The title compound, Dy(HP2O7)·3H2O, is isostructural with other members of the triclinic Ln(HP2O7)·3H2O (Ln = rare earth) family.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (P-O) = 0.004 Å
- H-atom completeness 72%
- Disorder in main residue
- R factor = 0.027
- wR factor = 0.068
- Data-to-parameter ratio = 24.3
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT021_ALERT_1_B Ratio Unique / Expected Reflections too High ... 1.90
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT213_ALERT_2_C Atom O2 has ADP max/min Ratio ............. 4.00 prola
PLAT301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O11
Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:H7 Dy1 O10 P2
Atom count from the _atom_site data: H5 Dy1 O10 P2
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 2
From the CIF: _chemical_formula_sum Dy1 H7 O10 P2
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
Dy 2.00 2.00 0.00
H 14.00 10.00 4.00
O 20.00 20.00 0.00
P 4.00 4.00 0.00
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
5 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
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduction: CrysAlis RED; program(s) used to solve structure: SIR2002 (Burla et al., 2003); program(s) used to refine structure: JANA2000 (Petricek et al., 2000); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: JANA2000.
dysprosium hydrogendiphosphate trihydrate
top
Crystal data top
Dy(HO7P2)·3H2O | Z = 2 |
Mr = 391.5 | F(000) = 362 |
Triclinic, P1 | Dx = 3.044 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 6.4371 (3) Å | Cell parameters from 10749 reflections |
b = 6.9284 (5) Å | θ = 3.0–26.6° |
c = 9.8164 (7) Å | µ = 9.16 mm−1 |
α = 81.593 (6)° | T = 294 K |
β = 80.377 (5)° | Plate, colorless |
γ = 88.368 (5)° | 0.07 × 0.05 × 0.01 mm |
V = 427.00 (5) Å3 | |
Data collection top
Oxford Diffraction CCD diffractometer | 3357 independent reflections |
Radiation source: X-ray tube | 2842 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.050 |
Detector resolution: 8.3438 pixels mm-1 | θmax = 26.6°, θmin = 3.0° |
Rotation method data acquisition using ω scans | h = −8→8 |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2005) | k = −8→8 |
Tmin = 0.438, Tmax = 0.691 | l = −12→12 |
10749 measured reflections | |
Refinement top
Refinement on F2 | 5 constraints |
R[F > 3σ(F)] = 0.027 | H atoms treated by a mixture of independent and constrained refinement |
wR(F) = 0.068 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0016I2] |
S = 1.09 | (Δ/σ)max = 0.009 |
3357 reflections | Δρmax = 0.63 e Å−3 |
138 parameters | Δρmin = −0.63 e Å−3 |
8 restraints | |
Special details top
Refinement. The refinement was carried out against all reflections. The conventional
R-factor is always based on F. The goodness of fit as well as
the weighted R-factor are based on F and F2 for
refinement carried out on F and F2, respectively. The
threshold expression is used only for calculating R-factors etc.
and it is not relevant to the choice of reflections for refinement. The program used for refinement, Jana2000, uses the weighting scheme based on
the experimental expectations, see _refine_ls_weighting_details, that does not
force S to be one. Therefore the values of S are usually larger
then the ones from the SHELX program. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Dy1 | 0.37284 (3) | 0.26096 (3) | 0.45268 (2) | 0.00921 (7) | |
P1 | −0.19330 (16) | 0.23307 (15) | 0.56100 (12) | 0.0084 (3) | |
P2 | 0.05652 (18) | 0.14188 (17) | 0.78811 (12) | 0.0132 (3) | |
O1 | −0.3361 (5) | 0.4106 (4) | 0.5584 (3) | 0.0147 (10) | |
O2 | −0.3286 (5) | 0.0722 (4) | 0.5327 (4) | 0.0155 (10) | |
O3 | 0.0681 (5) | −0.0737 (5) | 0.8355 (3) | 0.0201 (11) | |
O4 | 0.0141 (5) | 0.2585 (5) | 0.4663 (3) | 0.0149 (10) | |
O5 | 0.2414 (5) | 0.2330 (5) | 0.6886 (3) | 0.0185 (11) | |
O6 | −0.1523 (5) | 0.1807 (5) | 0.7182 (4) | 0.0192 (11) | |
O7 | 0.0099 (6) | 0.2598 (5) | 0.9125 (4) | 0.0250 (12) | |
O8 | 0.6683 (5) | 0.3610 (5) | 0.2673 (4) | 0.0220 (11) | |
O9 | 0.2877 (6) | 0.2687 (6) | 0.2262 (4) | 0.0282 (13) | |
O10 | 0.4985 (19) | 0.099 (2) | 0.0015 (13) | 0.072 (3) | 0.424 (7) |
O11 | 0.5101 (14) | 0.3274 (17) | −0.0449 (10) | 0.072 (3) | 0.576 (7) |
H71 | −0.015 (9) | 0.208 (8) | 0.994 (2) | 0.03* | |
H81 | 0.721 (6) | 0.464 (4) | 0.276 (6) | 0.0264* | |
H82 | 0.761 (5) | 0.279 (5) | 0.257 (6) | 0.0264* | |
H91 | 0.362 (6) | 0.255 (8) | 0.153 (3) | 0.0339* | |
H92 | 0.167 (3) | 0.239 (8) | 0.223 (5) | 0.0339* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Dy1 | 0.00649 (11) | 0.00744 (11) | 0.01406 (12) | −0.00012 (7) | −0.00178 (8) | −0.00254 (7) |
P1 | 0.0047 (5) | 0.0069 (5) | 0.0144 (6) | 0.0002 (4) | −0.0030 (4) | −0.0026 (4) |
P2 | 0.0113 (6) | 0.0165 (6) | 0.0116 (6) | −0.0024 (5) | −0.0020 (5) | −0.0010 (5) |
O1 | 0.0132 (15) | 0.0061 (15) | 0.0251 (18) | 0.0031 (12) | −0.0050 (14) | −0.0020 (13) |
O2 | 0.0106 (15) | 0.0068 (15) | 0.0310 (19) | −0.0050 (12) | −0.0106 (14) | 0.0004 (13) |
O3 | 0.0246 (19) | 0.0187 (17) | 0.0159 (17) | 0.0019 (14) | −0.0002 (14) | −0.0021 (14) |
O4 | 0.0093 (15) | 0.0190 (17) | 0.0169 (16) | 0.0013 (12) | −0.0032 (13) | −0.0037 (13) |
O5 | 0.0110 (16) | 0.0287 (19) | 0.0160 (17) | −0.0062 (14) | −0.0045 (13) | 0.0005 (14) |
O6 | 0.0109 (16) | 0.0258 (19) | 0.0216 (18) | −0.0007 (14) | −0.0062 (14) | −0.0023 (15) |
O7 | 0.041 (2) | 0.0208 (19) | 0.0139 (17) | −0.0014 (16) | −0.0048 (17) | −0.0028 (15) |
O8 | 0.0150 (17) | 0.0233 (19) | 0.0283 (19) | −0.0019 (14) | −0.0007 (15) | −0.0089 (16) |
O9 | 0.0207 (19) | 0.048 (2) | 0.0163 (18) | −0.0134 (18) | −0.0013 (15) | −0.0051 (17) |
O10 | 0.040 (4) | 0.127 (7) | 0.046 (4) | 0.005 (5) | 0.006 (3) | −0.016 (5) |
O11 | 0.040 (4) | 0.127 (7) | 0.046 (4) | 0.005 (5) | 0.006 (3) | −0.016 (5) |
Geometric parameters (Å, º) top
Dy1—O1i | 2.269 (3) | P2—O3 | 1.501 (3) |
Dy1—O1ii | 2.596 (3) | P2—O5 | 1.498 (3) |
Dy1—O2ii | 2.466 (3) | P2—O6 | 1.608 (4) |
Dy1—O2iii | 2.314 (3) | P2—O7 | 1.550 (4) |
Dy1—O4 | 2.291 (3) | O7—H71 | 0.82 (2) |
Dy1—O5 | 2.311 (3) | O8—H81 | 0.82 (3) |
Dy1—O8 | 2.441 (3) | O8—H82 | 0.81 (3) |
Dy1—O9 | 2.370 (4) | O9—H91 | 0.81 (3) |
P1—O1 | 1.514 (3) | O9—H92 | 0.82 (3) |
P1—O2 | 1.518 (3) | O10—O10iv | 1.38 (2) |
P1—O4 | 1.493 (3) | O10—O11 | 1.581 (18) |
P1—O6 | 1.596 (4) | | |
| | | |
O1ii—Dy1—O1i | 68.38 (11) | O2iii—Dy1—O9 | 83.80 (13) |
O1ii—Dy1—O2ii | 56.36 (10) | O4—Dy1—O5 | 75.14 (12) |
O1ii—Dy1—O2iii | 122.67 (10) | O4—Dy1—O8 | 134.66 (12) |
O1ii—Dy1—O4 | 140.90 (11) | O4—Dy1—O9 | 70.46 (12) |
O1ii—Dy1—O5 | 75.70 (11) | O5—Dy1—O8 | 146.53 (13) |
O1ii—Dy1—O8 | 70.86 (11) | O5—Dy1—O9 | 145.44 (12) |
O1ii—Dy1—O9 | 135.81 (11) | O8—Dy1—O9 | 67.08 (13) |
O1i—Dy1—O1ii | 68.38 (11) | O1—P1—O2 | 104.23 (18) |
O1i—Dy1—O2ii | 124.46 (11) | O1—P1—O4 | 115.54 (17) |
O1i—Dy1—O2iii | 167.05 (11) | O1—P1—O6 | 106.05 (19) |
O1i—Dy1—O4 | 85.30 (11) | O2—P1—O4 | 114.22 (19) |
O1i—Dy1—O5 | 88.35 (12) | O2—P1—O6 | 107.45 (18) |
O1i—Dy1—O8 | 81.03 (11) | O4—P1—O6 | 108.77 (18) |
O1i—Dy1—O9 | 91.96 (13) | O3—P2—O5 | 117.01 (19) |
O2ii—Dy1—O2iii | 67.50 (11) | O3—P2—O6 | 107.1 (2) |
O2ii—Dy1—O4 | 143.02 (10) | O3—P2—O7 | 112.20 (19) |
O2ii—Dy1—O5 | 83.61 (11) | O5—P2—O6 | 109.23 (18) |
O2ii—Dy1—O8 | 76.74 (11) | O5—P2—O7 | 108.2 (2) |
O2ii—Dy1—O9 | 123.20 (12) | O6—P2—O7 | 102.1 (2) |
O2iii—Dy1—O2ii | 67.50 (11) | P2—O7—H71 | 123 (4) |
O2iii—Dy1—O4 | 81.75 (11) | H81—O8—H82 | 109 (4) |
O2iii—Dy1—O5 | 88.26 (12) | H91—O9—H92 | 109 (5) |
O2iii—Dy1—O8 | 108.29 (11) | O10iv—O10—O11 | 162.5 (12) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x+1, y, z; (iii) −x, −y, −z+1; (iv) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H71···O3v | 0.82 (2) | 1.78 (3) | 2.593 (5) | 175 (6) |
O8—H82···O3vi | 0.82 (3) | 2.00 (4) | 2.772 (5) | 157 (5) |
O9—H91···O11 | 0.81 (3) | 2.01 (3) | 2.782 (10) | 158 (5) |
O9—H92···O3iii | 0.82 (2) | 2.12 (4) | 2.884 (5) | 155 (5) |
O9—H91···O10 | 0.81 (3) | 2.03 (5) | 2.785 (14) | 154 (5) |
Symmetry codes: (iii) −x, −y, −z+1; (v) −x, −y, −z+2; (vi) −x+1, −y, −z+1. |