Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802005421/ya6097sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802005421/ya6097Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (Ni-O) = 0.004 Å
- Disorder in solvent or counterion
- R factor = 0.040
- wR factor = 0.100
- Data-to-parameter ratio = 11.5
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry PLATON alerts of the form PLAT_7?? have been detected for an inorganic structure. These tests are under development for inorganics and comments are welcomed. It is not necessary to supply a data validation response form for these alerts at this time.
Alert Level B:
PLAT_420 Alert B D-H Without Acceptor O(11W) - H(111) ? PLAT_735 Alert B D-H Calc 0.85(5), Rep 0.847(10) .... 5.00 s.u-Ratio O1W -H11 1.555 1.555 PLAT_735 Alert B D-H Calc 0.84(5), Rep 0.849(10) .... 5.00 s.u-Ratio O11W -H111 1.555 1.555
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.245 0.290 Tmin and Tmax expected: 0.466 0.750 RR = 1.359 Please check that your absorption correction is appropriate. PLAT_302 Alert C Anion/Solvent Disorder ....................... 3.00 Perc. PLAT_735 Alert C D-H Calc 0.86(4), Rep 0.852(10) .... 4.00 s.u-Ratio O2W -H21 1.555 1.555 PLAT_735 Alert C D-H Calc 0.84(4), Rep 0.853(10) .... 4.00 s.u-Ratio O2W -H22 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.849(10) .... 4.00 s.u-Ratio O3W -H31 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.849(10) .... 4.00 s.u-Ratio O3W -H32 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.848(10) .... 4.00 s.u-Ratio O4W -H41 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.845(10) .... 4.00 s.u-Ratio O4W -H42 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.847(10) .... 4.00 s.u-Ratio O5W -H51 1.555 1.555 PLAT_735 Alert C D-H Calc 0.84(4), Rep 0.847(10) .... 4.00 s.u-Ratio O5W -H52 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.847(10) .... 4.00 s.u-Ratio O6W -H61 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.846(10) .... 3.00 s.u-Ratio O6W -H62 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.847(10) .... 4.00 s.u-Ratio O7W -H71 1.555 1.555 PLAT_735 Alert C D-H Calc 0.84(4), Rep 0.846(10) .... 4.00 s.u-Ratio O7W -H72 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.848(10) .... 4.00 s.u-Ratio O8W -H81 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.852(10) .... 4.00 s.u-Ratio O8W -H82 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.849(10) .... 4.00 s.u-Ratio O9W -H91 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.850(10) .... 4.00 s.u-Ratio O9W -H92 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.849(10) .... 4.00 s.u-Ratio O10W -H101 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.847(10) .... 4.00 s.u-Ratio O10W -H102 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.846(10) .... 4.00 s.u-Ratio O11W -H112 1.555 1.555 PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.844(10) .... 3.00 s.u-Ratio O12W -H121 1.555 1.555 PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.843(10) .... 3.00 s.u-Ratio O12W -H122 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.848(10) .... 3.00 s.u-Ratio O13W -H131 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.849(10) .... 4.00 s.u-Ratio O13W -H132 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.847(10) .... 3.00 s.u-Ratio O14W -H141 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.849(10) .... 4.00 s.u-Ratio O14W -H142 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.846(10) .... 4.00 s.u-Ratio O15W -H152 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.846(10) .... 4.00 s.u-Ratio O16W -H161 1.555 1.555 PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.845(10) .... 3.00 s.u-Ratio O16W -H162 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.848(10) .... 4.00 s.u-Ratio O17W -H172 1.555 1.555 PLAT_735 Alert C D-H Calc 0.84(3), Rep 0.843(10) .... 3.00 s.u-Ratio O18W -H181 1.555 1.555 PLAT_735 Alert C D-H Calc 0.84(4), Rep 0.848(10) .... 4.00 s.u-Ratio O18W -H182 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.845(10) .... 3.00 s.u-Ratio O19W -H191 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.846(10) .... 3.00 s.u-Ratio O19W -H192 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.843(10) .... 4.00 s.u-Ratio O20W -H201 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.847(10) .... 3.00 s.u-Ratio O20W -H202 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(4), Rep 0.846(10) .... 4.00 s.u-Ratio O21W -H211 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.847(10) .... 3.00 s.u-Ratio O21W -H212 1.555 1.555 PLAT_735 Alert C D-H Calc 0.85(3), Rep 0.845(10) .... 3.00 s.u-Ratio O22W -H221 1.555 1.555 PLAT_736 Alert C H...A Calc 2.11(4), Rep 2.112(19) .... 2.11 s.u-Ratio H21 -O7W 1.555 1.555 PLAT_736 Alert C H...A Calc 1.95(5), Rep 1.953(15) .... 3.33 s.u-Ratio H42 -O16W 1.555 1.555 PLAT_736 Alert C H...A Calc 2.05(4), Rep 2.052(17) .... 2.35 s.u-Ratio H52 -O21W 1.555 1.555 PLAT_736 Alert C H...A Calc 2.20(4), Rep 2.201(15) .... 2.67 s.u-Ratio H61 -O11 1.555 1.445 PLAT_736 Alert C H...A Calc 2.06(4), Rep 2.063(12) .... 3.33 s.u-Ratio H62 -O4 1.555 2.765 PLAT_736 Alert C H...A Calc 1.91(4), Rep 1.910(13) .... 3.08 s.u-Ratio H71 -O3 1.555 2.665 PLAT_736 Alert C H...A Calc 2.09(4), Rep 2.088(18) .... 2.22 s.u-Ratio H72 -O20 1.555 1.455 PLAT_736 Alert C H...A Calc 1.87(4), Rep 1.873(14) .... 2.86 s.u-Ratio H81 -O18 1.555 1.555 PLAT_736 Alert C H...A Calc 2.12(4), Rep 2.119(18) .... 2.22 s.u-Ratio H82 -O2 1.555 2.765 PLAT_736 Alert C H...A Calc 1.96(4), Rep 1.953(14) .... 2.86 s.u-Ratio H91 -O9 1.555 1.445 PLAT_736 Alert C H...A Calc 2.00(4), Rep 1.996(14) .... 2.86 s.u-Ratio H101 -O19 1.555 1.455 PLAT_736 Alert C H...A Calc 2.39(4), Rep 2.397(15) .... 2.67 s.u-Ratio H102 -O17 1.555 1.555 PLAT_736 Alert C H...A Calc 2.32(3), Rep 2.315(12) .... 2.50 s.u-Ratio H121 -O25 1.555 1.445 PLAT_736 Alert C H...A Calc 1.98(4), Rep 1.973(17) .... 2.35 s.u-Ratio H122 -O5 1.555 1.445 PLAT_736 Alert C H...A Calc 2.05(3), Rep 2.047(13) .... 2.31 s.u-Ratio H142 -O8W 1.555 1.555 PLAT_736 Alert C H...A Calc 1.86(4), Rep 1.862(14) .... 2.86 s.u-Ratio H152 -O21W 1.555 1.555 PLAT_736 Alert C H...A Calc 1.88(4), Rep 1.876(12) .... 3.33 s.u-Ratio H172 -O22W 1.555 1.555 PLAT_736 Alert C H...A Calc 1.95(4), Rep 1.946(15) .... 2.67 s.u-Ratio H182 -O12W 1.555 1.565 PLAT_736 Alert C H...A Calc 1.97(3), Rep 1.974(11) .... 2.73 s.u-Ratio H191 -O26 1.555 1.555 PLAT_736 Alert C H...A Calc 1.81(3), Rep 1.814(12) .... 2.50 s.u-Ratio H192 -O24 1.555 1.455 PLAT_736 Alert C H...A Calc 1.92(3), Rep 1.923(12) .... 2.50 s.u-Ratio H201 -O12 1.555 1.455 PLAT_736 Alert C H...A Calc 1.85(3), Rep 1.849(11) .... 2.73 s.u-Ratio H202 -O7 1.555 1.555 PLAT_743 Alert C Torsion Calc 0.03(13), Rep 0.00 .... Missing s.u. O1 -V5 -O1 -V5 2.775 1.555 1.555 2.775 General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 2.586 Tmax scaled 0.750 Tmin scaled 0.634
0 Alert Level A = Potentially serious problem
3 Alert Level B = Potential problem
63 Alert Level C = Please check
The title compound was the unexpected product of the reaction of equimolar amounts of ammonium metavanadate (0.12 g, 1 mmol), nickel nitrate hexahydrate (0.29 g, 1 mmol) and 1,2,4-benzenetricarboxylic acid anhydride (0.19 g, 1 mmol) in several ml of 50% aqueous ethanol. The pH of the solution was adjusted to approximately 8 by the addition of sodium hydroxide solution. Pink polyhedral crystals separated from the solution after one week.
The H atoms of the coordinated water molecules were located and refined subject to the following restraints: O—H = 0.85±0.01 and H···H = 1.39±0.01 Å; Uiso(H) = 1.2Ueq(O). Of the three lattice water molecules, one is disordered over two sites with equal occupancies. One of the H atoms, corresponding to one of the disordered sites, occupies a center of inversion.
Data collection: CAD-4 Software (Enraf-Nonius, 1988); cell refinement: CAD-4 Software; 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.
Na4Ni(V10O28)·23H2O | Z = 2 |
Mr = 1522.44 | F(000) = 1512 |
Triclinic, P1 | Dx = 2.303 Mg m−3 |
a = 8.925 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.862 (3) Å | Cell parameters from 25 reflections |
c = 18.341 (4) Å | θ = 12.8–13.9° |
α = 91.81 (3)° | µ = 2.62 mm−1 |
β = 91.85 (3)° | T = 298 K |
γ = 104.32 (3)° | Block, pink |
V = 2195.5 (8) Å3 | 0.50 × 0.25 × 0.11 mm |
Enraf-Nonius CAD-4 diffractometer | 6270 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.027 |
Graphite monochromator | θmax = 26.0°, θmin = 1.1° |
ω scans | h = 0→11 |
Absorption correction: ψ scan (North et al., 1968) | k = −17→16 |
Tmin = 0.245, Tmax = 0.290 | l = −22→22 |
9182 measured reflections | 3 standard reflections every 60 min |
8594 independent reflections | intensity decay: none |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.100 | Only H-atom coordinates refined |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0427P)2 + 1.0711P] where P = (Fo2 + 2Fc2)/3 |
8594 reflections | (Δ/σ)max < 0.001 |
748 parameters | Δρmax = 0.53 e Å−3 |
71 restraints | Δρmin = −0.56 e Å−3 |
Na4Ni(V10O28)·23H2O | γ = 104.32 (3)° |
Mr = 1522.44 | V = 2195.5 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 8.925 (2) Å | Mo Kα radiation |
b = 13.862 (3) Å | µ = 2.62 mm−1 |
c = 18.341 (4) Å | T = 298 K |
α = 91.81 (3)° | 0.50 × 0.25 × 0.11 mm |
β = 91.85 (3)° |
Enraf-Nonius CAD-4 diffractometer | 6270 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North et al., 1968) | Rint = 0.027 |
Tmin = 0.245, Tmax = 0.290 | 3 standard reflections every 60 min |
9182 measured reflections | intensity decay: none |
8594 independent reflections |
R[F2 > 2σ(F2)] = 0.040 | 71 restraints |
wR(F2) = 0.100 | Only H-atom coordinates refined |
S = 1.02 | Δρmax = 0.53 e Å−3 |
8594 reflections | Δρmin = −0.56 e Å−3 |
748 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.51980 (6) | 0.75713 (4) | 0.24874 (3) | 0.02339 (14) | |
V1 | 1.04483 (8) | 0.88632 (5) | −0.11579 (4) | 0.01989 (17) | |
V2 | 0.98071 (8) | 0.89853 (5) | 0.12389 (4) | 0.01966 (16) | |
V3 | 1.19773 (9) | 0.82060 (6) | 0.02127 (4) | 0.02303 (18) | |
V4 | 0.84823 (9) | 0.74714 (5) | −0.00557 (4) | 0.02337 (18) | |
V5 | 1.18889 (8) | 1.04061 (5) | 0.01413 (4) | 0.01687 (16) | |
V6 | 0.79087 (8) | 0.25867 (5) | 0.49586 (4) | 0.02219 (17) | |
V7 | 1.02179 (8) | 0.37485 (5) | 0.38700 (4) | 0.01882 (16) | |
V8 | 0.81267 (8) | 0.48000 (5) | 0.48244 (4) | 0.01634 (16) | |
V9 | 0.86214 (9) | 0.70758 (6) | 0.47248 (4) | 0.02267 (17) | |
V10 | 1.05245 (8) | 0.59845 (5) | 0.37444 (4) | 0.01836 (16) | |
Na1 | 0.5000 | 0.5000 | 0.0000 | 0.0481 (8) | |
Na2 | 0.7076 (2) | 0.44162 (16) | 0.15135 (11) | 0.0418 (5) | |
Na3 | 0.4850 (2) | 0.24783 (15) | 0.25365 (11) | 0.0342 (4) | |
Na4 | 0.2635 (2) | 0.04865 (16) | 0.35560 (12) | 0.0411 (5) | |
Na5 | 0.5000 | 0.0000 | 0.5000 | 0.0363 (7) | |
O1 | 1.0104 (3) | 0.9053 (2) | 0.00392 (15) | 0.0163 (6) | |
O2 | 1.0745 (4) | 0.8835 (2) | −0.20194 (16) | 0.0285 (7) | |
O3 | 0.8974 (3) | 0.7729 (2) | −0.10323 (16) | 0.0232 (7) | |
O4 | 1.2035 (3) | 0.8379 (2) | −0.07840 (16) | 0.0241 (7) | |
O5 | 0.9530 (4) | 0.9039 (2) | 0.21043 (16) | 0.0273 (7) | |
O6 | 1.1456 (3) | 0.8473 (2) | 0.11791 (16) | 0.0234 (7) | |
O7 | 0.8395 (3) | 0.7826 (2) | 0.09280 (16) | 0.0238 (7) | |
O8 | 0.8303 (3) | 0.9750 (2) | 0.08851 (15) | 0.0185 (6) | |
O9 | 1.1116 (3) | 1.0350 (2) | 0.11259 (15) | 0.0170 (6) | |
O10 | 1.3121 (3) | 0.9681 (2) | 0.02871 (16) | 0.0226 (7) | |
O11 | 1.2938 (3) | 1.1598 (2) | 0.02227 (16) | 0.0224 (7) | |
O12 | 1.3420 (4) | 0.7730 (2) | 0.03757 (18) | 0.0329 (8) | |
O13 | 1.0314 (4) | 0.7133 (2) | 0.01179 (17) | 0.0261 (7) | |
O14 | 0.7209 (4) | 0.6436 (2) | −0.01234 (19) | 0.0373 (8) | |
O15 | 0.9834 (3) | 0.4014 (2) | 0.50532 (15) | 0.0173 (6) | |
O16 | 0.6402 (4) | 0.1671 (2) | 0.48808 (19) | 0.0325 (8) | |
O17 | 0.6819 (3) | 0.3695 (2) | 0.47561 (16) | 0.0203 (6) | |
O18 | 0.8495 (3) | 0.2756 (2) | 0.39899 (16) | 0.0219 (6) | |
O19 | 1.1530 (3) | 0.3067 (2) | 0.42804 (16) | 0.0226 (7) | |
O20 | 1.0511 (4) | 0.3652 (2) | 0.30110 (17) | 0.0286 (7) | |
O21 | 0.8930 (3) | 0.4734 (2) | 0.38613 (15) | 0.0171 (6) | |
O22 | 0.9109 (3) | 0.6713 (2) | 0.37750 (16) | 0.0220 (6) | |
O23 | 1.0810 (3) | 0.5882 (2) | 0.28846 (16) | 0.0261 (7) | |
O24 | 1.2155 (3) | 0.7013 (2) | 0.40643 (16) | 0.0223 (7) | |
O25 | 1.0497 (3) | 0.7990 (2) | 0.48396 (16) | 0.0242 (7) | |
O26 | 0.7419 (4) | 0.7732 (2) | 0.45361 (18) | 0.0323 (8) | |
O27 | 0.7163 (3) | 0.5680 (2) | 0.46581 (16) | 0.0213 (6) | |
O28 | 0.8270 (3) | 0.4966 (2) | 0.58633 (15) | 0.0174 (6) | |
O1w | 0.7000 (6) | 0.4267 (3) | 0.0219 (2) | 0.0608 (12) | |
H11 | 0.783 (5) | 0.459 (3) | 0.004 (4) | 0.073* | |
H12 | 0.682 (6) | 0.3656 (13) | 0.009 (3) | 0.073* | |
O2w | 0.4840 (5) | 0.5001 (3) | 0.1301 (2) | 0.0467 (10) | |
H21 | 0.422 (6) | 0.449 (2) | 0.147 (3) | 0.056* | |
H22 | 0.481 (6) | 0.551 (2) | 0.156 (3) | 0.056* | |
O3w | 0.9320 (6) | 0.3839 (3) | 0.1567 (2) | 0.0566 (12) | |
H31 | 0.945 (7) | 0.333 (3) | 0.133 (2) | 0.068* | |
H32 | 0.979 (7) | 0.388 (4) | 0.1981 (16) | 0.068* | |
O4w | 0.8688 (5) | 0.6117 (3) | 0.1725 (2) | 0.0432 (9) | |
H41 | 0.900 (6) | 0.654 (3) | 0.140 (2) | 0.052* | |
H42 | 0.826 (6) | 0.637 (3) | 0.206 (2) | 0.052* | |
O5w | 0.6518 (4) | 0.4140 (3) | 0.27762 (19) | 0.0358 (8) | |
H51 | 0.724 (4) | 0.415 (4) | 0.3090 (19) | 0.043* | |
H52 | 0.586 (4) | 0.441 (4) | 0.296 (2) | 0.043* | |
O6w | 0.5611 (4) | 0.2584 (3) | 0.1279 (2) | 0.0374 (8) | |
H61 | 0.479 (3) | 0.234 (4) | 0.102 (2) | 0.045* | |
H62 | 0.633 (3) | 0.232 (3) | 0.115 (3) | 0.045* | |
O7w | 0.2999 (4) | 0.3351 (3) | 0.2117 (2) | 0.0414 (9) | |
H71 | 0.245 (4) | 0.303 (4) | 0.1761 (18) | 0.050* | |
H72 | 0.243 (4) | 0.352 (4) | 0.243 (2) | 0.050* | |
O8w | 0.6774 (4) | 0.1614 (3) | 0.2886 (2) | 0.0367 (8) | |
H81 | 0.734 (4) | 0.191 (4) | 0.3246 (17) | 0.044* | |
H82 | 0.734 (4) | 0.145 (4) | 0.2561 (18) | 0.044* | |
O9w | 0.3255 (4) | 0.0814 (3) | 0.23084 (19) | 0.0366 (8) | |
H91 | 0.254 (4) | 0.071 (4) | 0.1980 (19) | 0.044* | |
H92 | 0.400 (4) | 0.059 (4) | 0.216 (2) | 0.044* | |
O10w | 0.3988 (4) | 0.2292 (3) | 0.3776 (2) | 0.0397 (9) | |
H101 | 0.321 (3) | 0.251 (4) | 0.388 (3) | 0.048* | |
H102 | 0.476 (3) | 0.259 (3) | 0.405 (2) | 0.048* | |
O11w | 0.0305 (6) | 0.0964 (4) | 0.3530 (3) | 0.0678 (14) | |
H111 | −0.019 (6) | 0.117 (5) | 0.386 (2) | 0.081* | |
H112 | −0.019 (6) | 0.092 (5) | 0.3124 (15) | 0.081* | |
O12w | 0.1409 (4) | −0.1247 (3) | 0.3277 (2) | 0.0366 (8) | |
H121 | 0.104 (5) | −0.149 (4) | 0.3668 (14) | 0.044* | |
H122 | 0.070 (4) | −0.129 (4) | 0.2954 (17) | 0.044* | |
O13w | 0.2364 (5) | 0.0206 (3) | 0.4854 (2) | 0.0487 (10) | |
H131 | 0.172 (5) | −0.0341 (18) | 0.493 (3) | 0.058* | |
H132 | 0.214 (6) | 0.068 (2) | 0.510 (3) | 0.058* | |
O14w | 0.5033 (4) | 0.0001 (3) | 0.3708 (2) | 0.0395 (9) | |
H141 | 0.497 (6) | −0.0583 (13) | 0.354 (3) | 0.047* | |
H142 | 0.562 (5) | 0.042 (2) | 0.345 (2) | 0.047* | |
O15w | 0.3900 (4) | 0.6133 (3) | 0.25155 (18) | 0.0298 (7) | |
H151 | 0.2921 (13) | 0.602 (4) | 0.252 (2) | 0.036* | |
H152 | 0.423 (4) | 0.586 (3) | 0.2873 (18) | 0.036* | |
O16w | 0.7136 (4) | 0.7075 (3) | 0.2697 (2) | 0.0372 (9) | |
H161 | 0.763 (6) | 0.704 (3) | 0.3094 (15) | 0.045* | |
H162 | 0.700 (6) | 0.654 (2) | 0.245 (2) | 0.045* | |
O17w | 0.6469 (4) | 0.9018 (3) | 0.24623 (19) | 0.0325 (8) | |
H171 | 0.7435 (16) | 0.910 (4) | 0.242 (3) | 0.039* | |
H172 | 0.611 (4) | 0.935 (3) | 0.215 (2) | 0.039* | |
O18w | 0.3229 (4) | 0.8034 (3) | 0.22962 (19) | 0.0372 (9) | |
H181 | 0.275 (5) | 0.801 (4) | 0.1890 (12) | 0.045* | |
H182 | 0.279 (5) | 0.829 (4) | 0.2625 (16) | 0.045* | |
O19w | 0.4932 (4) | 0.7834 (3) | 0.35793 (16) | 0.0265 (7) | |
H191 | 0.568 (3) | 0.782 (3) | 0.3872 (19) | 0.032* | |
H192 | 0.408 (2) | 0.752 (3) | 0.375 (2) | 0.032* | |
O20w | 0.5485 (4) | 0.7312 (3) | 0.13999 (17) | 0.0295 (8) | |
H201 | 0.486 (3) | 0.748 (4) | 0.110 (2) | 0.035* | |
H202 | 0.6403 (19) | 0.749 (4) | 0.126 (2) | 0.035* | |
O21w | 0.4617 (4) | 0.5095 (3) | 0.36387 (19) | 0.0371 (9) | |
H211 | 0.532 (3) | 0.535 (4) | 0.3960 (19) | 0.044* | |
H212 | 0.373 (2) | 0.506 (4) | 0.381 (2) | 0.044* | |
O22w | 0.5382 (4) | 1.0058 (3) | 0.14203 (19) | 0.0378 (9) | |
H221 | 0.482 (4) | 0.984 (4) | 0.1041 (16) | 0.045* | |
H222 | 0.6317 (18) | 1.008 (4) | 0.134 (2) | 0.045* | |
O23w | 0.868 (2) | 0.4466 (15) | −0.0974 (11) | 0.141 (7) | 0.50 |
H231 | 0.90 (3) | 0.499 (9) | −0.122 (10) | 0.169* | 0.50 |
H232 | 0.90 (3) | 0.400 (10) | −0.115 (11) | 0.169* | 0.50 |
O23' | 0.968 (3) | 0.480 (2) | −0.0420 (12) | 0.225 (12) | 0.50 |
H233 | 1.0000 | 0.5000 | 0.0000 | 0.271* | |
H234 | 0.873 (15) | 0.45 (3) | −0.043 (5) | 0.271* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0214 (3) | 0.0301 (3) | 0.0203 (3) | 0.0092 (2) | 0.0011 (2) | 0.0027 (2) |
V1 | 0.0215 (4) | 0.0228 (4) | 0.0162 (4) | 0.0075 (3) | −0.0002 (3) | −0.0019 (3) |
V2 | 0.0216 (4) | 0.0215 (4) | 0.0154 (4) | 0.0045 (3) | −0.0005 (3) | 0.0026 (3) |
V3 | 0.0233 (4) | 0.0243 (4) | 0.0242 (4) | 0.0120 (3) | −0.0041 (3) | −0.0005 (3) |
V4 | 0.0251 (4) | 0.0183 (4) | 0.0243 (4) | 0.0010 (3) | −0.0020 (3) | 0.0008 (3) |
V5 | 0.0127 (3) | 0.0215 (4) | 0.0160 (4) | 0.0037 (3) | −0.0008 (3) | −0.0008 (3) |
V6 | 0.0228 (4) | 0.0181 (4) | 0.0225 (4) | −0.0005 (3) | −0.0021 (3) | 0.0013 (3) |
V7 | 0.0217 (4) | 0.0203 (4) | 0.0149 (4) | 0.0065 (3) | 0.0000 (3) | −0.0017 (3) |
V8 | 0.0129 (3) | 0.0204 (4) | 0.0155 (4) | 0.0040 (3) | −0.0012 (3) | 0.0000 (3) |
V9 | 0.0242 (4) | 0.0227 (4) | 0.0233 (4) | 0.0108 (3) | −0.0033 (3) | −0.0002 (3) |
V10 | 0.0195 (4) | 0.0199 (4) | 0.0151 (4) | 0.0036 (3) | 0.0005 (3) | 0.0022 (3) |
Na1 | 0.0464 (18) | 0.0416 (18) | 0.047 (2) | −0.0059 (14) | −0.0150 (15) | 0.0167 (15) |
Na2 | 0.0487 (13) | 0.0462 (13) | 0.0348 (12) | 0.0204 (10) | −0.0023 (10) | 0.0026 (10) |
Na3 | 0.0314 (10) | 0.0393 (11) | 0.0311 (11) | 0.0074 (9) | 0.0012 (8) | 0.0030 (9) |
Na4 | 0.0481 (13) | 0.0412 (12) | 0.0375 (12) | 0.0176 (10) | −0.0003 (10) | 0.0048 (10) |
Na5 | 0.0368 (15) | 0.0285 (14) | 0.0376 (17) | −0.0031 (12) | −0.0055 (13) | 0.0086 (12) |
O1 | 0.0155 (14) | 0.0172 (14) | 0.0163 (15) | 0.0048 (11) | −0.0004 (11) | −0.0010 (12) |
O2 | 0.0349 (18) | 0.0330 (18) | 0.0186 (17) | 0.0112 (15) | 0.0003 (14) | −0.0053 (14) |
O3 | 0.0272 (16) | 0.0213 (16) | 0.0198 (17) | 0.0049 (13) | −0.0052 (13) | −0.0047 (13) |
O4 | 0.0246 (16) | 0.0294 (17) | 0.0215 (17) | 0.0142 (13) | −0.0028 (13) | −0.0049 (13) |
O5 | 0.0301 (17) | 0.0347 (18) | 0.0168 (17) | 0.0073 (14) | −0.0008 (13) | 0.0028 (14) |
O6 | 0.0264 (16) | 0.0290 (17) | 0.0170 (16) | 0.0113 (14) | −0.0045 (13) | 0.0026 (13) |
O7 | 0.0259 (16) | 0.0211 (16) | 0.0222 (17) | 0.0009 (13) | 0.0016 (13) | 0.0056 (13) |
O8 | 0.0158 (14) | 0.0232 (15) | 0.0166 (15) | 0.0048 (12) | 0.0024 (11) | 0.0006 (12) |
O9 | 0.0162 (14) | 0.0213 (15) | 0.0137 (15) | 0.0055 (12) | −0.0011 (11) | −0.0002 (12) |
O10 | 0.0168 (15) | 0.0298 (17) | 0.0215 (17) | 0.0069 (13) | −0.0016 (12) | −0.0013 (13) |
O11 | 0.0170 (14) | 0.0271 (16) | 0.0209 (16) | 0.0013 (12) | 0.0009 (12) | 0.0010 (13) |
O12 | 0.0334 (18) | 0.0361 (19) | 0.034 (2) | 0.0194 (15) | −0.0098 (15) | −0.0031 (15) |
O13 | 0.0333 (18) | 0.0178 (15) | 0.0284 (18) | 0.0091 (13) | −0.0052 (14) | 0.0022 (13) |
O14 | 0.042 (2) | 0.0238 (18) | 0.039 (2) | −0.0051 (15) | −0.0050 (16) | 0.0005 (15) |
O15 | 0.0168 (14) | 0.0190 (15) | 0.0163 (15) | 0.0054 (12) | −0.0020 (11) | −0.0003 (12) |
O16 | 0.0297 (18) | 0.0250 (17) | 0.036 (2) | −0.0059 (14) | −0.0031 (15) | 0.0010 (15) |
O17 | 0.0144 (14) | 0.0259 (16) | 0.0185 (16) | 0.0014 (12) | −0.0026 (12) | 0.0002 (12) |
O18 | 0.0239 (16) | 0.0191 (15) | 0.0211 (17) | 0.0037 (12) | −0.0035 (12) | −0.0036 (12) |
O19 | 0.0256 (16) | 0.0264 (16) | 0.0182 (16) | 0.0116 (13) | −0.0004 (13) | −0.0034 (13) |
O20 | 0.0354 (18) | 0.0334 (18) | 0.0183 (17) | 0.0115 (15) | 0.0016 (14) | −0.0042 (14) |
O21 | 0.0165 (14) | 0.0207 (15) | 0.0149 (15) | 0.0064 (12) | −0.0004 (11) | −0.0011 (12) |
O22 | 0.0244 (16) | 0.0238 (16) | 0.0182 (16) | 0.0071 (13) | −0.0040 (12) | 0.0025 (12) |
O23 | 0.0282 (17) | 0.0303 (18) | 0.0183 (17) | 0.0041 (14) | 0.0010 (13) | 0.0028 (13) |
O24 | 0.0209 (15) | 0.0228 (16) | 0.0209 (16) | 0.0007 (12) | 0.0007 (12) | 0.0032 (13) |
O25 | 0.0293 (17) | 0.0208 (16) | 0.0213 (17) | 0.0043 (13) | −0.0021 (13) | 0.0022 (13) |
O26 | 0.0358 (19) | 0.0306 (18) | 0.036 (2) | 0.0186 (15) | −0.0057 (15) | 0.0022 (15) |
O27 | 0.0165 (14) | 0.0271 (16) | 0.0219 (16) | 0.0087 (12) | −0.0022 (12) | 0.0017 (13) |
O28 | 0.0142 (14) | 0.0241 (15) | 0.0148 (15) | 0.0066 (12) | 0.0019 (11) | 0.0010 (12) |
O1w | 0.099 (4) | 0.042 (2) | 0.048 (3) | 0.030 (2) | 0.001 (3) | 0.003 (2) |
O2w | 0.052 (3) | 0.041 (2) | 0.046 (3) | 0.014 (2) | −0.0086 (19) | −0.0107 (19) |
O3w | 0.076 (3) | 0.069 (3) | 0.038 (3) | 0.048 (3) | −0.017 (2) | −0.014 (2) |
O4w | 0.059 (3) | 0.039 (2) | 0.035 (2) | 0.0166 (19) | 0.0054 (19) | 0.0076 (17) |
O5w | 0.0301 (19) | 0.052 (2) | 0.028 (2) | 0.0161 (17) | −0.0096 (15) | −0.0072 (17) |
O6w | 0.034 (2) | 0.043 (2) | 0.037 (2) | 0.0143 (17) | 0.0023 (17) | −0.0035 (17) |
O7w | 0.0315 (19) | 0.060 (3) | 0.034 (2) | 0.0161 (18) | −0.0037 (16) | −0.0163 (19) |
O8w | 0.0284 (18) | 0.047 (2) | 0.032 (2) | 0.0079 (16) | −0.0047 (15) | −0.0134 (17) |
O9w | 0.0319 (19) | 0.050 (2) | 0.026 (2) | 0.0086 (17) | −0.0082 (15) | −0.0051 (16) |
O10w | 0.0295 (19) | 0.060 (3) | 0.032 (2) | 0.0158 (18) | 0.0004 (16) | −0.0091 (18) |
O11w | 0.079 (3) | 0.087 (3) | 0.053 (3) | 0.055 (3) | −0.026 (3) | −0.023 (3) |
O12w | 0.042 (2) | 0.041 (2) | 0.028 (2) | 0.0135 (17) | −0.0045 (16) | 0.0096 (17) |
O13w | 0.057 (3) | 0.048 (2) | 0.046 (3) | 0.024 (2) | 0.003 (2) | 0.001 (2) |
O14w | 0.047 (2) | 0.035 (2) | 0.036 (2) | 0.0111 (18) | −0.0021 (17) | −0.0037 (17) |
O15w | 0.0243 (17) | 0.0333 (19) | 0.032 (2) | 0.0069 (15) | 0.0037 (14) | 0.0061 (15) |
O16w | 0.034 (2) | 0.055 (2) | 0.029 (2) | 0.0240 (18) | −0.0063 (16) | 0.0008 (17) |
O17w | 0.0268 (17) | 0.0334 (19) | 0.038 (2) | 0.0080 (15) | 0.0021 (15) | 0.0063 (16) |
O18w | 0.035 (2) | 0.059 (2) | 0.0251 (19) | 0.0276 (18) | −0.0003 (16) | 0.0046 (18) |
O19w | 0.0223 (16) | 0.041 (2) | 0.0164 (17) | 0.0075 (15) | 0.0042 (13) | 0.0037 (14) |
O20w | 0.0196 (16) | 0.049 (2) | 0.0219 (18) | 0.0123 (16) | 0.0010 (13) | 0.0062 (15) |
O21w | 0.0228 (17) | 0.058 (2) | 0.031 (2) | 0.0108 (17) | 0.0019 (15) | 0.0021 (18) |
O22w | 0.0264 (18) | 0.055 (2) | 0.031 (2) | 0.0086 (18) | −0.0022 (15) | 0.0054 (18) |
O23w | 0.175 (17) | 0.142 (15) | 0.147 (16) | 0.101 (14) | 0.089 (13) | 0.072 (13) |
O23' | 0.24 (3) | 0.26 (3) | 0.15 (2) | 0.00 (2) | −0.03 (2) | 0.05 (2) |
Ni1—O18w | 2.038 (3) | V9—O25 | 1.834 (3) |
Ni1—O16w | 2.043 (3) | V9—O19ii | 1.847 (3) |
Ni1—O15w | 2.046 (3) | V9—O22 | 1.892 (3) |
Ni1—O17w | 2.048 (3) | V9—O27 | 2.045 (3) |
Ni1—O20w | 2.051 (3) | V9—O15ii | 2.320 (3) |
Ni1—O19w | 2.056 (3) | V10—O23 | 1.613 (3) |
V1—O2 | 1.612 (3) | V10—O22 | 1.803 (3) |
V1—O3 | 1.810 (3) | V10—O24 | 1.833 (3) |
V1—O4 | 1.834 (3) | V10—O21 | 1.975 (3) |
V1—O9i | 1.974 (3) | V10—O28ii | 2.030 (3) |
V1—O8i | 2.007 (3) | V10—O15ii | 2.238 (3) |
V1—O1 | 2.243 (3) | Na1—O1w | 2.292 (5) |
V2—O5 | 1.616 (3) | Na1—O1wiii | 2.292 (5) |
V2—O6 | 1.791 (3) | Na1—O2wiii | 2.396 (4) |
V2—O7 | 1.841 (3) | Na1—O2w | 2.396 (4) |
V2—O9 | 1.983 (3) | Na1—O14 | 2.453 (3) |
V2—O8 | 2.009 (3) | Na1—O14iii | 2.453 (3) |
V2—O1 | 2.227 (3) | Na2—O3w | 2.334 (4) |
V3—O12 | 1.609 (3) | Na2—O2w | 2.358 (5) |
V3—O13 | 1.822 (3) | Na2—O1w | 2.373 (5) |
V3—O4 | 1.852 (3) | Na2—O5w | 2.407 (4) |
V3—O6 | 1.895 (3) | Na2—O4w | 2.451 (5) |
V3—O10 | 2.045 (3) | Na2—O6w | 2.569 (4) |
V3—O1 | 2.288 (3) | Na3—O7w | 2.398 (4) |
V4—O14 | 1.594 (3) | Na3—O8w | 2.406 (4) |
V4—O13 | 1.830 (3) | Na3—O9w | 2.408 (4) |
V4—O7 | 1.864 (3) | Na3—O6w | 2.424 (4) |
V4—O3 | 1.882 (3) | Na3—O10w | 2.424 (4) |
V4—O11i | 2.043 (3) | Na3—O5w | 2.432 (4) |
V4—O1 | 2.307 (3) | Na4—O11w | 2.333 (5) |
V5—O10 | 1.684 (3) | Na4—O9w | 2.402 (4) |
V5—O11 | 1.685 (3) | Na4—O14w | 2.407 (4) |
V5—O8i | 1.886 (3) | Na4—O12w | 2.412 (4) |
V5—O9 | 1.951 (3) | Na4—O13w | 2.434 (5) |
V5—O1i | 2.115 (3) | Na4—O10w | 2.509 (5) |
V5—O1 | 2.138 (3) | Na5—O16iv | 2.365 (3) |
V6—O16 | 1.604 (3) | Na5—O16 | 2.365 (3) |
V6—O25ii | 1.830 (3) | Na5—O14w | 2.370 (4) |
V6—O24ii | 1.866 (3) | Na5—O14wiv | 2.370 (4) |
V6—O18 | 1.874 (3) | Na5—O13wiv | 2.447 (4) |
V6—O17 | 2.049 (3) | Na5—O13w | 2.447 (4) |
V6—O15 | 2.274 (3) | O1—V5i | 2.115 (3) |
V7—O20 | 1.612 (3) | O8—V5i | 1.886 (3) |
V7—O18 | 1.817 (3) | O8—V1i | 2.007 (3) |
V7—O19 | 1.834 (3) | O9—V1i | 1.974 (3) |
V7—O28ii | 1.987 (3) | O11—V4i | 2.043 (3) |
V7—O21 | 1.991 (3) | O15—V8ii | 2.130 (3) |
V7—O15 | 2.241 (3) | O15—V10ii | 2.238 (3) |
V8—O17 | 1.679 (3) | O15—V9ii | 2.320 (3) |
V8—O27 | 1.688 (3) | O19—V9ii | 1.847 (3) |
V8—O28 | 1.908 (3) | O24—V6ii | 1.866 (3) |
V8—O21 | 1.936 (3) | O25—V6ii | 1.830 (3) |
V8—O15 | 2.120 (3) | O28—V7ii | 1.987 (3) |
V8—O15ii | 2.130 (3) | O28—V10ii | 2.030 (3) |
V9—O26 | 1.606 (3) | O23'—O23'v | 1.66 (4) |
O18w—Ni1—O16w | 178.33 (16) | O23—V10—O21 | 100.04 (14) |
O18w—Ni1—O15w | 89.71 (15) | O22—V10—O21 | 91.94 (13) |
O16w—Ni1—O15w | 88.89 (15) | O24—V10—O21 | 153.93 (13) |
O18w—Ni1—O17w | 89.52 (15) | O23—V10—O28ii | 99.97 (14) |
O16w—Ni1—O17w | 91.88 (15) | O22—V10—O28ii | 155.19 (13) |
O15w—Ni1—O17w | 179.18 (14) | O24—V10—O28ii | 87.82 (13) |
O18w—Ni1—O20w | 93.46 (14) | O21—V10—O28ii | 75.86 (11) |
O16w—Ni1—O20w | 87.38 (14) | O23—V10—O15ii | 174.72 (14) |
O15w—Ni1—O20w | 88.08 (14) | O22—V10—O15ii | 81.01 (12) |
O17w—Ni1—O20w | 92.25 (14) | O24—V10—O15ii | 79.50 (12) |
O18w—Ni1—O19w | 87.02 (14) | O21—V10—O15ii | 76.78 (11) |
O16w—Ni1—O19w | 92.14 (14) | O28ii—V10—O15ii | 75.24 (11) |
O15w—Ni1—O19w | 92.18 (14) | O1w—Na1—O1wiii | 180.0 |
O17w—Ni1—O19w | 87.50 (14) | O1w—Na1—O2wiii | 96.36 (15) |
O20w—Ni1—O19w | 179.45 (12) | O1wiii—Na1—O2wiii | 83.64 (15) |
O2—V1—O3 | 104.04 (16) | O1w—Na1—O2w | 83.64 (15) |
O2—V1—O4 | 101.52 (15) | O1wiii—Na1—O2w | 96.36 (15) |
O3—V1—O4 | 94.47 (14) | O2wiii—Na1—O2w | 180.0 (2) |
O2—V1—O9i | 101.02 (14) | O1w—Na1—O14 | 79.99 (15) |
O3—V1—O9i | 90.72 (13) | O1wiii—Na1—O14 | 100.01 (15) |
O4—V1—O9i | 154.87 (13) | O2wiii—Na1—O14 | 79.68 (13) |
O2—V1—O8i | 99.55 (15) | O2w—Na1—O14 | 100.32 (13) |
O3—V1—O8i | 154.91 (13) | O1w—Na1—O14iii | 100.01 (15) |
O4—V1—O8i | 89.02 (13) | O1wiii—Na1—O14iii | 79.99 (15) |
O9i—V1—O8i | 76.39 (11) | O2wiii—Na1—O14iii | 100.32 (13) |
O2—V1—O1 | 174.82 (14) | O2w—Na1—O14iii | 79.68 (13) |
O3—V1—O1 | 80.58 (12) | O14—Na1—O14iii | 180.0 |
O4—V1—O1 | 80.24 (12) | O3w—Na2—O2w | 172.91 (18) |
O9i—V1—O1 | 76.39 (11) | O3w—Na2—O1w | 90.23 (17) |
O8i—V1—O1 | 75.54 (11) | O2w—Na2—O1w | 82.73 (16) |
O5—V2—O6 | 104.03 (15) | O3w—Na2—O5w | 94.70 (16) |
O5—V2—O7 | 102.53 (15) | O2w—Na2—O5w | 92.29 (15) |
O6—V2—O7 | 94.91 (14) | O1w—Na2—O5w | 162.99 (18) |
O5—V2—O9 | 99.68 (14) | O3w—Na2—O4w | 88.77 (17) |
O6—V2—O9 | 91.11 (13) | O2w—Na2—O4w | 91.74 (15) |
O7—V2—O9 | 154.79 (13) | O1w—Na2—O4w | 100.92 (17) |
O5—V2—O8 | 99.17 (14) | O5w—Na2—O4w | 95.47 (15) |
O6—V2—O8 | 155.13 (13) | O3w—Na2—O6w | 86.18 (16) |
O7—V2—O8 | 88.63 (13) | O2w—Na2—O6w | 93.18 (15) |
O9—V2—O8 | 76.14 (11) | O1w—Na2—O6w | 78.36 (16) |
O5—V2—O1 | 174.14 (14) | O5w—Na2—O6w | 85.72 (14) |
O6—V2—O1 | 80.86 (12) | O4w—Na2—O6w | 174.89 (15) |
O7—V2—O1 | 80.03 (12) | O7w—Na3—O8w | 176.54 (16) |
O9—V2—O1 | 76.80 (11) | O7w—Na3—O9w | 97.29 (14) |
O8—V2—O1 | 75.51 (11) | O8w—Na3—O9w | 83.12 (14) |
O12—V3—O13 | 104.21 (16) | O7w—Na3—O6w | 83.35 (14) |
O12—V3—O4 | 103.02 (16) | O8w—Na3—O6w | 93.20 (14) |
O13—V3—O4 | 93.04 (15) | O9w—Na3—O6w | 91.60 (14) |
O12—V3—O6 | 100.23 (15) | O7w—Na3—O10w | 96.49 (14) |
O13—V3—O6 | 90.59 (14) | O8w—Na3—O10w | 86.97 (14) |
O4—V3—O6 | 154.79 (13) | O9w—Na3—O10w | 85.42 (14) |
O12—V3—O10 | 98.91 (15) | O6w—Na3—O10w | 176.98 (16) |
O13—V3—O10 | 156.73 (13) | O7w—Na3—O5w | 84.25 (14) |
O4—V3—O10 | 84.21 (13) | O8w—Na3—O5w | 95.34 (13) |
O6—V3—O10 | 82.69 (13) | O9w—Na3—O5w | 178.46 (15) |
O12—V3—O1 | 173.30 (14) | O6w—Na3—O5w | 88.44 (14) |
O13—V3—O1 | 82.08 (12) | O10w—Na3—O5w | 94.54 (15) |
O4—V3—O1 | 78.66 (12) | O11w—Na4—O9w | 97.22 (17) |
O6—V3—O1 | 77.15 (11) | O11w—Na4—O14w | 174.50 (18) |
O10—V3—O1 | 74.72 (11) | O9w—Na4—O14w | 88.09 (14) |
O14—V4—O13 | 104.81 (17) | O11w—Na4—O12w | 93.86 (18) |
O14—V4—O7 | 101.27 (16) | O9w—Na4—O12w | 93.09 (15) |
O13—V4—O7 | 91.06 (14) | O14w—Na4—O12w | 87.26 (14) |
O14—V4—O3 | 103.02 (16) | O11w—Na4—O13w | 89.17 (17) |
O13—V4—O3 | 90.90 (14) | O9w—Na4—O13w | 172.63 (16) |
O7—V4—O3 | 154.25 (13) | O14w—Na4—O13w | 85.45 (15) |
O14—V4—O11i | 98.58 (16) | O12w—Na4—O13w | 90.15 (15) |
O13—V4—O11i | 156.61 (13) | O11w—Na4—O10w | 87.62 (17) |
O7—V4—O11i | 84.53 (13) | O9w—Na4—O10w | 83.70 (14) |
O3—V4—O11i | 83.55 (13) | O14w—Na4—O10w | 91.55 (14) |
O14—V4—O1 | 173.73 (15) | O12w—Na4—O10w | 176.62 (16) |
O13—V4—O1 | 81.40 (12) | O13w—Na4—O10w | 92.92 (15) |
O7—V4—O1 | 77.46 (12) | O16iv—Na5—O16 | 180.00 (8) |
O3—V4—O1 | 77.46 (12) | O16iv—Na5—O14w | 98.31 (13) |
O11i—V4—O1 | 75.21 (11) | O16—Na5—O14w | 81.69 (13) |
O10—V5—O11 | 107.03 (15) | O16iv—Na5—O14wiv | 81.69 (13) |
O10—V5—O8i | 98.10 (14) | O16—Na5—O14wiv | 98.31 (13) |
O11—V5—O8i | 99.47 (14) | O14w—Na5—O14wiv | 180.000 (1) |
O10—V5—O9 | 96.07 (13) | O16iv—Na5—O13wiv | 99.42 (13) |
O11—V5—O9 | 96.11 (14) | O16—Na5—O13wiv | 80.58 (13) |
O8i—V5—O9 | 154.82 (12) | O14w—Na5—O13wiv | 94.04 (14) |
O10—V5—O1i | 164.61 (13) | O14wiv—Na5—O13wiv | 85.96 (14) |
O11—V5—O1i | 88.24 (13) | O16iv—Na5—O13w | 80.58 (13) |
O8i—V5—O1i | 80.84 (12) | O16—Na5—O13w | 99.42 (13) |
O9—V5—O1i | 80.00 (11) | O14w—Na5—O13w | 85.96 (14) |
O10—V5—O1 | 86.37 (13) | O14wiv—Na5—O13w | 94.04 (14) |
O11—V5—O1 | 166.37 (13) | O13wiv—Na5—O13w | 180.000 (1) |
O8i—V5—O1 | 80.61 (12) | V5i—O1—V5 | 101.71 (11) |
O9—V5—O1 | 79.63 (11) | V5i—O1—V2 | 93.04 (11) |
O1i—V5—O1 | 78.29 (11) | V5—O1—V2 | 93.22 (11) |
O16—V6—O25ii | 104.52 (16) | V5i—O1—V1 | 93.19 (11) |
O16—V6—O24ii | 100.89 (16) | V5—O1—V1 | 92.53 (11) |
O25ii—V6—O24ii | 91.85 (14) | V2—O1—V1 | 170.51 (14) |
O16—V6—O18 | 102.49 (16) | V5i—O1—V3 | 170.28 (14) |
O25ii—V6—O18 | 90.87 (13) | V5—O1—V3 | 88.01 (10) |
O24ii—V6—O18 | 154.96 (13) | V2—O1—V3 | 86.67 (10) |
O16—V6—O17 | 97.21 (15) | V1—O1—V3 | 85.99 (10) |
O25ii—V6—O17 | 158.26 (13) | V5i—O1—V4 | 87.09 (10) |
O24ii—V6—O17 | 84.41 (13) | V5—O1—V4 | 171.18 (14) |
O18—V6—O17 | 83.90 (13) | V2—O1—V4 | 86.85 (10) |
O16—V6—O15 | 172.66 (14) | V1—O1—V4 | 86.31 (10) |
O25ii—V6—O15 | 82.78 (12) | V3—O1—V4 | 83.19 (9) |
O24ii—V6—O15 | 77.90 (12) | V1—O3—V4 | 114.91 (16) |
O18—V6—O15 | 77.76 (12) | V1—O4—V3 | 113.95 (15) |
O17—V6—O15 | 75.49 (11) | V2—O6—V3 | 114.41 (15) |
O20—V7—O18 | 103.30 (16) | V2—O7—V4 | 114.54 (15) |
O20—V7—O19 | 102.61 (15) | V5i—O8—V1i | 108.81 (14) |
O18—V7—O19 | 93.92 (14) | V5i—O8—V2 | 107.96 (14) |
O20—V7—O28ii | 100.28 (15) | V1i—O8—V2 | 99.01 (12) |
O18—V7—O28ii | 154.52 (13) | V5—O9—V1i | 107.58 (13) |
O19—V7—O28ii | 90.23 (13) | V5—O9—V2 | 107.49 (13) |
O20—V7—O21 | 100.30 (14) | V1i—O9—V2 | 101.04 (12) |
O18—V7—O21 | 89.84 (12) | V5—O10—V3 | 110.85 (15) |
O19—V7—O21 | 155.25 (13) | V5—O11—V4i | 109.42 (15) |
O28ii—V7—O21 | 76.49 (11) | V3—O13—V4 | 113.31 (15) |
O20—V7—O15 | 175.39 (14) | V4—O14—Na1 | 167.3 (2) |
O18—V7—O15 | 79.77 (12) | V8—O15—V8ii | 101.45 (12) |
O19—V7—O15 | 80.47 (12) | V8—O15—V10ii | 93.87 (11) |
O28ii—V7—O15 | 76.15 (11) | V8ii—O15—V10ii | 92.35 (11) |
O21—V7—O15 | 76.14 (11) | V8—O15—V7 | 93.33 (11) |
O17—V8—O27 | 106.93 (14) | V8ii—O15—V7 | 92.41 (11) |
O17—V8—O28 | 98.27 (14) | V10ii—O15—V7 | 170.41 (14) |
O27—V8—O28 | 97.45 (13) | V8—O15—V6 | 87.63 (10) |
O17—V8—O21 | 96.70 (14) | V8ii—O15—V6 | 170.92 (14) |
O27—V8—O21 | 97.05 (13) | V10ii—O15—V6 | 87.03 (10) |
O28—V8—O21 | 155.13 (12) | V7—O15—V6 | 86.96 (10) |
O17—V8—O15 | 87.77 (12) | V8—O15—V9ii | 170.77 (14) |
O27—V8—O15 | 165.29 (13) | V8ii—O15—V9ii | 87.76 (10) |
O28—V8—O15 | 80.63 (11) | V10ii—O15—V9ii | 86.20 (10) |
O21—V8—O15 | 80.23 (11) | V7—O15—V9ii | 85.68 (10) |
O17—V8—O15ii | 166.29 (12) | V6—O15—V9ii | 83.16 (9) |
O27—V8—O15ii | 86.74 (13) | V6—O16—Na5 | 154.7 (2) |
O28—V8—O15ii | 80.51 (12) | V8—O17—V6 | 109.10 (14) |
O21—V8—O15ii | 80.25 (12) | V7—O18—V6 | 114.68 (16) |
O15—V8—O15ii | 78.55 (12) | V7—O19—V9ii | 114.82 (15) |
O26—V9—O25 | 104.20 (16) | V8—O21—V10 | 107.45 (14) |
O26—V9—O19ii | 103.30 (16) | V8—O21—V7 | 107.81 (13) |
O25—V9—O19ii | 92.33 (14) | V10—O21—V7 | 101.01 (12) |
O26—V9—O22 | 100.72 (15) | V10—O22—V9 | 114.92 (15) |
O25—V9—O22 | 90.65 (14) | V10—O24—V6ii | 114.28 (15) |
O19ii—V9—O22 | 154.26 (13) | V6ii—O25—V9 | 112.63 (15) |
O26—V9—O27 | 100.13 (15) | V8—O27—V9 | 111.28 (14) |
O25—V9—O27 | 155.59 (13) | V8—O28—V7ii | 108.24 (14) |
O19ii—V9—O27 | 84.01 (13) | V8—O28—V10ii | 107.90 (13) |
O22—V9—O27 | 82.79 (13) | V7ii—O28—V10ii | 99.24 (12) |
O26—V9—O15ii | 174.07 (15) | Na1—O1w—Na2 | 97.70 (17) |
O25—V9—O15ii | 81.42 (12) | Na2—O2w—Na1 | 95.30 (15) |
O19ii—V9—O15ii | 78.09 (12) | Na2—O5w—Na3 | 94.37 (14) |
O22—V9—O15ii | 77.09 (11) | Na3—O6w—Na2 | 90.60 (14) |
O27—V9—O15ii | 74.20 (10) | Na4—O9w—Na3 | 96.56 (14) |
O23—V10—O22 | 103.43 (15) | Na3—O10w—Na4 | 93.39 (14) |
O23—V10—O24 | 102.75 (15) | Na4—O13w—Na5 | 92.28 (14) |
O22—V10—O24 | 94.91 (14) | Na5—O14w—Na4 | 94.86 (14) |
O10—V5—O1—V5i | 178.67 (14) | O28—V8—O15—V6 | 97.93 (12) |
O11—V5—O1—V5i | 9.0 (6) | O21—V8—O15—V6 | −98.02 (12) |
O8i—V5—O1—V5i | −82.50 (13) | O15ii—V8—O15—V6 | −179.95 (16) |
O9—V5—O1—V5i | 81.81 (12) | O18—V7—O15—V8 | −81.32 (12) |
O1i—V5—O1—V5i | 0.0 | O19—V7—O15—V8 | −177.10 (13) |
O10—V5—O1—V2 | 84.89 (13) | O28ii—V7—O15—V8 | 90.29 (12) |
O11—V5—O1—V2 | −84.8 (6) | O21—V7—O15—V8 | 11.06 (10) |
O8i—V5—O1—V2 | −176.28 (12) | O18—V7—O15—V8ii | 177.06 (13) |
O9—V5—O1—V2 | −11.96 (10) | O19—V7—O15—V8ii | 81.27 (12) |
O1i—V5—O1—V2 | −93.78 (12) | O28ii—V7—O15—V8ii | −11.34 (10) |
O10—V5—O1—V1 | −87.55 (13) | O21—V7—O15—V8ii | −90.56 (11) |
O11—V5—O1—V1 | 102.8 (5) | O18—V7—O15—V6 | 6.12 (11) |
O8i—V5—O1—V1 | 11.28 (10) | O19—V7—O15—V6 | −89.66 (12) |
O9—V5—O1—V1 | 175.60 (12) | O28ii—V7—O15—V6 | 177.73 (11) |
O1i—V5—O1—V1 | 93.78 (12) | O21—V7—O15—V6 | 98.51 (11) |
O10—V5—O1—V3 | −1.66 (12) | O18—V7—O15—V9ii | 89.48 (12) |
O11—V5—O1—V3 | −171.3 (5) | O19—V7—O15—V9ii | −6.30 (11) |
O8i—V5—O1—V3 | 97.17 (11) | O28ii—V7—O15—V9ii | −98.91 (11) |
O9—V5—O1—V3 | −98.51 (11) | O21—V7—O15—V9ii | −178.13 (11) |
O1i—V5—O1—V3 | 179.68 (16) | O25ii—V6—O15—V8 | 179.96 (13) |
O6—V2—O1—V5i | 176.65 (13) | O24ii—V6—O15—V8 | −86.57 (12) |
O7—V2—O1—V5i | 79.97 (12) | O18—V6—O15—V8 | 87.48 (12) |
O9—V2—O1—V5i | −90.03 (11) | O17—V6—O15—V8 | 0.70 (10) |
O8—V2—O1—V5i | −11.19 (10) | O25ii—V6—O15—V10ii | −86.04 (12) |
O6—V2—O1—V5 | −81.43 (13) | O24ii—V6—O15—V10ii | 7.43 (11) |
O7—V2—O1—V5 | −178.11 (13) | O18—V6—O15—V10ii | −178.51 (12) |
O9—V2—O1—V5 | 11.89 (10) | O17—V6—O15—V10ii | 94.71 (11) |
O8—V2—O1—V5 | 90.73 (12) | O25ii—V6—O15—V7 | 86.50 (12) |
O6—V2—O1—V3 | 6.39 (11) | O24ii—V6—O15—V7 | 179.96 (12) |
O7—V2—O1—V3 | −90.29 (12) | O18—V6—O15—V7 | −5.98 (11) |
O9—V2—O1—V3 | 99.71 (11) | O17—V6—O15—V7 | −92.76 (11) |
O8—V2—O1—V3 | 178.55 (12) | O25ii—V6—O15—V9ii | 0.49 (11) |
O6—V2—O1—V4 | 89.74 (12) | O24ii—V6—O15—V9ii | 93.95 (12) |
O7—V2—O1—V4 | −6.94 (11) | O18—V6—O15—V9ii | −91.99 (12) |
O9—V2—O1—V4 | −176.94 (11) | O17—V6—O15—V9ii | −178.77 (12) |
O8—V2—O1—V4 | −98.10 (11) | O25ii—V6—O16—Na5 | 13.2 (5) |
O3—V1—O1—V5i | −81.15 (12) | O24ii—V6—O16—Na5 | −81.6 (5) |
O4—V1—O1—V5i | −177.40 (13) | O18—V6—O16—Na5 | 107.4 (5) |
O9i—V1—O1—V5i | 11.90 (10) | O17—V6—O16—Na5 | −167.2 (4) |
O8i—V1—O1—V5i | 91.09 (12) | O14w—Na5—O16—V6 | −112.2 (5) |
O3—V1—O1—V5 | 176.97 (13) | O14wiv—Na5—O16—V6 | 67.8 (5) |
O4—V1—O1—V5 | 80.72 (12) | O13wiv—Na5—O16—V6 | −16.6 (5) |
O9i—V1—O1—V5 | −89.98 (11) | O13w—Na5—O16—V6 | 163.4 (5) |
O8i—V1—O1—V5 | −10.79 (10) | O27—V8—O17—V6 | −179.65 (14) |
O3—V1—O1—V3 | 89.14 (12) | O28—V8—O17—V6 | −79.21 (15) |
O4—V1—O1—V3 | −7.10 (11) | O21—V8—O17—V6 | 80.86 (15) |
O9i—V1—O1—V3 | −177.81 (12) | O15—V8—O17—V6 | 0.98 (14) |
O8i—V1—O1—V3 | −98.62 (11) | O15ii—V8—O17—V6 | 4.6 (6) |
O3—V1—O1—V4 | 5.72 (11) | O16—V6—O17—V8 | 178.29 (18) |
O4—V1—O1—V4 | −90.52 (12) | O25ii—V6—O17—V8 | −2.9 (4) |
O9i—V1—O1—V4 | 98.77 (11) | O24ii—V6—O17—V8 | 77.98 (16) |
O8i—V1—O1—V4 | 177.96 (11) | O18—V6—O17—V8 | −79.83 (16) |
O13—V3—O1—V5 | 179.66 (13) | O15—V6—O17—V8 | −0.94 (14) |
O4—V3—O1—V5 | −85.61 (13) | O20—V7—O18—V6 | 175.34 (17) |
O6—V3—O1—V5 | 87.23 (13) | O19—V7—O18—V6 | 71.39 (17) |
O10—V3—O1—V5 | 1.41 (10) | O28ii—V7—O18—V6 | −27.4 (4) |
O13—V3—O1—V2 | 86.32 (13) | O21—V7—O18—V6 | −84.12 (16) |
O4—V3—O1—V2 | −178.95 (13) | O15—V7—O18—V6 | −8.18 (14) |
O6—V3—O1—V2 | −6.11 (11) | O16—V6—O18—V7 | −179.39 (18) |
O10—V3—O1—V2 | −91.93 (12) | O25ii—V6—O18—V7 | −74.31 (17) |
O13—V3—O1—V1 | −87.66 (13) | O24ii—V6—O18—V7 | 22.0 (4) |
O4—V3—O1—V1 | 7.07 (11) | O17—V6—O18—V7 | 84.54 (16) |
O6—V3—O1—V1 | 179.91 (12) | O15—V6—O18—V7 | 8.12 (14) |
O10—V3—O1—V1 | 94.09 (12) | O20—V7—O19—V9ii | −174.79 (17) |
O13—V3—O1—V4 | −0.91 (12) | O18—V7—O19—V9ii | −70.22 (18) |
O4—V3—O1—V4 | 93.83 (12) | O28ii—V7—O19—V9ii | 84.62 (17) |
O6—V3—O1—V4 | −93.33 (12) | O21—V7—O19—V9ii | 27.9 (4) |
O10—V3—O1—V4 | −179.15 (12) | O15—V7—O19—V9ii | 8.71 (15) |
O13—V4—O1—V5i | −179.32 (13) | O17—V8—O21—V10 | 178.58 (14) |
O7—V4—O1—V5i | −86.29 (12) | O27—V8—O21—V10 | 70.52 (15) |
O3—V4—O1—V5i | 87.82 (12) | O28—V8—O21—V10 | −54.7 (3) |
O11i—V4—O1—V5i | 1.28 (10) | O15—V8—O21—V10 | −94.86 (13) |
O13—V4—O1—V2 | −86.11 (12) | O15ii—V8—O21—V10 | −14.93 (12) |
O7—V4—O1—V2 | 6.92 (11) | O17—V8—O21—V7 | −73.29 (15) |
O3—V4—O1—V2 | −178.97 (12) | O27—V8—O21—V7 | 178.65 (14) |
O11i—V4—O1—V2 | 94.49 (11) | O28—V8—O21—V7 | 53.4 (3) |
O13—V4—O1—V1 | 87.30 (12) | O15—V8—O21—V7 | 13.27 (12) |
O7—V4—O1—V1 | −179.68 (12) | O15ii—V8—O21—V7 | 93.20 (13) |
O3—V4—O1—V1 | −5.56 (11) | O23—V10—O21—V8 | −169.93 (15) |
O11i—V4—O1—V1 | −92.10 (11) | O22—V10—O21—V8 | −65.92 (15) |
O13—V4—O1—V3 | 0.91 (12) | O24—V10—O21—V8 | 39.4 (3) |
O7—V4—O1—V3 | 93.93 (12) | O28ii—V10—O21—V8 | 92.22 (14) |
O3—V4—O1—V3 | −91.95 (12) | O15ii—V10—O21—V8 | 14.38 (11) |
O11i—V4—O1—V3 | −178.50 (12) | O23—V10—O21—V7 | 77.26 (15) |
O2—V1—O3—V4 | 174.65 (17) | O22—V10—O21—V7 | −178.74 (13) |
O4—V1—O3—V4 | 71.59 (18) | O24—V10—O21—V7 | −73.4 (3) |
O9i—V1—O3—V4 | −83.80 (17) | O28ii—V10—O21—V7 | −20.60 (12) |
O8i—V1—O3—V4 | −25.7 (4) | O15ii—V10—O21—V7 | −98.44 (13) |
O1—V1—O3—V4 | −7.73 (15) | O20—V7—O21—V8 | 170.26 (15) |
O14—V4—O3—V1 | −178.82 (18) | O18—V7—O21—V8 | 66.76 (15) |
O13—V4—O3—V1 | −73.40 (18) | O19—V7—O21—V8 | −32.3 (4) |
O7—V4—O3—V1 | 20.9 (4) | O28ii—V7—O21—V8 | −91.53 (14) |
O11i—V4—O3—V1 | 83.82 (17) | O15—V7—O21—V8 | −12.73 (12) |
O1—V4—O3—V1 | 7.59 (14) | O20—V7—O21—V10 | −77.20 (16) |
O2—V1—O4—V3 | −175.35 (17) | O18—V7—O21—V10 | 179.31 (14) |
O3—V1—O4—V3 | −70.03 (18) | O19—V7—O21—V10 | 80.3 (3) |
O9i—V1—O4—V3 | 31.3 (4) | O28ii—V7—O21—V10 | 21.01 (12) |
O8i—V1—O4—V3 | 85.10 (17) | O15—V7—O21—V10 | 99.81 (13) |
O1—V1—O4—V3 | 9.60 (15) | O23—V10—O22—V9 | −174.95 (16) |
O12—V3—O4—V1 | 177.18 (18) | O24—V10—O22—V9 | −70.58 (18) |
O13—V3—O4—V1 | 71.83 (18) | O21—V10—O22—V9 | 84.25 (17) |
O6—V3—O4—V1 | −26.0 (4) | O28ii—V10—O22—V9 | 24.9 (4) |
O10—V3—O4—V1 | −84.99 (17) | O15ii—V10—O22—V9 | 7.96 (15) |
O1—V3—O4—V1 | −9.46 (15) | O26—V9—O22—V10 | 177.85 (18) |
O5—V2—O6—V3 | 174.82 (17) | O25—V9—O22—V10 | 73.27 (17) |
O7—V2—O6—V3 | 70.59 (18) | O19ii—V9—O22—V10 | −23.5 (4) |
O9—V2—O6—V3 | −84.91 (17) | O27—V9—O22—V10 | −83.15 (17) |
O8—V2—O6—V3 | −26.8 (4) | O15ii—V9—O22—V10 | −7.78 (14) |
O1—V2—O6—V3 | −8.47 (15) | O23—V10—O24—V6ii | 174.81 (17) |
O12—V3—O6—V2 | −177.95 (18) | O22—V10—O24—V6ii | 69.83 (17) |
O13—V3—O6—V2 | −73.39 (18) | O21—V10—O24—V6ii | −34.8 (4) |
O4—V3—O6—V2 | 25.0 (4) | O28ii—V10—O24—V6ii | −85.46 (16) |
O10—V3—O6—V2 | 84.26 (17) | O15ii—V10—O24—V6ii | −10.07 (15) |
O1—V3—O6—V2 | 8.34 (15) | O26—V9—O25—V6ii | −178.72 (17) |
O5—V2—O7—V4 | −175.93 (17) | O19ii—V9—O25—V6ii | 76.94 (17) |
O6—V2—O7—V4 | −70.36 (18) | O22—V9—O25—V6ii | −77.49 (17) |
O9—V2—O7—V4 | 32.8 (4) | O27—V9—O25—V6ii | −3.7 (4) |
O8—V2—O7—V4 | 84.98 (17) | O15ii—V9—O25—V6ii | −0.65 (15) |
O1—V2—O7—V4 | 9.45 (15) | O17—V8—O27—V9 | 179.91 (14) |
O14—V4—O7—V2 | 177.08 (18) | O28—V8—O27—V9 | 78.87 (16) |
O13—V4—O7—V2 | 71.75 (17) | O21—V8—O27—V9 | −80.86 (16) |
O3—V4—O7—V2 | −22.5 (4) | O15—V8—O27—V9 | −2.5 (6) |
O11i—V4—O7—V2 | −85.23 (17) | O15ii—V8—O27—V9 | −1.10 (15) |
O1—V4—O7—V2 | −9.20 (14) | O26—V9—O27—V8 | 179.28 (18) |
O5—V2—O8—V5i | −169.32 (15) | O25—V9—O27—V8 | 4.2 (4) |
O6—V2—O8—V5i | 31.9 (4) | O19ii—V9—O27—V8 | −78.24 (17) |
O7—V2—O8—V5i | −66.85 (15) | O22—V9—O27—V8 | 79.62 (17) |
O9—V2—O8—V5i | 92.88 (15) | O15ii—V9—O27—V8 | 1.05 (14) |
O1—V2—O8—V5i | 13.20 (12) | O17—V8—O28—V7ii | −179.99 (14) |
O5—V2—O8—V1i | 77.44 (15) | O27—V8—O28—V7ii | −71.58 (15) |
O6—V2—O8—V1i | −81.4 (3) | O21—V8—O28—V7ii | 53.6 (3) |
O7—V2—O8—V1i | 179.90 (13) | O15—V8—O28—V7ii | 93.67 (13) |
O9—V2—O8—V1i | −20.36 (11) | O15ii—V8—O28—V7ii | 13.83 (12) |
O1—V2—O8—V1i | −100.04 (12) | O17—V8—O28—V10ii | 73.51 (15) |
O10—V5—O9—V1i | −179.15 (14) | O27—V8—O28—V10ii | −178.08 (14) |
O11—V5—O9—V1i | 72.93 (15) | O21—V8—O28—V10ii | −52.9 (3) |
O8i—V5—O9—V1i | −55.2 (3) | O15—V8—O28—V10ii | −12.83 (12) |
O1i—V5—O9—V1i | −14.19 (12) | O15ii—V8—O28—V10ii | −92.67 (13) |
O1—V5—O9—V1i | −93.98 (13) | O2wiii—Na1—O1w—Na2 | 173.96 (16) |
O10—V5—O9—V2 | −71.07 (15) | O2w—Na1—O1w—Na2 | −6.04 (16) |
O11—V5—O9—V2 | −178.98 (14) | O14—Na1—O1w—Na2 | 95.65 (17) |
O8i—V5—O9—V2 | 52.9 (3) | O14iii—Na1—O1w—Na2 | −84.35 (17) |
O1i—V5—O9—V2 | 93.90 (13) | O3w—Na2—O1w—Na1 | −173.01 (19) |
O1—V5—O9—V2 | 14.10 (12) | O2w—Na2—O1w—Na1 | 6.15 (17) |
O5—V2—O9—V5 | 171.11 (15) | O5w—Na2—O1w—Na1 | 79.9 (6) |
O6—V2—O9—V5 | 66.67 (15) | O4w—Na2—O1w—Na1 | −84.22 (19) |
O7—V2—O9—V5 | −37.3 (4) | O6w—Na2—O1w—Na1 | 100.93 (18) |
O8—V2—O9—V5 | −91.74 (14) | O1w—Na2—O2w—Na1 | −5.86 (15) |
O1—V2—O9—V5 | −13.67 (11) | O5w—Na2—O2w—Na1 | −169.52 (14) |
O5—V2—O9—V1i | −76.29 (15) | O4w—Na2—O2w—Na1 | 94.93 (15) |
O6—V2—O9—V1i | 179.27 (13) | O6w—Na2—O2w—Na1 | −83.69 (15) |
O7—V2—O9—V1i | 75.2 (3) | O1w—Na1—O2w—Na2 | 6.05 (16) |
O8—V2—O9—V1i | 20.85 (12) | O1wiii—Na1—O2w—Na2 | −173.95 (16) |
O1—V2—O9—V1i | 98.92 (13) | O14—Na1—O2w—Na2 | −72.52 (15) |
O11—V5—O10—V3 | 179.45 (14) | O14iii—Na1—O2w—Na2 | 107.48 (15) |
O8i—V5—O10—V3 | −77.99 (16) | O3w—Na2—O5w—Na3 | −92.75 (17) |
O9—V5—O10—V3 | 81.14 (16) | O2w—Na2—O5w—Na3 | 86.07 (15) |
O1i—V5—O10—V3 | 6.9 (6) | O1w—Na2—O5w—Na3 | 13.6 (6) |
O1—V5—O10—V3 | 1.98 (15) | O4w—Na2—O5w—Na3 | 178.04 (14) |
O12—V3—O10—V5 | −179.81 (18) | O6w—Na2—O5w—Na3 | −6.95 (13) |
O13—V3—O10—V5 | −6.3 (4) | O7w—Na3—O5w—Na2 | −76.13 (14) |
O4—V3—O10—V5 | 77.88 (17) | O8w—Na3—O5w—Na2 | 100.42 (14) |
O6—V3—O10—V5 | −80.54 (17) | O6w—Na3—O5w—Na2 | 7.35 (14) |
O1—V3—O10—V5 | −1.92 (14) | O10w—Na3—O5w—Na2 | −172.21 (13) |
O10—V5—O11—V4i | −179.82 (14) | O7w—Na3—O6w—Na2 | 77.53 (14) |
O8i—V5—O11—V4i | 78.61 (16) | O8w—Na3—O6w—Na2 | −102.12 (13) |
O9—V5—O11—V4i | −81.54 (15) | O9w—Na3—O6w—Na2 | 174.68 (13) |
O1i—V5—O11—V4i | −1.80 (15) | O5w—Na3—O6w—Na2 | −6.86 (13) |
O1—V5—O11—V4i | −10.6 (6) | O3w—Na2—O6w—Na3 | 101.96 (16) |
O12—V3—O13—V4 | 178.89 (18) | O2w—Na2—O6w—Na3 | −85.11 (15) |
O4—V3—O13—V4 | −76.86 (18) | O1w—Na2—O6w—Na3 | −167.02 (17) |
O6—V3—O13—V4 | 78.18 (18) | O5w—Na2—O6w—Na3 | 6.95 (13) |
O10—V3—O13—V4 | 5.5 (5) | O11w—Na4—O9w—Na3 | 94.06 (18) |
O1—V3—O13—V4 | 1.24 (16) | O14w—Na4—O9w—Na3 | −84.50 (15) |
O14—V4—O13—V3 | 179.67 (19) | O12w—Na4—O9w—Na3 | −171.66 (14) |
O7—V4—O13—V3 | −78.38 (18) | O10w—Na4—O9w—Na3 | 7.27 (13) |
O3—V4—O13—V3 | 75.94 (18) | O7w—Na3—O9w—Na4 | −103.47 (15) |
O11i—V4—O13—V3 | 0.2 (5) | O8w—Na3—O9w—Na4 | 79.99 (15) |
O1—V4—O13—V3 | −1.23 (16) | O6w—Na3—O9w—Na4 | 173.02 (14) |
O13—V4—O14—Na1 | 120.9 (9) | O10w—Na3—O9w—Na4 | −7.50 (14) |
O7—V4—O14—Na1 | 26.8 (10) | O7w—Na3—O10w—Na4 | 103.98 (14) |
O3—V4—O14—Na1 | −144.6 (9) | O8w—Na3—O10w—Na4 | −76.18 (14) |
O11i—V4—O14—Na1 | −59.3 (10) | O9w—Na3—O10w—Na4 | 7.15 (13) |
O1w—Na1—O14—V4 | −118.9 (10) | O5w—Na3—O10w—Na4 | −171.30 (13) |
O1wiii—Na1—O14—V4 | 61.1 (10) | O11w—Na4—O10w—Na3 | −104.72 (17) |
O2wiii—Na1—O14—V4 | 142.7 (10) | O9w—Na4—O10w—Na3 | −7.19 (13) |
O2w—Na1—O14—V4 | −37.3 (10) | O14w—Na4—O10w—Na3 | 80.72 (14) |
O17—V8—O15—V8ii | 179.12 (14) | O13w—Na4—O10w—Na3 | 166.24 (14) |
O27—V8—O15—V8ii | 1.5 (6) | O11w—Na4—O13w—Na5 | −169.93 (18) |
O28—V8—O15—V8ii | −82.12 (13) | O14w—Na4—O13w—Na5 | 8.97 (14) |
O21—V8—O15—V8ii | 81.93 (13) | O12w—Na4—O13w—Na5 | 96.22 (14) |
O15ii—V8—O15—V8ii | 0.0 | O10w—Na4—O13w—Na5 | −82.35 (14) |
O17—V8—O15—V10ii | −87.69 (13) | O16iv—Na5—O13w—Na4 | −108.23 (15) |
O27—V8—O15—V10ii | 94.7 (5) | O16—Na5—O13w—Na4 | 71.77 (15) |
O28—V8—O15—V10ii | 11.07 (11) | O14w—Na5—O13w—Na4 | −9.11 (14) |
O21—V8—O15—V10ii | 175.12 (12) | O14wiv—Na5—O13w—Na4 | 170.89 (14) |
O15ii—V8—O15—V10ii | 93.19 (13) | O16iv—Na5—O14w—Na4 | 89.09 (14) |
O17—V8—O15—V7 | 85.98 (13) | O16—Na5—O14w—Na4 | −90.91 (14) |
O27—V8—O15—V7 | −91.7 (5) | O13wiv—Na5—O14w—Na4 | −170.77 (14) |
O28—V8—O15—V7 | −175.26 (12) | O13w—Na5—O14w—Na4 | 9.23 (14) |
O21—V8—O15—V7 | −11.21 (10) | O9w—Na4—O14w—Na5 | 167.16 (14) |
O15ii—V8—O15—V7 | −93.14 (13) | O12w—Na4—O14w—Na5 | −99.66 (14) |
O17—V8—O15—V6 | −0.83 (12) | O13w—Na4—O14w—Na5 | −9.29 (14) |
O27—V8—O15—V6 | −178.5 (5) | O10w—Na4—O14w—Na5 | 83.52 (14) |
Symmetry codes: (i) −x+2, −y+2, −z; (ii) −x+2, −y+1, −z+1; (iii) −x+1, −y+1, −z; (iv) −x+1, −y, −z+1; (v) −x+2, −y+1, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H11···O23w | 0.85 (1) | 2.05 (5) | 2.675 (15) | 131 (6) |
O1w—H12···O12v | 0.85 (1) | 2.04 (2) | 2.876 (5) | 170 (5) |
O2w—H21···O7w | 0.85 (1) | 2.11 (2) | 2.946 (6) | 166 (5) |
O2w—H22···O15w | 0.85 (1) | 2.19 (3) | 2.945 (5) | 148 (4) |
O3w—H31···O3v | 0.85 (1) | 2.34 (3) | 3.098 (5) | 149 (5) |
O3w—H32···O20 | 0.85 (1) | 2.04 (2) | 2.864 (5) | 165 (6) |
O4w—H41···O7 | 0.85 (1) | 2.19 (3) | 2.884 (5) | 140 (4) |
O4w—H42···O16w | 0.85 (1) | 1.95 (2) | 2.789 (5) | 170 (5) |
O5w—H51···O21 | 0.85 (1) | 2.03 (2) | 2.831 (4) | 158 (5) |
O5w—H52···O21w | 0.85 (1) | 2.05 (2) | 2.878 (5) | 165 (4) |
O6w—H61···O11vi | 0.85 (1) | 2.20 (2) | 3.039 (5) | 170 (4) |
O6w—H62···O4v | 0.85 (1) | 2.06 (1) | 2.908 (4) | 175 (4) |
O7w—H71···O3iii | 0.85 (1) | 1.91 (1) | 2.753 (5) | 174 (5) |
O7w—H72···O20vii | 0.85 (1) | 2.09 (2) | 2.906 (5) | 163 (4) |
O8w—H81···O18 | 0.85 (1) | 1.87 (1) | 2.713 (4) | 170 (5) |
O8w—H82···O2v | 0.85 (1) | 2.12 (2) | 2.943 (5) | 163 (4) |
O9w—H91···O9vi | 0.85 (1) | 1.95 (1) | 2.793 (4) | 170 (4) |
O9w—H92···O22wviii | 0.85 (1) | 2.09 (2) | 2.904 (5) | 159 (4) |
O10w—H101···O19vii | 0.85 (1) | 2.00 (1) | 2.838 (4) | 171 (5) |
O10w—H102···O17 | 0.85 (1) | 2.40 (2) | 3.233 (5) | 169 (5) |
O11w—H111···O19vii | 0.85 (1) | 2.76 (7) | 3.108 (6) | 106 (5) |
O11w—H112···O2iii | 0.85 (1) | 2.13 (2) | 2.940 (6) | 160 (7) |
O12w—H121···O25vi | 0.84 (1) | 2.32 (1) | 3.148 (5) | 169 (4) |
O12w—H122···O5vi | 0.84 (1) | 1.97 (2) | 2.783 (5) | 161 (4) |
O13w—H131···O25vi | 0.85 (1) | 2.30 (2) | 3.110 (5) | 160 (4) |
O13w—H132···O26ix | 0.85 (1) | 2.22 (2) | 2.994 (5) | 151 (4) |
O14w—H141···O19wviii | 0.85 (1) | 2.19 (2) | 2.985 (5) | 156 (5) |
O14w—H142···O8w | 0.85 (1) | 2.05 (1) | 2.886 (6) | 169 (5) |
O15w—H151···O23vii | 0.85 (1) | 1.99 (2) | 2.801 (4) | 160 (4) |
O15w—H152···O21w | 0.85 (1) | 1.86 (1) | 2.699 (5) | 170 (4) |
O16w—H161···O22 | 0.85 (1) | 1.94 (2) | 2.746 (4) | 160 (5) |
O16w—H162···O4w | 0.85 (1) | 2.21 (5) | 2.789 (5) | 126 (5) |
O17w—H171···O5 | 0.85 (1) | 1.99 (2) | 2.823 (5) | 165 (5) |
O17w—H172···O22w | 0.85 (1) | 1.88 (1) | 2.723 (5) | 177 (5) |
O18w—H181···O6vii | 0.84 (1) | 1.94 (2) | 2.723 (4) | 155 (4) |
O18w—H182···O12wx | 0.85 (1) | 1.95 (2) | 2.783 (5) | 169 (5) |
O19w—H191···O26 | 0.85 (1) | 1.97 (1) | 2.818 (4) | 177 (5) |
O19w—H192···O24vii | 0.85 (1) | 1.81 (1) | 2.653 (4) | 171 (4) |
O20w—H201···O12vii | 0.84 (1) | 1.92 (1) | 2.763 (4) | 174 (5) |
O20w—H202···O7 | 0.85 (1) | 1.85 (1) | 2.696 (4) | 178 (5) |
O21w—H211···O27 | 0.85 (1) | 2.00 (2) | 2.835 (5) | 167 (5) |
O21w—H212···O28ix | 0.85 (1) | 1.90 (1) | 2.744 (4) | 176 (5) |
O22w—H221···O10vii | 0.85 (1) | 1.99 (2) | 2.794 (5) | 160 (5) |
O22w—H222···O8 | 0.85 (1) | 2.13 (2) | 2.938 (4) | 161 (4) |
Symmetry codes: (iii) −x+1, −y+1, −z; (v) −x+2, −y+1, −z; (vi) x−1, y−1, z; (vii) x−1, y, z; (viii) x, y−1, z; (ix) −x+1, −y+1, −z+1; (x) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | Na4Ni(V10O28)·23H2O |
Mr | 1522.44 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 8.925 (2), 13.862 (3), 18.341 (4) |
α, β, γ (°) | 91.81 (3), 91.85 (3), 104.32 (3) |
V (Å3) | 2195.5 (8) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.62 |
Crystal size (mm) | 0.50 × 0.25 × 0.11 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | ψ scan (North et al., 1968) |
Tmin, Tmax | 0.245, 0.290 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 9182, 8594, 6270 |
Rint | 0.027 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.100, 1.02 |
No. of reflections | 8594 |
No. of parameters | 748 |
No. of restraints | 71 |
H-atom treatment | Only H-atom coordinates refined |
Δρmax, Δρmin (e Å−3) | 0.53, −0.56 |
Computer programs: CAD-4 Software (Enraf-Nonius, 1988), CAD-4 Software, XCAD4 (Harms, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.
The title compound, which has the empirical formulation of Na4Ni(V10O28).23H2O, is related to the water-soluble mineral huemulite, Na4Mg(V10O28).24H2O (Gordillo et al., 1966). Both compounds feature the polyhedral [V10O28]6- hexaanion, whose structure has been well documented: it contains eight terminal, 14 µ2-bridging, four µ3-bridging and two µ6-bridging O atoms linking ten V atoms into a D2 h point-symmetry hexa-anionic species (Capparelli et al., 1986).
In the title compound, the Ni atom is coordinated by six water molecules in the [Ni(H2O)6]2+ dication (Fig. 1). Three Na atoms (which are in general positions) and four pairs of bridging water molecules comprise a link between the two other independent Na atoms (which are located at the crystallographic inversion centers), and this unit then continues on to form infinite chains in the (011) direction (Fig. 2). Each of the Na atoms in general positions along with the four contacts with bridging water molecules has two terminal water ligands; however, the Na atoms in the inversion centers along with four bridging coordinations are additionally coordinated to the vanadyl atoms (O14 and O16) of each of the two independent [V10O28]6- anions (Figs. 3 and 4), these interaction linking the chains into layers. The numerous hydrogen bonds connect these negatively charged layers, as well as the otherwise isolated [Ni(H2O)6]2+ dications and lattice water molecules, into three-dimensional network.
Decavanadates having an aklylammonium cation as the counter-ion are also known; these are synthesized by the reaction of the amine and vanadium pentoxide (Averbuch-Pouchot, 1995; Averbuch-Pouchot & Durif, 1995).