Ytterbium hydrogendiphosphate trihydrate: synthesis and non-merohedral twinning

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

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

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Computing details

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

Crystal data

Yb(HO7P2^3^−)·3H2O	Z = 2
Mr = 402	F(000) = 370
Triclinic, P1	Dx = 3.197 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71069 Å
a = 6.3900 (6) Å	Cell parameters from 9895 reflections
b = 6.8324 (3) Å	θ = 3.0–26.6°
c = 9.8109 (8) Å	µ = 11.62 mm^−1
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) Å^3

Data collection

Oxford Diffraction CCD diffractometer	3288 independent reflections
Radiation source: X-ray tube	2824 reflections with I > 3σ(I)
Graphite monochromator	Rint = 0.036
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 = 0.176, Tmax = 0.576	l = −12→12
9895 measured reflections

Refinement

Refinement on F^2	5 constraints
R[F > 3σ(F)] = 0.026	H atoms treated by a mixture of independent and constrained refinement
wR(F) = 0.073	Weighting scheme based on measured s.u.'s w = 1/[σ^2(I) + 0.0016I^2]
S = 1.27	(Δ/σ)max = 0.038
3288 reflections	Δρmax = 0.79 e Å^−3
138 parameters	Δρmin = −0.63 e Å^−3
8 restraints

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Yb1	0.37153 (3)	0.25902 (3)	0.45353 (2)	0.00874 (7)
P1	−0.19429 (18)	0.23432 (17)	0.56243 (13)	0.0078 (3)
P2	0.05814 (19)	0.14260 (19)	0.78749 (13)	0.0119 (4)
O1	−0.3370 (5)	0.4158 (5)	0.5593 (4)	0.0148 (11)
O2	−0.3344 (5)	0.0723 (5)	0.5342 (4)	0.0143 (11)
O3	0.0686 (6)	−0.0761 (5)	0.8355 (4)	0.0178 (11)
O4	0.0154 (5)	0.2564 (5)	0.4669 (4)	0.0128 (10)
O5	0.2442 (5)	0.2339 (5)	0.6859 (4)	0.0168 (11)
O6	−0.1539 (5)	0.1804 (5)	0.7205 (4)	0.0186 (12)
O7	0.0141 (7)	0.2636 (6)	0.9120 (4)	0.0231 (13)
O8	0.6640 (6)	0.3595 (6)	0.2734 (4)	0.0201 (12)
O9	0.2880 (6)	0.2683 (7)	0.2310 (4)	0.0260 (13)
O10	0.4973 (19)	0.0944 (19)	0.0053 (13)	0.065 (3)	0.462 (8)
O11	0.5112 (16)	0.3377 (18)	−0.0425 (12)	0.065 (3)	0.538 (8)
H71	−0.011 (10)	0.206 (8)	0.992 (2)	0.0278*
H91	0.356 (7)	0.298 (9)	0.152 (2)	0.0312*
H92	0.169 (4)	0.231 (9)	0.225 (5)	0.0312*
H82	0.751 (5)	0.272 (5)	0.259 (7)	0.0241*
H81	0.726 (6)	0.463 (4)	0.273 (7)	0.0241*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00696 (12)	0.00699 (12)	0.01199 (13)	0.00014 (7)	−0.00078 (8)	−0.00143 (8)
P1	0.0057 (5)	0.0069 (6)	0.0117 (6)	0.0001 (4)	−0.0032 (5)	−0.0020 (5)
P2	0.0108 (6)	0.0151 (6)	0.0095 (6)	−0.0019 (5)	−0.0022 (5)	−0.0006 (5)
O1	0.0131 (16)	0.0058 (16)	0.026 (2)	0.0067 (13)	−0.0044 (15)	−0.0026 (15)
O2	0.0097 (16)	0.0063 (16)	0.028 (2)	−0.0038 (13)	−0.0074 (15)	0.0005 (15)
O3	0.0230 (19)	0.0149 (18)	0.0139 (19)	0.0015 (15)	−0.0009 (15)	0.0001 (15)
O4	0.0085 (16)	0.0165 (17)	0.0144 (18)	0.0000 (13)	−0.0037 (14)	−0.0032 (14)
O5	0.0115 (17)	0.029 (2)	0.0091 (18)	−0.0058 (15)	−0.0017 (14)	−0.0002 (15)
O6	0.0077 (16)	0.027 (2)	0.021 (2)	−0.0010 (15)	−0.0038 (15)	−0.0012 (16)
O7	0.035 (2)	0.022 (2)	0.0122 (19)	−0.0020 (17)	−0.0020 (18)	−0.0028 (16)
O8	0.0141 (17)	0.022 (2)	0.024 (2)	−0.0032 (15)	0.0025 (16)	−0.0068 (17)
O9	0.020 (2)	0.043 (2)	0.014 (2)	−0.0155 (18)	−0.0009 (16)	−0.0010 (19)
O10	0.042 (4)	0.107 (7)	0.041 (5)	0.003 (5)	0.008 (4)	−0.010 (5)
O11	0.042 (4)	0.107 (7)	0.041 (5)	0.003 (5)	0.008 (4)	−0.010 (5)

Geometric parameters (Å, º)

Yb1—O1^i	2.214 (3)	P2—O3	1.503 (4)
Yb1—O1^ii	2.607 (4)	P2—O5	1.500 (3)
Yb1—O2^ii	2.422 (3)	P2—O6	1.604 (4)
Yb1—O2^iii	2.267 (3)	P2—O7	1.555 (4)
Yb1—O4	2.257 (3)	O7—H71	0.82 (3)
Yb1—O5	2.268 (3)	O8—H82	0.82 (3)
Yb1—O8	2.381 (3)	O8—H81	0.82 (3)
Yb1—O9	2.327 (4)	O9—H91	0.82 (3)
P1—O1	1.518 (3)	O9—H92	0.82 (4)
P1—O2	1.528 (4)	O10—O10^iv	1.309 (19)
P1—O4	1.495 (3)	O10—O11	1.661 (18)
P1—O6	1.604 (4)
O1^ii—Yb1—O1^i	67.74 (12)	O4—Yb1—O5	75.95 (13)
O1^ii—Yb1—O2^ii	56.71 (11)	O4—Yb1—O8	134.83 (13)
O1^ii—Yb1—O2^iii	122.76 (12)	O4—Yb1—O9	70.25 (13)
O1^ii—Yb1—O4	140.48 (12)	O5—Yb1—O8	145.28 (14)
O1^ii—Yb1—O5	74.84 (12)	O5—Yb1—O9	146.11 (13)
O1^ii—Yb1—O8	70.50 (13)	O8—Yb1—O9	67.47 (14)
O1^ii—Yb1—O9	135.55 (12)	O1—P1—O2	103.64 (19)
O1^i—Yb1—O1^ii	67.74 (12)	O1—P1—O4	115.89 (19)
O1^i—Yb1—O2^ii	124.18 (13)	O1—P1—O6	106.4 (2)
O1^i—Yb1—O2^iii	168.23 (12)	O2—P1—O4	114.0 (2)
O1^i—Yb1—O4	85.54 (12)	O2—P1—O6	107.5 (2)
O1^i—Yb1—O5	88.53 (13)	O4—P1—O6	108.9 (2)
O1^i—Yb1—O8	80.23 (12)	O3—P2—O5	117.1 (2)
O1^i—Yb1—O9	91.25 (15)	O3—P2—O6	106.5 (2)
O2^ii—Yb1—O2^iii	66.98 (12)	O3—P2—O7	112.2 (2)
O2^ii—Yb1—O4	142.92 (11)	O5—P2—O6	109.6 (2)
O2^ii—Yb1—O5	82.65 (12)	O5—P2—O7	108.1 (2)
O2^ii—Yb1—O8	77.04 (12)	O6—P2—O7	102.3 (2)
O2^ii—Yb1—O9	124.08 (14)	P1—O6—P2	132.7 (2)
O2^iii—Yb1—O2^ii	66.98 (12)	P2—O7—H71	120 (4)
O2^iii—Yb1—O4	82.72 (12)	H82—O8—H81	109 (4)
O2^iii—Yb1—O5	89.46 (13)	H91—O9—H92	109 (5)
O2^iii—Yb1—O8	107.61 (13)	O10^iv—O10—O11	159.6 (12)
O2^iii—Yb1—O9	83.99 (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)

D—H···A	D—H	H···A	D···A	D—H···A
O7—H71···O3^v	0.82 (3)	1.78 (3)	2.593 (5)	179 (8)
O8—H82···O3^vi	0.82 (4)	1.97 (4)	2.755 (5)	161 (6)
O9—H91···O11	0.82 (3)	1.98 (3)	2.795 (12)	173 (6)
O9—H92···O3^iii	0.82 (3)	2.09 (4)	2.877 (6)	160 (6)
O9—H91···O10	0.82 (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.