Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802017828/ya6115sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802017828/ya6115Isup2.hkl |
CCDC reference: 194631
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- H-atom completeness 93%
- R factor = 0.020
- wR factor = 0.046
- Data-to-parameter ratio = 16.1
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry General Notes
FORMU_01 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:C24 H52 N2 O6 W1 Atom count from the _atom_site data: C24 H48 N2 O6 W1 ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.664 Tmax scaled 0.664 Tmin scaled 0.502 CELLZ_01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C24 H52 N2 O6 W TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 96.00 96.00 0.00 H 208.00 192.00 16.00 N 8.00 8.00 0.00 O 24.00 24.00 0.00 W 4.00 4.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional? REFLT_03 From the CIF: _diffrn_reflns_theta_max 25.00 From the CIF: _reflns_number_total 1243 Count of symmetry unique reflns 711 Completeness (_total/calc) 174.82% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 532 Fraction of Friedel pairs measured 0.748 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
Data collection: SMART (Siemens, 1994); cell refinement: SADABS (Siemens, 1996); data reduction: SAINT (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1996); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
(C12H24N)2[WO4]·2H2O | Dx = 1.500 Mg m−3 |
Mr = 648.54 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I42d | Cell parameters from 109 reflections |
a = 12.7053 (8) Å | θ = 2.0–25.0° |
c = 17.6737 (15) Å | µ = 4.09 mm−1 |
V = 2853.0 (4) Å3 | T = 293 K |
Z = 4 | Prism, colorless |
F(000) = 1328 | 0.45 × 0.15 × 0.10 mm |
Siemens SMART CCD diffractometer | 1243 independent reflections |
Radiation source: fine-focus sealed tube | 1106 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
ω scans | θmax = 25.0°, θmin = 2.0° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −9→15 |
Tmin = 0.756, Tmax = 1.000 | k = −14→9 |
3260 measured reflections | l = −19→20 |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.020 | w = 1/[σ2(Fo2) + (0.0129P)2 + 8.2983P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.046 | (Δ/σ)max < 0.001 |
S = 1.05 | Δρmax = 0.78 e Å−3 |
1243 reflections | Δρmin = −0.50 e Å−3 |
77 parameters | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00374 (15) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack, 1983 |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.020 (19) |
Experimental. empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) |
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 | ||
W | 1.0000 | 0.5000 | 0.2500 | 0.02651 (13) | |
O | 1.1098 (3) | 0.4674 (3) | 0.3071 (2) | 0.0493 (10) | |
O01 | 1.2500 | 0.3148 (6) | 0.3750 | 0.099 (3) | |
N | 1.1048 (4) | 0.2500 | 0.1250 | 0.0337 (13) | |
HN | 1.0627 | 0.2044 | 0.1005 | 0.040* | |
C1 | 1.1652 (4) | 0.1892 (4) | 0.1835 (3) | 0.0377 (12) | |
H1 | 1.2082 | 0.2386 | 0.2128 | 0.045* | |
C2 | 1.0850 (5) | 0.1374 (5) | 0.2369 (3) | 0.0499 (15) | |
H2A | 1.0383 | 0.0923 | 0.2080 | 0.060* | |
H2B | 1.0427 | 0.1914 | 0.2611 | 0.060* | |
C3 | 1.1420 (5) | 0.0718 (5) | 0.2978 (3) | 0.0563 (16) | |
H3A | 1.1833 | 0.1181 | 0.3297 | 0.068* | |
H3B | 1.0903 | 0.0368 | 0.3294 | 0.068* | |
C4 | 1.2134 (4) | −0.0096 (6) | 0.2621 (3) | 0.0562 (15) | |
H4A | 1.1715 | −0.0601 | 0.2340 | 0.067* | |
H4B | 1.2511 | −0.0474 | 0.3014 | 0.067* | |
C5 | 1.2928 (5) | 0.0439 (5) | 0.2085 (4) | 0.0606 (17) | |
H5A | 1.3385 | 0.0896 | 0.2376 | 0.073* | |
H5B | 1.3362 | −0.0095 | 0.1847 | 0.073* | |
C6 | 1.2375 (4) | 0.1082 (4) | 0.1475 (3) | 0.0487 (14) | |
H6A | 1.2895 | 0.1435 | 0.1163 | 0.058* | |
H6B | 1.1968 | 0.0618 | 0.1164 | 0.058* |
U11 | U22 | U33 | U12 | U13 | U23 | |
W | 0.02543 (14) | 0.02543 (14) | 0.02869 (17) | 0.000 | 0.000 | 0.000 |
O | 0.038 (2) | 0.048 (3) | 0.062 (2) | −0.0021 (15) | −0.0272 (17) | 0.0067 (17) |
O01 | 0.085 (6) | 0.049 (4) | 0.162 (9) | 0.000 | −0.048 (6) | 0.000 |
N | 0.027 (3) | 0.035 (3) | 0.039 (3) | 0.000 | 0.000 | −0.006 (3) |
C1 | 0.036 (3) | 0.034 (3) | 0.043 (3) | −0.002 (2) | −0.003 (2) | −0.006 (2) |
C2 | 0.046 (3) | 0.050 (3) | 0.054 (4) | 0.001 (3) | 0.013 (3) | −0.002 (3) |
C3 | 0.064 (4) | 0.058 (4) | 0.046 (3) | 0.003 (3) | 0.007 (3) | 0.011 (3) |
C4 | 0.064 (3) | 0.043 (3) | 0.062 (3) | 0.012 (4) | −0.007 (2) | 0.015 (5) |
C5 | 0.049 (3) | 0.068 (4) | 0.065 (4) | 0.018 (3) | 0.003 (3) | 0.010 (3) |
C6 | 0.042 (3) | 0.051 (3) | 0.053 (3) | 0.006 (3) | 0.007 (3) | 0.006 (3) |
W—Oi | 1.771 (3) | C2—H2B | 0.9700 |
W—Oii | 1.771 (3) | C3—C4 | 1.514 (9) |
W—Oiii | 1.771 (3) | C3—H3A | 0.9700 |
W—O | 1.771 (3) | C3—H3B | 0.9700 |
N—C1 | 1.502 (6) | C4—C5 | 1.541 (8) |
N—C1iv | 1.502 (6) | C4—H4A | 0.9700 |
N—HN | 0.900 | C4—H4B | 0.9700 |
C1—C6 | 1.519 (7) | C5—C6 | 1.524 (8) |
C1—C2 | 1.538 (7) | C5—H5A | 0.9700 |
C1—H1 | 0.9800 | C5—H5B | 0.9700 |
C2—C3 | 1.542 (8) | C6—H6A | 0.9700 |
C2—H2A | 0.9700 | C6—H6B | 0.9700 |
Oi—W—Oii | 110.5 (3) | C2—C3—H3A | 109.4 |
Oi—W—Oiii | 108.94 (13) | C4—C3—H3B | 109.4 |
Oii—W—Oiii | 108.94 (13) | C2—C3—H3B | 109.4 |
Oi—W—O | 108.94 (13) | H3A—C3—H3B | 108.0 |
Oii—W—O | 108.94 (13) | C3—C4—C5 | 110.3 (6) |
Oiii—W—O | 110.5 (3) | C3—C4—H4A | 109.6 |
C1—N—C1iv | 118.5 (6) | C5—C4—H4A | 109.6 |
C1—N—HN | 107.7 | C3—C4—H4B | 109.6 |
C1iv—N—HN | 107.7 | C5—C4—H4B | 109.6 |
N—C1—C6 | 111.7 (4) | H4A—C4—H4B | 108.1 |
N—C1—C2 | 107.7 (4) | C6—C5—C4 | 111.7 (5) |
C6—C1—C2 | 111.6 (4) | C6—C5—H5A | 109.3 |
N—C1—H1 | 108.6 | C4—C5—H5A | 109.3 |
C6—C1—H1 | 108.6 | C6—C5—H5B | 109.3 |
C2—C1—H1 | 108.6 | C4—C5—H5B | 109.3 |
C1—C2—C3 | 110.4 (5) | H5A—C5—H5B | 107.9 |
C1—C2—H2A | 109.6 | C1—C6—C5 | 110.2 (5) |
C3—C2—H2A | 109.6 | C1—C6—H6A | 109.6 |
C1—C2—H2B | 109.6 | C5—C6—H6A | 109.6 |
C3—C2—H2B | 109.6 | C1—C6—H6B | 109.6 |
H2A—C2—H2B | 108.1 | C5—C6—H6B | 109.6 |
C4—C3—C2 | 111.1 (5) | H6A—C6—H6B | 108.1 |
C4—C3—H3A | 109.4 |
Symmetry codes: (i) y+1/2, −x+3/2, −z+1/2; (ii) −y+3/2, x−1/2, −z+1/2; (iii) −x+2, −y+1, z; (iv) x, −y+1/2, −z+1/4. |