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The crystal structure of the title complex is built of di­cyclo­hexyl­ammonium cations, [NH2(C6H11)2]+, orthotungstate dianions, [WO4]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 \overline 4 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802017828/ya6115sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802017828/ya6115Isup2.hkl
Contains datablock I

CCDC reference: 194631

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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.

Computing details top

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]·2H2ODx = 1.500 Mg m3
Mr = 648.54Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I42dCell parameters from 109 reflections
a = 12.7053 (8) Åθ = 2.0–25.0°
c = 17.6737 (15) ŵ = 4.09 mm1
V = 2853.0 (4) Å3T = 293 K
Z = 4Prism, colorless
F(000) = 13280.45 × 0.15 × 0.10 mm
Data collection top
Siemens SMART CCD
diffractometer
1243 independent reflections
Radiation source: fine-focus sealed tube1106 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
ω scansθmax = 25.0°, θmin = 2.0°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 915
Tmin = 0.756, Tmax = 1.000k = 149
3260 measured reflectionsl = 1920
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-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 = 1.05Δρmax = 0.78 e Å3
1243 reflectionsΔρmin = 0.50 e Å3
77 parametersExtinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00374 (15)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack, 1983
Secondary atom site location: difference Fourier mapAbsolute 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
xyzUiso*/Ueq
W1.00000.50000.25000.02651 (13)
O1.1098 (3)0.4674 (3)0.3071 (2)0.0493 (10)
O011.25000.3148 (6)0.37500.099 (3)
N1.1048 (4)0.25000.12500.0337 (13)
HN1.06270.20440.10050.040*
C11.1652 (4)0.1892 (4)0.1835 (3)0.0377 (12)
H11.20820.23860.21280.045*
C21.0850 (5)0.1374 (5)0.2369 (3)0.0499 (15)
H2A1.03830.09230.20800.060*
H2B1.04270.19140.26110.060*
C31.1420 (5)0.0718 (5)0.2978 (3)0.0563 (16)
H3A1.18330.11810.32970.068*
H3B1.09030.03680.32940.068*
C41.2134 (4)0.0096 (6)0.2621 (3)0.0562 (15)
H4A1.17150.06010.23400.067*
H4B1.25110.04740.30140.067*
C51.2928 (5)0.0439 (5)0.2085 (4)0.0606 (17)
H5A1.33850.08960.23760.073*
H5B1.33620.00950.18470.073*
C61.2375 (4)0.1082 (4)0.1475 (3)0.0487 (14)
H6A1.28950.14350.11630.058*
H6B1.19680.06180.11640.058*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W0.02543 (14)0.02543 (14)0.02869 (17)0.0000.0000.000
O0.038 (2)0.048 (3)0.062 (2)0.0021 (15)0.0272 (17)0.0067 (17)
O010.085 (6)0.049 (4)0.162 (9)0.0000.048 (6)0.000
N0.027 (3)0.035 (3)0.039 (3)0.0000.0000.006 (3)
C10.036 (3)0.034 (3)0.043 (3)0.002 (2)0.003 (2)0.006 (2)
C20.046 (3)0.050 (3)0.054 (4)0.001 (3)0.013 (3)0.002 (3)
C30.064 (4)0.058 (4)0.046 (3)0.003 (3)0.007 (3)0.011 (3)
C40.064 (3)0.043 (3)0.062 (3)0.012 (4)0.007 (2)0.015 (5)
C50.049 (3)0.068 (4)0.065 (4)0.018 (3)0.003 (3)0.010 (3)
C60.042 (3)0.051 (3)0.053 (3)0.006 (3)0.007 (3)0.006 (3)
Geometric parameters (Å, º) top
W—Oi1.771 (3)C2—H2B0.9700
W—Oii1.771 (3)C3—C41.514 (9)
W—Oiii1.771 (3)C3—H3A0.9700
W—O1.771 (3)C3—H3B0.9700
N—C11.502 (6)C4—C51.541 (8)
N—C1iv1.502 (6)C4—H4A0.9700
N—HN0.900C4—H4B0.9700
C1—C61.519 (7)C5—C61.524 (8)
C1—C21.538 (7)C5—H5A0.9700
C1—H10.9800C5—H5B0.9700
C2—C31.542 (8)C6—H6A0.9700
C2—H2A0.9700C6—H6B0.9700
Oi—W—Oii110.5 (3)C2—C3—H3A109.4
Oi—W—Oiii108.94 (13)C4—C3—H3B109.4
Oii—W—Oiii108.94 (13)C2—C3—H3B109.4
Oi—W—O108.94 (13)H3A—C3—H3B108.0
Oii—W—O108.94 (13)C3—C4—C5110.3 (6)
Oiii—W—O110.5 (3)C3—C4—H4A109.6
C1—N—C1iv118.5 (6)C5—C4—H4A109.6
C1—N—HN107.7C3—C4—H4B109.6
C1iv—N—HN107.7C5—C4—H4B109.6
N—C1—C6111.7 (4)H4A—C4—H4B108.1
N—C1—C2107.7 (4)C6—C5—C4111.7 (5)
C6—C1—C2111.6 (4)C6—C5—H5A109.3
N—C1—H1108.6C4—C5—H5A109.3
C6—C1—H1108.6C6—C5—H5B109.3
C2—C1—H1108.6C4—C5—H5B109.3
C1—C2—C3110.4 (5)H5A—C5—H5B107.9
C1—C2—H2A109.6C1—C6—C5110.2 (5)
C3—C2—H2A109.6C1—C6—H6A109.6
C1—C2—H2B109.6C5—C6—H6A109.6
C3—C2—H2B109.6C1—C6—H6B109.6
H2A—C2—H2B108.1C5—C6—H6B109.6
C4—C3—C2111.1 (5)H6A—C6—H6B108.1
C4—C3—H3A109.4
Symmetry codes: (i) y+1/2, x+3/2, z+1/2; (ii) y+3/2, x1/2, z+1/2; (iii) x+2, y+1, z; (iv) x, y+1/2, z+1/4.
 

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