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Crystals of caesium molybdeno­methyl­enedi­phospho­nate, [CsMoO2(CH3O6P2)], were hydro­thermally synthesized at 473 K. The monoclinic structure, as determined from single-crystal X-ray diffraction, is two-dimensional and consists of stacked mixed layers of corner-sharing tetrahedral di­phosphon­ate groups and MoO6 octahedra, between which Cs+ cations are intercalated.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102003992/iz1019sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270102003992/iz1019Isup2.hkl
Contains datablock I

CCDC reference: 184481

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: SHELXTL.

Caesium molybdenomethylendiphosphonate top
Crystal data top
[CsMoO2(CH3O6P2)]F(000) = 800
Mr = 434Dx = 3.552 Mg m3
Dm = 3.423 (8) Mg m3
Dm measured by pycnometry
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 8.0859 (5) ÅCell parameters from 5728 reflections
b = 11.8567 (7) Åθ = 2.8–29.9°
c = 9.2347 (5) ŵ = 6.44 mm1
β = 113.512 (1)°T = 296 K
V = 811.84 (8) Å3Parallelepiped, blue
Z = 40.20 × 0.12 × 0.08 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
2142 independent reflections
Radiation source: fine-focus sealed tube1646 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ω scansθmax = 29.9°, θmin = 2.8°
Absorption correction: semi-empirical (using intensity measurements)
(SADABS; Blessing, 1995)
h = 106
Tmin = 0.390, Tmax = 0.597k = 1516
5609 measured reflectionsl = 1212
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033H-atom parameters constrained
wR(F2) = 0.081 w = 1/[σ2(Fo2) + (0.0487P)2 + 0.4123P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.001
2142 reflectionsΔρmax = 1.62 e Å3
119 parametersΔρmin = 1.58 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: 0.0013 (3)
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 on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating _R_factor_obs 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
Cs0.68614 (4)0.12463 (3)0.98461 (4)0.02315 (13)
Mo0.98806 (5)0.12786 (3)0.74580 (4)0.01204 (12)
P10.2533 (2)0.24800 (9)1.07243 (12)0.0121 (2)
P20.7315 (2)0.00573 (9)1.40591 (12)0.0119 (2)
O10.4390 (5)0.2234 (3)1.2024 (4)0.0214 (7)
O20.2154 (5)0.1576 (3)0.9430 (4)0.0157 (6)
O30.8023 (4)0.1033 (3)1.5250 (4)0.0159 (7)
O40.5394 (5)0.0321 (3)1.2937 (4)0.0222 (7)
O50.8509 (5)0.0134 (3)1.3170 (4)0.0184 (7)
O60.1041 (5)0.2547 (3)1.1318 (4)0.0162 (6)
O70.8717 (5)0.2374 (3)0.7776 (4)0.0190 (7)
O80.9228 (5)0.0189 (3)0.8290 (4)0.0196 (7)
C0.2711 (7)0.3802 (3)0.9863 (6)0.0148 (9)
HA0.17250.38510.88310.018*
HB0.38230.37970.96980.018*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs0.0286 (2)0.0256 (2)0.0145 (2)0.00188 (13)0.00780 (14)0.00111 (11)
Mo0.0163 (2)0.0129 (2)0.0073 (2)0.00014 (14)0.0052 (2)0.00119 (12)
P10.0161 (6)0.0117 (5)0.0081 (5)0.0007 (4)0.0044 (4)0.0006 (4)
P20.0148 (6)0.0119 (5)0.0084 (5)0.0011 (4)0.0041 (4)0.0010 (4)
O10.020 (2)0.020 (2)0.017 (2)0.0004 (14)0.0003 (15)0.0026 (13)
O20.019 (2)0.0162 (14)0.0111 (15)0.0016 (14)0.0053 (13)0.0020 (12)
O30.021 (2)0.0145 (14)0.010 (2)0.0013 (13)0.0038 (14)0.0019 (12)
O40.018 (2)0.017 (2)0.022 (2)0.0012 (14)0.0011 (15)0.0014 (14)
O50.029 (2)0.0154 (15)0.016 (2)0.0053 (14)0.0137 (15)0.0008 (13)
O60.022 (2)0.0158 (15)0.013 (2)0.0004 (14)0.0102 (13)0.0012 (12)
O70.024 (2)0.021 (2)0.013 (2)0.0033 (15)0.0082 (14)0.0011 (13)
O80.027 (2)0.021 (2)0.011 (2)0.0031 (15)0.0089 (14)0.0011 (13)
C0.026 (2)0.009 (2)0.017 (2)0.001 (2)0.017 (2)0.002 (2)
Geometric parameters (Å, º) top
Cs—O7i3.001 (3)P1—O21.543 (3)
Cs—O83.081 (3)P1—C1.790 (4)
Cs—O4ii3.106 (3)P2—O51.514 (3)
Cs—O1iii3.143 (3)P2—O41.516 (4)
Cs—O73.159 (3)P2—O31.540 (3)
Cs—O53.257 (3)P2—Cviii1.795 (4)
Cs—O3iii3.339 (3)P2—Csii4.1329 (12)
Cs—O8iv3.394 (4)O1—Csi3.143 (3)
Cs—O2ii3.443 (3)O2—Moix2.037 (3)
Cs—O6v3.461 (3)O2—Csii3.443 (3)
Cs—O13.552 (3)O3—Mox2.014 (3)
Cs—O43.669 (4)O3—Csi3.339 (3)
Mo—O81.692 (3)O4—Csii3.105 (3)
Mo—O71.697 (3)O5—Moiv2.115 (3)
Mo—O3vi2.014 (3)O6—Moxi2.172 (3)
Mo—O2v2.037 (3)O6—Csix3.461 (3)
Mo—O5iv2.115 (3)O7—Csiii3.001 (3)
Mo—O6vii2.172 (3)O8—Csiv3.394 (4)
Mo—Csiii3.9612 (5)C—P2xii1.795 (4)
Mo—Csiv4.1070 (5)C—HA0.97
P1—O61.513 (3)C—HB0.97
P1—O11.530 (4)
O7i—Cs—O8117.53 (9)O5iv—Mo—O6vii81.17 (12)
O7i—Cs—O4ii171.67 (9)O8—Mo—Cs49.81 (11)
O8—Cs—O4ii68.86 (9)O7—Mo—Cs52.58 (11)
O7i—Cs—O1iii111.04 (9)O3vi—Mo—Cs100.92 (9)
O8—Cs—O1iii98.87 (9)O2v—Mo—Cs92.39 (9)
O4ii—Cs—O1iii71.79 (9)O5iv—Mo—Cs138.01 (9)
O7i—Cs—O797.33 (7)O6vii—Mo—Cs140.51 (8)
O8—Cs—O749.97 (9)O8—Mo—Csiii127.89 (12)
O4ii—Cs—O790.94 (9)O7—Mo—Csiii44.66 (10)
O1iii—Cs—O763.51 (9)O3vi—Mo—Csiii57.39 (9)
O7i—Cs—O563.57 (8)O2v—Mo—Csiii122.23 (9)
O8—Cs—O597.96 (8)O5iv—Mo—Csiii127.27 (8)
O4ii—Cs—O5111.33 (9)O6vii—Mo—Csiii60.68 (9)
O1iii—Cs—O5162.78 (8)Cs—Mo—Csiii88.783 (11)
O7—Cs—O5131.93 (9)O8—Mo—Csiv53.77 (12)
O7i—Cs—O3iii49.88 (8)O7—Mo—Csiv135.96 (10)
O8—Cs—O3iii104.23 (8)O3vi—Mo—Csiv123.19 (9)
O4ii—Cs—O3iii135.78 (8)O2v—Mo—Csiv56.80 (9)
O1iii—Cs—O3iii66.19 (8)O5iv—Mo—Csiv51.86 (8)
O7—Cs—O3iii58.55 (8)O6vii—Mo—Csiv117.69 (9)
O5—Cs—O3iii112.89 (8)Cs—Mo—Csiv92.581 (10)
O7i—Cs—O8iv77.67 (9)Csiii—Mo—Csiv178.344 (11)
O8—Cs—O8iv53.57 (10)O6—P1—O1113.6 (2)
O4ii—Cs—O8iv103.92 (8)O6—P1—O2112.1 (2)
O1iii—Cs—O8iv149.74 (8)O1—P1—O2107.7 (2)
O7—Cs—O8iv87.01 (8)O6—P1—C109.4 (2)
O5—Cs—O8iv47.31 (7)O1—P1—C106.7 (2)
O3iii—Cs—O8iv105.32 (8)O2—P1—C106.9 (2)
O7i—Cs—O2ii111.15 (8)O6—P1—Cs160.59 (13)
O8—Cs—O2ii63.69 (8)O1—P1—Cs56.45 (13)
O4ii—Cs—O2ii66.00 (8)O2—P1—Cs61.76 (13)
O1iii—Cs—O2ii137.69 (8)C—P1—Cs89.88 (15)
O7—Cs—O2ii113.59 (8)O5—P2—O4111.2 (2)
O5—Cs—O2ii49.66 (7)O5—P2—O3111.3 (2)
O3iii—Cs—O2ii152.18 (8)O4—P2—O3108.7 (2)
O8iv—Cs—O2ii46.97 (8)O5—P2—Cviii109.1 (2)
O7i—Cs—O6v49.06 (8)O4—P2—Cviii108.3 (2)
O8—Cs—O6v70.95 (8)O3—P2—Cviii108.1 (2)
O4ii—Cs—O6v138.63 (8)O5—P2—Cs50.08 (12)
O1iii—Cs—O6v105.57 (8)O4—P2—Cs65.97 (14)
O7—Cs—O6v54.83 (8)O3—P2—Cs107.00 (12)
O5—Cs—O6v83.43 (8)Cviii—P2—Cs144.3 (2)
O3iii—Cs—O6v48.60 (8)O5—P2—Csii86.94 (14)
O8iv—Cs—O6v57.17 (8)O4—P2—Csii39.03 (13)
O2ii—Cs—O6v104.05 (8)O3—P2—Csii147.72 (13)
O7i—Cs—O160.11 (8)Cviii—P2—Csii89.3 (2)
O8—Cs—O1173.06 (8)Cs—P2—Csii63.82 (2)
O4ii—Cs—O1112.86 (9)P1—O1—Csi129.9 (2)
O1iii—Cs—O188.00 (7)P1—O1—Cs102.50 (15)
O7—Cs—O1135.50 (8)Csi—O1—Cs110.07 (10)
O5—Cs—O175.12 (8)P1—O2—Moix130.0 (2)
O3iii—Cs—O179.33 (8)P1—O2—Csii124.4 (2)
O8iv—Cs—O1119.94 (7)Moix—O2—Csii93.54 (11)
O2ii—Cs—O1110.44 (8)P1—O2—Cs96.63 (15)
O6v—Cs—O1108.22 (7)Moix—O2—Cs126.90 (12)
O7i—Cs—O470.25 (8)Csii—O2—Cs74.21 (6)
O8—Cs—O4134.03 (8)P2—O3—Mox138.3 (2)
O4ii—Cs—O4101.51 (8)P2—O3—Csi129.6 (2)
O1iii—Cs—O4121.37 (8)Mox—O3—Csi92.08 (10)
O7—Cs—O4167.50 (8)P2—O4—Csii123.1 (2)
O5—Cs—O441.79 (8)P2—O4—Cs91.86 (15)
O3iii—Cs—O4111.46 (7)Csii—O4—Cs78.49 (8)
O8iv—Cs—O488.88 (7)P2—O5—Moiv147.2 (2)
O2ii—Cs—O471.31 (7)P2—O5—Cs109.0 (2)
O6v—Cs—O4113.33 (7)Moiv—O5—Cs97.43 (10)
O1—Cs—O439.52 (8)P1—O6—Moxi140.4 (2)
O8—Mo—O7102.2 (2)P1—O6—Csix129.0 (2)
O8—Mo—O3vi96.16 (14)Moxi—O6—Csix86.15 (10)
O7—Mo—O3vi92.57 (14)Mo—O7—Csiii111.92 (13)
O8—Mo—O2v93.46 (15)Mo—O7—Cs102.17 (13)
O7—Mo—O2v94.47 (14)Csiii—O7—Cs126.08 (12)
O3vi—Mo—O2v166.62 (13)Mo—O8—Cs105.39 (14)
O8—Mo—O5iv88.39 (14)Mo—O8—Csiv102.53 (15)
O7—Mo—O5iv169.40 (13)Cs—O8—Csiv126.42 (9)
O3vi—Mo—O5iv85.51 (13)P1—C—P2xii117.3 (2)
O2v—Mo—O5iv85.49 (13)P1—C—HA108.0
O8—Mo—O6vii169.53 (14)P2xii—C—HA108.0
O7—Mo—O6vii88.27 (14)P1—C—HB108.0
O3vi—Mo—O6vii83.91 (12)P2xii—C—HB108.0
O2v—Mo—O6vii84.95 (13)HA—C—HB107.2
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x+1, y, z+2; (iii) x, y+1/2, z1/2; (iv) x+2, y, z+2; (v) x+1, y, z; (vi) x, y, z1; (vii) x+1, y+1/2, z1/2; (viii) x+1, y1/2, z+5/2; (ix) x1, y, z; (x) x, y, z+1; (xi) x1, y+1/2, z+1/2; (xii) x+1, y+1/2, z+5/2.
 

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