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The title compound, Yb(HP2O7)·3H2O, is isostructural with the other triclinic modifications of this stoichiometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807008331/hb2297sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807008331/hb2297Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](P-O) = 0.004 Å
  • H-atom completeness 72%
  • Disorder in main residue
  • R factor = 0.026
  • wR factor = 0.073
  • Data-to-parameter ratio = 23.8

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 O1 has ADP max/min Ratio ............. 3.80 oblat 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 Yb1 Atom count from the _atom_site data: H5 O10 P2 Yb1 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 Yb1 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 Yb 2.00 2.00 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

Computing details top

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.

ytterbium hydrogendiphosphate trihydrate top
Crystal data top
Yb(HO7P23)·3H2OZ = 2
Mr = 402F(000) = 370
Triclinic, P1Dx = 3.197 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 6.3900 (6) ÅCell parameters from 9895 reflections
b = 6.8324 (3) Åθ = 3.0–26.6°
c = 9.8109 (8) ŵ = 11.62 mm1
α = 81.662 (6)°T = 294 K
β = 80.070 (7)°Prism, colorless
γ = 88.354 (5)°0.14 × 0.09 × 0.02 mm
V = 417.45 (6) Å3
Data collection top
Oxford Diffraction CCD
diffractometer
3288 independent reflections
Radiation source: X-ray tube2824 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.036
Detector resolution: 8.3438 pixels mm-1θmax = 26.6°, θmin = 3.0°
Rotation method data acquisition using ω scansh = 88
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2005)
k = 88
Tmin = 0.176, Tmax = 0.576l = 1212
9895 measured reflections
Refinement top
Refinement on F25 constraints
R[F > 3σ(F)] = 0.026H atoms treated by a mixture of independent and constrained refinement
wR(F) = 0.073Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0016I2]
S = 1.27(Δ/σ)max = 0.038
3288 reflectionsΔρmax = 0.79 e Å3
138 parametersΔρmin = 0.63 e Å3
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
xyzUiso*/UeqOcc. (<1)
Yb10.37153 (3)0.25902 (3)0.45353 (2)0.00874 (7)
P10.19429 (18)0.23432 (17)0.56243 (13)0.0078 (3)
P20.05814 (19)0.14260 (19)0.78749 (13)0.0119 (4)
O10.3370 (5)0.4158 (5)0.5593 (4)0.0148 (11)
O20.3344 (5)0.0723 (5)0.5342 (4)0.0143 (11)
O30.0686 (6)0.0761 (5)0.8355 (4)0.0178 (11)
O40.0154 (5)0.2564 (5)0.4669 (4)0.0128 (10)
O50.2442 (5)0.2339 (5)0.6859 (4)0.0168 (11)
O60.1539 (5)0.1804 (5)0.7205 (4)0.0186 (12)
O70.0141 (7)0.2636 (6)0.9120 (4)0.0231 (13)
O80.6640 (6)0.3595 (6)0.2734 (4)0.0201 (12)
O90.2880 (6)0.2683 (7)0.2310 (4)0.0260 (13)
O100.4973 (19)0.0944 (19)0.0053 (13)0.065 (3)0.462 (8)
O110.5112 (16)0.3377 (18)0.0425 (12)0.065 (3)0.538 (8)
H710.011 (10)0.206 (8)0.992 (2)0.0278*
H910.356 (7)0.298 (9)0.152 (2)0.0312*
H920.169 (4)0.231 (9)0.225 (5)0.0312*
H820.751 (5)0.272 (5)0.259 (7)0.0241*
H810.726 (6)0.463 (4)0.273 (7)0.0241*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Yb10.00696 (12)0.00699 (12)0.01199 (13)0.00014 (7)0.00078 (8)0.00143 (8)
P10.0057 (5)0.0069 (6)0.0117 (6)0.0001 (4)0.0032 (5)0.0020 (5)
P20.0108 (6)0.0151 (6)0.0095 (6)0.0019 (5)0.0022 (5)0.0006 (5)
O10.0131 (16)0.0058 (16)0.026 (2)0.0067 (13)0.0044 (15)0.0026 (15)
O20.0097 (16)0.0063 (16)0.028 (2)0.0038 (13)0.0074 (15)0.0005 (15)
O30.0230 (19)0.0149 (18)0.0139 (19)0.0015 (15)0.0009 (15)0.0001 (15)
O40.0085 (16)0.0165 (17)0.0144 (18)0.0000 (13)0.0037 (14)0.0032 (14)
O50.0115 (17)0.029 (2)0.0091 (18)0.0058 (15)0.0017 (14)0.0002 (15)
O60.0077 (16)0.027 (2)0.021 (2)0.0010 (15)0.0038 (15)0.0012 (16)
O70.035 (2)0.022 (2)0.0122 (19)0.0020 (17)0.0020 (18)0.0028 (16)
O80.0141 (17)0.022 (2)0.024 (2)0.0032 (15)0.0025 (16)0.0068 (17)
O90.020 (2)0.043 (2)0.014 (2)0.0155 (18)0.0009 (16)0.0010 (19)
O100.042 (4)0.107 (7)0.041 (5)0.003 (5)0.008 (4)0.010 (5)
O110.042 (4)0.107 (7)0.041 (5)0.003 (5)0.008 (4)0.010 (5)
Geometric parameters (Å, º) top
Yb1—O1i2.214 (3)P2—O31.503 (4)
Yb1—O1ii2.607 (4)P2—O51.500 (3)
Yb1—O2ii2.422 (3)P2—O61.604 (4)
Yb1—O2iii2.267 (3)P2—O71.555 (4)
Yb1—O42.257 (3)O7—H710.82 (3)
Yb1—O52.268 (3)O8—H820.82 (3)
Yb1—O82.381 (3)O8—H810.82 (3)
Yb1—O92.327 (4)O9—H910.82 (3)
P1—O11.518 (3)O9—H920.82 (4)
P1—O21.528 (4)O10—O10iv1.309 (19)
P1—O41.495 (3)O10—O111.661 (18)
P1—O61.604 (4)
O1ii—Yb1—O1i67.74 (12)O4—Yb1—O575.95 (13)
O1ii—Yb1—O2ii56.71 (11)O4—Yb1—O8134.83 (13)
O1ii—Yb1—O2iii122.76 (12)O4—Yb1—O970.25 (13)
O1ii—Yb1—O4140.48 (12)O5—Yb1—O8145.28 (14)
O1ii—Yb1—O574.84 (12)O5—Yb1—O9146.11 (13)
O1ii—Yb1—O870.50 (13)O8—Yb1—O967.47 (14)
O1ii—Yb1—O9135.55 (12)O1—P1—O2103.64 (19)
O1i—Yb1—O1ii67.74 (12)O1—P1—O4115.89 (19)
O1i—Yb1—O2ii124.18 (13)O1—P1—O6106.4 (2)
O1i—Yb1—O2iii168.23 (12)O2—P1—O4114.0 (2)
O1i—Yb1—O485.54 (12)O2—P1—O6107.5 (2)
O1i—Yb1—O588.53 (13)O4—P1—O6108.9 (2)
O1i—Yb1—O880.23 (12)O3—P2—O5117.1 (2)
O1i—Yb1—O991.25 (15)O3—P2—O6106.5 (2)
O2ii—Yb1—O2iii66.98 (12)O3—P2—O7112.2 (2)
O2ii—Yb1—O4142.92 (11)O5—P2—O6109.6 (2)
O2ii—Yb1—O582.65 (12)O5—P2—O7108.1 (2)
O2ii—Yb1—O877.04 (12)O6—P2—O7102.3 (2)
O2ii—Yb1—O9124.08 (14)P1—O6—P2132.7 (2)
O2iii—Yb1—O2ii66.98 (12)P2—O7—H71120 (4)
O2iii—Yb1—O482.72 (12)H82—O8—H81109 (4)
O2iii—Yb1—O589.46 (13)H91—O9—H92109 (5)
O2iii—Yb1—O8107.61 (13)O10iv—O10—O11159.6 (12)
O2iii—Yb1—O983.99 (15)
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···AD—HH···AD···AD—H···A
O7—H71···O3v0.82 (3)1.78 (3)2.593 (5)179 (8)
O8—H82···O3vi0.82 (4)1.97 (4)2.755 (5)161 (6)
O9—H91···O110.82 (3)1.98 (3)2.795 (12)173 (6)
O9—H92···O3iii0.82 (3)2.09 (4)2.877 (6)160 (6)
O9—H91···O100.82 (3)2.21 (5)2.785 (14)128 (5)
Symmetry codes: (iii) x, y, z+1; (v) x, y, z+2; (vi) x+1, y, z+1.
 

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