The title compound, [Na2Ni(SO4)2(H2O)4] or Ni astrakanite, is part of an isostructural family containing the Mg (the original astrakanite mineral), Zn and Co species. The very regular NiO(H2O)4O(SO4)2 octahedra lie at centers of symmetry, while the rather distorted NaO(H2O)2O(SO4)4 octahedra are at general positions, linked into a three-dimensional network by the bridging water molecules and fully coordinated sulfate groups.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (S-O) = 0.002 Å
- R factor = 0.023
- wR factor = 0.067
- Data-to-parameter ratio = 11.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 39.34 Deg.
O2 -S1 -NA1 1.555 1.555 4.565
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2005).
Disodium nickel bis(sulfate) tetrahydrate
top
Crystal data top
[Na2Ni(SO4)2(H2O)4] | F(000) = 372 |
Mr = 368.87 | Dx = 2.494 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3942 reflections |
a = 5.5284 (6) Å | θ = 3.1–27.8° |
b = 8.189 (1) Å | µ = 2.55 mm−1 |
c = 11.0343 (13) Å | T = 294 K |
β = 100.468 (2)° | Plates, light_blue |
V = 491.23 (10) Å3 | 0.22 × 0.16 × 0.08 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD diffractometer | 1094 independent reflections |
Radiation source: fine-focus sealed tube | 1060 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
φ and ω scans | θmax = 27.8°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) | h = −7→7 |
Tmin = 0.604, Tmax = 0.822 | k = −10→10 |
3942 measured reflections | l = −14→14 |
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.067 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0476P)2 + 0.2019P] where P = (Fo2 + 2Fc2)/3 |
1094 reflections | (Δ/σ)max = 0.001 |
95 parameters | Δρmax = 0.39 e Å−3 |
6 restraints | Δρmin = −0.33 e Å−3 |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.0000 | 0.0000 | 0.0000 | 0.01453 (13) | |
Na1 | 0.12865 (15) | 0.06926 (10) | 0.36180 (7) | 0.0239 (2) | |
S1 | 0.37008 (8) | 0.28638 (5) | 0.13650 (4) | 0.01497 (14) | |
O1 | 0.3493 (3) | 0.26831 (18) | 0.26754 (13) | 0.0241 (3) | |
O2 | 0.2051 (3) | 0.41431 (18) | 0.07920 (13) | 0.0248 (3) | |
O3 | 0.3146 (3) | 0.12945 (18) | 0.07142 (14) | 0.0233 (3) | |
O4 | 0.6288 (3) | 0.32744 (18) | 0.13104 (14) | 0.0245 (3) | |
O1W | −0.1253 (3) | 0.03655 (19) | 0.16071 (13) | 0.0195 (3) | |
O2W | 0.1722 (3) | −0.20991 (17) | 0.08071 (13) | 0.0202 (3) | |
H1WA | −0.221 (4) | −0.039 (2) | 0.174 (3) | 0.037 (8)* | |
H1WB | −0.210 (4) | 0.1225 (19) | 0.151 (3) | 0.039 (8)* | |
H2WA | 0.299 (3) | −0.207 (4) | 0.1364 (19) | 0.043 (8)* | |
H2WB | 0.208 (5) | −0.277 (3) | 0.028 (2) | 0.057 (10)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0153 (2) | 0.0141 (2) | 0.01415 (19) | −0.00007 (11) | 0.00272 (13) | −0.00081 (11) |
Na1 | 0.0263 (4) | 0.0237 (4) | 0.0213 (4) | −0.0011 (3) | 0.0032 (3) | 0.0013 (3) |
S1 | 0.0143 (2) | 0.0152 (2) | 0.0152 (2) | 0.00061 (16) | 0.00202 (17) | −0.00081 (15) |
O1 | 0.0302 (8) | 0.0254 (8) | 0.0171 (7) | 0.0019 (6) | 0.0056 (6) | 0.0018 (5) |
O2 | 0.0275 (8) | 0.0253 (8) | 0.0211 (7) | 0.0104 (6) | 0.0025 (6) | 0.0027 (5) |
O3 | 0.0189 (7) | 0.0215 (7) | 0.0291 (8) | −0.0028 (5) | 0.0031 (6) | −0.0095 (6) |
O4 | 0.0178 (7) | 0.0217 (7) | 0.0350 (8) | −0.0035 (6) | 0.0074 (6) | −0.0032 (6) |
O1W | 0.0201 (7) | 0.0198 (7) | 0.0194 (7) | 0.0005 (6) | 0.0059 (5) | 0.0000 (6) |
O2W | 0.0202 (7) | 0.0181 (7) | 0.0201 (7) | 0.0021 (5) | −0.0018 (5) | −0.0011 (5) |
Geometric parameters (Å, º) top
Ni1—O1W | 2.0399 (14) | Na1—O2iv | 2.4237 (16) |
Ni1—O1Wi | 2.0399 (14) | Na1—O2Wv | 2.6120 (17) |
Ni1—O3 | 2.0669 (14) | S1—O2 | 1.4560 (15) |
Ni1—O3i | 2.0669 (14) | S1—O3 | 1.4769 (14) |
Ni1—O2Wi | 2.0848 (14) | S1—O1 | 1.4787 (14) |
Ni1—O2W | 2.0848 (14) | S1—O4 | 1.4812 (15) |
Na1—O2ii | 2.3627 (16) | O1W—H1WA | 0.841 (10) |
Na1—O4iii | 2.3848 (16) | O1W—H1WB | 0.842 (10) |
Na1—O1 | 2.3848 (17) | O2W—H2WA | 0.844 (10) |
Na1—O1W | 2.4155 (16) | O2W—H2WB | 0.846 (10) |
| | | |
O1W—Ni1—O1Wi | 180.00 (8) | O2iv—Na1—O2Wv | 75.39 (5) |
O1W—Ni1—O3 | 89.34 (6) | O2—S1—O3 | 110.89 (9) |
O1Wi—Ni1—O3 | 90.66 (6) | O2—S1—O1 | 110.04 (9) |
O1W—Ni1—O3i | 90.66 (6) | O3—S1—O1 | 110.01 (9) |
O1Wi—Ni1—O3i | 89.34 (6) | O2—S1—O4 | 110.64 (9) |
O3—Ni1—O3i | 180.00 (10) | O3—S1—O4 | 107.13 (8) |
O1W—Ni1—O2Wi | 92.84 (6) | O1—S1—O4 | 108.05 (9) |
O1Wi—Ni1—O2Wi | 87.16 (6) | O2—S1—Na1vi | 39.34 (6) |
O3—Ni1—O2Wi | 91.57 (6) | O3—S1—Na1vi | 81.46 (6) |
O3i—Ni1—O2Wi | 88.43 (6) | O1—S1—Na1vi | 147.51 (7) |
O1W—Ni1—O2W | 87.16 (6) | O4—S1—Na1vi | 96.53 (6) |
O1Wi—Ni1—O2W | 92.84 (6) | S1—O1—Na1 | 129.18 (9) |
O3—Ni1—O2W | 88.43 (6) | S1—O2—Na1vi | 117.66 (8) |
O3i—Ni1—O2W | 91.57 (6) | S1—O2—Na1v | 135.03 (9) |
O2Wi—Ni1—O2W | 180.00 (8) | Na1vi—O2—Na1v | 103.80 (6) |
O2ii—Na1—O4iii | 91.03 (6) | S1—O3—Ni1 | 135.86 (9) |
O2ii—Na1—O1 | 113.12 (6) | S1—O4—Na1vii | 136.76 (9) |
O4iii—Na1—O1 | 104.66 (6) | Ni1—O1W—Na1 | 125.61 (7) |
O2ii—Na1—O1W | 154.93 (6) | Ni1—O1W—H1WA | 112 (2) |
O4iii—Na1—O1W | 99.66 (6) | Na1—O1W—H1WA | 101 (2) |
O1—Na1—O1W | 86.17 (6) | Ni1—O1W—H1WB | 106 (2) |
O2ii—Na1—O2iv | 76.20 (6) | Na1—O1W—H1WB | 104 (2) |
O4iii—Na1—O2iv | 90.41 (6) | H1WA—O1W—H1WB | 106.3 (15) |
O1—Na1—O2iv | 161.73 (6) | Ni1—O2W—Na1iv | 114.40 (6) |
O1W—Na1—O2iv | 81.08 (5) | Ni1—O2W—H2WA | 123 (2) |
O2ii—Na1—O2Wv | 73.64 (5) | Na1iv—O2W—H2WA | 109 (2) |
O4iii—Na1—O2Wv | 161.06 (6) | Ni1—O2W—H2WB | 113 (2) |
O1—Na1—O2Wv | 91.80 (5) | Na1iv—O2W—H2WB | 88 (2) |
O1W—Na1—O2Wv | 90.59 (5) | H2WA—O2W—H2WB | 104.7 (15) |
Symmetry codes: (i) −x, −y, −z; (ii) x, −y+1/2, z+1/2; (iii) −x+1, y−1/2, −z+1/2; (iv) −x, y−1/2, −z+1/2; (v) −x, y+1/2, −z+1/2; (vi) x, −y+1/2, z−1/2; (vii) −x+1, y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WB···O4viii | 0.84 (1) | 1.89 (1) | 2.733 (2) | 174 (3) |
O1W—H1WA···O1iv | 0.84 (1) | 1.89 (1) | 2.709 (2) | 163 (3) |
O2W—H2WA···O1iii | 0.84 (1) | 2.05 (1) | 2.868 (2) | 163 (2) |
O2W—H2WB···O4ix | 0.85 (1) | 2.16 (2) | 2.921 (2) | 150 (3) |
Symmetry codes: (iii) −x+1, y−1/2, −z+1/2; (iv) −x, y−1/2, −z+1/2; (viii) x−1, y, z; (ix) −x+1, −y, −z. |