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LaP3O9·3H2O belongs to the REIIIP3O9·3H2O (RE = rare earth) polyphosphate family that crystallizes in space group P\overline 6. In these cyclotriphosphates, the cyclic P3O93− anion has a planar configuration with 3/m internal symmetry. The La3+ cation, located on one of the \overline 6 axes, is ninefold-coordinated by six polyphosphate O atoms at a distance of 2.518 (2) Å and by three water O atoms at 2.584 (3) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807004734/wm2090sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807004734/wm2090Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](P-O) = 0.003 Å
  • R factor = 0.014
  • wR factor = 0.037
  • Data-to-parameter ratio = 15.3

checkCIF/PLATON results

No syntax errors found



Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 30.02 From the CIF: _reflns_number_total 519 Count of symmetry unique reflns 264 Completeness (_total/calc) 196.59% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 255 Fraction of Friedel pairs measured 0.966 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CAD-4 EXPRESS (Duisenberg, 1992; Macíček & Yordanov, 1992); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

Lanthanum cyclotriphosphate trihydrate top
Crystal data top
LaP3O9·3H2ODx = 2.974 Mg m3
Mr = 429.87Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6Cell parameters from 25 reflections
Hall symbol: P -6θ = 2.0–15.0°
a = 6.7373 (5) ŵ = 5.01 mm1
c = 6.1048 (9) ÅT = 298 K
V = 239.98 (4) Å3Prism, colourless
Z = 10.15 × 0.14 × 0.13 mm
F(000) = 204
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.033
Radiation source: fine-focus sealed tubeθmax = 30.0°, θmin = 3.3°
Graphite monochromatorh = 99
ω/2θ scansk = 97
2476 measured reflectionsl = 88
519 independent reflections2 standard reflections every 120 min
518 reflections with I > 2σ(I) intensity decay: 2%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.015All H-atom parameters refined
wR(F2) = 0.037 w = 1/[σ2(Fo2) + (0.0234P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.16(Δ/σ)max < 0.001
519 reflectionsΔρmax = 1.04 e Å3
34 parametersΔρmin = 0.60 e Å3
0 restraintsAbsolute structure: Flack (1983), with 255 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.070 (18)
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
La0.33330.66670.00000.00786 (8)
P0.22015 (15)0.94258 (15)0.50000.00853 (17)
O10.2340 (5)1.1851 (5)0.50000.0199 (6)
O20.3189 (4)0.9238 (4)0.7088 (4)0.0235 (5)
O30.6938 (5)1.0698 (6)0.00000.0196 (6)
H0.760 (7)1.146 (8)0.099 (6)0.027 (12)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
La0.00762 (10)0.00762 (10)0.00832 (12)0.00381 (5)0.0000.000
P0.0086 (4)0.0082 (4)0.0103 (4)0.0054 (3)0.0000.000
O10.0117 (12)0.0101 (12)0.0393 (17)0.0065 (10)0.0000.000
O20.0220 (10)0.0207 (10)0.0220 (11)0.0063 (8)0.0081 (9)0.0094 (8)
O30.0170 (13)0.0140 (13)0.0121 (13)0.0040 (11)0.0000.000
Geometric parameters (Å, º) top
La—O2i2.518 (2)La—O3viii2.584 (3)
La—O2ii2.518 (2)P—O21.472 (2)
La—O2iii2.518 (2)P—O2iii1.472 (2)
La—O2iv2.518 (2)P—O11.590 (3)
La—O2v2.518 (2)P—O1ix1.595 (3)
La—O2vi2.518 (2)O1—Px1.595 (3)
La—O3vii2.584 (3)O2—Laxi2.518 (2)
La—O32.584 (3)O3—H0.77 (4)
O2i—La—O2ii138.52 (4)O2iii—La—O367.43 (7)
O2i—La—O2iii75.66 (9)O2iv—La—O3135.02 (6)
O2ii—La—O2iii89.83 (12)O2v—La—O371.12 (8)
O2i—La—O2iv89.83 (12)O2vi—La—O371.12 (8)
O2ii—La—O2iv75.66 (9)O3vii—La—O3120.0
O2iii—La—O2iv138.52 (4)O2i—La—O3viii71.12 (8)
O2i—La—O2v138.52 (4)O2ii—La—O3viii135.02 (6)
O2ii—La—O2v75.66 (9)O2iii—La—O3viii135.02 (6)
O2iii—La—O2v138.52 (4)O2iv—La—O3viii71.12 (8)
O2iv—La—O2v75.66 (9)O2v—La—O3viii67.43 (7)
O2i—La—O2vi75.66 (9)O2vi—La—O3viii67.43 (7)
O2ii—La—O2vi138.52 (4)O3vii—La—O3viii120.0
O2iii—La—O2vi75.66 (9)O3—La—O3viii120.0
O2iv—La—O2vi138.52 (4)O2—P—O2iii119.9 (2)
O2v—La—O2vi89.83 (12)O2—P—O1106.95 (11)
O2i—La—O3vii67.43 (7)O2iii—P—O1106.95 (11)
O2ii—La—O3vii71.12 (8)O2—P—O1ix109.26 (10)
O2iii—La—O3vii71.12 (8)O2iii—P—O1ix109.26 (10)
O2iv—La—O3vii67.43 (7)O1—P—O1ix103.14 (19)
O2v—La—O3vii135.02 (6)P—O1—Px136.86 (19)
O2vi—La—O3vii135.02 (6)P—O2—Laxi147.66 (13)
O2i—La—O3135.02 (6)La—O3—H129 (3)
O2ii—La—O367.43 (7)
Symmetry codes: (i) y+1, xy+1, z1; (ii) x, y, z+1; (iii) x, y, z1; (iv) y+1, xy+1, z+1; (v) x+y, x+1, z+1; (vi) x+y, x+1, z1; (vii) y+1, xy+1, z; (viii) x+y, x+1, z; (ix) x+y1, x+1, z; (x) y+1, xy+2, z; (xi) x, y, z1.
 

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