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The structure of di­ammonium tetramolybdate, [(NH4)2(Mo4O13)]n, consists of puckered layers built up from the self-assembly of chains of tetrameric units [Mo4O13]2− linked through corner-sharing octahedra. The ammonium cations are located between consecutive layers, yielding a three-dimensional array via extensive N—H...O hydrogen bonding, in which terminal oxo groups of the surface network are involved.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680400385X/wm6011sup1.cif
Contains datablocks I, pbcadi

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680400385X/wm6011Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Mo-O) = 0.005 Å
  • H-atom completeness 1%
  • R factor = 0.037
  • wR factor = 0.104
  • Data-to-parameter ratio = 11.4

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............ 24.99 Deg. PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. N1 = 2.87 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O3 .. N1 = 2.81 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O9 .. N2 = 2.86 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O10 .. N1 = 2.80 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O10 .. N2 = 2.85 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O13 .. N1 = 2.87 Ang.
Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 8 From the CIF: _chemical_formula_weight 627.84 TEST: Calculate formula weight from _atom_site_* atom mass num sum N 14.01 2.00 28.01 O 16.00 13.00 207.99 H 1.01 0.00 0.00 Mo 95.94 4.00 383.76 Calculated formula weight 619.76 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 627.84 PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT430_ALERT_2_C Short Inter D...A Contact O9 .. N2 = 2.90 Ang.
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: H8 Mo4 N2 O13 Atom count from _chemical_formula_moiety:H8260 N20 FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:H8 Mo4 N2 O13 Atom count from the _atom_site data: Mo4 N2 O13 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 8 From the CIF: _chemical_formula_sum H8 Mo4 N2 O13 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 64.00 0.00 64.00 Mo 32.00 32.00 0.00 N 16.00 16.00 0.00 O 104.00 104.00 0.00
0 ALERT level A = In general: serious problem 7 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 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: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXLTL-NT (Bruker, 1998); program(s) used to refine structure: SHELXLTL-NT; molecular graphics: SHELXLTL-NT; software used to prepare material for publication: SHELXLTL-NT.

(I) top
Crystal data top
(NH4)2[Mo4O13]F(000) = 2352
Mr = 627.84Dx = 3.724 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 25 reflections
a = 15.423 (2) Åθ = 39.3–39.8°
b = 19.0022 (9) ŵ = 4.45 mm1
c = 7.6423 (7) ÅT = 293 K
V = 2239.7 (4) Å3Prism, colorless
Z = 80.60 × 0.36 × 0.20 mm
Data collection top
Rigaku AFC-7S
diffractometer
1842 reflections with I > 2σ(I)
Radiation source: Normal-focus sealed tubeRint = 0.039
Graphite monochromatorθmax = 25.0°, θmin = 2.1°
ω–2θ scansh = 018
Absorption correction: empirical (using intensity measurements)
(Walker & Stuart 1983)
k = 222
Tmin = 0.160, Tmax = 0.411l = 09
2166 measured reflections3 standard reflections every 150 reflections
1968 independent reflections intensity decay: none
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037H-atom parameters not refined
wR(F2) = 0.104 w = 1/[σ2(Fo2) + (0.0611P)2 + 14.763P]
where P = (Fo2 + 2Fc2)/3
S = 1.24(Δ/σ)max < 0.001
1968 reflectionsΔρmax = 1.40 e Å3
172 parametersΔρmin = 2.81 e Å3
0 restraints
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
Mo10.14025 (4)0.39902 (3)0.20935 (8)0.00648 (19)
Mo20.27954 (4)0.24880 (3)0.42271 (7)0.00456 (19)
Mo30.06614 (3)0.38978 (3)0.11479 (8)0.00570 (19)
Mo40.07082 (4)0.24360 (3)0.32982 (8)0.00402 (19)
O10.1263 (3)0.4551 (3)0.3854 (7)0.0164 (11)
O20.0231 (3)0.3315 (2)0.2804 (6)0.0083 (10)
O30.3448 (3)0.1779 (3)0.4433 (7)0.0135 (11)
O40.1683 (3)0.1949 (2)0.4297 (6)0.0071 (9)
O50.1438 (3)0.3173 (2)0.1721 (6)0.0083 (10)
O60.1802 (3)0.3141 (2)0.3107 (6)0.0066 (9)
O70.0519 (3)0.4218 (2)0.0502 (6)0.0090 (10)
O80.2723 (3)0.2819 (2)0.6337 (6)0.0090 (10)
O90.2294 (3)0.4311 (3)0.1039 (7)0.0128 (11)
O100.1187 (3)0.4228 (3)0.0658 (7)0.0141 (11)
O110.0854 (3)0.4519 (3)0.2742 (7)0.0131 (10)
O120.0127 (3)0.1959 (2)0.4253 (6)0.0093 (10)
O130.0754 (3)0.2086 (3)0.1201 (7)0.0091 (10)
N10.0226 (4)0.4195 (3)0.3765 (8)0.0146 (13)
N20.2840 (5)0.4322 (3)0.2305 (9)0.0218 (15)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.0055 (3)0.0041 (3)0.0098 (3)0.0005 (2)0.0016 (2)0.0019 (2)
Mo20.0036 (3)0.0050 (3)0.0051 (3)0.0001 (2)0.0003 (2)0.0006 (2)
Mo30.0046 (3)0.0045 (3)0.0080 (3)0.0005 (2)0.0006 (2)0.0000 (2)
Mo40.0036 (3)0.0032 (3)0.0052 (3)0.0007 (2)0.0002 (2)0.0007 (2)
O10.016 (3)0.019 (3)0.015 (3)0.004 (2)0.001 (2)0.003 (2)
O20.006 (2)0.012 (2)0.007 (2)0.0012 (19)0.0011 (18)0.0028 (18)
O30.013 (2)0.012 (3)0.015 (3)0.005 (2)0.002 (2)0.002 (2)
O40.007 (2)0.005 (2)0.009 (2)0.0024 (19)0.0022 (18)0.0011 (18)
O50.008 (2)0.007 (2)0.010 (2)0.0035 (19)0.0000 (18)0.0022 (19)
O60.004 (2)0.005 (2)0.011 (2)0.0014 (18)0.0008 (18)0.0007 (18)
O70.006 (2)0.009 (2)0.012 (2)0.0001 (19)0.0018 (19)0.0032 (19)
O80.008 (2)0.012 (2)0.007 (2)0.0012 (19)0.0019 (18)0.001 (2)
O90.010 (2)0.009 (2)0.019 (3)0.0044 (19)0.001 (2)0.001 (2)
O100.013 (2)0.014 (3)0.015 (3)0.001 (2)0.002 (2)0.003 (2)
O110.012 (2)0.012 (2)0.015 (3)0.004 (2)0.003 (2)0.005 (2)
O120.008 (2)0.008 (2)0.012 (2)0.0013 (19)0.0021 (19)0.0012 (19)
O130.010 (2)0.008 (2)0.009 (2)0.0044 (19)0.0008 (19)0.001 (2)
N10.015 (3)0.011 (3)0.017 (3)0.003 (3)0.004 (3)0.004 (3)
N20.024 (4)0.021 (4)0.020 (3)0.002 (3)0.006 (3)0.007 (3)
Geometric parameters (Å, º) top
Mo1—O91.706 (5)Mo3—O71.982 (5)
Mo1—O11.730 (5)Mo3—O22.173 (5)
Mo1—O71.877 (5)Mo3—O12ii2.330 (5)
Mo1—O61.893 (5)Mo4—O121.735 (5)
Mo1—O22.281 (5)Mo4—O131.736 (5)
Mo2—O31.688 (5)Mo4—O21.865 (5)
Mo2—O81.734 (5)Mo4—O41.923 (4)
Mo2—O5i1.902 (5)Mo4—O62.158 (5)
Mo2—O41.999 (5)Mo4—O13iii2.398 (5)
Mo2—O62.149 (5)O5—Mo2iv1.902 (5)
Mo2—O8ii2.288 (5)O8—Mo2iii2.288 (5)
Mo3—O101.719 (5)O12—Mo3iii2.330 (5)
Mo3—O111.723 (5)O13—Mo4ii2.398 (5)
Mo3—O51.877 (5)
O9—Mo1—O1104.3 (2)O7—Mo3—O273.73 (18)
O9—Mo1—O7101.3 (2)O10—Mo3—O12ii85.6 (2)
O1—Mo1—O7105.7 (2)O11—Mo3—O12ii168.5 (2)
O9—Mo1—O6103.7 (2)O5—Mo3—O12ii81.81 (19)
O1—Mo1—O6104.3 (2)O7—Mo3—O12ii74.64 (18)
O7—Mo1—O6134.3 (2)O2—Mo3—O12ii77.41 (17)
O9—Mo1—O2162.1 (2)O12—Mo4—O13102.6 (2)
O1—Mo1—O293.6 (2)O12—Mo4—O2105.1 (2)
O7—Mo1—O273.09 (18)O13—Mo4—O299.9 (2)
O6—Mo1—O271.39 (18)O12—Mo4—O499.3 (2)
O3—Mo2—O8104.0 (2)O13—Mo4—O498.6 (2)
O3—Mo2—O5i102.2 (2)O2—Mo4—O4145.1 (2)
O8—Mo2—O5i98.4 (2)O12—Mo4—O6158.8 (2)
O3—Mo2—O495.8 (2)O13—Mo4—O698.2 (2)
O8—Mo2—O496.1 (2)O2—Mo4—O674.86 (18)
O5i—Mo2—O4153.45 (19)O4—Mo4—O673.42 (18)
O3—Mo2—O6157.3 (2)O12—Mo4—O13iii80.2 (2)
O8—Mo2—O696.6 (2)O13—Mo4—O13iii176.0 (3)
O5i—Mo2—O684.10 (18)O2—Mo4—O13iii81.93 (18)
O4—Mo2—O672.18 (18)O4—Mo4—O13iii77.99 (18)
O3—Mo2—O8ii85.2 (2)O6—Mo4—O13iii78.74 (17)
O8—Mo2—O8ii170.8 (2)Mo4—O2—Mo3145.5 (3)
O5i—Mo2—O8ii80.63 (19)Mo4—O2—Mo1103.8 (2)
O4—Mo2—O8ii81.55 (18)Mo3—O2—Mo194.40 (18)
O6—Mo2—O8ii74.22 (17)Mo4—O4—Mo2114.4 (2)
O10—Mo3—O11103.7 (2)Mo3—O5—Mo2iv144.1 (3)
O10—Mo3—O598.9 (2)Mo1—O6—Mo2152.5 (3)
O11—Mo3—O5103.2 (2)Mo1—O6—Mo4107.6 (2)
O10—Mo3—O797.0 (2)Mo2—O6—Mo499.92 (18)
O11—Mo3—O797.1 (2)Mo1—O7—Mo3115.7 (2)
O5—Mo3—O7150.4 (2)Mo2—O8—Mo2iii143.3 (3)
O10—Mo3—O2162.2 (2)Mo4—O12—Mo3iii152.7 (3)
O11—Mo3—O292.7 (2)Mo4—O13—Mo4ii135.0 (3)
O5—Mo3—O283.93 (19)
Symmetry codes: (i) x1/2, y, z1/2; (ii) x, y+1/2, z+1/2; (iii) x, y+1/2, z1/2; (iv) x+1/2, y, z1/2.
 

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