Sodium diiron(III) diphosphate hydroxide dihydrate

Gao, S.; Ng, S.W.

doi:10.1107/S1600536805036226

Sodium diiron(III) diphosphate hydroxide dihydrate

The title compound, poly[sodium [aqua-μ₃-hydroxo-di-μ₄-phosphatodiferrate(III)] hydrate], NaFe₂(OH)(PO₄)₂(H₂O)₂, is isostructural with the mineral leucophosphite, Fe₂H₅KO₁₁P₂.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805036226/br6221sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805036226/br6221Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 295 K
Mean (P-O) = 0.002 Å
R factor = 0.022
wR factor = 0.072
Data-to-parameter ratio = 12.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.50
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.86 Ratio
PLAT417_ALERT_2_C Short Inter D-H..H-D       H2     ..  H4      ..       2.13 Ang.
PLAT758_ALERT_4_C D-H..A  Calc      166.00, Rep      165(6) ......  Senseless su
              O9   -H9   -O2W     1.555   1.555   1.555

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 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
   3 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

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); 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.

Poly[sodium [aqua-µ₃-hydroxo-di-µ₄-phosphato-diferrate(III)] hydrate] top

Crystal data top

NaFe₂(OH)(PO₄)₂(H₂O)₂	F(000) = 744
M_r = 377.67	D_x = 2.767 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 8478 reflections
a = 9.766 (2) Å	θ = 3.0–27.5°
b = 9.692 (2) Å	µ = 3.65 mm⁻¹
c = 9.811 (2) Å	T = 295 K
β = 102.53 (2)°	Prism, light yellow
V = 906.4 (3) Å³	0.31 × 0.24 × 0.18 mm
Z = 4

Data collection top

Rigaku R-AXIS RAPID IP diffractometer	2070 independent reflections
Radiation source: fine-focus sealed tube	1955 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.015
ω scans	θ_max = 27.5°, θ_min = 3.0°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −12→12
T_min = 0.363, T_max = 0.518	k = −12→12
8694 measured reflections	l = −10→12

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)] = 0.022	Hydrogen site location: difference Fourier map
wR(F²) = 0.072	H-atom parameters constrained
S = 1.09	w = 1/[σ²(F_o²) + (0.0424P)² + 1.9035P] where P = (F_o² + 2F_c²)/3
2070 reflections	(Δ/σ)_max = 0.001
165 parameters	Δρ_max = 0.85 e Å⁻³
7 restraints	Δρ_min = −0.34 e Å⁻³

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe1	0.61052 (3)	0.04829 (4)	0.63047 (4)	0.0071 (1)
Fe2	0.59902 (3)	0.27125 (4)	0.31173 (4)	0.0069 (1)
P1	0.79049 (6)	0.31958 (6)	0.63035 (6)	0.0070 (1)
P2	0.79314 (6)	0.46961 (6)	0.14665 (6)	0.0070 (1)
Na1	1.0176 (1)	0.1960 (1)	0.3995 (1)	0.0205 (3)
O1	0.6982 (2)	0.2224 (2)	0.6948 (2)	0.0125 (4)
O2	0.7361 (2)	0.3348 (2)	0.4733 (2)	0.0116 (4)
O3	0.9420 (2)	0.2694 (2)	0.6570 (2)	0.0130 (4)
O4	0.7833 (2)	0.4635 (2)	0.6973 (2)	0.0102 (3)
O5	0.6800 (2)	0.3763 (2)	0.1797 (2)	0.0120 (4)
O6	0.9402 (2)	0.4069 (2)	0.1988 (2)	0.0101 (4)
O7	0.7613 (2)	0.4880 (2)	−0.0138 (2)	0.0100 (3)
O8	0.7858 (2)	0.6115 (2)	0.2158 (2)	0.0112 (4)
O9	0.4985 (2)	0.1420 (2)	0.4395 (2)	0.0079 (3)
O1w	0.4904 (2)	0.4498 (2)	0.3457 (3)	0.0226 (5)
O2w	0.3137 (3)	0.3500 (2)	0.5347 (3)	0.0287 (5)
H9	0.449	0.209	0.454	0.07*
H1	0.405	0.471	0.320	0.03*
H2	0.537	0.518	0.386	0.05*
H3	0.267	0.398	0.469	0.05*
H4	0.282	0.358	0.608	0.04*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0070 (2)	0.0081 (2)	0.0060 (2)	−0.0003 (1)	0.0011 (1)	−0.0002 (1)
Fe2	0.0064 (2)	0.0075 (2)	0.0067 (2)	−0.0005 (1)	0.0009 (1)	0.0003 (1)
P1	0.0069 (3)	0.0066 (3)	0.0067 (3)	0.0003 (2)	−0.0002 (2)	−0.0006 (2)
P2	0.0069 (3)	0.0070 (3)	0.0074 (3)	−0.0011 (2)	0.0021 (2)	0.0004 (2)
Na1	0.0192 (6)	0.0293 (6)	0.0125 (5)	0.0067 (5)	0.0023 (4)	0.0085 (5)
O1	0.0165 (9)	0.0094 (8)	0.0116 (9)	−0.0054 (7)	0.0034 (7)	−0.0014 (7)
O2	0.0132 (9)	0.0122 (9)	0.0080 (8)	−0.0023 (7)	−0.0009 (7)	−0.0006 (7)
O3	0.0091 (8)	0.0171 (9)	0.0113 (9)	0.0053 (7)	−0.0010 (7)	−0.0019 (7)
O4	0.0105 (8)	0.0076 (8)	0.0106 (8)	0.0006 (6)	−0.0015 (7)	−0.0025 (7)
O5	0.0117 (8)	0.0138 (9)	0.0112 (8)	−0.0043 (7)	0.0041 (7)	0.0016 (7)
O6	0.0080 (8)	0.0129 (9)	0.0098 (8)	0.0014 (7)	0.0029 (6)	0.0022 (7)
O7	0.0096 (8)	0.0133 (9)	0.0072 (8)	−0.0014 (7)	0.0019 (6)	0.0014 (7)
O8	0.0136 (9)	0.0089 (8)	0.0127 (9)	−0.0011 (7)	0.0066 (7)	−0.0016 (7)
O9	0.0084 (8)	0.0080 (8)	0.0078 (8)	0.0008 (6)	0.0026 (6)	0.0000 (6)
O1w	0.011 (1)	0.021 (1)	0.034 (1)	0.004 (1)	0.001 (1)	−0.012 (1)
O2w	0.044 (1)	0.020 (1)	0.027 (1)	0.008 (1)	0.018 (1)	0.009 (1)

Geometric parameters (Å, º) top

Fe1—O1	1.935 (2)	P2—O6	1.541 (2)
Fe1—O4ⁱ	1.961 (2)	P2—O7	1.547 (2)
Fe1—O6ⁱⁱ	1.972 (2)	P2—O8	1.542 (2)
Fe1—O7ⁱⁱⁱ	1.960 (2)	Na1—O1^vi	3.050 (2)
Fe1—O9	2.155 (2)	Na1—O2	3.280 (2)
Fe1—O9^iv	2.165 (2)	Na1—O3	2.872 (2)
Fe2—O2	1.940 (2)	Na1—O5^vii	2.945 (2)
Fe2—O3^v	1.950 (2)	Na1—O6	2.825 (2)
Fe2—O5	1.946 (2)	Na1—O7^vii	2.947 (2)
Fe2—O8ⁱⁱⁱ	1.967 (2)	Na1—O8ⁱⁱⁱ	3.045 (2)
Fe2—O9	2.154 (2)	Na1—O1wⁱⁱⁱ	3.376 (3)
Fe2—O1w	2.094 (2)	Na1—O2w^viii	3.269 (3)
P1—O1	1.532 (2)	O9—H9	0.84
P1—O2	1.524 (2)	O1w—H1	0.85
P1—O3	1.525 (2)	O1w—H2	0.85
P1—O4	1.550 (2)	O2w—H3	0.85
P2—O5	1.516 (2)	O2w—H4	0.84

O1—Fe1—O4ⁱ	88.29 (8)	O3—Na1—O1^vi	144.16 (7)
O1—Fe1—O6ⁱⁱ	92.48 (8)	O5^vii—Na1—O1^vi	113.88 (6)
O1—Fe1—O7ⁱⁱⁱ	99.05 (8)	O7^vii—Na1—O1^vi	78.53 (6)
O1—Fe1—O9	91.25 (8)	O8ⁱⁱⁱ—Na1—O1^vi	118.70 (6)
O1—Fe1—O9^iv	176.80 (7)	O6—Na1—O2w^viii	91.82 (7)
O4ⁱ—Fe1—O6ⁱⁱ	97.26 (8)	O3—Na1—O2w^viii	84.45 (7)
O4ⁱ—Fe1—O7ⁱⁱⁱ	95.35 (8)	O5^vii—Na1—O2w^viii	58.65 (6)
O4ⁱ—Fe1—O9	178.63 (7)	O7^vii—Na1—O2w^viii	64.61 (6)
O4ⁱ—Fe1—O9^iv	92.75 (7)	O8ⁱⁱⁱ—Na1—O2w^viii	167.74 (7)
O6ⁱⁱ—Fe1—O7ⁱⁱⁱ	163.14 (8)	O1^vi—Na1—O2w^viii	64.01 (6)
O6ⁱⁱ—Fe1—O9	84.05 (7)	O6—Na1—O2	75.32 (6)
O6ⁱⁱ—Fe1—O9^iv	84.39 (7)	O3—Na1—O2	46.84 (5)
O7ⁱⁱⁱ—Fe1—O9	83.44 (7)	O5^vii—Na1—O2	101.47 (6)
O7ⁱⁱⁱ—Fe1—O9^iv	83.86 (7)	O7^vii—Na1—O2	147.91 (6)
O9—Fe1—O9^iv	87.77 (7)	O8ⁱⁱⁱ—Na1—O2	52.98 (5)
O2—Fe2—O3^v	170.79 (8)	O1^vi—Na1—O2	132.14 (6)
O2—Fe2—O5	94.01 (8)	O2w^viii—Na1—O2	115.65 (7)
O2—Fe2—O8ⁱⁱⁱ	92.77 (8)	O6—Na1—O1wⁱⁱⁱ	93.07 (6)
O2—Fe2—O9	91.72 (7)	O3—Na1—O1wⁱⁱⁱ	146.23 (7)
O2—Fe2—O1w	83.74 (8)	O5^vii—Na1—O1wⁱⁱⁱ	114.94 (6)
O3^v—Fe2—O5	87.26 (8)	O7^vii—Na1—O1wⁱⁱⁱ	70.80 (6)
O3^v—Fe2—O8ⁱⁱⁱ	96.36 (8)	O8ⁱⁱⁱ—Na1—O1wⁱⁱⁱ	71.03 (6)
O3^v—Fe2—O9	87.39 (7)	O1^vi—Na1—O1wⁱⁱⁱ	69.02 (6)
O3^v—Fe2—O1w	87.19 (9)	O2w^viii—Na1—O1wⁱⁱⁱ	119.59 (7)
O5—Fe2—O8ⁱⁱⁱ	89.60 (8)	O2—Na1—O1wⁱⁱⁱ	123.79 (6)
O5—Fe2—O9	173.95 (7)	P1—O1—Fe1	131.3 (1)
O5—Fe2—O1w	88.09 (9)	P1—O2—Fe2	145.4 (1)
O8ⁱⁱⁱ—Fe2—O9	88.19 (7)	P1—O2—Na1	93.36 (9)
O8ⁱⁱⁱ—Fe2—O1w	175.67 (8)	Fe2—O2—Na1	98.74 (7)
O9—Fe2—O1w	94.46 (8)	P1—O3—Fe2^vii	140.2 (1)
O1—P1—O2	111.7 (1)	P1—O3—Na1	110.7 (1)
O1—P1—O3	111.6 (1)	Fe2^vii—O3—Na1	109.01 (8)
O1—P1—O4	107.1 (1)	P1—O4—Fe1^ix	132.7 (1)
O2—P1—O3	108.5 (1)	P2—O5—Fe2	151.0 (1)
O2—P1—O4	107.7 (1)	P2—O5—Na1^v	102.26 (9)
O3—P1—O4	110.2 (1)	Fe2—O5—Na1^v	106.43 (8)
O5—P2—O6	111.3 (1)	P2—O6—Fe1^vi	126.5 (1)
O5—P2—O7	106.9 (1)	P2—O6—Na1	127.3 (1)
O5—P2—O8	109.4 (1)	Fe1^vi—O6—Na1	106.17 (8)
O6—P2—O7	110.5 (1)	P2—O7—Fe1^x	128.0 (1)
O6—P2—O8	109.5 (1)	P2—O7—Na1^v	101.30 (9)
O7—P2—O8	109.1 (1)	Fe1^x—O7—Na1^v	126.13 (8)
O6—Na1—O3	110.65 (7)	P2—O8—Fe2^x	124.0 (1)
O6—Na1—O5^vii	146.21 (7)	Fe2—O9—Fe1	122.80 (8)
O3—Na1—O5^vii	55.03 (6)	Fe2—O9—Fe1^iv	124.46 (8)
O6—Na1—O7^vii	135.74 (7)	Fe1—O9—Fe1^iv	92.23 (7)
O3—Na1—O7^vii	103.97 (6)	Fe2—O9—H9	90
O5^vii—Na1—O7^vii	49.37 (5)	Fe1—O9—H9	112
O6—Na1—O8ⁱⁱⁱ	81.03 (6)	Fe1^iv—O9—H9	117
O3—Na1—O8ⁱⁱⁱ	88.75 (6)	Fe2—O1w—H1	131
O5^vii—Na1—O8ⁱⁱⁱ	124.50 (7)	Fe2—O1w—H2	119
O7^vii—Na1—O8ⁱⁱⁱ	127.18 (7)	H1—O1w—H2	110
O6—Na1—O1^vi	57.25 (5)	H3—O2w—H4	111

Symmetry codes: (i) −x+3/2, y−1/2, −z+3/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) −x+3/2, y−1/2, −z+1/2; (iv) −x+1, −y, −z+1; (v) x−1/2, −y+1/2, z−1/2; (vi) x+1/2, −y+1/2, z−1/2; (vii) x+1/2, −y+1/2, z+1/2; (viii) x+1, y, z; (ix) −x+3/2, y+1/2, −z+3/2; (x) −x+3/2, y+1/2, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O9—H9···O2w	0.84	2.16	2.988 (3)	165 (6)
O1w—H1···O4^xi	0.85	1.91	2.746 (3)	167 (4)
O1w—H2···O2w^xi	0.85	1.97	2.798 (3)	165 (4)
O2w—H3···O4^xi	0.85	2.09	2.900 (3)	162 (5)
O2w—H4···O8^xi	0.84	2.01	2.847 (3)	176 (5)

Symmetry code: (xi) −x+1, −y+1, −z+1.

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page