 (5) |
O1—V1—V1i | 89.91 (5) | O13—V5—O14 | 80.65 (5) |
O8—V1—V1i | 129.91 (4) | O12—V5—O14 | 80.24 (5) |
O9—V1—V1i | 129.29 (4) | O14i—V5—O14 | 78.77 (5) |
O12—V1—V1i | 40.08 (3) | O5i—V5—V3i | 38.69 (4) |
O12i—V1—V1i | 40.01 (4) | O6—V5—V3i | 145.41 (4) |
O14—V1—V1i | 85.14 (3) | O13—V5—V3i | 90.25 (4) |
O1—V1—V4 | 135.97 (5) | O12—V5—V3i | 90.17 (4) |
O8—V1—V4 | 82.81 (4) | O14i—V5—V3i | 49.41 (3) |
O9—V1—V4 | 33.14 (4) | O14—V5—V3i | 128.18 (3) |
O12—V1—V4 | 86.76 (4) | O5i—V5—V4 | 144.81 (4) |
O12i—V1—V4 | 123.32 (4) | O6—V5—V4 | 38.16 (4) |
O14—V1—V4 | 48.06 (3) | O13—V5—V4 | 90.22 (4) |
V1i—V1—V4 | 119.911 (11) | O12—V5—V4 | 87.88 (4) |
O2—V2—O11 | 102.68 (6) | O14i—V5—V4 | 127.03 (3) |
O2—V2—O10 | 103.11 (6) | O14—V5—V4 | 48.28 (3) |
O11—V2—O10 | 94.91 (6) | V3i—V5—V4 | 176.241 (13) |
O2—V2—O13 | 100.03 (6) | V3—O3—Naiv | 151.99 (8) |
O11—V2—O13 | 91.82 (6) | V4—O4—Na | 94.05 (6) |
O10—V2—O13 | 153.80 (6) | V5i—O5—V3 | 110.24 (6) |
O2—V2—O13i | 100.27 (6) | V5—O6—V4 | 111.10 (6) |
O11—V2—O13i | 155.35 (6) | V4—O7—V3 | 112.97 (7) |
O10—V2—O13i | 88.53 (5) | V1—O8—V3 | 115.80 (7) |
O13—V2—O13i | 75.33 (6) | V1—O9—V4 | 113.90 (7) |
O2—V2—O14 | 174.79 (6) | V2—O10—V3 | 115.55 (7) |
O11—V2—O14 | 81.26 (5) | V2—O11—V4 | 114.35 (7) |
O10—V2—O14 | 79.76 (5) | V2—O11—Na | 138.42 (7) |
O13—V2—O14 | 76.28 (5) | V4—O11—Na | 105.91 (6) |
O13i—V2—O14 | 75.33 (5) | V5—O12—V1 | 108.69 (6) |
O2—V2—V2i | 90.40 (4) | V5—O12—V1i | 107.74 (6) |
O11—V2—V2i | 131.71 (4) | V1—O12—V1i | 99.91 (5) |
O10—V2—V2i | 127.38 (4) | V5—O13—V2 | 107.51 (6) |
O13—V2—V2i | 39.91 (4) | V5—O13—V2i | 106.80 (6) |
O13i—V2—V2i | 38.85 (4) | V2—O13—V2i | 101.24 (6) |
O14—V2—V2i | 84.41 (3) | V5i—O14—V5 | 101.23 (5) |
O2—V2—V4 | 136.48 (5) | V5i—O14—V2 | 94.07 (5) |
O11—V2—V4 | 33.96 (4) | V5—O14—V2 | 92.55 (5) |
O10—V2—V4 | 83.41 (4) | V5i—O14—V1 | 93.31 (5) |
O13—V2—V4 | 88.25 (4) | V5—O14—V1 | 93.30 (5) |
O13i—V2—V4 | 123.07 (4) | V2—O14—V1 | 169.52 (6) |
O14—V2—V4 | 47.75 (3) | V5i—O14—V4 | 170.28 (6) |
V2i—V2—V4 | 119.934 (10) | V5—O14—V4 | 88.44 (4) |
O3—V3—O7 | 106.34 (6) | V2—O14—V4 | 86.49 (4) |
O3—V3—O10 | 103.38 (6) | V1—O14—V4 | 84.98 (4) |
O7—V3—O10 | 91.89 (6) | V5i—O14—V3 | 87.64 (4) |
O3—V3—O8 | 101.62 (6) | V5—O14—V3 | 171.13 (6) |
O7—V3—O8 | 90.27 (5) | V2—O14—V3 | 86.41 (4) |
O10—V3—O8 | 153.19 (6) | V1—O14—V3 | 86.47 (4) |
O3—V3—O5 | 98.01 (6) | V4—O14—V3 | 82.71 (4) |
O7—V3—O5 | 155.57 (6) | O18—Mg—O16 | 174.54 (7) |
O10—V3—O5 | 84.11 (5) | O18—Mg—O15 | 86.78 (7) |
O8—V3—O5 | 82.97 (5) | O16—Mg—O15 | 91.31 (7) |
O3—V3—O14 | 171.99 (6) | O18—Mg—O20 | 88.30 (7) |
O7—V3—O14 | 81.60 (5) | O16—Mg—O20 | 93.64 (7) |
O10—V3—O14 | 76.95 (5) | O15—Mg—O20 | 175.05 (7) |
O8—V3—O14 | 76.94 (5) | O18—Mg—O17 | 96.68 (6) |
O5—V3—O14 | 74.01 (5) | O16—Mg—O17 | 88.42 (6) |
O3—V3—V4 | 139.67 (5) | O15—Mg—O17 | 89.55 (6) |
O7—V3—V4 | 33.35 (4) | O20—Mg—O17 | 90.47 (6) |
O10—V3—V4 | 84.61 (4) | O18—Mg—O19 | 91.04 (6) |
O8—V3—V4 | 82.61 (4) | O16—Mg—O19 | 83.90 (6) |
O5—V3—V4 | 122.25 (4) | O15—Mg—O19 | 91.80 (6) |
O14—V3—V4 | 48.26 (3) | O20—Mg—O19 | 88.84 (6) |
O3—V3—V5i | 129.08 (5) | O17—Mg—O19 | 172.23 (6) |
O7—V3—V5i | 124.55 (4) | Mg—O15—H15A | 124 (2) |
O10—V3—V5i | 78.26 (4) | Mg—O15—H15B | 124 (2) |
O8—V3—V5i | 78.55 (4) | H15A—O15—H15B | 107 (3) |
O5—V3—V5i | 31.07 (4) | Mg—O16—H16A | 131 (3) |
O14—V3—V5i | 42.96 (3) | Mg—O16—H16B | 126 (2) |
V4—V3—V5i | 91.210 (11) | H16A—O16—H16B | 103 (3) |
O4—V4—O7 | 105.00 (6) | Mg—O17—H17A | 119.6 (17) |
O4—V4—O9 | 102.66 (6) | Mg—O17—H17B | 114 (2) |
O7—V4—O9 | 93.46 (6) | H17A—O17—H17B | 109 (3) |
O4—V4—O11 | 99.82 (6) | Mg—O18—H18A | 120 (2) |
O7—V4—O11 | 90.57 (6) | Mg—O18—H18B | 125 (2) |
O9—V4—O11 | 155.26 (6) | H18A—O18—H18B | 114 (3) |
O4—V4—O6 | 98.15 (6) | Mg—O19—H19A | 119 (2) |
O7—V4—O6 | 156.63 (5) | Mg—O19—H19B | 114 (2) |
O9—V4—O6 | 84.47 (5) | H19A—O19—H19B | 106 (3) |
O11—V4—O6 | 82.25 (5) | Mg—O20—H20A | 124 (2) |
O4—V4—O14 | 171.81 (6) | Mg—O20—H20B | 120 (2) |
O7—V4—O14 | 82.71 (5) | H20A—O20—H20B | 112 (3) |
O9—V4—O14 | 79.29 (5) | O22—Na—O21 | 87.75 (6) |
O11—V4—O14 | 77.03 (5) | O22—Na—O11 | 171.56 (6) |
O6—V4—O14 | 74.02 (5) | O21—Na—O11 | 84.71 (6) |
O4—V4—V3 | 138.65 (5) | O22—Na—O21ii | 79.37 (6) |
O7—V4—V3 | 33.68 (4) | O21—Na—O21ii | 86.51 (6) |
O9—V4—V3 | 86.29 (4) | O11—Na—O21ii | 96.36 (6) |
O11—V4—V3 | 83.62 (4) | O22—Na—O3iii | 75.39 (5) |
O6—V4—V3 | 123.03 (4) | O21—Na—O3iii | 143.59 (6) |
O14—V4—V3 | 49.03 (3) | O11—Na—O3iii | 113.00 (5) |
O4—V4—V1 | 135.60 (5) | O21ii—Na—O3iii | 120.57 (6) |
O7—V4—V1 | 83.28 (4) | O22—Na—O4 | 125.32 (6) |
O9—V4—V1 | 32.96 (4) | O21—Na—O4 | 133.54 (6) |
O11—V4—V1 | 123.98 (4) | O11—Na—O4 | 58.98 (4) |
O6—V4—V1 | 82.44 (4) | O21ii—Na—O4 | 71.38 (5) |
O14—V4—V1 | 46.96 (3) | O3iii—Na—O4 | 81.23 (4) |
V3—V4—V1 | 61.595 (9) | O22—Na—V4 | 152.77 (5) |
O4—V4—V5 | 128.89 (5) | O21—Na—V4 | 113.87 (5) |
O7—V4—V5 | 125.99 (4) | O11—Na—V4 | 31.93 (3) |
O9—V4—V5 | 79.57 (4) | O21ii—Na—V4 | 85.40 (4) |
O11—V4—V5 | 78.33 (4) | O3iii—Na—V4 | 93.61 (4) |
O6—V4—V5 | 30.75 (3) | O4—Na—V4 | 27.46 (3) |
O14—V4—V5 | 43.29 (3) | O22—Na—Naii | 80.98 (5) |
V3—V4—V5 | 92.319 (11) | O21—Na—Naii | 45.05 (4) |
V1—V4—V5 | 62.181 (10) | O11—Na—Naii | 91.00 (4) |
O4—V4—V2 | 131.50 (5) | O21ii—Na—Naii | 41.46 (4) |
O7—V4—V2 | 82.28 (4) | O3iii—Na—Naii | 153.44 (5) |
O9—V4—V2 | 125.04 (4) | O4—Na—Naii | 103.33 (4) |
O11—V4—V2 | 31.68 (4) | V4—Na—Naii | 102.21 (3) |
O6—V4—V2 | 79.98 (4) | Na—O21—Naii | 93.49 (6) |
O14—V4—V2 | 45.76 (3) | Na—O21—H21A | 116 (3) |
V3—V4—V2 | 60.834 (9) | Naii—O21—H21A | 115 (3) |
V1—V4—V2 | 92.548 (11) | Na—O21—H21B | 115 (2) |
V5—V4—V2 | 60.980 (9) | Naii—O21—H21B | 121 (2) |
O4—V4—Na | 58.49 (5) | H21A—O21—H21B | 98 (3) |
O7—V4—Na | 107.82 (4) | Na—O22—H22A | 124 (3) |
O9—V4—Na | 154.24 (4) | Na—O22—H22B | 124 (2) |
O11—V4—Na | 42.16 (4) | H22A—O22—H22B | 107 (3) |
O6—V4—Na | 81.52 (4) | H23A—O23—H23B | 98 (3) |
O14—V4—Na | 116.92 (4) | H24A—O24—H24B | 112 (3) |
V3—V4—Na | 119.467 (17) | | |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x+1/2, −y+3/2, −z+1; (iii) x, −y+1, z+1/2; (iv) x, −y+1, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O15—H15A···O8v | 0.72 (3) | 2.02 (3) | 2.7291 (19) | 169 (3) |
O15—H15B···O24vi | 0.72 (3) | 2.06 (3) | 2.749 (2) | 160 (3) |
O16—H16A···O12 | 0.67 (3) | 1.98 (3) | 2.6517 (19) | 175 (4) |
O16—H16B···O19vii | 0.75 (3) | 2.02 (3) | 2.774 (2) | 179 (3) |
O17—H17A···O9 | 0.77 (3) | 2.05 (3) | 2.7933 (19) | 164 (2) |
O17—H17B···O7viii | 0.71 (3) | 2.10 (3) | 2.8052 (19) | 174 (3) |
O18—H18A···O23v | 0.74 (3) | 1.99 (3) | 2.729 (2) | 176 (3) |
O18—H18B···O22ix | 0.69 (3) | 2.11 (3) | 2.800 (2) | 177 (3) |
O19—H19A···O2iii | 0.73 (3) | 2.26 (3) | 2.8600 (19) | 141 (3) |
O19—H19A···O1v | 0.73 (3) | 2.52 (3) | 3.037 (2) | 130 (2) |
O19—H19B···O24x | 0.72 (3) | 2.11 (3) | 2.822 (2) | 170 (3) |
O20—H20A···O6 | 0.68 (3) | 2.05 (3) | 2.725 (2) | 176 (3) |
O20—H20B···O10iii | 0.72 (3) | 1.97 (3) | 2.686 (2) | 171 (3) |
O21—H21A···O17xi | 0.72 (3) | 2.29 (4) | 3.007 (2) | 176 (4) |
O21—H21B···O2 | 0.80 (3) | 2.34 (3) | 3.052 (2) | 149 (3) |
O22—H22A···O23iii | 0.69 (3) | 2.09 (3) | 2.784 (2) | 174 (3) |
O22—H22B···O10ii | 0.77 (3) | 2.30 (3) | 2.950 (2) | 142 (3) |
O23—H23A···O8 | 0.69 (3) | 2.11 (3) | 2.756 (2) | 154 (3) |
O23—H23B···O4viii | 0.82 (3) | 2.19 (3) | 2.900 (2) | 146 (3) |
O24—H24A···O13 | 0.74 (3) | 1.95 (3) | 2.685 (2) | 172 (3) |
O24—H24B···O5iii | 0.67 (3) | 2.17 (3) | 2.827 (2) | 167 (3) |
Symmetry codes: (ii) −x+1/2, −y+3/2, −z+1; (iii) x, −y+1, z+1/2; (v) x, −y, z+1/2; (vi) x, y−1, z; (vii) −x, −y, −z+1; (viii) −x+1/2, −y+1/2, −z+1; (ix) −x+1/2, y−1/2, −z+3/2; (x) −x, −y+1, −z+1; (xi) x, y+1, z. |
(II) trimagnesium decavanadate octacosahydrate
top
Crystal data top
Mg3V10O28·28H2O | Z = 2 |
Mr = 1534.78 | F(000) = 1540 |
Triclinic, P1 | Dx = 2.220 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.4834 (1) Å | Cell parameters from 8192 reflections |
b = 10.7309 (2) Å | θ = 2.0–30.0° |
c = 21.2293 (4) Å | µ = 2.12 mm−1 |
α = 90.751 (1)° | T = 93 K |
β = 97.866 (1)° | Block, orange |
γ = 103.663 (1)° | 0.30 × 0.18 × 0.14 mm |
V = 2296.24 (6) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 13207 independent reflections |
Radiation source: Rigaku UltraX-18 rotating anode | 10950 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
Detector resolution: 10 pixels mm-1 | θmax = 30.0°, θmin = 2.0° |
ω scans | h = −14→14 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −9→15 |
Tmin = 0.518, Tmax = 0.743 | l = −27→29 |
22420 measured reflections | |
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)] = 0.032 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.086 | H-atom parameters not refined |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0467P)2] where P = (Fo2 + 2Fc2)/3 |
13207 reflections | (Δ/σ)max = 0.002 |
632 parameters | Δρmax = 0.99 e Å−3 |
0 restraints | Δρmin = −0.95 e Å−3 |
Crystal data top
Mg3V10O28·28H2O | γ = 103.663 (1)° |
Mr = 1534.78 | V = 2296.24 (6) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.4834 (1) Å | Mo Kα radiation |
b = 10.7309 (2) Å | µ = 2.12 mm−1 |
c = 21.2293 (4) Å | T = 93 K |
α = 90.751 (1)° | 0.30 × 0.18 × 0.14 mm |
β = 97.866 (1)° | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 13207 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 10950 reflections with I > 2σ(I) |
Tmin = 0.518, Tmax = 0.743 | Rint = 0.025 |
22420 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.032 | 0 restraints |
wR(F2) = 0.086 | H-atom parameters not refined |
S = 1.01 | Δρmax = 0.99 e Å−3 |
13207 reflections | Δρmin = −0.95 e Å−3 |
632 parameters | |
Special details top
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 of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) 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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
V1 | 0.01390 (3) | 0.24943 (3) | 0.023068 (16) | 0.00664 (7) | |
V2 | −0.12606 (3) | −0.14660 (3) | 0.086083 (16) | 0.00743 (7) | |
V3 | −0.24898 (3) | 0.09011 (3) | 0.065604 (16) | 0.00790 (7) | |
V4 | 0.01812 (3) | 0.12080 (3) | 0.152868 (16) | 0.00824 (7) | |
V5 | 0.14348 (3) | 0.01526 (3) | 0.047124 (15) | 0.00594 (7) | |
O1 | 0.06339 (15) | 0.39143 (14) | −0.00221 (7) | 0.0118 (3) | |
O2 | −0.17465 (16) | −0.29019 (15) | 0.10872 (8) | 0.0140 (3) | |
O3 | −0.39140 (15) | 0.11831 (16) | 0.07086 (7) | 0.0129 (3) | |
O4 | 0.07879 (16) | 0.17042 (16) | 0.22535 (7) | 0.0156 (3) | |
O5 | −0.28150 (14) | 0.02503 (14) | −0.02698 (7) | 0.0094 (3) | |
O6 | 0.17817 (14) | 0.06983 (15) | 0.12320 (7) | 0.0097 (3) | |
O7 | −0.15061 (14) | 0.14006 (14) | 0.14536 (7) | 0.0096 (3) | |
O8 | −0.15803 (14) | 0.24264 (14) | 0.03364 (7) | 0.0090 (3) | |
O9 | 0.07406 (14) | 0.26798 (14) | 0.10794 (7) | 0.0095 (3) | |
O10 | −0.27488 (14) | −0.08202 (15) | 0.08441 (7) | 0.0101 (3) | |
O11 | −0.04116 (14) | −0.05820 (14) | 0.16011 (7) | 0.0097 (3) | |
O12 | 0.16761 (13) | 0.17856 (14) | 0.00828 (7) | 0.0075 (3) | |
O13 | 0.04842 (13) | −0.15684 (14) | 0.06161 (7) | 0.0073 (3) | |
O14 | −0.04905 (13) | 0.04609 (13) | 0.04770 (6) | 0.0066 (3) | |
V6 | 0.34035 (3) | 0.37841 (3) | 0.395074 (16) | 0.00610 (7) | |
V7 | 0.42408 (3) | 0.39064 (3) | 0.607632 (15) | 0.00640 (7) | |
V8 | 0.17308 (3) | 0.35497 (3) | 0.507868 (16) | 0.00697 (7) | |
V9 | 0.36096 (3) | 0.17784 (3) | 0.497797 (16) | 0.00725 (7) | |
V10 | 0.60101 (3) | 0.40431 (3) | 0.496502 (15) | 0.00539 (7) | |
O15 | 0.31059 (15) | 0.37189 (15) | 0.31834 (7) | 0.0109 (3) | |
O16 | 0.45553 (14) | 0.39772 (15) | 0.68425 (7) | 0.0108 (3) | |
O17 | 0.01814 (14) | 0.33846 (15) | 0.51011 (7) | 0.0114 (3) | |
O18 | 0.35272 (15) | 0.02545 (15) | 0.49510 (7) | 0.0120 (3) | |
O19 | 0.23428 (14) | 0.54803 (14) | 0.50650 (7) | 0.0083 (3) | |
O20 | 0.56095 (14) | 0.24272 (14) | 0.49581 (7) | 0.0076 (3) | |
O21 | 0.19249 (14) | 0.18854 (14) | 0.50297 (7) | 0.0086 (3) | |
O22 | 0.17835 (14) | 0.36437 (14) | 0.41832 (7) | 0.0081 (3) | |
O23 | 0.34650 (14) | 0.21115 (14) | 0.41172 (7) | 0.0084 (3) | |
O24 | 0.24568 (14) | 0.37590 (14) | 0.59340 (7) | 0.0087 (3) | |
O25 | 0.41177 (14) | 0.22076 (14) | 0.58628 (7) | 0.0082 (3) | |
O26 | 0.54268 (13) | 0.42214 (14) | 0.40752 (6) | 0.0070 (3) | |
O27 | 0.61069 (13) | 0.43407 (14) | 0.58771 (6) | 0.0067 (3) | |
O28 | 0.39959 (13) | 0.39754 (13) | 0.50125 (6) | 0.0068 (3) | |
Mg1 | 0.36814 (7) | 0.64111 (7) | 0.11116 (3) | 0.00893 (13) | |
O29 | 0.20417 (15) | 0.70626 (16) | 0.13009 (7) | 0.0133 (3) | |
H29A | 0.1628 | 0.7522 | 0.1137 | 0.020* | |
H29B | 0.1900 | 0.7178 | 0.1642 | 0.020* | |
O30 | 0.28291 (15) | 0.59050 (15) | 0.01891 (7) | 0.0119 (3) | |
H30A | 0.2205 | 0.5238 | 0.0131 | 0.018* | |
H30B | 0.2432 | 0.6377 | −0.0051 | 0.018* | |
O31 | 0.45800 (14) | 0.82080 (15) | 0.08286 (8) | 0.0134 (3) | |
H31A | 0.4236 | 0.8815 | 0.0703 | 0.020* | |
H31B | 0.5358 | 0.8530 | 0.0881 | 0.020* | |
O32 | 0.47023 (14) | 0.70467 (15) | 0.20146 (7) | 0.0109 (3) | |
H32A | 0.5426 | 0.7466 | 0.2038 | 0.016* | |
H32B | 0.4738 | 0.6560 | 0.2314 | 0.016* | |
O33 | 0.29112 (14) | 0.46667 (15) | 0.14471 (8) | 0.0132 (3) | |
H33A | 0.3384 | 0.4274 | 0.1681 | 0.020* | |
H33B | 0.2229 | 0.4083 | 0.1388 | 0.020* | |
O34 | 0.52740 (15) | 0.56597 (15) | 0.08970 (7) | 0.0131 (3) | |
H34A | 0.5030 | 0.4927 | 0.0740 | 0.020* | |
H34B | 0.5489 | 0.5944 | 0.0509 | 0.020* | |
Mg2 | 0.23696 (7) | 0.85624 (7) | 0.31211 (3) | 0.00920 (13) | |
O35 | 0.07560 (14) | 0.79128 (15) | 0.24116 (7) | 0.0109 (3) | |
H35A | 0.0472 | 0.8420 | 0.2168 | 0.016* | |
H35B | 0.0116 | 0.7494 | 0.2541 | 0.016* | |
O36 | 0.27165 (15) | 0.67493 (15) | 0.30863 (7) | 0.0143 (3) | |
H36A | 0.2218 | 0.6072 | 0.2889 | 0.021* | |
H36B | 0.3060 | 0.6361 | 0.3432 | 0.021* | |
O37 | 0.21552 (15) | 1.04021 (15) | 0.31645 (7) | 0.0135 (3) | |
H37A | 0.1804 | 1.0755 | 0.2880 | 0.020* | |
H37B | 0.2551 | 1.0936 | 0.3485 | 0.020* | |
O38 | 0.35812 (15) | 0.90049 (15) | 0.24374 (8) | 0.0143 (3) | |
H38A | 0.3946 | 0.9771 | 0.2304 | 0.021* | |
H38B | 0.3872 | 0.8367 | 0.2327 | 0.021* | |
O39 | 0.40325 (14) | 0.91515 (16) | 0.38250 (7) | 0.0126 (3) | |
H39A | 0.4594 | 0.8714 | 0.3881 | 0.019* | |
H39B | 0.3912 | 0.9412 | 0.4221 | 0.019* | |
O40 | 0.12096 (16) | 0.80419 (15) | 0.38227 (7) | 0.0147 (3) | |
H40A | 0.0904 | 0.8621 | 0.3985 | 0.022* | |
H40B | 0.0858 | 0.7251 | 0.3875 | 0.022* | |
Mg3 | 0.75884 (7) | 0.17655 (7) | 0.34686 (4) | 0.01084 (14) | |
O41 | 0.55648 (15) | 0.15355 (17) | 0.34636 (8) | 0.0159 (3) | |
H41A | 0.5000 | 0.1857 | 0.3613 | 0.024* | |
H41B | 0.4994 | 0.0674 | 0.3576 | 0.024* | |
O42 | 0.72967 (17) | −0.02248 (15) | 0.34442 (7) | 0.0158 (3) | |
H42A | 0.7349 | −0.0480 | 0.3095 | 0.024* | |
H42B | 0.6958 | −0.0803 | 0.3673 | 0.024* | |
O43 | 0.79438 (15) | 0.17481 (16) | 0.44430 (7) | 0.0145 (3) | |
H43A | 0.8552 | 0.2404 | 0.4684 | 0.022* | |
H43B | 0.7326 | 0.1316 | 0.4647 | 0.022* | |
O44 | 0.76817 (18) | 0.37020 (17) | 0.35071 (8) | 0.0207 (4) | |
H44A | 0.8449 | 0.3895 | 0.3510 | 0.031* | |
H44B | 0.7034 | 0.4001 | 0.3731 | 0.031* | |
O45 | 0.72756 (16) | 0.16439 (17) | 0.24970 (7) | 0.0168 (3) | |
H45A | 0.7818 | 0.1741 | 0.2246 | 0.025* | |
H45B | 0.6590 | 0.1508 | 0.2335 | 0.025* | |
O46 | 0.96004 (17) | 0.1961 (2) | 0.34707 (11) | 0.0421 (7) | |
H46A | 1.0279 | 0.2606 | 0.3681 | 0.063* | |
H46B | 0.9784 | 0.1952 | 0.3137 | 0.063* | |
O47 | 0.84110 (15) | 0.67127 (16) | 0.28246 (7) | 0.0143 (3) | |
H47A | 0.7985 | 0.6085 | 0.2618 | 0.022* | |
H47B | 0.8250 | 0.6574 | 0.3191 | 0.022* | |
O48 | 0.45585 (15) | 0.35168 (16) | 0.21830 (7) | 0.0145 (3) | |
H48A | 0.5403 | 0.3916 | 0.2203 | 0.022* | |
H48B | 0.4338 | 0.3631 | 0.2537 | 0.022* | |
O49 | 0.72061 (16) | 0.85099 (16) | 0.22993 (7) | 0.0142 (3) | |
H49A | 0.7611 | 0.8841 | 0.2026 | 0.021* | |
H49B | 0.7740 | 0.8019 | 0.2485 | 0.021* | |
O50 | 0.47564 (16) | 0.11250 (16) | 0.18493 (8) | 0.0158 (3) | |
H50A | 0.4809 | 0.0987 | 0.1465 | 0.024* | |
H50B | 0.4540 | 0.1865 | 0.1957 | 0.024* | |
O51 | 0.01521 (17) | 0.53150 (17) | 0.36980 (8) | 0.0196 (3) | |
H51A | 0.0360 | 0.5202 | 0.3320 | 0.029* | |
H51B | 0.0719 | 0.5020 | 0.3987 | 0.029* | |
O52 | 0.90891 (18) | 0.46003 (16) | 0.13737 (8) | 0.0196 (3) | |
H52A | 0.9151 | 0.5284 | 0.1173 | 0.029* | |
H52B | 0.9120 | 0.4046 | 0.1194 | 0.029* | |
O53 | 0.00594 (16) | 0.98053 (17) | 0.42894 (9) | 0.0203 (4) | |
H53A | 0.0582 | 1.0612 | 0.4413 | 0.030* | |
H53B | −0.0711 | 0.9261 | 0.4567 | 0.030* | |
O54 | 0.08233 (17) | 0.46651 (17) | 0.25104 (8) | 0.0209 (4) | |
H54A | 0.0343 | 0.4784 | 0.2160 | 0.031* | |
H54B | 0.1085 | 0.3954 | 0.2455 | 0.031* | |
O55A | 0.4295 (2) | 0.3204 (2) | 0.0293 (2) | 0.0140 (9) | 0.685 (12) |
H55A | 0.3529 | 0.2812 | 0.0311 | 0.021* | 0.685 |
H55B | 0.4774 | 0.2720 | 0.0316 | 0.021* | 0.685 |
O55B | 0.4337 (6) | 0.3084 (6) | 0.0593 (5) | 0.0162 (17)* | 0.315 (12) |
O56A | 0.6925 (2) | 0.4934 (2) | 0.19051 (12) | 0.0149 (7) | 0.657 (6) |
H56A | 0.7525 | 0.4536 | 0.1859 | 0.022* | 0.657 |
H56B | 0.6704 | 0.5417 | 0.1605 | 0.022* | 0.657 |
O56B | 0.7229 (5) | 0.4420 (5) | 0.2211 (2) | 0.0159 (14)* | 0.343 (6) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.00690 (14) | 0.00442 (15) | 0.00841 (15) | 0.00097 (11) | 0.00102 (11) | 0.00095 (12) |
V2 | 0.00825 (15) | 0.00641 (16) | 0.00835 (15) | 0.00193 (12) | 0.00315 (11) | 0.00322 (12) |
V3 | 0.00663 (14) | 0.00810 (16) | 0.00975 (16) | 0.00250 (12) | 0.00251 (12) | 0.00216 (12) |
V4 | 0.01062 (15) | 0.00869 (16) | 0.00560 (15) | 0.00372 (12) | −0.00059 (11) | −0.00024 (12) |
V5 | 0.00472 (13) | 0.00586 (15) | 0.00672 (15) | 0.00114 (11) | −0.00077 (11) | 0.00091 (11) |
O1 | 0.0118 (7) | 0.0068 (7) | 0.0172 (7) | 0.0025 (5) | 0.0033 (5) | 0.0020 (6) |
O2 | 0.0177 (7) | 0.0102 (7) | 0.0159 (8) | 0.0034 (6) | 0.0076 (6) | 0.0052 (6) |
O3 | 0.0100 (7) | 0.0154 (8) | 0.0149 (7) | 0.0052 (6) | 0.0035 (5) | 0.0030 (6) |
O4 | 0.0220 (8) | 0.0153 (8) | 0.0096 (7) | 0.0084 (6) | −0.0047 (6) | −0.0028 (6) |
O5 | 0.0070 (6) | 0.0103 (7) | 0.0107 (7) | 0.0027 (5) | −0.0002 (5) | 0.0013 (5) |
O6 | 0.0097 (6) | 0.0104 (7) | 0.0085 (7) | 0.0032 (5) | −0.0021 (5) | −0.0002 (5) |
O7 | 0.0117 (7) | 0.0100 (7) | 0.0086 (7) | 0.0042 (5) | 0.0033 (5) | 0.0020 (5) |
O8 | 0.0092 (6) | 0.0087 (7) | 0.0100 (7) | 0.0039 (5) | 0.0012 (5) | 0.0023 (5) |
O9 | 0.0097 (6) | 0.0072 (7) | 0.0105 (7) | 0.0010 (5) | −0.0006 (5) | −0.0012 (5) |
O10 | 0.0075 (6) | 0.0110 (7) | 0.0126 (7) | 0.0021 (5) | 0.0039 (5) | 0.0027 (6) |
O11 | 0.0126 (7) | 0.0105 (7) | 0.0072 (6) | 0.0046 (5) | 0.0027 (5) | 0.0026 (5) |
O12 | 0.0057 (6) | 0.0057 (6) | 0.0102 (7) | −0.0002 (5) | 0.0008 (5) | 0.0003 (5) |
O13 | 0.0074 (6) | 0.0073 (7) | 0.0071 (6) | 0.0024 (5) | 0.0000 (5) | 0.0031 (5) |
O14 | 0.0060 (6) | 0.0068 (7) | 0.0070 (6) | 0.0014 (5) | 0.0005 (5) | 0.0014 (5) |
V6 | 0.00659 (14) | 0.00563 (15) | 0.00543 (14) | 0.00070 (11) | −0.00008 (11) | 0.00045 (11) |
V7 | 0.00611 (14) | 0.00720 (16) | 0.00543 (15) | 0.00099 (11) | 0.00018 (11) | 0.00168 (11) |
V8 | 0.00490 (14) | 0.00793 (16) | 0.00744 (15) | 0.00051 (11) | 0.00044 (11) | 0.00095 (12) |
V9 | 0.00746 (14) | 0.00472 (15) | 0.00866 (15) | 0.00048 (11) | −0.00036 (11) | 0.00118 (12) |
V10 | 0.00507 (14) | 0.00527 (15) | 0.00600 (15) | 0.00177 (11) | 0.00043 (11) | 0.00063 (11) |
O15 | 0.0122 (7) | 0.0116 (7) | 0.0078 (7) | 0.0015 (6) | 0.0001 (5) | 0.0001 (5) |
O16 | 0.0103 (6) | 0.0144 (7) | 0.0076 (7) | 0.0030 (6) | 0.0010 (5) | 0.0023 (5) |
O17 | 0.0074 (6) | 0.0132 (8) | 0.0130 (7) | 0.0014 (5) | 0.0008 (5) | 0.0015 (6) |
O18 | 0.0135 (7) | 0.0064 (7) | 0.0142 (7) | 0.0008 (5) | −0.0013 (5) | 0.0011 (6) |
O19 | 0.0072 (6) | 0.0091 (7) | 0.0089 (7) | 0.0031 (5) | 0.0003 (5) | 0.0006 (5) |
O20 | 0.0084 (6) | 0.0058 (7) | 0.0085 (6) | 0.0022 (5) | 0.0004 (5) | 0.0007 (5) |
O21 | 0.0085 (6) | 0.0061 (7) | 0.0100 (7) | −0.0005 (5) | 0.0005 (5) | 0.0013 (5) |
O22 | 0.0076 (6) | 0.0080 (7) | 0.0079 (6) | 0.0010 (5) | −0.0006 (5) | 0.0010 (5) |
O23 | 0.0100 (6) | 0.0052 (6) | 0.0087 (7) | 0.0008 (5) | −0.0010 (5) | 0.0000 (5) |
O24 | 0.0075 (6) | 0.0114 (7) | 0.0076 (6) | 0.0022 (5) | 0.0015 (5) | 0.0022 (5) |
O25 | 0.0081 (6) | 0.0060 (7) | 0.0097 (7) | 0.0004 (5) | 0.0009 (5) | 0.0017 (5) |
O26 | 0.0072 (6) | 0.0081 (7) | 0.0062 (6) | 0.0027 (5) | 0.0009 (5) | 0.0003 (5) |
O27 | 0.0072 (6) | 0.0070 (7) | 0.0061 (6) | 0.0023 (5) | 0.0004 (5) | 0.0013 (5) |
O28 | 0.0071 (6) | 0.0062 (7) | 0.0075 (6) | 0.0021 (5) | 0.0007 (5) | 0.0009 (5) |
Mg1 | 0.0095 (3) | 0.0075 (3) | 0.0090 (3) | 0.0020 (3) | −0.0017 (2) | 0.0014 (3) |
O29 | 0.0147 (7) | 0.0152 (8) | 0.0117 (7) | 0.0087 (6) | −0.0010 (5) | 0.0015 (6) |
O30 | 0.0126 (7) | 0.0076 (7) | 0.0130 (7) | 0.0012 (5) | −0.0051 (5) | 0.0011 (6) |
O31 | 0.0086 (7) | 0.0101 (7) | 0.0202 (8) | 0.0009 (5) | 0.0000 (6) | 0.0053 (6) |
O32 | 0.0105 (7) | 0.0130 (7) | 0.0079 (7) | 0.0016 (5) | −0.0015 (5) | 0.0025 (6) |
O33 | 0.0093 (7) | 0.0089 (7) | 0.0187 (8) | −0.0003 (5) | −0.0033 (6) | 0.0042 (6) |
O34 | 0.0120 (7) | 0.0117 (7) | 0.0158 (7) | 0.0022 (6) | 0.0041 (6) | 0.0003 (6) |
Mg2 | 0.0078 (3) | 0.0098 (3) | 0.0093 (3) | 0.0017 (3) | −0.0004 (2) | 0.0016 (3) |
O35 | 0.0087 (6) | 0.0113 (7) | 0.0118 (7) | 0.0017 (5) | −0.0008 (5) | 0.0035 (6) |
O36 | 0.0159 (7) | 0.0110 (7) | 0.0143 (7) | 0.0037 (6) | −0.0048 (6) | 0.0019 (6) |
O37 | 0.0163 (7) | 0.0103 (7) | 0.0115 (7) | 0.0034 (6) | −0.0065 (6) | −0.0005 (6) |
O38 | 0.0157 (7) | 0.0093 (7) | 0.0186 (8) | 0.0021 (6) | 0.0069 (6) | 0.0017 (6) |
O39 | 0.0099 (7) | 0.0181 (8) | 0.0098 (7) | 0.0049 (6) | −0.0016 (5) | 0.0020 (6) |
O40 | 0.0168 (7) | 0.0114 (8) | 0.0155 (8) | 0.0008 (6) | 0.0059 (6) | 0.0025 (6) |
Mg3 | 0.0100 (3) | 0.0088 (3) | 0.0133 (3) | 0.0007 (3) | 0.0030 (3) | −0.0027 (3) |
O41 | 0.0109 (7) | 0.0238 (9) | 0.0147 (8) | 0.0070 (6) | 0.0038 (6) | −0.0019 (6) |
O42 | 0.0270 (9) | 0.0081 (7) | 0.0109 (7) | −0.0007 (6) | 0.0071 (6) | −0.0022 (6) |
O43 | 0.0125 (7) | 0.0136 (8) | 0.0137 (7) | −0.0021 (6) | −0.0014 (6) | −0.0019 (6) |
O44 | 0.0299 (9) | 0.0129 (8) | 0.0211 (9) | 0.0043 (7) | 0.0117 (7) | −0.0011 (7) |
O45 | 0.0151 (7) | 0.0273 (9) | 0.0120 (7) | 0.0103 (7) | 0.0061 (6) | 0.0032 (7) |
O46 | 0.0094 (8) | 0.0625 (16) | 0.0461 (13) | −0.0068 (9) | 0.0071 (8) | −0.0450 (12) |
O47 | 0.0110 (7) | 0.0168 (8) | 0.0135 (7) | 0.0000 (6) | 0.0016 (5) | 0.0003 (6) |
O48 | 0.0146 (7) | 0.0167 (8) | 0.0138 (7) | 0.0060 (6) | 0.0040 (6) | 0.0028 (6) |
O49 | 0.0177 (7) | 0.0136 (8) | 0.0109 (7) | 0.0007 (6) | 0.0060 (6) | 0.0001 (6) |
O50 | 0.0197 (8) | 0.0131 (8) | 0.0139 (8) | 0.0015 (6) | 0.0046 (6) | −0.0005 (6) |
O51 | 0.0206 (8) | 0.0196 (9) | 0.0181 (8) | 0.0047 (7) | 0.0012 (6) | 0.0044 (7) |
O52 | 0.0286 (9) | 0.0139 (8) | 0.0173 (8) | 0.0070 (7) | 0.0042 (7) | −0.0025 (6) |
O53 | 0.0106 (7) | 0.0158 (8) | 0.0333 (10) | 0.0017 (6) | 0.0019 (7) | 0.0023 (7) |
O54 | 0.0211 (8) | 0.0169 (9) | 0.0242 (9) | 0.0078 (7) | −0.0035 (7) | −0.0027 (7) |
O55A | 0.0107 (11) | 0.0131 (12) | 0.019 (2) | 0.0025 (8) | 0.0030 (9) | 0.0013 (10) |
O56A | 0.0138 (11) | 0.0155 (13) | 0.0146 (13) | 0.0035 (9) | −0.0008 (9) | 0.0040 (10) |
Geometric parameters (Å, º) top
V1—O1 | 1.6134 (15) | O26—V7ii | 1.9946 (15) |
V1—O9 | 1.8177 (15) | O27—V6ii | 1.9718 (15) |
V1—O8 | 1.8312 (14) | O28—V10ii | 2.1277 (14) |
V1—O13i | 1.9927 (14) | Mg1—O33 | 2.0351 (17) |
V1—O12 | 1.9962 (14) | Mg1—O30 | 2.0474 (16) |
V1—O14 | 2.2168 (14) | Mg1—O31 | 2.0721 (17) |
V1—V2i | 3.0432 (5) | Mg1—O32 | 2.0846 (16) |
V1—V4 | 3.0977 (5) | Mg1—O29 | 2.0868 (17) |
V2—O2 | 1.6063 (16) | Mg1—O34 | 2.1165 (17) |
V2—O11 | 1.8279 (15) | O29—H29A | 0.7849 |
V2—O10 | 1.8471 (15) | O29—H29B | 0.7732 |
V2—O13 | 1.9953 (14) | O30—H30A | 0.8426 |
V2—O12i | 1.9984 (14) | O30—H30B | 0.8591 |
V2—O14 | 2.2421 (14) | O31—H31A | 0.8454 |
V2—V1i | 3.0433 (5) | O31—H31B | 0.7988 |
V2—V3 | 3.1182 (5) | O32—H32A | 0.7799 |
V3—O3 | 1.6098 (15) | O32—H32B | 0.8304 |
V3—O7 | 1.8587 (15) | O33—H33A | 0.8408 |
V3—O10 | 1.8593 (16) | O33—H33B | 0.8254 |
V3—O8 | 1.8756 (15) | O34—H34A | 0.8182 |
V3—O5 | 2.0335 (15) | O34—H34B | 0.9205 |
V3—O14 | 2.3327 (14) | Mg2—O37 | 2.0413 (17) |
V3—V5i | 3.0778 (5) | Mg2—O38 | 2.0453 (17) |
V3—V4 | 3.0838 (5) | Mg2—O40 | 2.0509 (17) |
V4—O4 | 1.6144 (15) | Mg2—O36 | 2.0643 (18) |
V4—O7 | 1.8148 (15) | Mg2—O35 | 2.0818 (16) |
V4—O9 | 1.8717 (15) | Mg2—O39 | 2.1008 (16) |
V4—O11 | 1.8892 (15) | O35—H35A | 0.8331 |
V4—O6 | 2.0554 (15) | O35—H35B | 0.7993 |
V4—O14 | 2.3193 (14) | O36—H36A | 0.8540 |
V4—V5 | 3.0811 (5) | O36—H36B | 0.9212 |
V5—O6 | 1.6725 (14) | O37—H37A | 0.8091 |
V5—O5i | 1.7097 (14) | O37—H37B | 0.8739 |
V5—O12 | 1.9236 (15) | O38—H38A | 0.8884 |
V5—O13 | 1.9307 (15) | O38—H38B | 0.8549 |
V5—O14 | 2.1226 (14) | O39—H39A | 0.8329 |
V5—O14i | 2.1396 (14) | O39—H39B | 0.9168 |
V5—V3i | 3.0778 (5) | O40—H40A | 0.8522 |
O5—V5i | 1.7097 (14) | O40—H40B | 0.8569 |
O12—V2i | 1.9983 (14) | Mg3—O45 | 2.0414 (17) |
O13—V1i | 1.9927 (14) | Mg3—O43 | 2.0521 (17) |
O14—V5i | 2.1397 (14) | Mg3—O44 | 2.0571 (19) |
V6—O15 | 1.6135 (15) | Mg3—O46 | 2.0692 (19) |
V6—O22 | 1.8058 (14) | Mg3—O41 | 2.0756 (17) |
V6—O23 | 1.8481 (15) | Mg3—O42 | 2.0837 (17) |
V6—O27ii | 1.9717 (15) | Mg3—H44A | 2.2456 |
V6—O26 | 2.0402 (14) | O41—H41A | 0.8459 |
V6—O28 | 2.2479 (14) | O41—H41B | 1.0263 |
V6—V7ii | 3.0652 (5) | O42—H42A | 0.8003 |
V6—V9 | 3.1062 (5) | O42—H42B | 0.8356 |
V7—O16 | 1.6119 (15) | O43—H43A | 0.9236 |
V7—O24 | 1.8217 (14) | O43—H43B | 0.8731 |
V7—O25 | 1.8429 (15) | O44—H44A | 0.7809 |
V7—O26ii | 1.9946 (15) | O44—H44B | 0.9886 |
V7—O27 | 2.0060 (14) | O45—H45A | 0.8212 |
V7—O28 | 2.2420 (14) | O45—H45B | 0.7332 |
V7—V6ii | 3.0652 (5) | O46—H46A | 0.9259 |
V7—V8 | 3.0877 (5) | O46—H46B | 0.7594 |
V8—O17 | 1.5992 (15) | O47—H47A | 0.8013 |
V8—O21 | 1.8478 (15) | O47—H47B | 0.8262 |
V8—O24 | 1.8593 (14) | O48—H48A | 0.8827 |
V8—O22 | 1.9128 (14) | O48—H48B | 0.8317 |
V8—O19 | 2.0207 (15) | O49—H49A | 0.8029 |
V8—O28 | 2.3340 (14) | O49—H49B | 0.9112 |
V8—V9 | 3.0677 (5) | O50—H50A | 0.8389 |
V8—V10ii | 3.0768 (5) | O50—H50B | 0.9105 |
V9—O18 | 1.6169 (16) | O51—H51A | 0.8739 |
V9—O21 | 1.8147 (15) | O51—H51B | 0.9079 |
V9—O23 | 1.8592 (15) | O52—H52A | 0.8468 |
V9—O25 | 1.9005 (14) | O52—H52B | 0.7122 |
V9—O20 | 2.0537 (14) | O53—H53A | 0.9215 |
V9—O28 | 2.2943 (15) | O53—H53B | 1.1210 |
V9—V10 | 3.0613 (5) | O54—H54A | 0.8680 |
V10—O20 | 1.6843 (15) | O54—H54B | 0.8813 |
V10—O19ii | 1.6914 (14) | O55A—H55A | 0.8200 |
V10—O26 | 1.9306 (14) | O55A—H55B | 0.8012 |
V10—O27 | 1.9432 (14) | O55B—H55A | 0.9488 |
V10—O28 | 2.1120 (14) | O55B—H55B | 0.9278 |
V10—O28ii | 2.1277 (14) | O56A—H56A | 0.8539 |
V10—V8ii | 3.0768 (5) | O56A—H56B | 0.8683 |
O19—V10ii | 1.6914 (14) | O56B—H56A | 0.8467 |
| | | |
O1—V1—O9 | 103.89 (7) | O21—V8—O24 | 92.03 (7) |
O1—V1—O8 | 102.95 (7) | O17—V8—O22 | 101.01 (7) |
O9—V1—O8 | 93.88 (7) | O21—V8—O22 | 89.08 (6) |
O1—V1—O13i | 97.56 (7) | O24—V8—O22 | 154.91 (6) |
O9—V1—O13i | 156.66 (7) | O17—V8—O19 | 100.71 (7) |
O8—V1—O13i | 90.15 (6) | O21—V8—O19 | 154.97 (6) |
O1—V1—O12 | 98.92 (7) | O24—V8—O19 | 85.59 (6) |
O9—V1—O12 | 90.23 (6) | O22—V8—O19 | 82.93 (6) |
O8—V1—O12 | 156.04 (6) | O17—V8—O28 | 174.82 (7) |
O13i—V1—O12 | 77.30 (6) | O21—V8—O28 | 80.71 (6) |
O1—V1—O14 | 173.59 (7) | O24—V8—O28 | 78.56 (6) |
O9—V1—O14 | 81.21 (6) | O22—V8—O28 | 76.90 (5) |
O8—V1—O14 | 80.33 (6) | O19—V8—O28 | 74.40 (5) |
O13i—V1—O14 | 76.82 (6) | O17—V8—V9 | 136.85 (6) |
O12—V1—O14 | 76.99 (5) | O21—V8—V9 | 32.78 (4) |
O1—V1—V2i | 87.98 (6) | O24—V8—V9 | 84.97 (5) |
O9—V1—V2i | 130.63 (5) | O22—V8—V9 | 82.48 (5) |
O8—V1—V2i | 130.44 (5) | O19—V8—V9 | 122.30 (4) |
O13i—V1—V2i | 40.29 (4) | O28—V8—V9 | 47.93 (4) |
O12—V1—V2i | 40.40 (4) | O17—V8—V10ii | 131.44 (6) |
O14—V1—V2i | 85.73 (4) | O21—V8—V10ii | 124.37 (5) |
O1—V1—V4 | 137.13 (6) | O24—V8—V10ii | 80.10 (5) |
O9—V1—V4 | 33.45 (5) | O22—V8—V10ii | 78.64 (4) |
O8—V1—V4 | 82.53 (5) | O19—V8—V10ii | 30.73 (4) |
O13i—V1—V4 | 125.14 (4) | O28—V8—V10ii | 43.68 (4) |
O12—V1—V4 | 88.10 (4) | V9—V8—V10ii | 91.609 (12) |
O14—V1—V4 | 48.33 (4) | O17—V8—V7 | 135.57 (6) |
V2i—V1—V4 | 120.938 (14) | O21—V8—V7 | 82.43 (5) |
O2—V2—O11 | 102.69 (8) | O24—V8—V7 | 32.61 (4) |
O2—V2—O10 | 103.24 (7) | O22—V8—V7 | 123.21 (4) |
O11—V2—O10 | 94.37 (7) | O19—V8—V7 | 82.25 (4) |
O2—V2—O13 | 99.44 (7) | O28—V8—V7 | 46.32 (3) |
O11—V2—O13 | 90.01 (6) | V9—V8—V7 | 61.183 (11) |
O10—V2—O13 | 155.31 (6) | V10ii—V8—V7 | 61.864 (11) |
O2—V2—O12i | 100.07 (7) | O18—V9—O21 | 104.43 (7) |
O11—V2—O12i | 155.43 (6) | O18—V9—O23 | 101.12 (7) |
O10—V2—O12i | 89.29 (6) | O21—V9—O23 | 92.99 (6) |
O13—V2—O12i | 77.19 (6) | O18—V9—O25 | 101.73 (7) |
O2—V2—O14 | 174.62 (7) | O21—V9—O25 | 91.02 (6) |
O11—V2—O14 | 80.49 (6) | O23—V9—O25 | 155.01 (7) |
O10—V2—O14 | 80.68 (6) | O18—V9—O20 | 98.27 (7) |
O13—V2—O14 | 76.10 (5) | O21—V9—O20 | 157.24 (6) |
O12i—V2—O14 | 76.14 (5) | O23—V9—O20 | 84.04 (6) |
O2—V2—V1i | 89.95 (6) | O25—V9—O20 | 82.79 (6) |
O11—V2—V1i | 130.23 (5) | O18—V9—O28 | 173.07 (7) |
O10—V2—V1i | 129.62 (5) | O21—V9—O28 | 82.49 (6) |
O13—V2—V1i | 40.23 (4) | O23—V9—O28 | 78.42 (6) |
O12i—V2—V1i | 40.34 (4) | O25—V9—O28 | 77.68 (6) |
O14—V2—V1i | 84.70 (4) | O20—V9—O28 | 74.80 (5) |
O2—V2—V3 | 135.95 (6) | O18—V9—V10 | 129.49 (6) |
O11—V2—V3 | 83.78 (5) | O21—V9—V10 | 126.07 (5) |
O10—V2—V3 | 32.84 (5) | O23—V9—V10 | 78.87 (5) |
O13—V2—V3 | 124.31 (4) | O25—V9—V10 | 78.86 (4) |
O12i—V2—V3 | 86.29 (4) | O20—V9—V10 | 31.23 (4) |
O14—V2—V3 | 48.26 (4) | O28—V9—V10 | 43.59 (3) |
V1i—V2—V3 | 119.130 (14) | O18—V9—V8 | 137.88 (6) |
O3—V3—O7 | 104.53 (7) | O21—V9—V8 | 33.45 (5) |
O3—V3—O10 | 102.63 (7) | O23—V9—V8 | 86.20 (5) |
O7—V3—O10 | 91.08 (7) | O25—V9—V8 | 83.64 (5) |
O3—V3—O8 | 102.39 (7) | O20—V9—V8 | 123.82 (4) |
O7—V3—O8 | 89.42 (6) | O28—V9—V8 | 49.04 (3) |
O10—V3—O8 | 154.01 (6) | V10—V9—V8 | 92.622 (13) |
O3—V3—O5 | 99.34 (7) | O18—V9—V6 | 133.99 (6) |
O7—V3—O5 | 156.07 (6) | O21—V9—V6 | 82.15 (5) |
O10—V3—O5 | 85.36 (6) | O23—V9—V6 | 32.97 (5) |
O8—V3—O5 | 83.74 (6) | O25—V9—V6 | 123.90 (5) |
O3—V3—O14 | 174.61 (7) | O20—V9—V6 | 83.22 (4) |
O7—V3—O14 | 80.77 (6) | O28—V9—V6 | 46.23 (3) |
O10—V3—O14 | 78.02 (6) | V10—V9—V6 | 62.356 (11) |
O8—V3—O14 | 76.42 (6) | V8—V9—V6 | 61.029 (11) |
O5—V3—O14 | 75.34 (5) | O20—V10—O19ii | 107.46 (7) |
O3—V3—V5i | 130.73 (6) | O20—V10—O26 | 97.62 (7) |
O7—V3—V5i | 124.73 (5) | O19ii—V10—O26 | 96.82 (6) |
O10—V3—V5i | 79.52 (5) | O20—V10—O27 | 96.95 (7) |
O8—V3—V5i | 78.90 (5) | O19ii—V10—O27 | 96.94 (6) |
O5—V3—V5i | 31.39 (4) | O26—V10—O27 | 155.94 (6) |
O14—V3—V5i | 43.96 (3) | O20—V10—O28 | 87.70 (6) |
O3—V3—V4 | 137.00 (6) | O19ii—V10—O28 | 164.85 (7) |
O7—V3—V4 | 32.48 (4) | O26—V10—O28 | 81.08 (6) |
O10—V3—V4 | 84.27 (5) | O27—V10—O28 | 80.49 (6) |
O8—V3—V4 | 82.29 (4) | O20—V10—O28ii | 165.68 (6) |
O5—V3—V4 | 123.62 (4) | O19ii—V10—O28ii | 86.86 (6) |
O14—V3—V4 | 48.29 (3) | O26—V10—O28ii | 80.43 (6) |
V5i—V3—V4 | 92.252 (12) | O27—V10—O28ii | 80.72 (6) |
O3—V3—V2 | 135.19 (6) | O28—V10—O28ii | 77.99 (6) |
O7—V3—V2 | 81.54 (5) | O20—V10—V9 | 39.21 (5) |
O10—V3—V2 | 32.60 (4) | O19ii—V10—V9 | 146.65 (5) |
O8—V3—V2 | 122.23 (5) | O26—V10—V9 | 89.26 (4) |
O5—V3—V2 | 82.81 (4) | O27—V10—V9 | 90.02 (4) |
O14—V3—V2 | 45.82 (4) | O28—V10—V9 | 48.50 (4) |
V5i—V3—V2 | 61.720 (11) | O28ii—V10—V9 | 126.48 (4) |
V4—V3—V2 | 60.580 (11) | O20—V10—V8ii | 145.06 (5) |
O4—V4—O7 | 103.53 (8) | O19ii—V10—V8ii | 37.62 (5) |
O4—V4—O9 | 102.04 (8) | O26—V10—V8ii | 88.50 (4) |
O7—V4—O9 | 92.36 (7) | O27—V10—V8ii | 90.44 (4) |
O4—V4—O11 | 102.49 (8) | O28—V10—V8ii | 127.23 (4) |
O7—V4—O11 | 91.26 (7) | O28ii—V10—V8ii | 49.25 (4) |
O9—V4—O11 | 153.61 (6) | V9—V10—V8ii | 175.513 (15) |
O4—V4—O6 | 100.51 (7) | V10ii—O19—V8 | 111.65 (7) |
O7—V4—O6 | 155.95 (6) | V10—O20—V9 | 109.57 (7) |
O9—V4—O6 | 83.33 (6) | V9—O21—V8 | 113.77 (7) |
O11—V4—O6 | 82.78 (6) | V6—O22—V8 | 114.91 (7) |
O4—V4—O14 | 174.44 (7) | V6—O23—V9 | 113.83 (7) |
O7—V4—O14 | 82.03 (6) | V7—O24—V8 | 114.03 (7) |
O9—V4—O14 | 77.39 (6) | V7—O25—V9 | 113.61 (8) |
O11—V4—O14 | 77.25 (6) | V10—O26—V7ii | 107.65 (7) |
O6—V4—O14 | 73.93 (5) | V10—O26—V6 | 107.02 (6) |
O4—V4—V5 | 130.94 (6) | V7ii—O26—V6 | 98.87 (6) |
O7—V4—V5 | 125.53 (5) | V10—O27—V6ii | 107.02 (7) |
O9—V4—V5 | 78.26 (5) | V10—O27—V7 | 107.20 (6) |
O11—V4—V5 | 78.40 (4) | V6ii—O27—V7 | 100.81 (6) |
O6—V4—V5 | 30.43 (4) | V10—O28—V10ii | 102.01 (6) |
O14—V4—V5 | 43.50 (3) | V10—O28—V7 | 93.75 (5) |
O4—V4—V3 | 136.89 (6) | V10ii—O28—V7 | 92.92 (5) |
O7—V4—V3 | 33.36 (5) | V10—O28—V6 | 94.12 (5) |
O9—V4—V3 | 84.91 (5) | V10ii—O28—V6 | 91.96 (5) |
O11—V4—V3 | 83.85 (5) | V7—O28—V6 | 169.68 (7) |
O6—V4—V3 | 122.59 (4) | V10—O28—V9 | 87.91 (5) |
O14—V4—V3 | 48.67 (3) | V10ii—O28—V9 | 170.03 (7) |
V5—V4—V3 | 92.167 (12) | V7—O28—V9 | 87.34 (5) |
O4—V4—V1 | 134.33 (6) | V6—O28—V9 | 86.28 (5) |
O7—V4—V1 | 82.60 (5) | V10—O28—V8 | 170.88 (7) |
O9—V4—V1 | 32.36 (4) | V10ii—O28—V8 | 87.07 (5) |
O11—V4—V1 | 122.81 (5) | V7—O28—V8 | 84.85 (5) |
O6—V4—V1 | 81.20 (4) | V6—O28—V8 | 86.33 (5) |
O14—V4—V1 | 45.56 (4) | V9—O28—V8 | 83.03 (5) |
V5—V4—V1 | 61.146 (11) | O33—Mg1—O30 | 94.51 (7) |
V3—V4—V1 | 60.952 (11) | O33—Mg1—O31 | 175.63 (7) |
O6—V5—O5i | 107.64 (7) | O30—Mg1—O31 | 89.47 (7) |
O6—V5—O12 | 97.94 (7) | O33—Mg1—O32 | 90.32 (7) |
O5i—V5—O12 | 97.49 (7) | O30—Mg1—O32 | 174.35 (7) |
O6—V5—O13 | 97.28 (7) | O31—Mg1—O32 | 85.61 (7) |
O5i—V5—O13 | 96.50 (7) | O33—Mg1—O29 | 90.62 (7) |
O12—V5—O13 | 155.12 (6) | O30—Mg1—O29 | 91.27 (7) |
O6—V5—O14 | 87.28 (6) | O31—Mg1—O29 | 91.10 (7) |
O5i—V5—O14 | 165.06 (6) | O32—Mg1—O29 | 91.60 (6) |
O12—V5—O14 | 80.84 (6) | O33—Mg1—O34 | 87.28 (7) |
O13—V5—O14 | 80.35 (6) | O30—Mg1—O34 | 86.69 (7) |
O6—V5—O14i | 164.89 (6) | O31—Mg1—O34 | 91.15 (7) |
O5i—V5—O14i | 87.45 (6) | O32—Mg1—O34 | 90.63 (6) |
O12—V5—O14i | 80.18 (6) | O29—Mg1—O34 | 176.95 (7) |
O13—V5—O14i | 80.00 (6) | Mg1—O29—H29A | 135.3 |
O14—V5—O14i | 77.62 (6) | Mg1—O29—H29B | 123.0 |
O6—V5—V3i | 145.92 (5) | H29A—O29—H29B | 96.1 |
O5i—V5—V3i | 38.29 (5) | Mg1—O30—H30A | 116.5 |
O12—V5—V3i | 88.72 (4) | Mg1—O30—H30B | 124.0 |
O13—V5—V3i | 89.62 (4) | H30A—O30—H30B | 96.0 |
O14—V5—V3i | 126.80 (4) | Mg1—O31—H31A | 129.4 |
O14i—V5—V3i | 49.18 (4) | Mg1—O31—H31B | 126.0 |
O6—V5—V4 | 38.50 (5) | H31A—O31—H31B | 103.6 |
O5i—V5—V4 | 146.15 (5) | Mg1—O32—H32A | 117.9 |
O12—V5—V4 | 89.88 (4) | Mg1—O32—H32B | 122.6 |
O13—V5—V4 | 89.87 (4) | H32A—O32—H32B | 103.9 |
O14—V5—V4 | 48.78 (4) | Mg1—O33—H33A | 121.9 |
O14i—V5—V4 | 126.40 (4) | Mg1—O33—H33B | 139.8 |
V3i—V5—V4 | 175.553 (15) | H33A—O33—H33B | 97.5 |
V5i—O5—V3 | 110.32 (7) | Mg1—O34—H34A | 112.8 |
V5—O6—V4 | 111.06 (7) | Mg1—O34—H34B | 108.7 |
V4—O7—V3 | 114.16 (7) | H34A—O34—H34B | 89.1 |
V1—O8—V3 | 115.51 (8) | O37—Mg2—O38 | 91.00 (7) |
V1—O9—V4 | 114.19 (8) | O37—Mg2—O40 | 91.80 (7) |
V2—O10—V3 | 114.56 (7) | O38—Mg2—O40 | 176.81 (8) |
V2—O11—V4 | 114.61 (8) | O37—Mg2—O36 | 176.32 (7) |
V5—O12—V1 | 106.59 (7) | O38—Mg2—O36 | 86.78 (7) |
V5—O12—V2i | 108.25 (7) | O40—Mg2—O36 | 90.35 (7) |
V1—O12—V2i | 99.26 (6) | O37—Mg2—O35 | 94.97 (7) |
V5—O13—V1i | 107.50 (7) | O38—Mg2—O35 | 89.63 (7) |
V5—O13—V2 | 107.64 (7) | O40—Mg2—O35 | 91.66 (7) |
V1i—O13—V2 | 99.48 (6) | O36—Mg2—O35 | 87.95 (7) |
V5—O14—V5i | 102.38 (6) | O37—Mg2—O39 | 87.34 (7) |
V5—O14—V1 | 92.79 (5) | O38—Mg2—O39 | 89.34 (7) |
V5i—O14—V1 | 93.14 (5) | O40—Mg2—O39 | 89.25 (7) |
V5—O14—V2 | 93.08 (5) | O36—Mg2—O39 | 89.70 (7) |
V5i—O14—V2 | 92.97 (5) | O35—Mg2—O39 | 177.49 (7) |
V1—O14—V2 | 170.43 (7) | Mg2—O35—H35A | 121.1 |
V5—O14—V4 | 87.72 (5) | Mg2—O35—H35B | 113.5 |
V5i—O14—V4 | 169.90 (7) | H35A—O35—H35B | 105.1 |
V1—O14—V4 | 86.11 (5) | Mg2—O36—H36A | 127.8 |
V2—O14—V4 | 86.58 (5) | Mg2—O36—H36B | 124.4 |
V5—O14—V3 | 170.75 (7) | H36A—O36—H36B | 97.6 |
V5i—O14—V3 | 86.86 (5) | Mg2—O37—H37A | 125.9 |
V1—O14—V3 | 87.08 (5) | Mg2—O37—H37B | 121.6 |
V2—O14—V3 | 85.91 (5) | H37A—O37—H37B | 112.0 |
V4—O14—V3 | 83.04 (5) | Mg2—O38—H38A | 128.9 |
O15—V6—O22 | 103.15 (7) | Mg2—O38—H38B | 112.3 |
O15—V6—O23 | 101.80 (7) | H38A—O38—H38B | 117.7 |
O22—V6—O23 | 95.03 (7) | Mg2—O39—H39A | 119.9 |
O15—V6—O27ii | 100.25 (7) | Mg2—O39—H39B | 118.9 |
O22—V6—O27ii | 92.11 (6) | H39A—O39—H39B | 106.7 |
O23—V6—O27ii | 154.58 (6) | Mg2—O40—H40A | 117.4 |
O15—V6—O26 | 99.81 (7) | Mg2—O40—H40B | 121.0 |
O22—V6—O26 | 155.91 (6) | H40A—O40—H40B | 119.2 |
O23—V6—O26 | 87.28 (6) | O45—Mg3—O43 | 175.38 (8) |
O27ii—V6—O26 | 76.62 (6) | O45—Mg3—O44 | 93.00 (8) |
O15—V6—O28 | 175.03 (7) | O43—Mg3—O44 | 91.41 (7) |
O22—V6—O28 | 81.27 (6) | O45—Mg3—O46 | 90.61 (8) |
O23—V6—O28 | 79.87 (6) | O43—Mg3—O46 | 87.59 (8) |
O27ii—V6—O28 | 77.15 (6) | O44—Mg3—O46 | 95.69 (9) |
O26—V6—O28 | 75.53 (5) | O45—Mg3—O41 | 89.20 (7) |
O15—V6—V7ii | 90.30 (6) | O43—Mg3—O41 | 92.53 (7) |
O22—V6—V7ii | 132.09 (5) | O44—Mg3—O41 | 85.30 (7) |
O23—V6—V7ii | 127.29 (5) | O46—Mg3—O41 | 179.01 (9) |
O27ii—V6—V7ii | 40.00 (4) | O45—Mg3—O42 | 87.78 (7) |
O26—V6—V7ii | 40.01 (4) | O43—Mg3—O42 | 87.96 (7) |
O28—V6—V7ii | 85.01 (4) | O44—Mg3—O42 | 174.27 (8) |
O15—V6—V9 | 134.72 (6) | O46—Mg3—O42 | 89.98 (9) |
O22—V6—V9 | 82.95 (5) | O41—Mg3—O42 | 89.04 (7) |
O23—V6—V9 | 33.20 (4) | O45—Mg3—H44A | 93.1 |
O27ii—V6—V9 | 124.58 (4) | O43—Mg3—H44A | 90.5 |
O26—V6—V9 | 86.09 (4) | O44—Mg3—H44A | 20.3 |
O28—V6—V9 | 47.48 (4) | O46—Mg3—H44A | 75.4 |
V7ii—V6—V9 | 118.923 (13) | O41—Mg3—H44A | 105.6 |
O16—V7—O24 | 102.60 (7) | O42—Mg3—H44A | 165.3 |
O16—V7—O25 | 103.35 (7) | Mg3—O41—H41A | 142.8 |
O24—V7—O25 | 94.66 (7) | Mg3—O41—H41B | 120.0 |
O16—V7—O26ii | 99.38 (7) | H41A—O41—H41B | 84.8 |
O24—V7—O26ii | 90.51 (6) | Mg3—O42—H42A | 109.7 |
O25—V7—O26ii | 154.95 (6) | Mg3—O42—H42B | 134.3 |
O16—V7—O27 | 98.99 (7) | H42A—O42—H42B | 113.7 |
O24—V7—O27 | 156.53 (6) | Mg3—O43—H43A | 121.8 |
O25—V7—O27 | 89.18 (6) | Mg3—O43—H43B | 119.2 |
O26ii—V7—O27 | 76.90 (6) | H43A—O43—H43B | 114.4 |
O16—V7—O28 | 173.97 (7) | Mg3—O44—H44A | 93.6 |
O24—V7—O28 | 81.82 (6) | Mg3—O44—H44B | 117.9 |
O25—V7—O28 | 80.19 (6) | H44A—O44—H44B | 136.2 |
O26ii—V7—O28 | 76.31 (5) | Mg3—O45—H45A | 129.4 |
O27—V7—O28 | 76.03 (5) | Mg3—O45—H45B | 118.2 |
O16—V7—V6ii | 89.17 (6) | H45A—O45—H45B | 112.4 |
O24—V7—V6ii | 131.63 (5) | Mg3—O46—H46A | 126.4 |
O25—V7—V6ii | 128.37 (5) | Mg3—O46—H46B | 112.5 |
O26ii—V7—V6ii | 41.12 (4) | H46A—O46—H46B | 102.5 |
O27—V7—V6ii | 39.19 (4) | H47A—O47—H47B | 104.4 |
O28—V7—V6ii | 84.82 (4) | H48A—O48—H48B | 107.1 |
O16—V7—V8 | 135.88 (5) | H49A—O49—H49B | 102.4 |
O24—V7—V8 | 33.37 (4) | H50A—O50—H50B | 117.5 |
O25—V7—V8 | 83.95 (5) | H51A—O51—H51B | 108.1 |
O26ii—V7—V8 | 87.07 (4) | H52A—O52—H52B | 115.8 |
O27—V7—V8 | 124.84 (4) | H53A—O53—H53B | 123.7 |
O28—V7—V8 | 48.84 (4) | H54A—O54—H54B | 107.8 |
V6ii—V7—V8 | 120.461 (14) | H55A—O55A—H55B | 110.3 |
O17—V8—O21 | 104.09 (7) | H55A—O55B—H55B | 90.3 |
O17—V8—O24 | 103.00 (7) | H56A—O56A—H56B | 118.7 |
Symmetry codes: (i) −x, −y, −z; (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 |
O29—H29A···O13iii | 0.78 | 1.96 | 2.734 (2) | 170.2 |
O29—H29B···O35 | 0.77 | 2.38 | 3.099 (2) | 154.6 |
O30—H30A···O1 | 0.84 | 1.89 | 2.726 (2) | 171.3 |
O30—H30B···O8iv | 0.86 | 1.80 | 2.631 (2) | 163.5 |
O31—H31A···O5iv | 0.85 | 2.10 | 2.909 (2) | 159.2 |
O31—H31B···O10v | 0.80 | 1.95 | 2.743 (2) | 168.9 |
O32—H32A···O49 | 0.78 | 1.94 | 2.704 (2) | 167.1 |
O32—H32B···O16ii | 0.83 | 1.99 | 2.767 (2) | 155.9 |
O33—H33A···O48 | 0.84 | 1.86 | 2.695 (2) | 174.9 |
O33—H33B···O9 | 0.83 | 1.93 | 2.741 (2) | 168.2 |
O34—H34A···O55B | 0.82 | 1.94 | 2.742 (6) | 164.7 |
O34—H34A···O55A | 0.82 | 2.00 | 2.813 (3) | 174.0 |
O34—H34B···O55Avi | 0.92 | 1.96 | 2.865 (5) | 167.9 |
O34—H34B···O55Bvi | 0.92 | 2.59 | 3.492 (11) | 168.4 |
O35—H35A···O11iii | 0.83 | 1.91 | 2.738 (2) | 172.1 |
O35—H35B···O47vii | 0.80 | 1.96 | 2.756 (2) | 170.3 |
O36—H36A···O54 | 0.85 | 1.91 | 2.757 (2) | 168.6 |
O36—H36B···O27ii | 0.92 | 1.86 | 2.782 (2) | 175.2 |
O37—H37A···O4iii | 0.81 | 2.03 | 2.829 (2) | 172.5 |
O37—H37B···O23iii | 0.87 | 1.83 | 2.701 (2) | 175.8 |
O38—H38A···O50iii | 0.89 | 1.86 | 2.725 (2) | 165.5 |
O38—H38B···O32 | 0.85 | 1.98 | 2.830 (2) | 172.8 |
O39—H39A···O25ii | 0.83 | 1.88 | 2.709 (2) | 171.5 |
O39—H39B···O18iii | 0.92 | 1.92 | 2.822 (2) | 167.3 |
O40—H40A···O53 | 0.85 | 1.87 | 2.715 (2) | 173.8 |
O40—H40B···O51 | 0.86 | 2.05 | 2.869 (2) | 160.9 |
O40—H40B···O17viii | 0.86 | 2.59 | 3.105 (2) | 119.6 |
O41—H41A···O23 | 0.85 | 2.12 | 2.934 (2) | 162.4 |
O41—H41B···O39ix | 1.03 | 1.83 | 2.857 (2) | 176.5 |
O42—H42A···O49ix | 0.80 | 1.96 | 2.748 (2) | 166.2 |
O42—H42B···O25x | 0.84 | 2.01 | 2.842 (2) | 171.3 |
O43—H43A···O17xi | 0.92 | 1.88 | 2.762 (2) | 160.0 |
O43—H43B···O18x | 0.87 | 1.98 | 2.775 (2) | 151.6 |
O43—H43B···O20 | 0.87 | 2.53 | 3.045 (2) | 118.3 |
O44—H44A···O51xi | 0.78 | 2.04 | 2.728 (2) | 146.5 |
O44—H44B···O26 | 0.99 | 1.99 | 2.956 (2) | 166.0 |
O44—H44B···O24ii | 0.99 | 2.41 | 3.000 (2) | 117.6 |
O44—H44B···O19ii | 0.99 | 2.57 | 3.150 (2) | 117.4 |
O45—H45A···O7xi | 0.82 | 1.97 | 2.743 (2) | 155.5 |
O45—H45B···O50 | 0.73 | 2.00 | 2.732 (2) | 176.9 |
O46—H46A···O22xi | 0.93 | 1.88 | 2.796 (2) | 168.5 |
O46—H46B···O4xi | 0.76 | 2.31 | 3.054 (2) | 164.9 |
O47—H47A···O56B | 0.80 | 1.92 | 2.705 (5) | 168.4 |
O47—H47A···O56A | 0.80 | 1.97 | 2.747 (3) | 162.2 |
O47—H47B···O24ii | 0.83 | 2.10 | 2.916 (2) | 171.1 |
O48—H48A···O56B | 0.88 | 1.86 | 2.730 (5) | 168.2 |
O48—H48A···O56A | 0.88 | 1.90 | 2.731 (3) | 156.2 |
O48—H48B···O15 | 0.83 | 2.02 | 2.812 (2) | 157.6 |
O49—H49A···O11v | 0.80 | 2.33 | 3.047 (2) | 149.7 |
O49—H49A···O10v | 0.80 | 2.53 | 3.185 (2) | 139.7 |
O49—H49B···O47 | 0.91 | 1.83 | 2.717 (2) | 165.2 |
O50—H50A···O3xi | 0.84 | 2.21 | 2.949 (2) | 147.2 |
O50—H50B···O48 | 0.91 | 1.83 | 2.716 (2) | 165.4 |
O51—H51A···O54 | 0.87 | 1.96 | 2.830 (2) | 170.8 |
O51—H51B···O22 | 0.91 | 2.07 | 2.867 (2) | 146.5 |
O52—H52A···O2v | 0.85 | 2.35 | 3.054 (2) | 140.5 |
O52—H52B···O8xi | 0.71 | 2.41 | 3.075 (2) | 155.3 |
O52—H52B···O9xi | 0.71 | 2.52 | 3.096 (2) | 138.7 |
O53—H53A···O21iii | 0.92 | 2.03 | 2.878 (2) | 153.1 |
O53—H53B···O21viii | 1.12 | 1.86 | 2.969 (2) | 170.4 |
O54—H54A···O52vii | 0.87 | 1.95 | 2.805 (2) | 166.0 |
O54—H54B···O4 | 0.88 | 2.39 | 3.207 (2) | 155.3 |
O54—H54B···O15 | 0.88 | 2.51 | 3.008 (2) | 116.3 |
O55A—H55A···O12 | 0.82 | 1.98 | 2.780 (3) | 163.1 |
O55A—H55B···O3xi | 0.80 | 2.47 | 3.245 (3) | 163.1 |
O56A—H56A···O52 | 0.85 | 2.04 | 2.760 (3) | 141.4 |
O56A—H56B···O34 | 0.87 | 2.04 | 2.802 (3) | 146.3 |
O56A—H56B···O2v | 0.87 | 2.50 | 3.097 (3) | 126.4 |
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (iv) −x, −y+1, −z; (v) x+1, y+1, z; (vi) −x+1, −y+1, −z; (vii) x−1, y, z; (viii) −x, −y+1, −z+1; (ix) x, y−1, z; (x) −x+1, −y, −z+1; (xi) x+1, y, z. |
Experimental details
| (I) | (II) |
Crystal data |
Chemical formula | Mg2Na2V10O28·20H2O | Mg3V10O28·28H2O |
Mr | 1412.32 | 1534.78 |
Crystal system, space group | Monoclinic, C2/c | Triclinic, P1 |
Temperature (K) | 93 | 93 |
a, b, c (Å) | 23.8384 (6), 11.0248 (2), 16.9332 (4) | 10.4834 (1), 10.7309 (2), 21.2293 (4) |
α, β, γ (°) | 90, 118.005 (1), 90 | 90.751 (1), 97.866 (1), 103.663 (1) |
V (Å3) | 3929.18 (15) | 2296.24 (6) |
Z | 4 | 2 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 2.46 | 2.12 |
Crystal size (mm) | 0.20 × 0.18 × 0.08 | 0.30 × 0.18 × 0.14 |
|
Data collection |
Diffractometer | Bruker SMART CCD area-detector system diffractometer | Bruker SMART CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.640, 0.821 | 0.518, 0.743 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 18758, 5746, 4522 | 22420, 13207, 10950 |
Rint | 0.034 | 0.025 |
(sin θ/λ)max (Å−1) | 0.704 | 0.704 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.075, 1.01 | 0.032, 0.086, 1.01 |
No. of reflections | 5746 | 13207 |
No. of parameters | 360 | 632 |
H-atom treatment | All H-atom parameters refined | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.72, −1.24 | 0.99, −0.95 |
Selected bond lengths (Å) for (I) topV1—O1 | 1.6008 (13) | V4—O11 | 1.9117 (13) |
V1—O8 | 1.8356 (12) | V4—O6 | 2.0506 (13) |
V1—O9 | 1.8425 (12) | V4—O14 | 2.3120 (12) |
V1—O12 | 2.0005 (12) | V5—O5i | 1.6932 (13) |
V1—O12i | 2.0036 (12) | V5—O6 | 1.6967 (13) |
V1—O14 | 2.2717 (13) | V5—O13 | 1.9168 (13) |
V2—O2 | 1.6140 (14) | V5—O12 | 1.9349 (13) |
V2—O11 | 1.7973 (13) | V5—O14i | 2.0995 (12) |
V2—O10 | 1.8496 (13) | V5—O14 | 2.1239 (12) |
V2—O13 | 1.9923 (13) | Mg—O18 | 2.0234 (15) |
V2—O13i | 2.0373 (12) | Mg—O16 | 2.0298 (15) |
V2—O14 | 2.2376 (13) | Mg—O15 | 2.0500 (16) |
V3—O3 | 1.6097 (13) | Mg—O20 | 2.0523 (16) |
V3—O7 | 1.8512 (13) | Mg—O17 | 2.1082 (15) |
V3—O10 | 1.8557 (13) | Mg—O19 | 2.1398 (15) |
V3—O8 | 1.8933 (13) | Na—O22 | 2.3481 (17) |
V3—O5 | 2.0510 (13) | Na—O21 | 2.4195 (19) |
V3—O14 | 2.3396 (12) | Na—O11 | 2.4264 (15) |
V4—O4 | 1.6071 (13) | Na—O21ii | 2.5864 (19) |
V4—O7 | 1.8349 (13) | Na—O3iii | 2.6620 (15) |
V4—O9 | 1.8516 (13) | Na—O4 | 2.9714 (16) |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x+1/2, −y+3/2, −z+1; (iii) x, −y+1, z+1/2. |
Hydrogen-bond geometry (Å, º) for (I) top
D—H···A | D—H | H···A | D···A | D—H···A |
O15—H15A···O8iv | 0.72 (3) | 2.02 (3) | 2.7291 (19) | 169 (3) |
O15—H15B···O24v | 0.72 (3) | 2.06 (3) | 2.749 (2) | 160 (3) |
O16—H16A···O12 | 0.67 (3) | 1.98 (3) | 2.6517 (19) | 175 (4) |
O16—H16B···O19vi | 0.75 (3) | 2.02 (3) | 2.774 (2) | 179 (3) |
O17—H17A···O9 | 0.77 (3) | 2.05 (3) | 2.7933 (19) | 164 (2) |
O17—H17B···O7vii | 0.71 (3) | 2.10 (3) | 2.8052 (19) | 174 (3) |
O18—H18A···O23iv | 0.74 (3) | 1.99 (3) | 2.729 (2) | 176 (3) |
O18—H18B···O22viii | 0.69 (3) | 2.11 (3) | 2.800 (2) | 177 (3) |
O19—H19A···O2iii | 0.73 (3) | 2.26 (3) | 2.8600 (19) | 141 (3) |
O19—H19A···O1iv | 0.73 (3) | 2.52 (3) | 3.037 (2) | 130 (2) |
O19—H19B···O24ix | 0.72 (3) | 2.11 (3) | 2.822 (2) | 170 (3) |
O20—H20A···O6 | 0.68 (3) | 2.05 (3) | 2.725 (2) | 176 (3) |
O20—H20B···O10iii | 0.72 (3) | 1.97 (3) | 2.686 (2) | 171 (3) |
O21—H21A···O17x | 0.72 (3) | 2.29 (4) | 3.007 (2) | 176 (4) |
O21—H21B···O2 | 0.80 (3) | 2.34 (3) | 3.052 (2) | 149 (3) |
O22—H22A···O23iii | 0.69 (3) | 2.09 (3) | 2.784 (2) | 174 (3) |
O22—H22B···O10ii | 0.77 (3) | 2.30 (3) | 2.950 (2) | 142 (3) |
O23—H23A···O8 | 0.69 (3) | 2.11 (3) | 2.756 (2) | 154 (3) |
O23—H23B···O4vii | 0.82 (3) | 2.19 (3) | 2.900 (2) | 146 (3) |
O24—H24A···O13 | 0.74 (3) | 1.95 (3) | 2.685 (2) | 172 (3) |
O24—H24B···O5iii | 0.67 (3) | 2.17 (3) | 2.827 (2) | 167 (3) |
Symmetry codes: (ii) −x+1/2, −y+3/2, −z+1; (iii) x, −y+1, z+1/2; (iv) x, −y, z+1/2; (v) x, y−1, z; (vi) −x, −y, −z+1; (vii) −x+1/2, −y+1/2, −z+1; (viii) −x+1/2, y−1/2, −z+3/2; (ix) −x, −y+1, −z+1; (x) x, y+1, z. |
Selected bond lengths (Å) for (II) topV1—O1 | 1.6134 (15) | V7—O26ii | 1.9946 (15) |
V1—O9 | 1.8177 (15) | V7—O27 | 2.0060 (14) |
V1—O8 | 1.8312 (14) | V7—O28 | 2.2420 (14) |
V1—O13i | 1.9927 (14) | V8—O17 | 1.5992 (15) |
V1—O12 | 1.9962 (14) | V8—O21 | 1.8478 (15) |
V1—O14 | 2.2168 (14) | V8—O24 | 1.8593 (14) |
V2—O2 | 1.6063 (16) | V8—O22 | 1.9128 (14) |
V2—O11 | 1.8279 (15) | V8—O19 | 2.0207 (15) |
V2—O10 | 1.8471 (15) | V8—O28 | 2.3340 (14) |
V2—O13 | 1.9953 (14) | V9—O18 | 1.6169 (16) |
V2—O12i | 1.9984 (14) | V9—O21 | 1.8147 (15) |
V2—O14 | 2.2421 (14) | V9—O23 | 1.8592 (15) |
V3—O3 | 1.6098 (15) | V9—O25 | 1.9005 (14) |
V3—O7 | 1.8587 (15) | V9—O20 | 2.0537 (14) |
V3—O10 | 1.8593 (16) | V9—O28 | 2.2943 (15) |
V3—O8 | 1.8756 (15) | V10—O20 | 1.6843 (15) |
V3—O5 | 2.0335 (15) | V10—O19ii | 1.6914 (14) |
V3—O14 | 2.3327 (14) | V10—O26 | 1.9306 (14) |
V4—O4 | 1.6144 (15) | V10—O27 | 1.9432 (14) |
V4—O7 | 1.8148 (15) | V10—O28 | 2.1120 (14) |
V4—O9 | 1.8717 (15) | V10—O28ii | 2.1277 (14) |
V4—O11 | 1.8892 (15) | Mg1—O33 | 2.0351 (17) |
V4—O6 | 2.0554 (15) | Mg1—O30 | 2.0474 (16) |
V4—O14 | 2.3193 (14) | Mg1—O31 | 2.0721 (17) |
V5—O6 | 1.6725 (14) | Mg1—O32 | 2.0846 (16) |
V5—O5i | 1.7097 (14) | Mg1—O29 | 2.0868 (17) |
V5—O12 | 1.9236 (15) | Mg1—O34 | 2.1165 (17) |
V5—O13 | 1.9307 (15) | Mg2—O37 | 2.0413 (17) |
V5—O14 | 2.1226 (14) | Mg2—O38 | 2.0453 (17) |
V5—O14i | 2.1396 (14) | Mg2—O40 | 2.0509 (17) |
V6—O15 | 1.6135 (15) | Mg2—O36 | 2.0643 (18) |
V6—O22 | 1.8058 (14) | Mg2—O35 | 2.0818 (16) |
V6—O23 | 1.8481 (15) | Mg2—O39 | 2.1008 (16) |
V6—O27ii | 1.9717 (15) | Mg3—O45 | 2.0414 (17) |
V6—O26 | 2.0402 (14) | Mg3—O43 | 2.0521 (17) |
V6—O28 | 2.2479 (14) | Mg3—O44 | 2.0571 (19) |
V7—O16 | 1.6119 (15) | Mg3—O46 | 2.0692 (19) |
V7—O24 | 1.8217 (14) | Mg3—O41 | 2.0756 (17) |
V7—O25 | 1.8429 (15) | Mg3—O42 | 2.0837 (17) |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) for (II) top
D—H···A | D—H | H···A | D···A | D—H···A |
O29—H29A···O13iii | 0.78 | 1.96 | 2.734 (2) | 170.2 |
O29—H29B···O35 | 0.77 | 2.38 | 3.099 (2) | 154.6 |
O30—H30A···O1 | 0.84 | 1.89 | 2.726 (2) | 171.3 |
O30—H30B···O8iv | 0.86 | 1.80 | 2.631 (2) | 163.5 |
O31—H31A···O5iv | 0.85 | 2.10 | 2.909 (2) | 159.2 |
O31—H31B···O10v | 0.80 | 1.95 | 2.743 (2) | 168.9 |
O32—H32A···O49 | 0.78 | 1.94 | 2.704 (2) | 167.1 |
O32—H32B···O16ii | 0.83 | 1.99 | 2.767 (2) | 155.9 |
O33—H33A···O48 | 0.84 | 1.86 | 2.695 (2) | 174.9 |
O33—H33B···O9 | 0.83 | 1.93 | 2.741 (2) | 168.2 |
O34—H34A···O55B | 0.82 | 1.94 | 2.742 (6) | 164.7 |
O34—H34A···O55A | 0.82 | 2.00 | 2.813 (3) | 174.0 |
O34—H34B···O55Avi | 0.92 | 1.96 | 2.865 (5) | 167.9 |
O34—H34B···O55Bvi | 0.92 | 2.59 | 3.492 (11) | 168.4 |
O35—H35A···O11iii | 0.83 | 1.91 | 2.738 (2) | 172.1 |
O35—H35B···O47vii | 0.80 | 1.96 | 2.756 (2) | 170.3 |
O36—H36A···O54 | 0.85 | 1.91 | 2.757 (2) | 168.6 |
O36—H36B···O27ii | 0.92 | 1.86 | 2.782 (2) | 175.2 |
O37—H37A···O4iii | 0.81 | 2.03 | 2.829 (2) | 172.5 |
O37—H37B···O23iii | 0.87 | 1.83 | 2.701 (2) | 175.8 |
O38—H38A···O50iii | 0.89 | 1.86 | 2.725 (2) | 165.5 |
O38—H38B···O32 | 0.85 | 1.98 | 2.830 (2) | 172.8 |
O39—H39A···O25ii | 0.83 | 1.88 | 2.709 (2) | 171.5 |
O39—H39B···O18iii | 0.92 | 1.92 | 2.822 (2) | 167.3 |
O40—H40A···O53 | 0.85 | 1.87 | 2.715 (2) | 173.8 |
O40—H40B···O51 | 0.86 | 2.05 | 2.869 (2) | 160.9 |
O40—H40B···O17viii | 0.86 | 2.59 | 3.105 (2) | 119.6 |
O41—H41A···O23 | 0.85 | 2.12 | 2.934 (2) | 162.4 |
O41—H41B···O39ix | 1.03 | 1.83 | 2.857 (2) | 176.5 |
O42—H42A···O49ix | 0.80 | 1.96 | 2.748 (2) | 166.2 |
O42—H42B···O25x | 0.84 | 2.01 | 2.842 (2) | 171.3 |
O43—H43A···O17xi | 0.92 | 1.88 | 2.762 (2) | 160.0 |
O43—H43B···O18x | 0.87 | 1.98 | 2.775 (2) | 151.6 |
O43—H43B···O20 | 0.87 | 2.53 | 3.045 (2) | 118.3 |
O44—H44A···O51xi | 0.78 | 2.04 | 2.728 (2) | 146.5 |
O44—H44B···O26 | 0.99 | 1.99 | 2.956 (2) | 166.0 |
O44—H44B···O24ii | 0.99 | 2.41 | 3.000 (2) | 117.6 |
O44—H44B···O19ii | 0.99 | 2.57 | 3.150 (2) | 117.4 |
O45—H45A···O7xi | 0.82 | 1.97 | 2.743 (2) | 155.5 |
O45—H45B···O50 | 0.73 | 2.00 | 2.732 (2) | 176.9 |
O46—H46A···O22xi | 0.93 | 1.88 | 2.796 (2) | 168.5 |
O46—H46B···O4xi | 0.76 | 2.31 | 3.054 (2) | 164.9 |
O47—H47A···O56B | 0.80 | 1.92 | 2.705 (5) | 168.4 |
O47—H47A···O56A | 0.80 | 1.97 | 2.747 (3) | 162.2 |
O47—H47B···O24ii | 0.83 | 2.10 | 2.916 (2) | 171.1 |
O48—H48A···O56B | 0.88 | 1.86 | 2.730 (5) | 168.2 |
O48—H48A···O56A | 0.88 | 1.90 | 2.731 (3) | 156.2 |
O48—H48B···O15 | 0.83 | 2.02 | 2.812 (2) | 157.6 |
O49—H49A···O11v | 0.80 | 2.33 | 3.047 (2) | 149.7 |
O49—H49A···O10v | 0.80 | 2.53 | 3.185 (2) | 139.7 |
O49—H49B···O47 | 0.91 | 1.83 | 2.717 (2) | 165.2 |
O50—H50A···O3xi | 0.84 | 2.21 | 2.949 (2) | 147.2 |
O50—H50B···O48 | 0.91 | 1.83 | 2.716 (2) | 165.4 |
O51—H51A···O54 | 0.87 | 1.96 | 2.830 (2) | 170.8 |
O51—H51B···O22 | 0.91 | 2.07 | 2.867 (2) | 146.5 |
O52—H52A···O2v | 0.85 | 2.35 | 3.054 (2) | 140.5 |
O52—H52B···O8xi | 0.71 | 2.41 | 3.075 (2) | 155.3 |
O52—H52B···O9xi | 0.71 | 2.52 | 3.096 (2) | 138.7 |
O53—H53A···O21iii | 0.92 | 2.03 | 2.878 (2) | 153.1 |
O53—H53B···O21viii | 1.12 | 1.86 | 2.969 (2) | 170.4 |
O54—H54A···O52vii | 0.87 | 1.95 | 2.805 (2) | 166.0 |
O54—H54B···O4 | 0.88 | 2.39 | 3.207 (2) | 155.3 |
O54—H54B···O15 | 0.88 | 2.51 | 3.008 (2) | 116.3 |
O55A—H55A···O12 | 0.82 | 1.98 | 2.780 (3) | 163.1 |
O55A—H55B···O3xi | 0.80 | 2.47 | 3.245 (3) | 163.1 |
O56A—H56A···O52 | 0.85 | 2.04 | 2.760 (3) | 141.4 |
O56A—H56B···O34 | 0.87 | 2.04 | 2.802 (3) | 146.3 |
O56A—H56B···O2v | 0.87 | 2.50 | 3.097 (3) | 126.4 |
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x, y+1, z; (iv) −x, −y+1, −z; (v) x+1, y+1, z; (vi) −x+1, −y+1, −z; (vii) x−1, y, z; (viii) −x, −y+1, −z+1; (ix) x, y−1, z; (x) −x+1, −y, −z+1; (xi) x+1, y, z. |
Coordination geometries of the water molecules around the Mg2+ cations. top | Mg | O | ε/°(a) | Classification(b) |
Compound I | | | | |
| Mg | O15 | 19.0 | Class 1, Type D |
| | O16 | 0.0 | Class 1, Type D |
| | O17 | 36.5 | Class 2, Type H |
| | O18 | 8.6 | Class 1, Type D |
| | O19 | 40.1 | Class 2, Type H |
| | O20 | 17.2 | Class 1, Type D |
| | | | |
Compound II | | | | |
| Mg1 | O29 | 18.9 | Class 1, Type D |
| | O30 | 40.7 | Class 1", Type J |
| | O31 | 8.3 | Class 1, Type D |
| | O32 | 34.0 | Class 2, Type H |
| | O33 | 7.0 | Class 1, Type D |
| | O34 | 60.0 | Class 2, Type H |
| Mg2 | O35 | 39.2 | Class 2, Type H |
| | O36 | 26.3 | Class 1, Type D |
| | O37 | 6.0 | Class 1, Type D |
| | O38 | 8.9 | Class 1, Type D |
| | O39 | 33.0 | Class 2, Type H |
| | O40 | 13.4 | Class 1, Type D |
| Mg3 | O41 | 25.1 | Class 1, Type D |
| | O42 | 12.6 | Class 1, Type D |
| | O43 | 18.6 | Class 1, Type D |
| | O44 | 27.5 | Class 1, Type D |
| | O45 | 0.0 | Class 1, Type D |
| | O46 | 36.6 | Class 1", Type J |
(a) Angle between the Mg—O bond and the plane defined by the water molecule. (b) Classification defined by Ferraris and Franchini-Angela (1972). |
When precipitated with more than one cationic species, the decavanadate anion, [V10O28]6−, crystallizes into double salts with various kinds of three- dimensional arrangements of the constituent ions. Typical examples are the mineral hummerite, K2Mg2[V10O28].16H2O (Avtamonova et al., 1988), and its isomorphous compounds K2Zn2[V10O28].16H2O (Evans, 1966), (NH4)2Mg2[V10O28].16H2O and Rb2Mg2[V10O28].16H2O (Avtamonova et al., 1988) where the monovalent cations link the decavanadate anions into layers that sandwich the hydrated M(H2O)62+ cations. Recently, various new extended structures have been observed in some double decavanadate salts, such as one-dimensional chains in [Ni(H2O)6]2[Na(H2O)3]2[V10O28]·4H2O (Higami et al., 2002), two-dimensional networks in Na4Ni[V10O28].23H2O (Sun et al., 2002) and three-dimensional structures in K2Ba2[V10O28]·8H2O (Rastsvetaeva, 1999), CuNa4V10O28.23H2O (Iida & Ozeki, 2003) and K4Na2[V10O28].10H2O (Lee & Joo, 2003). We report here the crystal structure of Mg2Na2V10O28.20H2O, (I), as a new addition to the family of alkali magnesium decavanadates. In the structure of (I), the decavanadate anions are linked into a three-dimensional structure by the Na+ cations. Also reported here is the crystal structure of Mg3V10O28.28H2O, (II), which complements the known alkaline earth decavanadates, including Ca3V10O28.17H2O (Swallow et al., 1966), Ca2(H3O)2[V10O28].16H2O (Strukan et al., 1999), Sr3V10O28.22H2O (Nieto et al., 1993) and Ba3V10O28.19H2O (Kamenar et al., 1996).
From solutions containing Mg2+ and Na+ cations, the decavanadate anion crystallizes with both cations to produce (I). An asymmetric unit of (I) includes one-half of a [V10O28]6− anion, an Mg2+ cation, an Na+ cation and water molecules. The decavanadate anion is located on a twofold axis and has a metal–oxygen framework the same as that reported by Evans (1966) (Fig. 1). The Mg2+ cation is octahedrally coordinated by six water molecules, with Mg—O distances of 2.0234 (15)–2.1398 (15) Å. The coordination environment of the Na+ cation consists of two O atoms from two separate [V10O28]6− anions (at 2.6264 and 2.6620 Å) and three water molecules (at 2.3481–2.5864 Å), yielding a coordination geometry between square-pyramidal and trigonal-bipyramidal, with a τ parameter of 0.466 [τ is defined as the difference of the two largest bond angles at the metal center divided by 60 and is expected to be 1 for the ideal trigonal-bipyramidal geometry and 0 for the ideal square-pyramidal geometry (Addison et al., 1984)]. The sixth O atom approaches Na+ at a distance of 2.9714 Å, capping a triangular face of the square pyramid. Each Na+ cation shares two water molecules with its symmetry equivalent, forming a dimeric cation, [Na2(H2O)4]2+, that links the decavanadate anions into a three-dimensional array (Fig. 2). The structure of this array is different from that in other decavanadates, such as (K2Mg2[V10O28].16H2O, (NH4)2Mg2[V10O28].16H2O and Rb2Mg2[V10O28].16H2O (Avtamonova et al., 1988), reflecting the different ionic radius and coordination requirement of the Na+ ion.
From solutions containing only Mg2+ as the cationic species, crystallization with the decavanadate anion gives (II). An asymmetric unit of (II) consists of two half [V10O28]6− anions, each located on an inversion center, three Mg2+ cations and water molecules of crystallization. The metal–oxygen framework of the decavanadate anion is also identical to that reported by Evans (1966) (Fig. 3). Each Mg2+ cation is octahedrally coordinated by six water molecules, with Mg—O distances ranging from 2.0351 (17) to 2.1165 (17) Å. The hydrated Mg+ cations do not bind to the decavanadate anions; this situation is unlike that observed in other alkaline earth decavanadates or in the para-dodecatungstates Mg5[H2W12O42].38H2O (Tsay & Silverton, 1973) and (NH4)2[Mg4(H2O)18(H2W12O42)].10H2O (Li et al., 1999). In contrast, the hydrated Cu2+ cation binds to the decavanadate anion in its simple salt but not in its double salt with Na+ (Iida & Ozeki, 2003). The three [Mg(OH2)6]2+ octahedra in (II) are linked together by hydrogen bonds. The coordination geometry of the water molecules around the Mg2+ cations is summarized in Table 1. According to the classification of Ferraris & Franchini-Angela (1972), most of the H2O molecules adopt a Class 1 Type D geometry (coordinating only the Mg2+ cation approximately along the bisectrix of the lone-pair orbitals) or a Class 2 Type H geometry (coordinating the Mg2+ cation and accepting a hydrogen bond). However, atoms O30 and O46 adopt a Class 1' Type J geometry (coordinating the Mg2+ cation along a lone-pair orbital), which was not found in MgSO4·7H2O (Ferraris & Jones, 1973) or MgSO4·4H2O (Baur, 1964).