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Single-crystal X-ray diffraction analysis has been performed on dysprosium ultraphosphate, DyP5O14, prepared by the flux method. The atomic arrangement is built up of layers of independent P8O24 rings perpendicular to the b axis inter­connected by PO4 groups to form a three-dimensional network of PO4 tetra­hedra. Two sites are located on the twofold axis for the Dy atoms, which have almost regular dodeca­hedral coordination.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807008410/br2028sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807008410/br2028Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](P-O) = 0.004 Å
  • R factor = 0.028
  • wR factor = 0.063
  • Data-to-parameter ratio = 12.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT021_ALERT_1_C Ratio Unique / Expected Reflections too High ... 1.04 PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.90 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96 PLAT213_ALERT_2_C Atom O4 has ADP max/min Ratio ............. 3.30 prola PLAT213_ALERT_2_C Atom O12 has ADP max/min Ratio ............. 3.10 oblat PLAT395_ALERT_2_C Deviating X-O-Y Angle from 120 Deg for O6 141.60 Deg.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 0 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: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

dysprosium ultraphosphate top
Crystal data top
DyP5O14F(000) = 2024
Mr = 541.35Dx = 3.510 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1946 reflections
a = 12.8934 (6) Åθ = 2.9–26.9°
b = 12.7756 (5) ŵ = 8.16 mm1
c = 12.4415 (5) ÅT = 298 K
β = 91.313 (3)°Cubic, colourless
V = 2048.84 (15) Å30.15 × 0.15 × 0.15 mm
Z = 8
Data collection top
Nonius KappaCCD area-detector
diffractometer
2290 independent reflections
Radiation source: fine-focus sealed tube1682 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
Detector resolution: 9 pixels mm-1θmax = 26.8°, θmin = 3.9°
ω/2θ scansh = 1616
Absorption correction: part of the refinement model (ΔF)
(Parkin et al., 1995)
k = 016
Tmin = 0.286, Tmax = 0.306l = 016
3807 measured reflections
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.028Secondary atom site location: difference Fourier map
wR(F2) = 0.063 w = 1/[σ2(Fo2) + (0.0082P]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max < 0.001
2290 reflectionsΔρmax = 1.65 e Å3
182 parametersΔρmin = 1.27 e Å3
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
Dy11.00000.52187 (2)0.25000.00472 (10)
Dy21.00000.03118 (2)0.25000.00456 (10)
P11.02500 (9)0.15233 (9)0.03255 (11)0.0054 (3)
P21.18169 (9)0.13795 (9)0.39145 (12)0.0055 (3)
P31.14714 (9)0.46602 (9)0.49867 (12)0.0064 (3)
P41.14896 (9)0.33223 (9)0.10313 (11)0.0059 (3)
P51.32072 (9)0.25021 (9)0.24096 (11)0.0055 (3)
O11.0257 (2)0.1032 (3)0.0736 (3)0.0123 (8)
O21.0607 (2)0.0973 (3)0.1306 (3)0.0105 (8)
O31.0865 (2)0.2617 (2)0.0210 (3)0.0085 (8)
O41.0914 (2)0.1981 (2)0.4457 (3)0.0095 (8)
O51.1526 (2)0.0497 (3)0.3226 (3)0.0119 (8)
O61.2398 (3)0.2283 (2)0.3355 (3)0.0118 (8)
O71.2490 (2)0.1041 (3)0.4914 (3)0.0083 (7)
O81.1159 (3)0.4636 (2)0.3857 (3)0.0104 (8)
O91.0768 (2)0.4342 (3)0.5843 (3)0.0133 (8)
O101.1946 (2)0.4182 (2)0.0282 (3)0.0078 (7)
O111.0896 (3)0.3714 (3)0.1921 (3)0.0134 (8)
O121.2437 (2)0.2633 (2)0.1365 (3)0.0090 (8)
O131.3680 (2)0.3509 (3)0.2684 (3)0.0125 (8)
O141.3833 (3)0.1578 (3)0.2183 (3)0.0154 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Dy10.00347 (16)0.00437 (16)0.0063 (2)0.0000.00080 (13)0.000
Dy20.00375 (16)0.00378 (16)0.0062 (2)0.0000.00043 (13)0.000
P10.0032 (5)0.0054 (5)0.0077 (8)0.0009 (5)0.0006 (5)0.0004 (5)
P20.0042 (6)0.0046 (5)0.0076 (8)0.0005 (5)0.0009 (5)0.0003 (5)
P30.0055 (6)0.0049 (5)0.0087 (8)0.0014 (5)0.0002 (5)0.0015 (5)
P40.0055 (6)0.0039 (5)0.0082 (8)0.0006 (5)0.0009 (5)0.0004 (5)
P50.0037 (5)0.0054 (5)0.0075 (8)0.0009 (5)0.0016 (5)0.0017 (5)
O10.0150 (18)0.0144 (17)0.008 (2)0.0024 (16)0.0013 (15)0.0023 (15)
O20.0095 (17)0.0105 (16)0.011 (2)0.0003 (15)0.0030 (15)0.0036 (15)
O30.0076 (16)0.0080 (16)0.010 (2)0.0024 (14)0.0012 (14)0.0003 (14)
O40.0038 (16)0.0077 (16)0.017 (2)0.0009 (14)0.0056 (15)0.0016 (15)
O50.0077 (16)0.0125 (16)0.016 (2)0.0004 (15)0.0035 (15)0.0035 (15)
O60.0132 (18)0.0079 (16)0.015 (2)0.0049 (15)0.0080 (16)0.0004 (15)
O70.0103 (16)0.0083 (16)0.006 (2)0.0054 (14)0.0037 (14)0.0027 (14)
O80.0120 (17)0.0135 (16)0.006 (2)0.0066 (15)0.0052 (15)0.0026 (14)
O90.0151 (17)0.0096 (16)0.015 (2)0.0030 (16)0.0059 (16)0.0005 (16)
O100.0077 (16)0.0049 (15)0.011 (2)0.0024 (14)0.0032 (14)0.0011 (14)
O110.0133 (17)0.0093 (17)0.018 (2)0.0082 (15)0.0033 (16)0.0025 (15)
O120.0046 (16)0.0127 (17)0.010 (2)0.0046 (14)0.0024 (14)0.0017 (14)
O130.0115 (17)0.0111 (16)0.015 (2)0.0064 (15)0.0006 (16)0.0026 (15)
O140.0143 (18)0.0171 (18)0.015 (2)0.0047 (16)0.0022 (16)0.0038 (16)
Geometric parameters (Å, º) top
Dy1—O14i2.326 (3)P2—O71.561 (4)
Dy1—O14ii2.326 (3)P2—O41.562 (3)
Dy1—O8iii2.350 (3)P3—O81.454 (4)
Dy1—O82.350 (3)P3—O91.472 (4)
Dy1—O11iii2.364 (3)P3—O7x1.614 (3)
Dy1—O112.364 (3)P3—O10xi1.640 (3)
Dy1—O9iv2.375 (4)P4—O111.450 (4)
Dy1—O9v2.375 (4)P4—O121.554 (3)
Dy2—O13vi2.288 (3)P4—O101.564 (3)
Dy2—O13vii2.288 (3)P4—O31.570 (4)
Dy2—O2iii2.359 (3)P5—O131.460 (3)
Dy2—O22.359 (3)P5—O141.461 (4)
Dy2—O52.382 (3)P5—O61.615 (4)
Dy2—O5iii2.382 (3)P5—O121.626 (4)
Dy2—O1viii2.396 (4)O1—Dy2ix2.396 (4)
Dy2—O1ix2.396 (4)O4—P1iii1.638 (3)
P1—O11.462 (4)O7—P3x1.614 (3)
P1—O21.473 (4)O9—Dy1iv2.375 (4)
P1—O31.615 (3)O10—P3v1.640 (3)
P1—O4iii1.638 (3)O13—Dy2xii2.288 (3)
P2—O51.459 (4)O14—Dy1xiii2.326 (3)
P2—O61.550 (4)
O14i—Dy1—O14ii83.40 (17)O13vii—Dy2—O1ix75.10 (12)
O14i—Dy1—O8iii139.20 (13)O2iii—Dy2—O1ix143.43 (11)
O14ii—Dy1—O8iii73.51 (12)O2—Dy2—O1ix74.42 (12)
O14i—Dy1—O873.51 (12)O5—Dy2—O1ix127.57 (12)
O14ii—Dy1—O8139.20 (13)O5iii—Dy2—O1ix73.96 (12)
O8iii—Dy1—O8143.05 (15)O1viii—Dy2—O1ix134.80 (16)
O14i—Dy1—O11iii150.97 (13)O1—P1—O2122.3 (2)
O14ii—Dy1—O11iii109.89 (12)O1—P1—O3106.1 (2)
O8iii—Dy1—O11iii69.76 (12)O2—P1—O3110.0 (2)
O8—Dy1—O11iii80.24 (12)O1—P1—O4iii109.1 (2)
O14i—Dy1—O11109.89 (12)O2—P1—O4iii107.7 (2)
O14ii—Dy1—O11150.97 (13)O3—P1—O4iii99.15 (17)
O8iii—Dy1—O1180.24 (12)O5—P2—O6115.6 (2)
O8—Dy1—O1169.76 (12)O5—P2—O7112.6 (2)
O11iii—Dy1—O1171.14 (17)O6—P2—O7107.35 (19)
O14i—Dy1—O9iv87.55 (12)O5—P2—O4116.74 (18)
O14ii—Dy1—O9iv71.94 (13)O6—P2—O4101.58 (18)
O8iii—Dy1—O9iv115.31 (12)O7—P2—O4101.4 (2)
O8—Dy1—O9iv73.87 (12)O8—P3—O9122.2 (2)
O11iii—Dy1—O9iv73.22 (12)O8—P3—O7x105.87 (19)
O11—Dy1—O9iv132.30 (12)O9—P3—O7x108.4 (2)
O14i—Dy1—O9v71.94 (13)O8—P3—O10xi109.2 (2)
O14ii—Dy1—O9v87.55 (12)O9—P3—O10xi108.6 (2)
O8iii—Dy1—O9v73.87 (12)O7x—P3—O10xi100.33 (17)
O8—Dy1—O9v115.31 (12)O11—P4—O12114.7 (2)
O11iii—Dy1—O9v132.30 (12)O11—P4—O10115.18 (19)
O11—Dy1—O9v73.22 (12)O12—P4—O10104.65 (18)
O9iv—Dy1—O9v152.68 (16)O11—P4—O3115.0 (2)
O13vi—Dy2—O13vii97.64 (17)O12—P4—O3103.71 (18)
O13vi—Dy2—O2iii97.86 (12)O10—P4—O3102.1 (2)
O13vii—Dy2—O2iii141.19 (12)O13—P5—O14121.8 (2)
O13vi—Dy2—O2141.19 (12)O13—P5—O6104.8 (2)
O13vii—Dy2—O297.86 (12)O14—P5—O6111.7 (2)
O2iii—Dy2—O291.85 (17)O13—P5—O12109.89 (19)
O13vi—Dy2—O5149.04 (13)O14—P5—O12105.0 (2)
O13vii—Dy2—O573.38 (11)O6—P5—O12101.96 (18)
O2iii—Dy2—O575.08 (11)P1—O1—Dy2ix171.3 (2)
O2—Dy2—O569.75 (12)P1—O2—Dy2138.75 (19)
O13vi—Dy2—O5iii73.38 (11)P4—O3—P1133.2 (3)
O13vii—Dy2—O5iii149.04 (13)P2—O4—P1iii126.2 (2)
O2iii—Dy2—O5iii69.75 (12)P2—O5—Dy2139.2 (2)
O2—Dy2—O5iii75.08 (11)P2—O6—P5141.6 (2)
O5—Dy2—O5iii128.56 (17)P2—O7—P3x131.3 (2)
O13vi—Dy2—O1viii75.10 (12)P3—O8—Dy1147.7 (2)
O13vii—Dy2—O1viii75.58 (12)P3—O9—Dy1iv147.1 (2)
O2iii—Dy2—O1viii74.42 (12)P4—O10—P3v128.6 (2)
O2—Dy2—O1viii143.43 (11)P4—O11—Dy1141.6 (2)
O5—Dy2—O1viii73.96 (12)P4—O12—P5137.2 (2)
O5iii—Dy2—O1viii127.57 (12)P5—O13—Dy2xii149.8 (2)
O13vi—Dy2—O1ix75.58 (12)P5—O14—Dy1xiii158.2 (3)
Symmetry codes: (i) x+5/2, y+1/2, z+1/2; (ii) x1/2, y+1/2, z; (iii) x+2, y, z+1/2; (iv) x+2, y+1, z+1; (v) x, y+1, z1/2; (vi) x1/2, y1/2, z; (vii) x+5/2, y1/2, z+1/2; (viii) x, y, z+1/2; (ix) x+2, y, z; (x) x+5/2, y+1/2, z+1; (xi) x, y+1, z+1/2; (xii) x+1/2, y+1/2, z; (xiii) x+1/2, y1/2, z.
 

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