Download citation
Download citation
link to html
The crystal structure of cerium catena-polyphosphate, CeP3O9, is isotypic with the previously reported structures of La, Pr, Nd and Gd C-type polyphosphates. The absolute configuration of CeP3O9 was determined reliably. The structure contains helical polyphosphate chains with a period of six tetra­hedra running along the c axis, and the Ce cation is in an eightfold coordination by terminal O atoms of the polyphosphate chains. Ce, one P and one O atom are located on twofold rotation axes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807020703/wm2096sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807020703/wm2096Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 180 K
  • Mean [sigma](P-O) = 0.003 Å
  • R factor = 0.025
  • wR factor = 0.055
  • Data-to-parameter ratio = 11.2

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.92
Author Response: This is only just on the low side for any global regulation; and 0.92 coverage is satisfactory for this sized-compound. There were time limitations, and it was thought better to collect a few Friedels than concentrate on excessive coverage.

Alert level B PLAT213_ALERT_2_B Atom O3 has ADP max/min Ratio ............. 4.20 prola
Alert level C PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.91
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 27.43 From the CIF: _reflns_number_total 686 Count of symmetry unique reflns 488 Completeness (_total/calc) 140.57% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 198 Fraction of Friedel pairs measured 0.406 Are heavy atom types Z>Si present yes PLAT794_ALERT_5_G Check Predicted Bond Valency for Ce1 (3) 3.33
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2006); software used to prepare material for publication: SHELXL97.

Cerium catena-polyphosphate top
Crystal data top
CeP3O9F(000) = 700
Mr = 377.03Dx = 3.524 Mg m3
Orthorhombic, C2221Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c 2Cell parameters from 1840 reflections
a = 11.236 (2) Åθ = 1.0–27.5°
b = 8.6110 (17) ŵ = 7.10 mm1
c = 7.3458 (15) ÅT = 180 K
V = 710.7 (2) Å3Trianglar plate, translucent white
Z = 40.15 × 0.10 × 0.05 mm
Data collection top
Nonius Kappa-CCD
diffractometer
686 independent reflections
Radiation source: fine-focus sealed tube658 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
φ scansθmax = 27.4°, θmin = 4.1°
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
h = 1014
Tmin = 0.461, Tmax = 0.700k = 1010
1045 measured reflectionsl = 99
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)] = 0.025 w = 1/[σ2(Fo2) + 0.1886P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055(Δ/σ)max < 0.001
S = 1.05Δρmax = 0.78 e Å3
686 reflectionsΔρmin = 1.38 e Å3
61 parametersAbsolute structure: Flack (1983), 198 Friedel pairs
0 restraintsAbsolute structure parameter: 0.06 (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 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
Ce11.00000.62768 (4)0.25000.00805 (15)
P11.00000.2484 (2)0.25000.0085 (3)
P20.82530 (12)0.9927 (2)0.20267 (15)0.0104 (3)
O10.6957 (3)0.0244 (5)0.2102 (4)0.0158 (9)
O20.8732 (4)0.8506 (5)0.2873 (5)0.0195 (11)
O30.8751 (4)1.00001.00000.0168 (12)
O40.0185 (3)0.3450 (4)0.4175 (4)0.0111 (9)
O50.8915 (4)0.1381 (4)0.2904 (5)0.0158 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ce10.0117 (2)0.0098 (2)0.0026 (2)0.0000.00012 (17)0.000
P10.0136 (8)0.0098 (7)0.0022 (7)0.0000.0010 (9)0.000
P20.0135 (7)0.0118 (6)0.0059 (6)0.0002 (7)0.0005 (4)0.0015 (6)
O10.0138 (19)0.023 (2)0.011 (2)0.0011 (19)0.0020 (14)0.0009 (18)
O20.025 (2)0.0152 (19)0.018 (3)0.0050 (18)0.0039 (17)0.0012 (18)
O30.016 (3)0.033 (3)0.002 (2)0.0000.0000.002 (3)
O40.016 (2)0.0145 (15)0.0026 (16)0.0024 (18)0.0027 (15)0.0005 (12)
O50.019 (2)0.023 (2)0.006 (2)0.005 (2)0.0039 (15)0.0044 (17)
Geometric parameters (Å, º) top
Ce1—O1i2.390 (4)P2—O21.475 (4)
Ce1—O1ii2.390 (4)P2—O1viii1.483 (4)
Ce1—O2iii2.406 (4)P2—O3ix1.592 (2)
Ce1—O22.406 (4)P2—O5viii1.593 (4)
Ce1—O4iv2.462 (3)O1—P2x1.483 (4)
Ce1—O4v2.462 (3)O1—Ce1xi2.390 (4)
Ce1—O4vi2.735 (3)O3—P2xii1.592 (2)
Ce1—O4vii2.735 (3)O3—P2xiii1.592 (2)
Ce1—P13.2660 (19)O4—P1xiv1.500 (3)
P1—O4vii1.500 (3)O4—Ce1xv2.462 (3)
P1—O4vi1.500 (3)O4—Ce1xiv2.735 (3)
P1—O51.573 (4)O5—P2x1.593 (4)
P1—O5iii1.573 (4)
O1i—Ce1—O1ii136.3 (2)O2iii—Ce1—P1142.91 (11)
O1i—Ce1—O2iii148.83 (16)O2—Ce1—P1142.91 (11)
O1ii—Ce1—O2iii74.81 (14)O4iv—Ce1—P195.47 (8)
O1i—Ce1—O274.81 (14)O4v—Ce1—P195.47 (8)
O1ii—Ce1—O2148.83 (16)O4vi—Ce1—P127.15 (6)
O2iii—Ce1—O274.2 (2)O4vii—Ce1—P127.15 (6)
O1i—Ce1—O4iv94.56 (11)O4vii—P1—O4vi112.6 (3)
O1ii—Ce1—O4iv89.52 (12)O4vii—P1—O5106.69 (18)
O2iii—Ce1—O4iv82.00 (12)O4vi—P1—O5112.5 (2)
O2—Ce1—O4iv89.25 (13)O4vii—P1—O5iii112.5 (2)
O1i—Ce1—O4v89.52 (12)O4vi—P1—O5iii106.69 (18)
O1ii—Ce1—O4v94.56 (11)O5—P1—O5iii105.8 (3)
O2iii—Ce1—O4v89.25 (13)O4vii—P1—Ce156.30 (14)
O2—Ce1—O4v82.00 (12)O4vi—P1—Ce156.30 (14)
O4iv—Ce1—O4v169.05 (16)O5—P1—Ce1127.12 (15)
O1i—Ce1—O4vi69.77 (12)O5iii—P1—Ce1127.12 (15)
O1ii—Ce1—O4vi71.56 (13)O2—P2—O1viii119.7 (3)
O2iii—Ce1—O4vi134.71 (13)O2—P2—O3ix107.39 (19)
O2—Ce1—O4vi135.74 (13)O1viii—P2—O3ix111.9 (2)
O4iv—Ce1—O4vi68.42 (12)O2—P2—O5viii108.2 (2)
O4v—Ce1—O4vi122.52 (8)O1viii—P2—O5viii107.4 (2)
O1i—Ce1—O4vii71.56 (13)O3ix—P2—O5viii100.56 (17)
O1ii—Ce1—O4vii69.77 (12)P2x—O1—Ce1xi167.6 (3)
O2iii—Ce1—O4vii135.74 (13)P2—O2—Ce1146.1 (2)
O2—Ce1—O4vii134.71 (13)P2xii—O3—P2xiii138.8 (3)
O4iv—Ce1—O4vii122.52 (8)P1xiv—O4—Ce1xv148.8 (2)
O4v—Ce1—O4vii68.42 (12)P1xiv—O4—Ce1xiv96.55 (15)
O4vi—Ce1—O4vii54.29 (12)Ce1xv—O4—Ce1xiv110.79 (13)
O1i—Ce1—P168.16 (11)P1—O5—P2x139.5 (3)
O1ii—Ce1—P168.16 (11)
Symmetry codes: (i) x+3/2, y+1/2, z+1/2; (ii) x+1/2, y+1/2, z; (iii) x+2, y, z+1/2; (iv) x+1, y+1, z1/2; (v) x+1, y+1, z+1; (vi) x+1, y, z+1/2; (vii) x+1, y, z; (viii) x, y+1, z; (ix) x, y, z1; (x) x, y1, z; (xi) x1/2, y1/2, z; (xii) x, y+2, z+1; (xiii) x, y, z+1; (xiv) x1, y, z; (xv) x+1, y+1, z+1/2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds