Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804002302/wm6009sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804002302/wm6009Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (W-O) = 0.008 Å
- H-atom completeness 1%
- R factor = 0.039
- wR factor = 0.098
- Data-to-parameter ratio = 17.6
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O25
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O26
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O27
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O28
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O29
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O30
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O31
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O32
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O33
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O34
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O35
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O36
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O37
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O38
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O39
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O40
Author Response: Explained in _publ_section_exptl_refinement |
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O41
Author Response: Explained in _publ_section_exptl_refinement |
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O1 = 2.60 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 O2 .. O32 = 2.80 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 .. O14 = 2.56 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 O4 .. O33 = 2.82 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 .. O15 = 2.60 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 O6 .. O30 = 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 O7 .. O28 = 2.83 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 O8 .. O25 = 2.82 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 .. O34 = 2.82 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 O10 .. O35 = 2.81 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 O10 .. O36 = 2.83 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 O11 .. O41 = 2.77 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 .. O27 = 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 O21 .. O26 = 2.84 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 O24 .. O41 = 2.80 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 O26 .. O31 = 2.80 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 O27 .. O41 = 2.76 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 O27 .. O37 = 2.80 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 O30 .. O41 = 2.83 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 O32 .. O36 = 2.81 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 O33 .. O34 = 2.80 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 2 From the CIF: _chemical_formula_weight 2117.43 TEST: Calculate formula weight from _atom_site_* atom mass num sum H 1.01 0.00 0.00 Na 22.99 5.50 126.44 Pt 195.08 1.00 195.08 W 183.85 6.00 1103.10 O 16.00 41.00 655.96 Calculated formula weight 2080.58 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
Author Response: Because H atoms of H2O were not included. |
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
Author Response: Because H atoms of H2O were not included.: |
PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 2117.43
Author Response: Because H atoms of H2O were not 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. |
PLAT430_ALERT_2_C Short Inter D...A Contact O19 .. O26 = 2.89 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT430_ALERT_2_C Short Inter D...A Contact O24 .. O31 = 2.90 Ang.
Author Response: Those are normal values in the polyoxometalates or it means strong hydrogen-bonding interaction. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 O
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7 O
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 8 O
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 9 O
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 10 O
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 11 O
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 15 O
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 17 O
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 20 Na
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 21 Na
Author Response: Because of groupping to related atoms. |
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 22 Na
Author Response: Because of groupping to related atoms. |
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: H36.5 Na5.5 O41 Pt1 W6 Atom count from _chemical_formula_moiety:H36.5 Na5.5 O41 Pt1 W65 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:H36.5 Na5.5 O41 Pt1 W6 Atom count from the _atom_site data: Na5.5 O41 Pt1 W6 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 H36.50 Na5.50 O41 Pt W6 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 73.00 0.00 73.00 Na 11.00 11.00 0.00 O 82.00 82.00 0.00 Pt 2.00 2.00 0.00 W 12.00 12.00 0.00
17 ALERT level A = In general: serious problem 21 ALERT level B = Potentially serious problem 20 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 42 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 11 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: STADI4 (Stoe & Coe, 1996); cell refinement: STADI4; data reduction: X-RED (STOE, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.
Na5.5[H2.5PtW6O24](H2O)17] | Z = 2 |
Mr = 2117.43 | F(000) = 1967 |
Triclinic, P1 | Dx = 3.785 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 10.736 (2) Å | Cell parameters from 30 reflections |
b = 12.803 (3) Å | θ = 9.5–10.5° |
c = 14.877 (3) Å | µ = 22.43 mm−1 |
α = 105.50 (3)° | T = 298 K |
β = 105.13 (3)° | Triclinic, pale yellow |
γ = 97.43 (3)° | 0.30 × 0.25 × 0.24 mm |
V = 1858.1 (9) Å3 |
Stoe Stadi-4 diffractometer | 7210 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 27.5°, θmin = 1.7° |
ω/2θ scans | h = 0→13 |
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996) | k = −16→16 |
Tmin = 0.005, Tmax = 0.010 | l = −19→18 |
8526 measured reflections | 3 standard reflections every 60 min |
8526 independent reflections | intensity decay: 3.5% |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.039 | w = 1/[σ2(Fo2) + (0.042P)2 + 22.4365P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.098 | (Δ/σ)max = 0.001 |
S = 1.13 | Δρmax = 1.89 e Å−3 |
8526 reflections | Δρmin = −2.38 e Å−3 |
485 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00196 (5) |
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 | ||
Pt | 0.53177 (3) | 0.63934 (3) | 0.19396 (2) | 0.01129 (9) | |
W1 | 0.36598 (4) | 0.38366 (3) | 0.12171 (3) | 0.01673 (10) | |
W2 | 0.23581 (4) | 0.57111 (3) | 0.03140 (3) | 0.01545 (10) | |
W3 | 0.39646 (4) | 0.82623 (3) | 0.11042 (3) | 0.01574 (10) | |
W4 | 0.68999 (4) | 0.90412 (3) | 0.29045 (3) | 0.01498 (10) | |
W5 | 0.81131 (4) | 0.72228 (3) | 0.38136 (3) | 0.01662 (10) | |
W6 | 0.64513 (4) | 0.45429 (3) | 0.29557 (3) | 0.01810 (10) | |
Na1 | 0.9679 (7) | 0.3308 (6) | 0.2866 (5) | 0.0588 (17) | |
Na2 | 1.1374 (5) | 0.6005 (4) | 0.3672 (4) | 0.0339 (11) | |
Na3 | 1.2834 (5) | 0.8758 (4) | 0.4486 (3) | 0.0347 (11) | |
Na4 | 1.1614 (8) | 0.9366 (10) | 0.2435 (5) | 0.092 (3) | |
Na5 | 1.0000 | 1.0000 | 0.0000 | 0.102 (5) | |
Na6 | 0.6471 (5) | 1.0511 (4) | 0.0975 (4) | 0.0415 (13) | |
O1 | 0.4369 (7) | 0.5191 (6) | 0.0644 (5) | 0.0152 (13) | |
O2 | 0.3617 (6) | 0.6889 (6) | 0.1682 (5) | 0.0140 (13) | |
O3 | 0.5885 (7) | 0.7630 (6) | 0.1426 (5) | 0.0162 (14) | |
O4 | 0.6228 (7) | 0.7577 (6) | 0.3235 (5) | 0.0150 (13) | |
O5 | 0.7028 (7) | 0.5885 (5) | 0.2258 (5) | 0.0141 (13) | |
O6 | 0.4734 (7) | 0.5227 (6) | 0.2484 (5) | 0.0178 (14) | |
O7 | 0.2291 (7) | 0.4688 (6) | 0.1056 (5) | 0.0177 (14) | |
O8 | 0.3245 (8) | 0.6930 (6) | −0.0012 (5) | 0.0230 (16) | |
O9 | 0.5065 (7) | 0.9080 (6) | 0.2446 (5) | 0.0182 (14) | |
O10 | 0.8360 (7) | 0.8270 (6) | 0.3089 (5) | 0.0185 (15) | |
O11 | 0.7105 (7) | 0.5968 (6) | 0.3980 (5) | 0.0178 (14) | |
O12 | 0.5452 (8) | 0.3609 (6) | 0.1633 (6) | 0.0242 (16) | |
O13 | 0.2935 (9) | 0.3086 (7) | 0.1839 (6) | 0.0286 (18) | |
O14 | 0.3209 (8) | 0.2907 (7) | 0.0023 (6) | 0.0265 (17) | |
O15 | 0.1908 (8) | 0.4777 (6) | −0.0885 (5) | 0.0236 (16) | |
O16 | 0.0945 (7) | 0.6179 (7) | 0.0403 (6) | 0.0258 (17) | |
O17 | 0.2549 (8) | 0.8732 (6) | 0.1204 (6) | 0.0238 (16) | |
O18 | 0.4644 (8) | 0.9031 (6) | 0.0468 (6) | 0.0254 (17) | |
O19 | 0.7564 (8) | 0.9812 (7) | 0.2249 (6) | 0.0276 (17) | |
O20 | 0.7245 (8) | 0.9943 (6) | 0.4067 (6) | 0.0274 (17) | |
O21 | 0.8523 (9) | 0.8128 (7) | 0.4990 (6) | 0.0289 (18) | |
O22 | 0.9538 (8) | 0.6742 (7) | 0.3755 (7) | 0.0315 (19) | |
O23 | 0.7940 (9) | 0.4162 (7) | 0.2964 (7) | 0.034 (2) | |
O24 | 0.5830 (9) | 0.3808 (7) | 0.3637 (6) | 0.0323 (19) | |
O25 | 0.8137 (10) | 0.2156 (8) | 0.1400 (8) | 0.048 (3) | |
O26 | 0.9144 (9) | 0.1930 (7) | 0.3596 (7) | 0.037 (2) | |
O27 | 1.1494 (16) | 0.2316 (14) | 0.2846 (11) | 0.092 (5) | |
O28 | 1.0415 (9) | 0.4652 (8) | 0.2085 (7) | 0.038 (2) | |
O29 | 1.0884 (12) | 0.4576 (9) | 0.4445 (8) | 0.054 (3) | |
O30 | 1.3557 (9) | 0.5721 (8) | 0.3922 (7) | 0.038 (2) | |
O31 | 1.2492 (10) | 0.7337 (8) | 0.5287 (7) | 0.038 (2) | |
O32 | 1.2049 (9) | 0.7390 (8) | 0.2911 (6) | 0.035 (2) | |
O33 | 1.4869 (10) | 0.8070 (8) | 0.4632 (7) | 0.041 (2) | |
O34 | 1.3742 (10) | 1.0077 (9) | 0.3741 (9) | 0.052 (3) | |
O35 | 1.0953 (8) | 0.9555 (7) | 0.3831 (6) | 0.0329 (19) | |
O36 | 0.9662 (10) | 0.7575 (9) | 0.1681 (8) | 0.049 (3) | |
O37 | 1.0069 (15) | 1.0182 (14) | 0.1657 (11) | 0.083 (4) | |
O38 | 1.0083 (13) | 1.1993 (12) | 0.0359 (10) | 0.073 (4) | |
O39 | 0.7485 (12) | 0.9397 (9) | −0.0179 (8) | 0.054 (3) | |
O40 | 0.5149 (16) | 1.1390 (10) | 0.1937 (11) | 0.089 (5) | |
O41 | 0.3661 (12) | 0.3701 (10) | 0.4343 (8) | 0.055 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt | 0.01289 (17) | 0.01005 (16) | 0.00966 (16) | 0.00129 (13) | 0.00292 (13) | 0.00215 (12) |
W1 | 0.0203 (2) | 0.01261 (18) | 0.01477 (19) | −0.00064 (15) | 0.00584 (15) | 0.00185 (15) |
W2 | 0.01495 (19) | 0.01546 (19) | 0.01234 (18) | −0.00012 (14) | 0.00307 (14) | 0.00125 (14) |
W3 | 0.0167 (2) | 0.01366 (19) | 0.01556 (19) | 0.00221 (15) | 0.00228 (15) | 0.00568 (15) |
W4 | 0.0170 (2) | 0.01145 (18) | 0.01356 (18) | 0.00074 (14) | 0.00223 (14) | 0.00275 (14) |
W5 | 0.0157 (2) | 0.01604 (19) | 0.01526 (19) | 0.00286 (15) | 0.00078 (15) | 0.00449 (15) |
W6 | 0.0203 (2) | 0.01458 (19) | 0.0190 (2) | 0.00452 (15) | 0.00367 (16) | 0.00663 (15) |
Na1 | 0.054 (4) | 0.054 (4) | 0.060 (4) | 0.003 (3) | 0.011 (3) | 0.015 (3) |
Na2 | 0.029 (3) | 0.036 (3) | 0.034 (3) | 0.009 (2) | 0.009 (2) | 0.007 (2) |
Na3 | 0.044 (3) | 0.036 (3) | 0.021 (2) | 0.011 (2) | 0.011 (2) | 0.003 (2) |
Na4 | 0.068 (5) | 0.190 (10) | 0.047 (4) | 0.068 (6) | 0.031 (4) | 0.052 (5) |
Na5 | 0.149 (13) | 0.068 (8) | 0.074 (8) | −0.017 (8) | 0.052 (9) | 0.000 (6) |
Na6 | 0.039 (3) | 0.039 (3) | 0.039 (3) | −0.007 (2) | −0.004 (2) | 0.025 (2) |
O1 | 0.014 (3) | 0.016 (3) | 0.012 (3) | 0.000 (3) | 0.002 (3) | 0.002 (3) |
O2 | 0.008 (3) | 0.017 (3) | 0.013 (3) | 0.001 (3) | −0.001 (2) | 0.004 (3) |
O3 | 0.025 (4) | 0.017 (3) | 0.010 (3) | 0.004 (3) | 0.009 (3) | 0.006 (3) |
O4 | 0.017 (3) | 0.017 (3) | 0.008 (3) | 0.002 (3) | 0.004 (3) | −0.001 (3) |
O5 | 0.019 (3) | 0.013 (3) | 0.010 (3) | 0.003 (3) | 0.005 (3) | 0.003 (3) |
O6 | 0.019 (4) | 0.019 (3) | 0.017 (3) | 0.003 (3) | 0.007 (3) | 0.007 (3) |
O7 | 0.017 (3) | 0.021 (4) | 0.015 (3) | 0.001 (3) | 0.006 (3) | 0.007 (3) |
O8 | 0.027 (4) | 0.019 (4) | 0.020 (4) | −0.003 (3) | 0.006 (3) | 0.005 (3) |
O9 | 0.016 (3) | 0.015 (3) | 0.021 (4) | 0.003 (3) | 0.005 (3) | 0.002 (3) |
O10 | 0.010 (3) | 0.018 (3) | 0.021 (4) | −0.004 (3) | −0.004 (3) | 0.007 (3) |
O11 | 0.017 (3) | 0.017 (3) | 0.014 (3) | 0.001 (3) | −0.001 (3) | 0.004 (3) |
O12 | 0.031 (4) | 0.011 (3) | 0.024 (4) | 0.007 (3) | 0.005 (3) | −0.002 (3) |
O13 | 0.034 (5) | 0.023 (4) | 0.036 (5) | 0.004 (3) | 0.017 (4) | 0.017 (4) |
O14 | 0.028 (4) | 0.028 (4) | 0.024 (4) | 0.003 (3) | 0.007 (3) | 0.010 (3) |
O15 | 0.023 (4) | 0.023 (4) | 0.016 (4) | 0.000 (3) | 0.002 (3) | −0.001 (3) |
O16 | 0.020 (4) | 0.029 (4) | 0.031 (4) | 0.006 (3) | 0.007 (3) | 0.014 (4) |
O17 | 0.020 (4) | 0.024 (4) | 0.027 (4) | 0.008 (3) | 0.003 (3) | 0.010 (3) |
O18 | 0.027 (4) | 0.019 (4) | 0.028 (4) | −0.001 (3) | 0.007 (3) | 0.007 (3) |
O19 | 0.031 (4) | 0.030 (4) | 0.026 (4) | 0.001 (3) | 0.013 (3) | 0.012 (3) |
O20 | 0.035 (5) | 0.021 (4) | 0.018 (4) | 0.009 (3) | 0.001 (3) | 0.000 (3) |
O21 | 0.035 (5) | 0.025 (4) | 0.022 (4) | 0.008 (4) | 0.002 (3) | 0.005 (3) |
O22 | 0.021 (4) | 0.035 (5) | 0.043 (5) | 0.011 (4) | 0.009 (4) | 0.019 (4) |
O23 | 0.030 (5) | 0.031 (5) | 0.043 (5) | 0.015 (4) | 0.011 (4) | 0.013 (4) |
O24 | 0.037 (5) | 0.031 (5) | 0.035 (5) | 0.006 (4) | 0.010 (4) | 0.021 (4) |
O25 | 0.045 (6) | 0.042 (6) | 0.047 (6) | −0.004 (5) | −0.006 (5) | 0.022 (5) |
O26 | 0.039 (5) | 0.031 (5) | 0.036 (5) | 0.008 (4) | 0.002 (4) | 0.010 (4) |
O27 | 0.086 (11) | 0.099 (12) | 0.077 (10) | −0.021 (9) | 0.044 (9) | 0.005 (9) |
O28 | 0.039 (5) | 0.046 (6) | 0.035 (5) | 0.011 (4) | 0.017 (4) | 0.017 (4) |
O29 | 0.075 (8) | 0.051 (6) | 0.036 (6) | 0.005 (6) | 0.015 (5) | 0.019 (5) |
O30 | 0.035 (5) | 0.053 (6) | 0.040 (5) | 0.021 (4) | 0.022 (4) | 0.021 (5) |
O31 | 0.048 (6) | 0.044 (5) | 0.033 (5) | 0.022 (5) | 0.021 (4) | 0.018 (4) |
O32 | 0.041 (5) | 0.039 (5) | 0.027 (4) | 0.013 (4) | 0.018 (4) | 0.005 (4) |
O33 | 0.039 (5) | 0.048 (6) | 0.036 (5) | 0.008 (5) | 0.021 (4) | 0.006 (4) |
O34 | 0.036 (6) | 0.056 (7) | 0.061 (7) | 0.004 (5) | 0.025 (5) | 0.008 (5) |
O35 | 0.020 (4) | 0.034 (5) | 0.034 (5) | 0.000 (4) | 0.003 (3) | 0.002 (4) |
O36 | 0.043 (6) | 0.046 (6) | 0.047 (6) | 0.007 (5) | 0.007 (5) | 0.004 (5) |
O37 | 0.075 (9) | 0.126 (13) | 0.075 (9) | 0.046 (9) | 0.031 (8) | 0.056 (9) |
O38 | 0.061 (8) | 0.092 (10) | 0.077 (9) | 0.014 (7) | 0.020 (7) | 0.047 (8) |
O39 | 0.068 (8) | 0.037 (6) | 0.048 (6) | 0.015 (5) | 0.003 (6) | 0.013 (5) |
O40 | 0.120 (13) | 0.030 (6) | 0.091 (11) | 0.024 (7) | 0.007 (10) | 0.001 (7) |
O41 | 0.058 (7) | 0.068 (8) | 0.040 (6) | 0.007 (6) | 0.020 (5) | 0.017 (5) |
Pt—W1 | 3.264 (1) | W6—O6 | 2.174 (7) |
Pt—W2 | 3.2939 (9) | W6—O11 | 1.942 (7) |
Pt—W3 | 3.305 (1) | W6—O12 | 1.939 (8) |
Pt—W4 | 3.328 (2) | W6—O23 | 1.729 (8) |
Pt—W5 | 3.3366 (9) | W6—O24 | 1.749 (8) |
Pt—W6 | 3.329 (1) | Na1—Na2 | 3.420 (8) |
W1—W2 | 3.336 (1) | Na1—Na6i | 4.355 (9) |
W1—W6 | 3.239 (2) | Na2—Na3 | 3.412 (7) |
W2—W3 | 3.234 (1) | Na3—Na4 | 3.328 (9) |
W3—W4 | 3.384 (2) | Na4—Na5 | 3.931 (8) |
W4—W5 | 3.239 (1) | Na5—Na6 | 4.460 (6) |
W5—W6 | 3.387 (2) | Na6—Na6ii | 3.50 (1) |
Pt—O1 | 2.026 (7) | Na1—O23 | 2.30 (1) |
Pt—O2 | 1.987 (7) | Na1—O25 | 2.33 (1) |
Pt—O3 | 2.025 (7) | Na1—O26 | 2.39 (1) |
Pt—O4 | 2.009 (6) | Na1—O27 | 2.46 (2) |
Pt—O5 | 2.010 (7) | Na1—O28 | 2.48 (1) |
Pt—O6 | 1.988 (7) | Na1—O29 | 2.38 (1) |
W1—O1 | 2.259 (7) | Na2—O22 | 2.31 (1) |
W1—O6 | 2.143 (7) | Na2—O28 | 2.39 (1) |
W1—O7 | 1.943 (7) | Na2—O29 | 2.48 (1) |
W1—O12 | 1.946 (8) | Na2—O30 | 2.37 (1) |
W1—O13 | 1.745 (7) | Na2—O31 | 2.43 (1) |
W1—O14 | 1.755 (8) | Na2—O32 | 2.47 (1) |
W2—O1 | 2.311 (7) | Na3—O20iii | 2.372 (9) |
W2—O2 | 2.154 (7) | Na3—O31 | 2.47 (1) |
W2—O7 | 1.931 (7) | Na3—O32 | 2.38 (1) |
W2—O8 | 1.959 (7) | Na3—O33 | 2.44 (1) |
W2—O15 | 1.763 (7) | Na3—O35 | 2.47 (1) |
W2—O16 | 1.725 (8) | Na3—O34 | 2.48 (1) |
W3—O2 | 2.185 (7) | Na4—O17iv | 2.32 (1) |
W3—O3 | 2.293 (7) | Na4—O32 | 2.86 (1) |
W3—O8 | 1.933 (7) | Na4—O34 | 2.45 (2) |
W3—O9 | 1.952 (7) | Na4—O35 | 2.33 (1) |
W3—O17 | 1.733 (8) | Na4—O36 | 2.66 (2) |
W3—O18 | 1.751 (8) | Na4—O37 | 2.30 (2) |
W4—O3 | 2.325 (7) | Na5—O37v | 2.39 (1) |
W4—O4 | 2.145 (7) | Na5—O37 | 2.39 (1) |
W4—O9 | 1.921 (7) | Na5—O38 | 2.45 (2) |
W4—O10 | 1.956 (7) | Na5—O38v | 2.45 (2) |
W4—O19 | 1.769 (8) | Na5—O39v | 2.63 (1) |
W4—O20 | 1.717 (7) | Na5—O39 | 2.63 (1) |
W5—O4 | 2.140 (7) | Na6—O18 | 2.348 (9) |
W5—O5 | 2.368 (7) | Na6—O18ii | 2.43 (1) |
W5—O10 | 1.965 (7) | Na6—O19 | 2.41 (1) |
W5—O11 | 1.928 (7) | Na6—O25vi | 2.40 (1) |
W5—O21 | 1.726 (8) | Na6—O40 | 2.44 (2) |
W5—O22 | 1.735 (8) | Na6—O39 | 2.50 (1) |
W6—O5 | 2.330 (7) | ||
W1—O1—W2 | 93.8 (2) | O23—W6—O12 | 96.9 (4) |
W2—O2—W3 | 96.4 (3) | O24—W6—O12 | 100.5 (4) |
W3—O3—W4 | 94.3 (3) | O23—W6—O11 | 99.1 (4) |
W5—O4—W4 | 98.2 (3) | O24—W6—O11 | 97.2 (4) |
W6—O5—W5 | 92.3 (2) | O12—W6—O11 | 152.4 (3) |
W1—O6—W6 | 97.2 (3) | O23—W6—O6 | 157.6 (4) |
W2—O7—W1 | 118.9 (3) | O24—W6—O6 | 97.6 (3) |
W3—O8—W2 | 112.4 (4) | O12—W6—O6 | 72.9 (3) |
W4—O9—W3 | 121.8 (4) | O11—W6—O6 | 84.1 (3) |
W4—O10—W5 | 111.4 (3) | O23—W6—O5 | 88.4 (4) |
W5—O11—W6 | 122.2 (4) | O24—W6—O5 | 164.7 (3) |
W6—O12—W1 | 113.0 (4) | O12—W6—O5 | 86.7 (3) |
W1—Pt—W2 | 61.15 (3) | O11—W6—O5 | 71.5 (3) |
W1—Pt—W3 | 119.79 (3) | O6—W6—O5 | 71.5 (2) |
W2—Pt—W3 | 58.68 (3) | Na2—Na1—Na6i | 154.7 (2) |
W1—Pt—W4 | 173.46 (2) | Na3—Na2—Na1 | 175.4 (2) |
W2—Pt—W4 | 119.86 (4) | Na4—Na3—Na2 | 98.7 (3) |
W3—Pt—W4 | 61.35 (3) | Na3—Na4—Na5 | 177.2 (3) |
W1—Pt—W6 | 58.85 (3) | Na4v—Na5—Na6 | 90.7 (1) |
W2—Pt—W6 | 119.78 (3) | Na4—Na5—Na6 | 89.3 (1) |
W3—Pt—W6 | 173.11 (2) | Na6ii—Na6—Na5 | 112.1 (2) |
W4—Pt—W6 | 119.14 (3) | O23—Na1—O25 | 82.1 (4) |
W1—Pt—W5 | 119.84 (4) | O23—Na1—O29 | 87.3 (5) |
W2—Pt—W5 | 172.14 (2) | O25—Na1—O29 | 168.8 (5) |
W3—Pt—W5 | 119.39 (3) | O23—Na1—O26 | 97.7 (4) |
W4—Pt—W5 | 58.16 (3) | O25—Na1—O26 | 87.6 (4) |
W6—Pt—W5 | 61.08 (3) | O29—Na1—O26 | 90.2 (4) |
W6—W1—W2 | 121.21 (3) | O23—Na1—O27 | 175.6 (5) |
W3—W2—W1 | 119.77 (3) | O25—Na1—O27 | 98.4 (5) |
W2—W3—W4 | 119.95 (4) | O29—Na1—O27 | 91.8 (5) |
W5—W4—W3 | 119.93 (3) | O26—Na1—O27 | 77.9 (5) |
W4—W5—W6 | 120.02 (3) | O23—Na1—O28 | 87.8 (4) |
W1—W6—W5 | 119.06 (4) | O25—Na1—O28 | 92.9 (4) |
O2—Pt—O6 | 95.6 (3) | O29—Na1—O28 | 90.4 (4) |
O2—Pt—O4 | 96.3 (3) | O26—Na1—O28 | 174.5 (5) |
O6—Pt—O4 | 96.5 (3) | O27—Na1—O28 | 96.6 (5) |
O2—Pt—O5 | 177.4 (3) | O23—Na1—Na2 | 81.5 (3) |
O6—Pt—O5 | 82.4 (3) | O22—Na2—O30 | 164.2 (4) |
O4—Pt—O5 | 82.3 (3) | O22—Na2—O28 | 97.7 (4) |
O2—Pt—O3 | 82.9 (3) | O30—Na2—O28 | 97.1 (4) |
O6—Pt—O3 | 177.5 (3) | O22—Na2—O31 | 86.3 (4) |
O4—Pt—O3 | 81.7 (3) | O30—Na2—O31 | 78.9 (4) |
O5—Pt—O3 | 99.1 (3) | O28—Na2—O31 | 176.0 (4) |
O2—Pt—O1 | 83.0 (3) | O22—Na2—O32 | 89.1 (3) |
O6—Pt—O1 | 82.6 (3) | O30—Na2—O32 | 85.5 (4) |
O4—Pt—O1 | 178.8 (3) | O28—Na2—O32 | 90.1 (3) |
O5—Pt—O1 | 98.3 (3) | O31—Na2—O32 | 89.9 (3) |
O3—Pt—O1 | 99.1 (3) | O22—Na2—O29 | 95.7 (4) |
O13—W1—O14 | 103.4 (4) | O30—Na2—O29 | 89.7 (4) |
O13—W1—O7 | 93.8 (3) | O28—Na2—O29 | 90.0 (4) |
O14—W1—O7 | 99.9 (3) | O31—Na2—O29 | 89.7 (4) |
O13—W1—O12 | 99.2 (4) | O32—Na2—O29 | 175.1 (4) |
O14—W1—O12 | 96.3 (3) | O20iii—Na3—O32 | 158.5 (4) |
O7—W1—O12 | 156.2 (3) | O20iii—Na3—O33 | 115.3 (4) |
O13—W1—O6 | 96.0 (3) | O32—Na3—O33 | 84.8 (4) |
O14—W1—O6 | 159.3 (3) | O20iii—Na3—O31 | 86.3 (3) |
O7—W1—O6 | 85.5 (3) | O32—Na3—O31 | 91.2 (4) |
O12—W1—O6 | 73.4 (3) | O33—Na3—O31 | 77.9 (4) |
O13—W1—O1 | 163.8 (3) | O20iii—Na3—O35 | 78.4 (3) |
O14—W1—O1 | 88.5 (3) | O32—Na3—O35 | 84.3 (3) |
O7—W1—O1 | 73.1 (3) | O33—Na3—O35 | 159.9 (4) |
O12—W1—O1 | 90.2 (3) | O31—Na3—O35 | 119.1 (4) |
O6—W1—O1 | 74.0 (2) | O20iii—Na3—O34 | 98.8 (4) |
O16—W2—O15 | 104.8 (4) | O32—Na3—O34 | 88.9 (4) |
O16—W2—O7 | 98.1 (3) | O33—Na3—O34 | 87.6 (4) |
O15—W2—O7 | 100.6 (3) | O31—Na3—O34 | 165.5 (4) |
O16—W2—O8 | 99.2 (3) | O35—Na3—O34 | 75.3 (4) |
O15—W2—O8 | 94.1 (3) | O37—Na4—O17iv | 100.0 (5) |
O7—W2—O8 | 153.5 (3) | O37—Na4—O35 | 97.0 (5) |
O16—W2—O2 | 94.8 (3) | O17iv—Na4—O35 | 161.7 (6) |
O15—W2—O2 | 158.3 (3) | O37—Na4—O34 | 134.2 (7) |
O7—W2—O2 | 85.4 (3) | O17iv—Na4—O34 | 94.3 (4) |
O8—W2—O2 | 73.4 (3) | O35—Na4—O34 | 78.5 (4) |
O16—W2—O1 | 164.6 (3) | O37—Na4—O36 | 83.8 (6) |
O15—W2—O1 | 88.9 (3) | O17iv—Na4—O36 | 91.7 (5) |
O7—W2—O1 | 72.1 (3) | O35—Na4—O36 | 83.2 (4) |
O8—W2—O1 | 86.4 (3) | O34—Na4—O36 | 139.2 (5) |
O2—W2—O1 | 73.0 (2) | O37—Na4—O32 | 144.8 (7) |
O17—W3—O18 | 105.5 (4) | O17iv—Na4—O32 | 85.2 (4) |
O17—W3—O8 | 101.5 (4) | O35—Na4—O32 | 76.9 (4) |
O18—W3—O8 | 94.8 (3) | O34—Na4—O32 | 79.3 (4) |
O17—W3—O9 | 96.3 (3) | O36—Na4—O32 | 61.1 (4) |
O18—W3—O9 | 100.0 (3) | O37v—Na5—O37 | 180.00 (7) |
O8—W3—O9 | 152.9 (3) | O37v—Na5—O38 | 91.1 (5) |
O17—W3—O2 | 96.0 (3) | O37—Na5—O38 | 88.9 (5) |
O18—W3—O2 | 157.2 (3) | O37v—Na5—O38v | 88.9 (5) |
O8—W3—O2 | 73.1 (3) | O37—Na5—O38v | 91.1 (5) |
O9—W3—O2 | 84.9 (3) | O38—Na5—O38v | 180.000 (1) |
O17—W3—O3 | 163.2 (3) | O37v—Na5—O39v | 77.9 (4) |
O18—W3—O3 | 87.8 (3) | O37—Na5—O39v | 102.1 (4) |
O8—W3—O3 | 87.2 (3) | O38—Na5—O39v | 83.0 (4) |
O9—W3—O3 | 70.9 (3) | O38v—Na5—O39v | 97.0 (4) |
O2—W3—O3 | 72.7 (2) | O37v—Na5—O39 | 102.1 (4) |
O20—W4—O19 | 105.7 (4) | O37—Na5—O39 | 77.9 (4) |
O20—W4—O9 | 97.3 (4) | O38—Na5—O39 | 97.0 (4) |
O19—W4—O9 | 100.6 (4) | O38v—Na5—O39 | 83.0 (4) |
O20—W4—O10 | 100.9 (3) | O39v—Na5—O39 | 180.0 (5) |
O19—W4—O10 | 93.6 (4) | O18—Na6—O25vi | 172.4 (4) |
O9—W4—O10 | 153.0 (3) | O18—Na6—O19 | 89.9 (3) |
O20—W4—O4 | 96.1 (3) | O25vi—Na6—O19 | 96.9 (4) |
O19—W4—O4 | 156.2 (3) | O18—Na6—O18ii | 85.9 (3) |
O9—W4—O4 | 85.9 (3) | O25vi—Na6—O18ii | 87.6 (3) |
O10—W4—O4 | 72.5 (3) | O19—Na6—O18ii | 172.0 (4) |
O20—W4—O3 | 163.4 (3) | O18—Na6—O40 | 80.8 (4) |
O19—W4—O3 | 88.2 (3) | O25vi—Na6—O40 | 95.6 (5) |
O9—W4—O3 | 70.7 (3) | O19—Na6—O40 | 92.6 (4) |
O10—W4—O3 | 87.1 (3) | O18ii—Na6—O40 | 93.5 (4) |
O4—W4—O3 | 72.2 (2) | O18—Na6—O39 | 90.5 (4) |
O21—W5—O22 | 104.7 (4) | O25vi—Na6—O39 | 92.7 (4) |
O21—W5—O11 | 98.8 (4) | O19—Na6—O39 | 90.5 (4) |
O22—W5—O11 | 100.0 (4) | O18ii—Na6—O39 | 82.7 (4) |
O21—W5—O10 | 100.6 (4) | O40—Na6—O39 | 170.8 (5) |
O22—W5—O10 | 94.7 (4) | Pt—O1—W1 | 99.1 (3) |
O11—W5—O10 | 151.8 (3) | Pt—O1—W2 | 98.6 (3) |
O21—W5—O4 | 98.0 (3) | Pt—O2—W2 | 105.3 (3) |
O22—W5—O4 | 155.7 (4) | Pt—O2—W3 | 104.7 (3) |
O11—W5—O4 | 84.7 (3) | Pt—O3—W3 | 99.7 (3) |
O10—W5—O4 | 72.5 (3) | Pt—O3—W4 | 99.6 (3) |
O21—W5—O5 | 165.6 (3) | Pt—O4—W5 | 107.0 (3) |
O22—W5—O5 | 87.3 (4) | Pt—O4—W4 | 106.4 (3) |
O11—W5—O5 | 70.8 (3) | Pt—O5—W6 | 99.9 (3) |
O10—W5—O5 | 86.1 (3) | Pt—O5—W5 | 99.0 (3) |
O4—W5—O5 | 71.6 (2) | Pt—O6—W1 | 104.4 (3) |
O23—W6—O24 | 103.9 (4) | Pt—O6—W6 | 106.1 (3) |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+2, −z; (iii) −x+2, −y+2, −z+1; (iv) x+1, y, z; (v) −x+2, −y+2, −z; (vi) x, y+1, z. |
D—H···A | D···A |
O1···O1vii | 2.60 (1) |
O3···O14vii | 2.56 (1) |
O5···O15vii | 2.60 (1) |
O25···O8vii | 2.82 (1) |
O25···O23 | 3.04 (2) |
O25···O38i | 2.90 (2) |
O26···O19i | 2.90 (1) |
O26···O21viii | 2.84 (1) |
O26···O27 | 3.05 (2) |
O26···O31viii | 2.80 (1) |
O27···O13iv | 2.68 (2) |
O27···O37i | 2.80 (2) |
O27···O41iv | 2.76 (2) |
O28···O7iv | 2.83 (1) |
O28···O15vii | 2.96 (1) |
O29···O11viii | 3.04 (1) |
O29···O29viii | 2.95 (2) |
O30···O6iv | 2.73 (1) |
O30···O31 | 3.05 (1) |
O30···O33 | 2.93 (1) |
O30···O41iv | 2.83 (1) |
O31···O24viii | 2.90 (1) |
O31···O33 | 3.08 (1) |
O32···O2iv | 2.80 (1) |
O32···O36 | 2.81 (2) |
O33···O4iv | 2.82 (1) |
O33···O34ix | 2.80 (2) |
O34···O9iv | 2.82 (1) |
O34···O35 | 3.03 (1) |
O35···O10 | 2.81 (1) |
O35···O20iii | 3.06 (1) |
O35···O21iii | 2.91 (1) |
O36···O10 | 2.83 (1) |
O36···O15vii | 3.01 (1) |
O36···O16iv | 2.98 (1) |
O37···O19 | 3.06 (2) |
O38···O16ii | 3.07 (2) |
O38···O17ii | 3.00 (2) |
O39···O14vii | 3.03 (1) |
O40···O12vi | 2.98 (2) |
Symmetry codes: (i) x, y−1, z; (ii) −x+1, −y+2, −z; (iii) −x+2, −y+2, −z+1; (iv) x+1, y, z; (vi) x, y+1, z; (vii) −x+1, −y+1, −z; (viii) −x+2, −y+1, −z+1; (ix) −x+3, −y+2, −z+1. |
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