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The title compound was prepared hydrothermally at 453 K. The structure consists of a three-dimensional framework built up from centrosymmetric Co2(HP2O7)2 clusters, linked through P-O-Co corners, delimiting interconnected tunnels. The Na+ cations partially occupy two independent positions in the tunnels at a distance of 0.58 (2) Å from each other. The structure of NaCoHP2O7 in the solid state is similar to that of NaZnHP2O7 and CaCoP2O7.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (P-O) = 0.002 Å
- Disorder in solvent or counterion
- R factor = 0.018
- wR factor = 0.057
- Data-to-parameter ratio = 9.9
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level B:
CHEMS_01 Alert B The sum formula contains elements in the wrong order.
H precedes Co
Sequence must be C, H, then alphabetical.
Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 50.00 Perc.
PLAT_745 Alert C D-H Calc 0.80(2), Rep 0.80000 .... Missing su
O4 -H 1.555 1.555
PLAT_745 Alert C D-H Calc 0.80(2), Rep 0.80000 .... Missing su
O4 -H 1.555 1.555
PLAT_746 Alert C H...A Calc 1.66(3), Rep 1.66000 .... Missing su
H -O7 1.555 2.666
PLAT_746 Alert C H...A Calc 2.57(4), Rep 2.56000 .... Missing su
H -O1 1.555 2.666
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
5 Alert Level C = Please check
Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: MolEN (Fair, 1990); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.
Sodium Cobalt Phosphate Hydrogendiphosphate
top
Crystal data top
NaCoHP2O7 | Z = 2 |
Mr = 256.87 | F(000) = 250 |
Triclinic, P1 | Dx = 3.264 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 6.5629 (7) Å | Cell parameters from 25 reflections |
b = 6.643 (1) Å | θ = 10.1–14.0° |
c = 6.5309 (6) Å | µ = 3.96 mm−1 |
α = 112.60 (1)° | T = 293 K |
β = 87.935 (8)° | Parallelepiped, pink |
γ = 96.14 (1)° | 0.25 × 0.18 × 0.14 mm |
V = 261.35 (5) Å3 | |
Data collection top
Enraf-Nonius CAD-4 diffractometer | 1123 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.011 |
Graphite monochromator | θmax = 27.0°, θmin = 3.1° |
ω/2θ scans | h = 0→8 |
Absorption correction: ψ scan (North et al., 1968) | k = −8→8 |
Tmin = 0.411, Tmax = 0.574 | l = −8→8 |
1246 measured reflections | 2 standard reflections every 120 min |
1142 independent reflections | intensity decay: none |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.018 | Only H-atom coordinates refined |
wR(F2) = 0.057 | w = 1/[σ2(Fo2) + (0.0379P)2 + 0.5277P] where P = (Fo2 + 2Fc2)/3 |
S = 0.96 | (Δ/σ)max < 0.001 |
1142 reflections | Δρmax = 0.44 e Å−3 |
115 parameters | Δρmin = −0.44 e Å−3 |
1 restraint | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.065 (4) |
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) |
Co1 | 0.14557 (4) | 0.38935 (4) | 0.28318 (4) | 0.00892 (13) | |
P1 | 0.12068 (8) | 0.86406 (9) | 0.16792 (9) | 0.00787 (15) | |
P2 | 0.64276 (8) | 0.28014 (8) | 0.25330 (8) | 0.00711 (15) | |
Na | 0.6582 (18) | 0.7594 (10) | 0.302 (3) | 0.0242 (18) | 0.65 (5) |
Na' | 0.613 (3) | 0.7404 (13) | 0.221 (5) | 0.023 (3) | 0.35 (5) |
O1 | 0.8274 (2) | 0.4464 (2) | 0.3630 (2) | 0.0099 (3) | |
O2 | 0.1139 (2) | 0.0960 (3) | 0.3312 (3) | 0.0124 (3) | |
O3 | 0.4643 (2) | 0.3913 (3) | 0.2215 (3) | 0.0130 (3) | |
O4 | 0.2102 (3) | 0.7202 (3) | 0.2764 (3) | 0.0128 (3) | |
O5 | 0.9229 (2) | 0.7475 (3) | 0.0489 (2) | 0.0116 (3) | |
O6 | 0.7117 (2) | 0.1209 (3) | 0.0136 (2) | 0.0111 (3) | |
O7 | 0.5890 (2) | 0.1272 (3) | 0.3791 (2) | 0.0111 (3) | |
H | 0.262 (6) | 0.780 (6) | 0.397 (3) | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.00891 (18) | 0.00918 (18) | 0.00716 (18) | 0.00045 (11) | −0.00017 (11) | 0.00158 (12) |
P1 | 0.0088 (3) | 0.0080 (3) | 0.0060 (2) | 0.00102 (19) | 0.00036 (19) | 0.0019 (2) |
P2 | 0.0075 (3) | 0.0071 (3) | 0.0060 (3) | 0.00080 (19) | 0.00021 (18) | 0.0017 (2) |
Na | 0.026 (2) | 0.0162 (11) | 0.031 (4) | 0.0057 (11) | 0.014 (3) | 0.0093 (16) |
Na' | 0.020 (3) | 0.0145 (18) | 0.032 (8) | 0.0007 (18) | 0.012 (4) | 0.008 (3) |
O1 | 0.0091 (7) | 0.0098 (7) | 0.0080 (7) | −0.0018 (6) | 0.0003 (5) | 0.0012 (6) |
O2 | 0.0162 (8) | 0.0093 (7) | 0.0102 (7) | 0.0025 (6) | 0.0036 (6) | 0.0020 (6) |
O3 | 0.0098 (7) | 0.0137 (7) | 0.0163 (8) | 0.0022 (6) | 0.0003 (6) | 0.0064 (6) |
O4 | 0.0186 (8) | 0.0101 (7) | 0.0101 (7) | 0.0014 (6) | −0.0041 (6) | 0.0040 (6) |
O5 | 0.0104 (7) | 0.0157 (8) | 0.0077 (7) | 0.0003 (6) | −0.0008 (6) | 0.0035 (6) |
O6 | 0.0118 (7) | 0.0108 (7) | 0.0070 (7) | −0.0008 (6) | 0.0027 (5) | 0.0003 (6) |
O7 | 0.0138 (7) | 0.0113 (7) | 0.0094 (7) | −0.0011 (6) | −0.0015 (6) | 0.0056 (6) |
Geometric parameters (Å, º) top
Co1—O5i | 2.0495 (15) | Na—O5 | 2.341 (4) |
Co1—O2 | 2.0782 (16) | Na—O7iv | 2.389 (4) |
Co1—O3 | 2.1156 (16) | Na—O3 | 2.503 (7) |
Co1—O1ii | 2.1474 (15) | Na—O7ii | 2.519 (6) |
Co1—O1iii | 2.1713 (15) | Na—O1 | 2.622 (10) |
Co1—O4 | 2.2104 (16) | Na—O2ii | 2.66 (2) |
P1—O2iv | 1.5036 (16) | Na—O4 | 2.929 (13) |
P1—O5iii | 1.5112 (16) | Na'—O5 | 2.295 (6) |
P1—O4 | 1.5593 (16) | Na'—O7iv | 2.393 (7) |
P1—O6i | 1.6121 (16) | Na'—O3 | 2.418 (6) |
P2—O3 | 1.5103 (16) | Na'—O4 | 2.649 (14) |
P2—O1 | 1.5394 (15) | Na'—O3i | 2.73 (3) |
P2—O7 | 1.5414 (16) | Na'—O7ii | 2.75 (2) |
P2—O6 | 1.5978 (15) | Na'—O1 | 2.95 (2) |
Na—Na' | 0.580 (17) | | |
| | | |
O5i—Co1—O2 | 95.83 (6) | O1iii—Co1—O4 | 90.30 (6) |
O5i—Co1—O3 | 92.13 (6) | O2iv—P1—O5iii | 116.81 (9) |
O2—Co1—O3 | 95.57 (6) | O2iv—P1—O4 | 111.27 (9) |
O5i—Co1—O1ii | 171.12 (6) | O5iii—P1—O4 | 109.37 (9) |
O2—Co1—O1ii | 87.35 (6) | O2iv—P1—O6i | 105.19 (9) |
O3—Co1—O1ii | 95.82 (6) | O5iii—P1—O6i | 108.62 (9) |
O5i—Co1—O1iii | 90.90 (6) | O4—P1—O6i | 104.79 (9) |
O2—Co1—O1iii | 93.18 (6) | O3—P2—O1 | 111.82 (9) |
O3—Co1—O1iii | 170.40 (6) | O3—P2—O7 | 114.19 (9) |
O1ii—Co1—O1iii | 80.63 (6) | O1—P2—O7 | 110.46 (9) |
O5i—Co1—O4 | 92.04 (6) | O3—P2—O6 | 107.65 (9) |
O2—Co1—O4 | 171.33 (6) | O1—P2—O6 | 107.99 (8) |
O3—Co1—O4 | 80.48 (6) | O7—P2—O6 | 104.24 (8) |
O1ii—Co1—O4 | 85.39 (6) | | |
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) x, y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H···O7ii | 0.80 | 1.66 | 2.450 (2) | 168 |
O4—H···O1ii | 0.80 | 2.56 | 2.955 (2) | 111 |
Symmetry code: (ii) −x+1, −y+1, −z+1. |
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