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
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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
DyP5O14 | F(000) = 2024 |
Mr = 541.35 | Dx = 3.510 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1946 reflections |
a = 12.8934 (6) Å | θ = 2.9–26.9° |
b = 12.7756 (5) Å | µ = 8.16 mm−1 |
c = 12.4415 (5) Å | T = 298 K |
β = 91.313 (3)° | Cubic, colourless |
V = 2048.84 (15) Å3 | 0.15 × 0.15 × 0.15 mm |
Z = 8 | |
Data collection top
Nonius KappaCCD area-detector diffractometer | 2290 independent reflections |
Radiation source: fine-focus sealed tube | 1682 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.000 |
Detector resolution: 9 pixels mm-1 | θmax = 26.8°, θmin = 3.9° |
ω/2θ scans | h = −16→16 |
Absorption correction: part of the refinement model (ΔF) (Parkin et al., 1995) | k = 0→16 |
Tmin = 0.286, Tmax = 0.306 | l = 0→16 |
3807 measured reflections | |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.028 | Secondary 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 reflections | Δρmax = 1.65 e Å−3 |
182 parameters | Δρmin = −1.27 e Å−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 | x | y | z | Uiso*/Ueq | |
Dy1 | 1.0000 | 0.52187 (2) | 0.2500 | 0.00472 (10) | |
Dy2 | 1.0000 | −0.03118 (2) | 0.2500 | 0.00456 (10) | |
P1 | 1.02500 (9) | 0.15233 (9) | 0.03255 (11) | 0.0054 (3) | |
P2 | 1.18169 (9) | 0.13795 (9) | 0.39145 (12) | 0.0055 (3) | |
P3 | 1.14714 (9) | 0.46602 (9) | 0.49867 (12) | 0.0064 (3) | |
P4 | 1.14896 (9) | 0.33223 (9) | 0.10313 (11) | 0.0059 (3) | |
P5 | 1.32072 (9) | 0.25021 (9) | 0.24096 (11) | 0.0055 (3) | |
O1 | 1.0257 (2) | 0.1032 (3) | −0.0736 (3) | 0.0123 (8) | |
O2 | 1.0607 (2) | 0.0973 (3) | 0.1306 (3) | 0.0105 (8) | |
O3 | 1.0865 (2) | 0.2617 (2) | 0.0210 (3) | 0.0085 (8) | |
O4 | 1.0914 (2) | 0.1981 (2) | 0.4457 (3) | 0.0095 (8) | |
O5 | 1.1526 (2) | 0.0497 (3) | 0.3226 (3) | 0.0119 (8) | |
O6 | 1.2398 (3) | 0.2283 (2) | 0.3355 (3) | 0.0118 (8) | |
O7 | 1.2490 (2) | 0.1041 (3) | 0.4914 (3) | 0.0083 (7) | |
O8 | 1.1159 (3) | 0.4636 (2) | 0.3857 (3) | 0.0104 (8) | |
O9 | 1.0768 (2) | 0.4342 (3) | 0.5843 (3) | 0.0133 (8) | |
O10 | 1.1946 (2) | 0.4182 (2) | 0.0282 (3) | 0.0078 (7) | |
O11 | 1.0896 (3) | 0.3714 (3) | 0.1921 (3) | 0.0134 (8) | |
O12 | 1.2437 (2) | 0.2633 (2) | 0.1365 (3) | 0.0090 (8) | |
O13 | 1.3680 (2) | 0.3509 (3) | 0.2684 (3) | 0.0125 (8) | |
O14 | 1.3833 (3) | 0.1578 (3) | 0.2183 (3) | 0.0154 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Dy1 | 0.00347 (16) | 0.00437 (16) | 0.0063 (2) | 0.000 | 0.00080 (13) | 0.000 |
Dy2 | 0.00375 (16) | 0.00378 (16) | 0.0062 (2) | 0.000 | 0.00043 (13) | 0.000 |
P1 | 0.0032 (5) | 0.0054 (5) | 0.0077 (8) | −0.0009 (5) | 0.0006 (5) | −0.0004 (5) |
P2 | 0.0042 (6) | 0.0046 (5) | 0.0076 (8) | 0.0005 (5) | 0.0009 (5) | 0.0003 (5) |
P3 | 0.0055 (6) | 0.0049 (5) | 0.0087 (8) | 0.0014 (5) | −0.0002 (5) | −0.0015 (5) |
P4 | 0.0055 (6) | 0.0039 (5) | 0.0082 (8) | 0.0006 (5) | 0.0009 (5) | −0.0004 (5) |
P5 | 0.0037 (5) | 0.0054 (5) | 0.0075 (8) | −0.0009 (5) | 0.0016 (5) | 0.0017 (5) |
O1 | 0.0150 (18) | 0.0144 (17) | 0.008 (2) | −0.0024 (16) | 0.0013 (15) | −0.0023 (15) |
O2 | 0.0095 (17) | 0.0105 (16) | 0.011 (2) | −0.0003 (15) | −0.0030 (15) | 0.0036 (15) |
O3 | 0.0076 (16) | 0.0080 (16) | 0.010 (2) | −0.0024 (14) | 0.0012 (14) | −0.0003 (14) |
O4 | 0.0038 (16) | 0.0077 (16) | 0.017 (2) | −0.0009 (14) | 0.0056 (15) | −0.0016 (15) |
O5 | 0.0077 (16) | 0.0125 (16) | 0.016 (2) | 0.0004 (15) | 0.0035 (15) | −0.0035 (15) |
O6 | 0.0132 (18) | 0.0079 (16) | 0.015 (2) | −0.0049 (15) | 0.0080 (16) | −0.0004 (15) |
O7 | 0.0103 (16) | 0.0083 (16) | 0.006 (2) | 0.0054 (14) | −0.0037 (14) | −0.0027 (14) |
O8 | 0.0120 (17) | 0.0135 (16) | 0.006 (2) | 0.0066 (15) | −0.0052 (15) | −0.0026 (14) |
O9 | 0.0151 (17) | 0.0096 (16) | 0.015 (2) | −0.0030 (16) | 0.0059 (16) | −0.0005 (16) |
O10 | 0.0077 (16) | 0.0049 (15) | 0.011 (2) | −0.0024 (14) | 0.0032 (14) | 0.0011 (14) |
O11 | 0.0133 (17) | 0.0093 (17) | 0.018 (2) | 0.0082 (15) | 0.0033 (16) | 0.0025 (15) |
O12 | 0.0046 (16) | 0.0127 (17) | 0.010 (2) | 0.0046 (14) | 0.0024 (14) | −0.0017 (14) |
O13 | 0.0115 (17) | 0.0111 (16) | 0.015 (2) | −0.0064 (15) | 0.0006 (16) | 0.0026 (15) |
O14 | 0.0143 (18) | 0.0171 (18) | 0.015 (2) | 0.0047 (16) | 0.0022 (16) | 0.0038 (16) |
Geometric parameters (Å, º) top
Dy1—O14i | 2.326 (3) | P2—O7 | 1.561 (4) |
Dy1—O14ii | 2.326 (3) | P2—O4 | 1.562 (3) |
Dy1—O8iii | 2.350 (3) | P3—O8 | 1.454 (4) |
Dy1—O8 | 2.350 (3) | P3—O9 | 1.472 (4) |
Dy1—O11iii | 2.364 (3) | P3—O7x | 1.614 (3) |
Dy1—O11 | 2.364 (3) | P3—O10xi | 1.640 (3) |
Dy1—O9iv | 2.375 (4) | P4—O11 | 1.450 (4) |
Dy1—O9v | 2.375 (4) | P4—O12 | 1.554 (3) |
Dy2—O13vi | 2.288 (3) | P4—O10 | 1.564 (3) |
Dy2—O13vii | 2.288 (3) | P4—O3 | 1.570 (4) |
Dy2—O2iii | 2.359 (3) | P5—O13 | 1.460 (3) |
Dy2—O2 | 2.359 (3) | P5—O14 | 1.461 (4) |
Dy2—O5 | 2.382 (3) | P5—O6 | 1.615 (4) |
Dy2—O5iii | 2.382 (3) | P5—O12 | 1.626 (4) |
Dy2—O1viii | 2.396 (4) | O1—Dy2ix | 2.396 (4) |
Dy2—O1ix | 2.396 (4) | O4—P1iii | 1.638 (3) |
P1—O1 | 1.462 (4) | O7—P3x | 1.614 (3) |
P1—O2 | 1.473 (4) | O9—Dy1iv | 2.375 (4) |
P1—O3 | 1.615 (3) | O10—P3v | 1.640 (3) |
P1—O4iii | 1.638 (3) | O13—Dy2xii | 2.288 (3) |
P2—O5 | 1.459 (4) | O14—Dy1xiii | 2.326 (3) |
P2—O6 | 1.550 (4) | | |
| | | |
O14i—Dy1—O14ii | 83.40 (17) | O13vii—Dy2—O1ix | 75.10 (12) |
O14i—Dy1—O8iii | 139.20 (13) | O2iii—Dy2—O1ix | 143.43 (11) |
O14ii—Dy1—O8iii | 73.51 (12) | O2—Dy2—O1ix | 74.42 (12) |
O14i—Dy1—O8 | 73.51 (12) | O5—Dy2—O1ix | 127.57 (12) |
O14ii—Dy1—O8 | 139.20 (13) | O5iii—Dy2—O1ix | 73.96 (12) |
O8iii—Dy1—O8 | 143.05 (15) | O1viii—Dy2—O1ix | 134.80 (16) |
O14i—Dy1—O11iii | 150.97 (13) | O1—P1—O2 | 122.3 (2) |
O14ii—Dy1—O11iii | 109.89 (12) | O1—P1—O3 | 106.1 (2) |
O8iii—Dy1—O11iii | 69.76 (12) | O2—P1—O3 | 110.0 (2) |
O8—Dy1—O11iii | 80.24 (12) | O1—P1—O4iii | 109.1 (2) |
O14i—Dy1—O11 | 109.89 (12) | O2—P1—O4iii | 107.7 (2) |
O14ii—Dy1—O11 | 150.97 (13) | O3—P1—O4iii | 99.15 (17) |
O8iii—Dy1—O11 | 80.24 (12) | O5—P2—O6 | 115.6 (2) |
O8—Dy1—O11 | 69.76 (12) | O5—P2—O7 | 112.6 (2) |
O11iii—Dy1—O11 | 71.14 (17) | O6—P2—O7 | 107.35 (19) |
O14i—Dy1—O9iv | 87.55 (12) | O5—P2—O4 | 116.74 (18) |
O14ii—Dy1—O9iv | 71.94 (13) | O6—P2—O4 | 101.58 (18) |
O8iii—Dy1—O9iv | 115.31 (12) | O7—P2—O4 | 101.4 (2) |
O8—Dy1—O9iv | 73.87 (12) | O8—P3—O9 | 122.2 (2) |
O11iii—Dy1—O9iv | 73.22 (12) | O8—P3—O7x | 105.87 (19) |
O11—Dy1—O9iv | 132.30 (12) | O9—P3—O7x | 108.4 (2) |
O14i—Dy1—O9v | 71.94 (13) | O8—P3—O10xi | 109.2 (2) |
O14ii—Dy1—O9v | 87.55 (12) | O9—P3—O10xi | 108.6 (2) |
O8iii—Dy1—O9v | 73.87 (12) | O7x—P3—O10xi | 100.33 (17) |
O8—Dy1—O9v | 115.31 (12) | O11—P4—O12 | 114.7 (2) |
O11iii—Dy1—O9v | 132.30 (12) | O11—P4—O10 | 115.18 (19) |
O11—Dy1—O9v | 73.22 (12) | O12—P4—O10 | 104.65 (18) |
O9iv—Dy1—O9v | 152.68 (16) | O11—P4—O3 | 115.0 (2) |
O13vi—Dy2—O13vii | 97.64 (17) | O12—P4—O3 | 103.71 (18) |
O13vi—Dy2—O2iii | 97.86 (12) | O10—P4—O3 | 102.1 (2) |
O13vii—Dy2—O2iii | 141.19 (12) | O13—P5—O14 | 121.8 (2) |
O13vi—Dy2—O2 | 141.19 (12) | O13—P5—O6 | 104.8 (2) |
O13vii—Dy2—O2 | 97.86 (12) | O14—P5—O6 | 111.7 (2) |
O2iii—Dy2—O2 | 91.85 (17) | O13—P5—O12 | 109.89 (19) |
O13vi—Dy2—O5 | 149.04 (13) | O14—P5—O12 | 105.0 (2) |
O13vii—Dy2—O5 | 73.38 (11) | O6—P5—O12 | 101.96 (18) |
O2iii—Dy2—O5 | 75.08 (11) | P1—O1—Dy2ix | 171.3 (2) |
O2—Dy2—O5 | 69.75 (12) | P1—O2—Dy2 | 138.75 (19) |
O13vi—Dy2—O5iii | 73.38 (11) | P4—O3—P1 | 133.2 (3) |
O13vii—Dy2—O5iii | 149.04 (13) | P2—O4—P1iii | 126.2 (2) |
O2iii—Dy2—O5iii | 69.75 (12) | P2—O5—Dy2 | 139.2 (2) |
O2—Dy2—O5iii | 75.08 (11) | P2—O6—P5 | 141.6 (2) |
O5—Dy2—O5iii | 128.56 (17) | P2—O7—P3x | 131.3 (2) |
O13vi—Dy2—O1viii | 75.10 (12) | P3—O8—Dy1 | 147.7 (2) |
O13vii—Dy2—O1viii | 75.58 (12) | P3—O9—Dy1iv | 147.1 (2) |
O2iii—Dy2—O1viii | 74.42 (12) | P4—O10—P3v | 128.6 (2) |
O2—Dy2—O1viii | 143.43 (11) | P4—O11—Dy1 | 141.6 (2) |
O5—Dy2—O1viii | 73.96 (12) | P4—O12—P5 | 137.2 (2) |
O5iii—Dy2—O1viii | 127.57 (12) | P5—O13—Dy2xii | 149.8 (2) |
O13vi—Dy2—O1ix | 75.58 (12) | P5—O14—Dy1xiii | 158.2 (3) |
Symmetry codes: (i) −x+5/2, y+1/2, −z+1/2; (ii) x−1/2, y+1/2, z; (iii) −x+2, y, −z+1/2; (iv) −x+2, −y+1, −z+1; (v) x, −y+1, z−1/2; (vi) x−1/2, y−1/2, z; (vii) −x+5/2, y−1/2, −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, y−1/2, z. |