The title compound, Tb(HP2O7)·3H2O, is isostructural with Y(HP2O7)·3H2O and Gd(HP2O7)·3H2O. The crystal studied exhibited non-merohedral twinning.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (P-O) = 0.003 Å
- H-atom completeness 72%
- Disorder in main residue
- R factor = 0.026
- wR factor = 0.056
- Data-to-parameter ratio = 23.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT021_ALERT_1_B Ratio Unique / Expected Reflections too High ... 1.89
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 600 Deg.
PLAT213_ALERT_2_C Atom O1 has ADP max/min Ratio ............. 3.50 oblat
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.56 Ratio
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 Tb1
Atom count from the _atom_site data: H5 O10 P2 Tb1
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 Tb1
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
Tb 2.00 2.00 0.00
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
4 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.
terbium hydrogendiphosphate trihydrate
top
Crystal data top
Tb(HP2O7)·3H2O | Z = 2 |
Mr = 387.9 | F(000) = 360 |
Triclinic, P1 | Dx = 2.991 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 6.4551 (5) Å | Cell parameters from 10460 reflections |
b = 6.9597 (4) Å | θ = 3.2–26.6° |
c = 9.8253 (7) Å | µ = 8.61 mm−1 |
α = 81.621 (6)° | T = 294 K |
β = 80.464 (6)° | Prism, colorless |
γ = 88.341 (6)° | 0.08 × 0.05 × 0.02 mm |
V = 430.66 (5) Å3 | |
Data collection top
Oxford Diffraction CCD diffractometer | 3399 independent reflections |
Radiation source: X-ray tube | 2737 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.049 |
Detector resolution: 8.3438 pixels mm-1 | θmax = 26.6°, θmin = 3.2° |
Rotation method data acquisition using ω scans | h = −8→8 |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2005) | k = −8→8 |
Tmin = 0.419, Tmax = 0.659 | l = −12→12 |
10460 measured reflections | |
Refinement top
Refinement on F2 | 5 constraints |
R[F > 3σ(F)] = 0.026 | H atoms treated by a mixture of independent and constrained refinement |
wR(F) = 0.056 | Weighting scheme based on measured s.u.'s w = 1/[σ2(I) + 0.0004I2] |
S = 1.13 | (Δ/σ)max = 0.019 |
3399 reflections | Δρmax = 0.97 e Å−3 |
144 parameters | Δρmin = −0.66 e Å−3 |
6 restraints | |
Special details top
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F2, conventional
R-factors are based on F, with F set to zero for negative
F2. The threshold expression of F2 > n*σ(F2) is
used only for calculating R-factors etc. and is not relevant to
the choice of reflections for refinement. The hydrogen atoms were localized from the difference Fourier map. Their
coordinates were refined independently. The O—H distances were restrained to
0.82 Å with σ 0.01. The isotropic temperature parameters of hydrogen atoms
were calculated as 1.2*Ueq of the parent atom. The structure was a twin with partial overlaps of reflections. Both twin
domains were used in the refinement. The angular limit for complete overlap
was chosen 0.1°. One water molecule was disordered. The oxygen of this molecule was split in two
partially occupied positions clearly visible in the difference Fourier map.
The occupation of the split positions was refined. The ADP parameters of split
O atoms were kept identical. The hydrogen atoms of the disordered water
molecule could not be determined. 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) |
Tb1 | 0.37274 (4) | 0.26131 (3) | 0.45245 (3) | 0.01008 (7) | |
P1 | −0.19255 (17) | 0.23305 (16) | 0.56073 (12) | 0.0088 (3) | |
P2 | 0.05658 (18) | 0.14173 (17) | 0.78786 (12) | 0.0135 (4) | |
O1 | −0.3366 (4) | 0.4087 (4) | 0.5581 (3) | 0.0123 (10) | |
O2 | −0.3303 (4) | 0.0720 (4) | 0.5328 (3) | 0.0126 (10) | |
O3 | 0.0676 (5) | −0.0735 (4) | 0.8359 (3) | 0.0206 (11) | |
O4 | 0.0126 (4) | 0.2583 (4) | 0.4667 (3) | 0.0137 (10) | |
O5 | 0.2409 (5) | 0.2314 (5) | 0.6891 (3) | 0.0186 (11) | |
O6 | −0.1506 (5) | 0.1800 (5) | 0.7171 (3) | 0.0191 (11) | |
O7 | 0.0087 (6) | 0.2585 (5) | 0.9129 (3) | 0.0261 (13) | |
O8 | 0.6688 (5) | 0.3618 (5) | 0.2657 (4) | 0.0237 (13) | |
O9 | 0.2861 (6) | 0.2700 (6) | 0.2249 (4) | 0.0317 (14) | |
O10 | 0.500 (2) | 0.107 (3) | 0.0007 (15) | 0.103 (11) | 0.452 (16) |
O11 | 0.5102 (13) | 0.327 (2) | −0.0466 (9) | 0.066 (5) | 0.548 (16) |
H71 | −0.031 (8) | 0.198 (7) | 0.990 (2) | 0.0313* | |
H81 | 0.740 (7) | 0.457 (5) | 0.266 (5) | 0.0284* | |
H82 | 0.732 (7) | 0.260 (4) | 0.255 (6) | 0.0284* | |
H91 | 0.370 (7) | 0.260 (8) | 0.155 (4) | 0.038* | |
H92 | 0.186 (6) | 0.212 (7) | 0.210 (6) | 0.038* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Tb1 | 0.00869 (11) | 0.00724 (12) | 0.01377 (12) | 0.00016 (7) | −0.00118 (8) | −0.00046 (8) |
P1 | 0.0064 (5) | 0.0068 (6) | 0.0132 (6) | 0.0006 (4) | −0.0026 (5) | −0.0006 (5) |
P2 | 0.0126 (6) | 0.0171 (7) | 0.0106 (6) | −0.0015 (5) | −0.0025 (5) | −0.0006 (5) |
O1 | 0.0083 (14) | 0.0074 (16) | 0.0206 (18) | 0.0058 (12) | −0.0036 (14) | −0.0002 (13) |
O2 | 0.0119 (15) | 0.0078 (16) | 0.0195 (18) | −0.0061 (12) | −0.0076 (14) | 0.0009 (13) |
O3 | 0.0313 (19) | 0.0156 (18) | 0.0141 (18) | 0.0043 (15) | −0.0047 (16) | 0.0013 (14) |
O4 | 0.0076 (15) | 0.0190 (17) | 0.0144 (17) | 0.0012 (13) | −0.0019 (13) | −0.0016 (13) |
O5 | 0.0152 (16) | 0.029 (2) | 0.0108 (18) | −0.0040 (14) | −0.0027 (14) | 0.0014 (14) |
O6 | 0.0095 (16) | 0.0235 (19) | 0.025 (2) | 0.0009 (14) | −0.0050 (15) | −0.0019 (15) |
O7 | 0.046 (2) | 0.020 (2) | 0.0118 (19) | −0.0022 (17) | −0.0036 (18) | −0.0018 (15) |
O8 | 0.0198 (19) | 0.024 (2) | 0.025 (2) | −0.0024 (15) | 0.0029 (16) | −0.0046 (18) |
O9 | 0.027 (2) | 0.048 (3) | 0.020 (2) | −0.0146 (19) | −0.0051 (17) | −0.0018 (19) |
O10 | 0.046 (4) | 0.142 (8) | 0.042 (4) | 0.014 (6) | 0.007 (4) | −0.017 (5) |
O11 | 0.046 (4) | 0.142 (8) | 0.042 (4) | 0.014 (6) | 0.007 (4) | −0.017 (5) |
Geometric parameters (Å, º) top
Tb1—O1i | 2.291 (3) | P2—O3 | 1.507 (3) |
Tb1—O1ii | 2.592 (3) | P2—O5 | 1.494 (3) |
Tb1—O2ii | 2.467 (3) | P2—O6 | 1.605 (3) |
Tb1—O2iii | 2.324 (3) | P2—O7 | 1.554 (4) |
Tb1—O4 | 2.306 (3) | O7—H71 | 0.82 (3) |
Tb1—O5 | 2.321 (3) | O8—H81 | 0.82 (4) |
Tb1—O8 | 2.459 (3) | O8—H82 | 0.82 (3) |
Tb1—O9 | 2.385 (4) | O9—H91 | 0.81 (4) |
P1—O1 | 1.514 (3) | O9—H92 | 0.82 (5) |
P1—O2 | 1.533 (3) | O10—O10iv | 1.49 (3) |
P1—O4 | 1.483 (3) | O10—O11 | 1.53 (3) |
P1—O6 | 1.593 (4) | | |
| | | |
O1ii—Tb1—O1i | 68.37 (10) | O2iii—Tb1—O8 | 108.16 (11) |
O1ii—Tb1—O2ii | 56.34 (9) | O2iii—Tb1—O9 | 84.07 (13) |
O1ii—Tb1—O2iii | 122.19 (10) | O4—Tb1—O5 | 74.87 (11) |
O1ii—Tb1—O4 | 141.03 (10) | O4—Tb1—O8 | 134.73 (11) |
O1ii—Tb1—O5 | 75.98 (10) | O4—Tb1—O9 | 70.49 (11) |
O1ii—Tb1—O8 | 70.91 (11) | O5—Tb1—O8 | 146.84 (12) |
O1ii—Tb1—O9 | 135.87 (11) | O5—Tb1—O9 | 145.19 (12) |
O1i—Tb1—O1ii | 68.37 (10) | O8—Tb1—O9 | 67.07 (12) |
O1i—Tb1—O2ii | 124.47 (10) | O1—P1—O2 | 103.35 (17) |
O1i—Tb1—O2iii | 167.52 (10) | O1—P1—O4 | 115.85 (16) |
O1i—Tb1—O4 | 85.58 (10) | O1—P1—O6 | 106.54 (18) |
O1i—Tb1—O5 | 88.58 (11) | O2—P1—O4 | 114.68 (18) |
O1i—Tb1—O8 | 80.95 (11) | O2—P1—O6 | 107.20 (17) |
O1i—Tb1—O9 | 92.01 (13) | O4—P1—O6 | 108.61 (17) |
O2ii—Tb1—O2iii | 66.97 (10) | O3—P2—O5 | 117.02 (18) |
O2ii—Tb1—O4 | 142.59 (9) | O3—P2—O6 | 106.99 (19) |
O2ii—Tb1—O5 | 83.42 (10) | O3—P2—O7 | 111.68 (18) |
O2ii—Tb1—O8 | 77.06 (10) | O5—P2—O6 | 109.19 (18) |
O2ii—Tb1—O9 | 123.40 (12) | O5—P2—O7 | 108.6 (2) |
O2iii—Tb1—O2ii | 66.97 (10) | O6—P2—O7 | 102.2 (2) |
O2iii—Tb1—O4 | 81.94 (10) | P2—O7—H71 | 118 (3) |
O2iii—Tb1—O5 | 87.93 (11) | O10iv—O10—O11 | 162.3 (13) |
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 (3) | 1.78 (3) | 2.588 (4) | 169 (5) |
O8—H82···O3vi | 0.82 (3) | 2.00 (4) | 2.782 (5) | 159 (5) |
O9—H91···O11 | 0.81 (4) | 2.03 (4) | 2.795 (9) | 157 (5) |
O9—H92···O3iii | 0.82 (4) | 2.07 (4) | 2.883 (5) | 177 (6) |
O9—H91···O10 | 0.81 (4) | 2.03 (5) | 2.770 (17) | 151 (5) |
Symmetry codes: (iii) −x, −y, −z+1; (v) −x, −y, −z+2; (vi) −x+1, −y, −z+1. |