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The crystal structure of the title complex is built of dicyclohexylammonium cations, [NH
2(C
6H
11)
2]
+, orthotungstate dianions, [WO
4]
2-, and lattice water molecules. The cations and coordinated water molecules occupy special positions on twofold axes; the tetrahedral orthotungstate dianion is located on a
axis. Hydrogen bonds involving all N- and O-bound H atoms link the cations, anions and water molecules into an infinite three-dimensional aggregate. The crystal is isostructural with its molybdenum analog [Thiele & Fuchs (1979).
Z. Naturforsch. Teil B,
34, 145-154].
Supporting information
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.
Bis(dicyclohexylammonium) tungstate dihydrate
top
Crystal data top
(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 |
Data collection top
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 top
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) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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* | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |
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