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A new compound with an open framework, (NH4)[Fe(MoO4)2], was synthesized through hydro­thermal reaction. It contains 10 non-H atoms in the asymmetric unit and the structure comprises a network of FeO6 octahedra and MoO4 tetrahedra that strictly alternate and involve only Fe-O-Mo linkages. The ammonium cations sit in the middle of the channels formed by these linkages.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803019597/br6116sup1.cif
Contains datablocks I, raxis

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803019597/br6116Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Fe-O) = 0.002 Å
  • R factor = 0.021
  • wR factor = 0.055
  • Data-to-parameter ratio = 13.1

checkCIF/PLATON results

No syntax errors found



Alert level A DIFF012_ALERT_1_A _diffrn_reflns_av_R_equivalents is missing R factor for symmetry-equivalent intensities. The following tests will not be performed RINTA DIFF020_ALERT_1_A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards. DIFF022_ALERT_1_A _diffrn_standards_decay_% is missing Percentage decrease in standards intensity.
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
3 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: TEXRAY software (Molecular Structure Corporation, 1999); cell refinement: TEXRAY software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEX (McArdle, 1995); software used to prepare material for publication: SHELXL97.

ammonium iron molybdate top
Crystal data top
(NH4)[Fe(MoO4)2]F(000) = 740
Mr = 393.77Dx = 3.556 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ac 2nCell parameters from 25 reflections
a = 14.782 (3) Åθ = 12–18°
b = 5.6774 (11) ŵ = 5.31 mm1
c = 8.7653 (18) ÅT = 293 K
V = 735.6 (3) Å3Block, brown
Z = 40.15 × 0.14 × 0.14 mm
Data collection top
Rigaku Weissenberg IP
diffractometer
870 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeθmax = 27.5°, θmin = 2.7°
Graphite monochromatorh = 019
scintillation counter scansk = 07
932 measured reflectionsl = 011
932 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021H-atom parameters not refined
wR(F2) = 0.055 w = 1/[σ2(Fo2) + (0.0268P)2 + 0.1878P]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
932 reflectionsΔρmax = 1.35 e Å3
71 parametersΔρmin = 1.20 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0084 (5)
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
xyzUiso*/Ueq
Mo10.032854 (17)0.25000.29379 (3)0.00992 (12)
Mo20.281400 (18)0.25000.99826 (4)0.01173 (13)
Fe30.11699 (3)0.25000.69048 (6)0.00928 (15)
N10.3824 (2)0.25000.5398 (4)0.0207 (7)
O10.05096 (18)0.25000.4921 (3)0.0160 (6)
O20.03143 (9)0.0006 (3)0.2315 (2)0.0160 (4)
O30.36644 (18)0.25000.8674 (4)0.0276 (7)
O40.17752 (15)0.25000.8922 (3)0.0188 (6)
O50.13360 (17)0.25000.1968 (3)0.0201 (6)
O60.29668 (11)0.0097 (4)1.1099 (2)0.0191 (4)
H10.43040.25000.60440.059 (19)*
H20.32860.25000.56570.06 (2)*
H30.39040.13210.47260.068 (15)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.00913 (17)0.01062 (17)0.01000 (19)0.0000.00015 (9)0.000
Mo20.01073 (18)0.01119 (18)0.0133 (2)0.0000.00328 (10)0.000
Fe30.0093 (2)0.0087 (2)0.0099 (3)0.0000.00115 (17)0.000
N10.0217 (15)0.0225 (17)0.0179 (18)0.0000.0016 (14)0.000
O10.0210 (11)0.0177 (13)0.0093 (13)0.0000.0019 (9)0.000
O20.0186 (7)0.0134 (9)0.0161 (8)0.0055 (7)0.0029 (6)0.0005 (9)
O30.0192 (12)0.0387 (17)0.0248 (16)0.0000.0032 (12)0.000
O40.0149 (11)0.0284 (14)0.0133 (13)0.0000.0041 (10)0.000
O50.0149 (10)0.0220 (13)0.0235 (16)0.0000.0055 (10)0.000
O60.0195 (6)0.0171 (9)0.0207 (10)0.0072 (7)0.0017 (6)0.0042 (10)
Geometric parameters (Å, º) top
Mo1—O51.715 (3)Fe3—O41.981 (3)
Mo1—O11.758 (3)Fe3—O11.994 (3)
Mo1—O21.7959 (17)Fe3—O6ii1.9972 (18)
Mo1—O2i1.7959 (17)Fe3—O6iii1.9972 (18)
Mo2—O31.702 (3)Fe3—O2iv2.0178 (17)
Mo2—O6i1.784 (2)Fe3—O2v2.0178 (17)
Mo2—O61.784 (2)O2—Fe3iv2.0178 (17)
Mo2—O41.795 (2)O6—Fe3vi1.9972 (18)
O5—Mo1—O1110.96 (13)O1—Fe3—O6iii90.26 (8)
O5—Mo1—O2108.00 (8)O6ii—Fe3—O6iii86.18 (12)
O1—Mo1—O2112.39 (8)O4—Fe3—O2iv88.90 (7)
O5—Mo1—O2i108.00 (8)O1—Fe3—O2iv89.35 (8)
O1—Mo1—O2i112.39 (8)O6ii—Fe3—O2iv92.34 (7)
O2—Mo1—O2i104.79 (11)O6iii—Fe3—O2iv178.47 (9)
O3—Mo2—O6i106.04 (8)O4—Fe3—O2v88.90 (7)
O3—Mo2—O6106.04 (8)O1—Fe3—O2v89.35 (8)
O6i—Mo2—O6111.46 (13)O6ii—Fe3—O2v178.47 (9)
O3—Mo2—O4106.42 (13)O6iii—Fe3—O2v92.34 (7)
O6i—Mo2—O4113.11 (7)O2iv—Fe3—O2v89.13 (10)
O6—Mo2—O4113.11 (7)Mo1—O1—Fe3159.45 (16)
O4—Fe3—O1177.54 (11)Mo1—O2—Fe3iv141.69 (12)
O4—Fe3—O6ii91.54 (8)Mo2—O4—Fe3148.04 (15)
O1—Fe3—O6ii90.26 (8)Mo2—O6—Fe3vi147.08 (10)
O4—Fe3—O6iii91.54 (8)
Symmetry codes: (i) x, y+1/2, z; (ii) x+1/2, y, z1/2; (iii) x+1/2, y+1/2, z1/2; (iv) x, y, z+1; (v) x, y+1/2, z+1; (vi) x+1/2, y, z+1/2.
 

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