The title compound, Y(HP
2O
7)·3H
2O, is isostructural with
Ln(HP
2O
7)·3H
2O (
Ln = Gd, Er). The YO
8 units and (HP
2O
7)
3− anions form sheets parallel to
ab and a network of O—H
O hydrogen bonds helps to establish the crystal packing.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (P-O) = 0.002 Å
- H-atom completeness 72%
- Disorder in main residue
- R factor = 0.021
- wR factor = 0.048
- Data-to-parameter ratio = 12.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
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 O10 P2 Y1
Atom count from the _atom_site data: H5 O10 P2 Y1
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 H7 O10 P2 Y1
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
H 14.00 10.00 4.00
O 20.00 20.00 0.00
P 4.00 4.00 0.00
Y 2.00 2.00 0.00
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
4 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
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, K. & Putz, 2005); software used to prepare material for publication: JANA2000.
yttrium hydrogendiphosphate trihydrate
top
Crystal data top
Y(HP2O7)·3H2O | Z = 2 |
Mr = 317.9 | F(000) = 308 |
Triclinic, P1 | Dx = 2.481 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 6.4297 (7) Å | Cell parameters from 5359 reflections |
b = 6.9042 (4) Å | θ = 3.2–26.6° |
c = 9.8272 (10) Å | µ = 7.26 mm−1 |
α = 81.612 (7)° | T = 294 K |
β = 80.306 (9)° | Blade, colourless |
γ = 88.413 (7)° | 0.19 × 0.08 × 0.02 mm |
V = 425.42 (7) Å3 | |
Data collection top
Oxford Diffraction CCD diffractometer | 1746 independent reflections |
Radiation source: X-ray tube | 1485 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.030 |
Detector resolution: 8.3438 pixels mm-1 | θmax = 26.6°, θmin = 3.2° |
rotation method data acquisition using ω scans | h = −8→7 |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2005) | k = −8→8 |
Tmin = 0.335, Tmax = 0.721 | l = −12→12 |
5359 measured reflections | |
Refinement top
Refinement on F2 | 5 constraints |
R[F > 3σ(F)] = 0.021 | H atoms treated by a mixture of independent and constrained refinement |
wR(F) = 0.048 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
S = 1.21 | (Δ/σ)max = 0.020 |
1746 reflections | Δρmax = 0.32 e Å−3 |
137 parameters | Δρmin = −0.38 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) |
Y1 | 0.37257 (4) | 0.26045 (4) | 0.45331 (3) | 0.00917 (9) | |
P1 | −0.19333 (11) | 0.23357 (10) | 0.56158 (8) | 0.0093 (2) | |
P2 | 0.05684 (11) | 0.14192 (11) | 0.78774 (8) | 0.0130 (2) | |
O1 | −0.3372 (3) | 0.4128 (3) | 0.5584 (2) | 0.0133 (6) | |
O2 | −0.3314 (3) | 0.0712 (3) | 0.5339 (2) | 0.0145 (7) | |
O3 | 0.0671 (3) | −0.0742 (3) | 0.8353 (2) | 0.0190 (7) | |
O4 | 0.0146 (3) | 0.2582 (3) | 0.4672 (2) | 0.0145 (6) | |
O5 | 0.2422 (3) | 0.2328 (3) | 0.6874 (2) | 0.0186 (7) | |
O6 | −0.1529 (3) | 0.1807 (3) | 0.7195 (2) | 0.0175 (7) | |
O7 | 0.0109 (4) | 0.2607 (3) | 0.9125 (2) | 0.0239 (7) | |
O8 | 0.6667 (3) | 0.3602 (3) | 0.2693 (2) | 0.0219 (7) | |
O9 | 0.2880 (3) | 0.2676 (4) | 0.2275 (2) | 0.0273 (8) | |
O10 | 0.4997 (11) | 0.1008 (12) | 0.0009 (7) | 0.0687 (19) | 0.427 (4) |
O11 | 0.5105 (8) | 0.3288 (10) | −0.0454 (5) | 0.0687 (19) | 0.573 (4) |
H71 | −0.008 (5) | 0.200 (4) | 0.9915 (15) | 0.0287* | |
H91 | 0.364 (3) | 0.267 (5) | 0.1520 (16) | 0.0327* | |
H92 | 0.170 (2) | 0.229 (5) | 0.223 (3) | 0.0327* | |
H81 | 0.732 (3) | 0.462 (2) | 0.262 (3) | 0.0263* | |
H82 | 0.748 (3) | 0.274 (3) | 0.244 (3) | 0.0263* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Y1 | 0.00798 (14) | 0.00697 (13) | 0.01242 (15) | −0.00029 (10) | −0.00163 (10) | −0.00099 (10) |
P1 | 0.0073 (3) | 0.0073 (3) | 0.0137 (4) | −0.0002 (3) | −0.0032 (3) | −0.0014 (3) |
P2 | 0.0122 (4) | 0.0159 (4) | 0.0109 (4) | −0.0016 (3) | −0.0030 (3) | −0.0003 (3) |
O1 | 0.0102 (10) | 0.0089 (10) | 0.0207 (11) | 0.0018 (8) | −0.0016 (8) | −0.0028 (8) |
O2 | 0.0123 (10) | 0.0081 (10) | 0.0250 (12) | −0.0007 (8) | −0.0080 (9) | −0.0035 (8) |
O3 | 0.0236 (12) | 0.0189 (11) | 0.0134 (11) | 0.0013 (9) | −0.0027 (9) | 0.0001 (9) |
O4 | 0.0085 (10) | 0.0207 (11) | 0.0145 (11) | 0.0001 (8) | −0.0025 (8) | −0.0024 (8) |
O5 | 0.0123 (10) | 0.0283 (12) | 0.0140 (11) | −0.0069 (9) | −0.0025 (8) | 0.0021 (9) |
O6 | 0.0101 (10) | 0.0274 (12) | 0.0137 (11) | −0.0010 (9) | −0.0029 (8) | 0.0025 (9) |
O7 | 0.0388 (13) | 0.0199 (12) | 0.0124 (11) | −0.0038 (10) | −0.0022 (10) | −0.0022 (9) |
O8 | 0.0162 (11) | 0.0238 (12) | 0.0247 (13) | −0.0034 (9) | 0.0019 (10) | −0.0051 (10) |
O9 | 0.0202 (12) | 0.0463 (15) | 0.0157 (12) | −0.0144 (11) | −0.0032 (9) | −0.0028 (11) |
O10 | 0.042 (2) | 0.121 (4) | 0.037 (3) | 0.003 (3) | 0.0030 (19) | −0.008 (3) |
O11 | 0.042 (2) | 0.121 (4) | 0.037 (3) | 0.003 (3) | 0.0030 (19) | −0.008 (3) |
Geometric parameters (Å, º) top
Y1—O1i | 2.2493 (19) | P2—O3 | 1.500 (2) |
Y1—O1ii | 2.594 (2) | P2—O5 | 1.5006 (19) |
Y1—O2ii | 2.4549 (19) | P2—O6 | 1.604 (2) |
Y1—O2iii | 2.2951 (19) | P2—O7 | 1.556 (2) |
Y1—O4 | 2.2827 (18) | O7—H71 | 0.818 (17) |
Y1—O5 | 2.2940 (19) | O8—H81 | 0.817 (18) |
Y1—O8 | 2.4245 (19) | O8—H82 | 0.82 (2) |
Y1—O9 | 2.366 (2) | O9—H91 | 0.817 (17) |
P1—O1 | 1.5241 (19) | O9—H92 | 0.818 (19) |
P1—O2 | 1.531 (2) | O10—O10iv | 1.395 (12) |
P1—O4 | 1.4921 (18) | O10—O11 | 1.573 (11) |
P1—O6 | 1.604 (2) | | |
| | | |
O1ii—Y1—O1i | 68.00 (6) | O4—Y1—O5 | 75.19 (7) |
O1ii—Y1—O2ii | 56.78 (6) | O4—Y1—O8 | 134.71 (7) |
O1ii—Y1—O2iii | 122.87 (6) | O4—Y1—O9 | 70.55 (7) |
O1ii—Y1—O4 | 140.61 (7) | O5—Y1—O8 | 146.41 (8) |
O1ii—Y1—O5 | 75.61 (7) | O5—Y1—O9 | 145.58 (7) |
O1ii—Y1—O8 | 70.84 (7) | O8—Y1—O9 | 67.09 (8) |
O1ii—Y1—O9 | 135.72 (7) | O1—P1—O2 | 103.80 (11) |
O1i—Y1—O1ii | 68.00 (6) | O1—P1—O4 | 115.73 (11) |
O1i—Y1—O2ii | 124.52 (7) | O1—P1—O6 | 106.23 (11) |
O1i—Y1—O2iii | 167.60 (7) | O2—P1—O4 | 114.54 (12) |
O1i—Y1—O4 | 85.39 (7) | O2—P1—O6 | 107.18 (11) |
O1i—Y1—O5 | 88.53 (7) | O4—P1—O6 | 108.75 (11) |
O1i—Y1—O8 | 80.81 (7) | O3—P2—O5 | 117.12 (12) |
O1i—Y1—O9 | 91.93 (8) | O3—P2—O6 | 106.80 (12) |
O2ii—Y1—O2iii | 67.10 (7) | O3—P2—O7 | 112.06 (12) |
O2ii—Y1—O4 | 142.75 (6) | O5—P2—O6 | 109.51 (11) |
O2ii—Y1—O5 | 83.24 (7) | O5—P2—O7 | 108.35 (13) |
O2ii—Y1—O8 | 77.06 (6) | O6—P2—O7 | 101.89 (12) |
O2ii—Y1—O9 | 123.33 (7) | P1—O6—P2 | 133.11 (12) |
O2iii—Y1—O2ii | 67.10 (7) | P2—O7—H71 | 118 (2) |
O2iii—Y1—O4 | 82.23 (7) | H81—O8—H82 | 109 (2) |
O2iii—Y1—O5 | 88.80 (7) | H91—O9—H92 | 109 (3) |
O2iii—Y1—O8 | 107.71 (7) | O10iv—O10—O11 | 162.9 (7) |
O2iii—Y1—O9 | 83.48 (8) | | |
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 | 0.818 (17) | 1.779 (17) | 2.596 (3) | 176 (3) |
O8—H82···O3vi | 0.82 (2) | 1.96 (2) | 2.775 (3) | 174 (3) |
O9—H91···O11 | 0.817 (17) | 2.000 (17) | 2.798 (5) | 165 (3) |
O9—H92···O3iii | 0.821 (17) | 2.09 (2) | 2.874 (3) | 160 (3) |
O9—H91···O10 | 0.817 (17) | 2.07 (3) | 2.789 (8) | 146 (3) |
Symmetry codes: (iii) −x, −y, −z+1; (v) −x, −y, −z+2; (vi) −x+1, −y, −z+1. |