Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804007445/br6144sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804007445/br6144Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (Mo-O) = 0.005 Å
- H-atom completeness 1%
- Disorder in solvent or counterion
- R factor = 0.030
- wR factor = 0.074
- Data-to-parameter ratio = 16.7
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT220_ALERT_2_A Large Non-Solvent O Ueq(max)/Ueq(min) ... 5.51 Ratio
Author Response: Because disorderd O20 and O21 atoms. Explained in Comment. |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O18
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O19
Author Response: Explained in _publ_section_exptl_refinement |
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O19 .. 2.69 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_B Short Inter D...A Contact O3 .. O18 .. 2.73 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_B Short Inter D...A Contact O5 .. O16 .. 2.78 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_B Short Inter D...A Contact O9 .. O20 .. 2.72 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_B Short Inter D...A Contact O12 .. O20 .. 2.65 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_B Short Inter D...A Contact O13 .. O21 .. 2.75 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_B Short Inter D...A Contact O14 .. O20 .. 2.72 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_B Short Inter D...A Contact O17 .. O19 .. 2.67 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_B Short Inter D...A Contact O18 .. O19 .. 2.81 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
Alert level C CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 1722.82 TEST: Calculate formula weight from _atom_site_* atom mass num sum La 138.91 2.00 277.81 Pt 195.08 1.00 195.08 Mo 95.94 6.00 575.64 O 16.00 40.00 639.96 H 1.01 0.00 0.00 Calculated formula weight 1688.49
Author Response: Because H atoms of H2O were not included. |
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
Author Response: Because H atoms of H2O were not included. |
PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 1722.82
Author Response: Because H atoms of H2O were included. |
PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ?
Author Response: Because H atoms of H2O were not included. |
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
Author Response: Because H atoms of H2O were not included. |
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... La PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc.
Author Response: Explained in Comment. |
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:H32 La2 Mo6 O40 Pt1 Atom count from the _atom_site data: La2 Mo6 O40 Pt1 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 4 From the CIF: _chemical_formula_sum H32 La2 Mo6 O40 Pt TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 128.00 0.00 128.00 La 8.00 8.00 0.00 Mo 24.00 24.00 0.00 O 160.00 160.00 0.00 Pt 4.00 4.00 0.00
3 ALERT level A = In general: serious problem 9 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 15 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Version 1.07; Farrugia, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.
La2[H2PtMo6O24]·16H2O | F(000) = 3192 |
Mr = 1722.82 | Dx = 3.378 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -C 2yc | Cell parameters from 25 reflections |
a = 21.147 (2) Å | θ = 9.5–10.4° |
b = 10.664 (1) Å | µ = 8.85 mm−1 |
c = 15.949 (2) Å | T = 298 K |
β = 109.62 (1)° | Monoclinic, colourless |
V = 3387.9 (7) Å3 | 0.20 × 0.13 × 0.13 mm |
Z = 4 |
Stoe Stadi-4 diffractometer | 3493 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 27.5°, θmin = 2.0° |
ω/2–θ scans | h = −27→25 |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996) | k = 0→13 |
Tmin = 0.251, Tmax = 0.357 | l = 0→20 |
3894 measured reflections | 3 standard reflections every 60 min |
3893 independent reflections | intensity decay: 3.7% |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.030 | w = 1/[σ2(Fo2) + (0.0295P)2 + 55.4435P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.074 | (Δ/σ)max = 0.001 |
S = 1.11 | Δρmax = 1.33 e Å−3 |
3893 reflections | Δρmin = −0.82 e Å−3 |
233 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.000281 (19) |
Primary atom site location: structure-invariant direct methods |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pt | 0.2500 | 0.2500 | 0.5000 | 0.01213 (9) | |
La | 0.601598 (17) | 0.27720 (3) | 0.64673 (2) | 0.01518 (10) | |
Mo1 | 0.39971 (2) | 0.32474 (5) | 0.63074 (3) | 0.01384 (12) | |
Mo2 | 0.30275 (3) | 0.54582 (5) | 0.51727 (3) | 0.01511 (12) | |
Mo3 | 0.15164 (3) | 0.46547 (5) | 0.36834 (3) | 0.01594 (12) | |
O1 | 0.29311 (19) | 0.3833 (4) | 0.5895 (3) | 0.0135 (8) | |
O2 | 0.3450 (2) | 0.1867 (4) | 0.5385 (3) | 0.0151 (8) | |
O3 | 0.2592 (2) | 0.3795 (4) | 0.4137 (3) | 0.0151 (8) | |
O4 | 0.3883 (2) | 0.4478 (5) | 0.5413 (3) | 0.0194 (9) | |
O5 | 0.2075 (2) | 0.5537 (4) | 0.4767 (3) | 0.0190 (9) | |
O6 | 0.3752 (2) | 0.1867 (4) | 0.7027 (3) | 0.0173 (9) | |
O7 | 0.4166 (2) | 0.4135 (4) | 0.7271 (3) | 0.0195 (9) | |
O8 | 0.4769 (2) | 0.2723 (5) | 0.6303 (3) | 0.0198 (9) | |
O9 | 0.3222 (2) | 0.6416 (5) | 0.6077 (3) | 0.0262 (11) | |
O10 | 0.3231 (2) | 0.6299 (5) | 0.4367 (3) | 0.0224 (10) | |
O11 | 0.1747 (2) | 0.5489 (5) | 0.2913 (3) | 0.0257 (10) | |
O12 | 0.0748 (2) | 0.5226 (5) | 0.3645 (3) | 0.0278 (11) | |
O13 | 0.5640 (3) | 0.4993 (5) | 0.5921 (4) | 0.0357 (13) | |
O14 | 0.5395 (4) | 0.2502 (9) | 0.4799 (4) | 0.075 (3) | |
O15 | 0.7114 (3) | 0.3698 (6) | 0.7468 (3) | 0.0341 (13) | |
O16 | 0.6823 (3) | 0.1067 (5) | 0.6335 (4) | 0.0321 (12) | |
O17 | 0.5465 (3) | 0.0615 (5) | 0.6201 (4) | 0.0385 (14) | |
O18 | 0.3237 (3) | 0.3380 (6) | 0.2938 (4) | 0.0430 (14) | |
O19 | 0.6009 (4) | 0.8474 (7) | 0.5901 (4) | 0.062 (2) | |
O20 | 0.0528 (7) | 0.7611 (14) | 0.3162 (10) | 0.056 (4) | 0.50 |
O21 | 0.5173 (7) | 0.3698 (16) | 0.3355 (10) | 0.061 (4) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt | 0.00976 (15) | 0.01609 (17) | 0.01060 (15) | −0.00088 (11) | 0.00349 (11) | −0.00021 (12) |
La | 0.01294 (17) | 0.01972 (19) | 0.01329 (17) | −0.00044 (13) | 0.00495 (13) | −0.00054 (13) |
Mo1 | 0.0102 (2) | 0.0187 (3) | 0.0127 (2) | −0.00076 (19) | 0.00390 (18) | −0.00007 (19) |
Mo2 | 0.0156 (2) | 0.0172 (3) | 0.0134 (2) | −0.00153 (19) | 0.00600 (19) | −0.00024 (19) |
Mo3 | 0.0124 (2) | 0.0185 (3) | 0.0171 (2) | −0.00043 (19) | 0.00508 (19) | 0.0002 (2) |
O1 | 0.0105 (18) | 0.017 (2) | 0.0141 (19) | −0.0021 (16) | 0.0052 (15) | −0.0008 (16) |
O2 | 0.0100 (19) | 0.021 (2) | 0.015 (2) | −0.0004 (16) | 0.0049 (16) | −0.0006 (17) |
O3 | 0.0138 (19) | 0.019 (2) | 0.0132 (19) | −0.0005 (17) | 0.0053 (16) | 0.0017 (17) |
O4 | 0.016 (2) | 0.030 (3) | 0.014 (2) | −0.0016 (19) | 0.0069 (17) | 0.0046 (19) |
O5 | 0.017 (2) | 0.021 (2) | 0.021 (2) | 0.0009 (18) | 0.0089 (18) | −0.0045 (18) |
O6 | 0.018 (2) | 0.021 (2) | 0.014 (2) | −0.0028 (18) | 0.0071 (17) | −0.0007 (17) |
O7 | 0.023 (2) | 0.023 (2) | 0.015 (2) | −0.0027 (19) | 0.0080 (17) | −0.0036 (18) |
O8 | 0.011 (2) | 0.024 (2) | 0.023 (2) | −0.0014 (18) | 0.0036 (17) | 0.0010 (19) |
O9 | 0.028 (3) | 0.028 (3) | 0.022 (2) | −0.005 (2) | 0.009 (2) | −0.006 (2) |
O10 | 0.019 (2) | 0.026 (3) | 0.024 (2) | 0.0000 (19) | 0.0104 (18) | 0.009 (2) |
O11 | 0.023 (2) | 0.029 (3) | 0.021 (2) | −0.005 (2) | 0.0033 (19) | 0.004 (2) |
O12 | 0.017 (2) | 0.028 (3) | 0.039 (3) | 0.004 (2) | 0.010 (2) | −0.001 (2) |
O13 | 0.040 (3) | 0.032 (3) | 0.045 (3) | 0.012 (3) | 0.027 (3) | 0.016 (3) |
O14 | 0.073 (5) | 0.121 (8) | 0.027 (3) | −0.062 (5) | 0.010 (3) | −0.020 (4) |
O15 | 0.026 (3) | 0.060 (4) | 0.017 (2) | −0.019 (3) | 0.008 (2) | −0.007 (2) |
O16 | 0.034 (3) | 0.031 (3) | 0.039 (3) | 0.009 (2) | 0.022 (2) | 0.005 (2) |
O17 | 0.026 (3) | 0.023 (3) | 0.069 (4) | −0.004 (2) | 0.020 (3) | −0.013 (3) |
O18 | 0.057 (4) | 0.041 (4) | 0.033 (3) | 0.003 (3) | 0.017 (3) | 0.003 (3) |
O19 | 0.095 (6) | 0.060 (5) | 0.048 (4) | 0.046 (4) | 0.046 (4) | 0.018 (3) |
O20 | 0.053 (8) | 0.052 (9) | 0.053 (8) | −0.004 (7) | 0.005 (7) | 0.003 (7) |
O21 | 0.055 (9) | 0.070 (11) | 0.064 (9) | −0.002 (8) | 0.027 (7) | −0.001 (8) |
Pt—Mo1 | 3.2516 (6) | Mo1—O1 | 2.216 (4) |
Pt—Mo2 | 3.3265 (6) | Mo1—O2 | 2.128 (4) |
Pt—Mo3 | 3.3291 (6) | Mo1—O4 | 1.893 (5) |
Mo1—Mo2 | 3.2475 (8) | Mo1—O6 | 2.037 (4) |
Mo1—Mo3i | 3.2814 (8) | Mo1—O7 | 1.737 (4) |
Mo2—Mo3 | 3.3897 (8) | Mo1—O8 | 1.729 (4) |
Pt—O1 | 2.004 (4) | Mo2—O1 | 2.129 (4) |
Pt—O2 | 2.011 (4) | Mo2—O3 | 2.387 (4) |
Pt—O3 | 2.006 (4) | Mo2—O4 | 2.012 (5) |
La—O6ii | 2.479 (4) | Mo2—O5 | 1.899 (4) |
La—O7ii | 2.614 (4) | Mo2—O9 | 1.701 (5) |
La—O8 | 2.561 (4) | Mo2—O10 | 1.736 (4) |
La—O10iii | 2.590 (4) | Mo3—O2i | 2.186 (4) |
La—O13 | 2.556 (6) | Mo3—O3 | 2.331 (4) |
La—O14 | 2.557 (7) | Mo3—O5 | 1.973 (5) |
La—O15 | 2.535 (5) | Mo3—O6i | 1.952 (5) |
La—O16 | 2.550 (5) | Mo3—O11 | 1.716 (5) |
La—O17 | 2.549 (5) | Mo3—O12 | 1.716 (5) |
Mo2—Mo1—Pt | 61.57 (1) | O14—La—O7ii | 134.9 (3) |
Mo2—Mo1—Mo3i | 122.63 (2) | O10iii—La—O7ii | 117.3 (2) |
Pt—Mo1—Mo3i | 61.27 (1) | O8—Mo1—O7 | 105.4 (2) |
Mo1—Mo2—Pt | 59.28 (2) | O8—Mo1—O4 | 95.9 (2) |
Mo1—Mo2—Mo3 | 118.51 (2) | O7—Mo1—O4 | 103.0 (2) |
O1—Pt—O1i | 180.000 (1) | O8—Mo1—O6 | 100.8 (2) |
O1—Pt—O3i | 97.2 (2) | O7—Mo1—O6 | 84.9 (2) |
O1—Pt—O3 | 82.8 (2) | O4—Mo1—O6 | 158.9 (2) |
O3i—Pt—O3 | 180.0 | O8—Mo1—O2 | 93.9 (2) |
O1—Pt—O2 | 81.5 (2) | O7—Mo1—O2 | 153.1 (2) |
O1i—Pt—O2 | 98.5 (2) | O4—Mo1—O2 | 93.2 (2) |
O3i—Pt—O2 | 82.9 (2) | O6—Mo1—O2 | 73.0 (2) |
O3—Pt—O2 | 97.1 (2) | O8—Mo1—O1 | 163.5 (2) |
O1—Pt—O2i | 98.5 (2) | O7—Mo1—O1 | 89.8 (2) |
O1i—Pt—O2i | 81.5 (2) | O4—Mo1—O1 | 73.8 (2) |
O3i—Pt—O2i | 97.1 (2) | O6—Mo1—O1 | 86.9 (2) |
O3—Pt—O2i | 82.9 (2) | O2—Mo1—O1 | 74.2 (2) |
O2—Pt—O2i | 180.000 (1) | O9—Mo2—O10 | 105.5 (2) |
Mo1—Pt—Mo2 | 59.15 (1) | O9—Mo2—O5 | 100.9 (2) |
O6ii—La—O15 | 72.6 (1) | O10—Mo2—O5 | 102.9 (2) |
O6ii—La—O8 | 87.3 (1) | O9—Mo2—O4 | 101.8 (2) |
O15—La—O8 | 140.0 (2) | O10—Mo2—O4 | 88.8 (2) |
O6ii—La—O16 | 83.3 (2) | O5—Mo2—O4 | 150.5 (2) |
O15—La—O16 | 80.4 (2) | O9—Mo2—O1 | 94.0 (2) |
O8—La—O16 | 132.2 (2) | O10—Mo2—O1 | 156.1 (2) |
O6ii—La—O17 | 75.0 (2) | O5—Mo2—O1 | 86.4 (2) |
O15—La—O17 | 136.7 (2) | O4—Mo2—O1 | 73.6 (2) |
O8—La—O17 | 64.4 (2) | O9—Mo2—O3 | 163.7 (2) |
O16—La—O17 | 67.9 (2) | O10—Mo2—O3 | 90.3 (2) |
O6ii—La—O13 | 128.9 (2) | O5—Mo2—O3 | 71.3 (2) |
O15—La—O13 | 88.2 (2) | O4—Mo2—O3 | 81.9 (2) |
O8—La—O13 | 78.0 (2) | O1—Mo2—O3 | 71.7 (2) |
O16—La—O13 | 140.6 (2) | O12—Mo3—O11 | 106.5 (2) |
O17—La—O13 | 135.0 (2) | O12—Mo3—O6i | 100.8 (2) |
O6ii—La—O14 | 146.0 (2) | O11—Mo3—O6i | 96.5 (2) |
O15—La—O14 | 137.8 (2) | O12—Mo3—O5 | 98.2 (2) |
O8—La—O14 | 74.9 (2) | O11—Mo3—O5 | 98.6 (2) |
O16—La—O14 | 87.6 (3) | O6i—Mo3—O5 | 151.3 (2) |
O17—La—O14 | 71.3 (2) | O12—Mo3—O2i | 95.8 (2) |
O13—La—O14 | 75.9 (3) | O11—Mo3—O2i | 157.0 (2) |
O6ii—La—O10iii | 133.7 (1) | O6i—Mo3—O2i | 73.4 (2) |
O15—La—O10iii | 65.4 (2) | O5—Mo3—O2i | 83.4 (2) |
O8—La—O10iii | 138.1 (2) | O12—Mo3—O3 | 164.6 (2) |
O16—La—O10iii | 71.7 (2) | O11—Mo3—O3 | 86.7 (2) |
O17—La—O10iii | 125.8 (2) | O6i—Mo3—O3 | 85.2 (2) |
O13—La—O10iii | 69.2 (2) | O5—Mo3—O3 | 71.4 (2) |
O14—La—O10iii | 72.4 (2) | O2i—Mo3—O3 | 72.1 (2) |
O6ii—La—O7ii | 60.2 (1) | Mo2—O1—Mo1 | 96.7 (2) |
O15—La—O7ii | 68.8 (2) | Mo1—O2—Mo3i | 99.1 (2) |
O8—La—O7ii | 71.2 (2) | Mo3—O3—Mo2 | 91.8 (2) |
O16—La—O7ii | 137.4 (2) | Mo1—O4—Mo2 | 112.5 (2) |
O17—La—O7ii | 116.9 (2) | Mo2—O5—Mo3 | 122.1 (2) |
O13—La—O7ii | 68.8 (2) | Mo3i—O6—Mo1 | 110.7 (2) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (ii) −x+1, y, −z+3/2; (iii) −x+1, −y+1, −z+1. |
D—H···A | D···A |
O13···O4iii | 2.703 (7) |
O13···O7ii | 2.920 (7) |
O13···O10iii | 2.923 (7) |
O13···O21iii | 2.75 (2) |
O14···O17 | 2.98 (1) |
O14···O19iii | 2.99 (1) |
O14···O20iv | 2.72 (2) |
O14···O21 | 2.54 (2) |
O15···O6ii | 2.967 (7) |
O15···O7ii | 2.911 (7) |
O15···O1ii | 2.647 (6) |
O15···O10iii | 2.770 (7) |
O15···O11iii | 2.811 (7) |
O16···O5iv | 2.785 (7) |
O16···O17 | 2.849 (7) |
O17···O8 | 2.721 (7) |
O17···O12i | 2.805 (7) |
O17···O19v | 2.673 (9) |
O18···O3 | 2.732 (7) |
O18···O9vi | 2.964 (7) |
O18···O19iii | 2.809 (9) |
O19···O2iii | 2.685 (7) |
O20···O9vii | 2.72 (2) |
O20···O12 | 2.65 (2) |
O20···O14viii | 2.72 (2) |
O20···O21ix | 2.64 (2) |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (ii) −x+1, y, −z+3/2; (iii) −x+1, −y+1, −z+1; (iv) x+1/2, y−1/2, z; (v) x, y−1, z; (vi) x, −y+1, z−1/2; (vii) −x+1/2, −y+3/2, −z+1; (viii) x−1/2, y+1/2, z; (ix) −x+1/2, y+1/2, −z+1/2. |