Sodium cobalt(II) hydrogendiphosphate, NaCoHP₂O₇

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.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](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

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Computing details

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

Crystal data

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) Å^3

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.018	Only H-atom coordinates refined
wR(F^2) = 0.057	w = 1/[σ^2(Fo^2) + (0.0379P)^2 + 0.5277P] where P = (Fo^2 + 2Fc^2)/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+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.065 (4)

Special details

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Co1—O5^i	2.0495 (15)	Na—O5	2.341 (4)
Co1—O2	2.0782 (16)	Na—O7^iv	2.389 (4)
Co1—O3	2.1156 (16)	Na—O3	2.503 (7)
Co1—O1^ii	2.1474 (15)	Na—O7^ii	2.519 (6)
Co1—O1^iii	2.1713 (15)	Na—O1	2.622 (10)
Co1—O4	2.2104 (16)	Na—O2^ii	2.66 (2)
P1—O2^iv	1.5036 (16)	Na—O4	2.929 (13)
P1—O5^iii	1.5112 (16)	Na'—O5	2.295 (6)
P1—O4	1.5593 (16)	Na'—O7^iv	2.393 (7)
P1—O6^i	1.6121 (16)	Na'—O3	2.418 (6)
P2—O3	1.5103 (16)	Na'—O4	2.649 (14)
P2—O1	1.5394 (15)	Na'—O3^i	2.73 (3)
P2—O7	1.5414 (16)	Na'—O7^ii	2.75 (2)
P2—O6	1.5978 (15)	Na'—O1	2.95 (2)
Na—Na'	0.580 (17)
O5^i—Co1—O2	95.83 (6)	O1^iii—Co1—O4	90.30 (6)
O5^i—Co1—O3	92.13 (6)	O2^iv—P1—O5^iii	116.81 (9)
O2—Co1—O3	95.57 (6)	O2^iv—P1—O4	111.27 (9)
O5^i—Co1—O1^ii	171.12 (6)	O5^iii—P1—O4	109.37 (9)
O2—Co1—O1^ii	87.35 (6)	O2^iv—P1—O6^i	105.19 (9)
O3—Co1—O1^ii	95.82 (6)	O5^iii—P1—O6^i	108.62 (9)
O5^i—Co1—O1^iii	90.90 (6)	O4—P1—O6^i	104.79 (9)
O2—Co1—O1^iii	93.18 (6)	O3—P2—O1	111.82 (9)
O3—Co1—O1^iii	170.40 (6)	O3—P2—O7	114.19 (9)
O1^ii—Co1—O1^iii	80.63 (6)	O1—P2—O7	110.46 (9)
O5^i—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)
O1^ii—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)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H···O7^ii	0.80	1.66	2.450 (2)	168
O4—H···O1^ii	0.80	2.56	2.955 (2)	111

Symmetry code: (ii) −x+1, −y+1, −z+1.