Download citation
Download citation
link to html
A novel ammonium 1,6-hexane­di­ammonium dodecatungstate, (NH4)2(NH3(CH2)6NH3)4[H2W12O42]·8H2O, contains centrosymmetric [H2W12O42]10- anions separated by the ammonium and 1,6-hexane­di­ammonium cations, and water mol­ecules, in a pseudo-layer structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802015799/tk6077sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802015799/tk6077Isup2.hkl
Contains datablock I

CCDC reference: 198293

Key indicators

  • Single-crystal synchrotron study
  • T = 100 K
  • Mean [sigma](C-C) = 0.018 Å
  • H-atom completeness 49%
  • R factor = 0.038
  • wR factor = 0.103
  • Data-to-parameter ratio = 20.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
ATOM_007 Alert A _atom_site_aniso_label is missing Unique label identifying the atom site.
Author response: All atoms were refined with isotropic thermal parameters.
REFLT_03
         From the CIF: _diffrn_reflns_theta_max           30.00
         From the CIF: _reflns_number_total               3953
         TEST2: Reflns within _diffrn_reflns_theta_max
         Count of symmetry unique reflns         4709
         Completeness (_total/calc)             83.95%
          Alert A: < 85% complete (theta max?)

THETM_01  Alert A The value of sine(theta_max)/wavelength is less than 0.550
          Calculated sin(theta_max)/wavelength =    0.5432
Author response: The CCD detector plate was placed as close to the crystal as was practicable (55 cm); this limited the maximum theta_max value.

Yellow Alert Alert Level C:
PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 21 General Notes
FORMU_01 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: C12 H49 N5 O25 W6 Atom count from _chemical_formula_moiety: 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:C12 H49 N5 O25 W6 Atom count from the _atom_site data: C12 H24 N5 O25 W6 ABSMU_01 Radiation type not identified. Calculation of _exptl_absorpt_correction_mu not performed. CELLZ_01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C12 H49 N5 O25 W6 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 24.00 24.00 0.00 H 98.00 48.00 50.00 N 10.00 10.00 0.00 O 50.00 50.00 0.00 W 12.00 12.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional? CHEMW_03 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 1766.66 TEST: Calculate formula weight from _atom_site_* atom mass num sum O 16.00 25.00 399.97 H 1.01 24.00 24.19 C 12.01 12.00 144.13 N 14.01 5.00 70.04 W 183.85 6.00 1103.10 Calculated formula weight 1741.43 The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01
3 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

The title compound, (I), was prepared as part of a study into the use of organic amine inter-layer spacer molecules for inorganic oxide-layered compounds. The crystal structure comprises [H2W12O42]10− anions bound in an infinite three-dimensional network through hydrogen bonding with 1,6-hexanediammonium2+ and NH4+ cations and water molecules, as shown in Fig. 1. There are at least 34 contacts between the anion oxygen atoms, amine nitrogen atoms and water O atoms within normal hydrogen-bonding distances, e.g. O6···O3W 2.814 (12) Å. Other minor intermolecular interactions are also found, e.g. C11—H···O3 with C11···O3 3.38 (2) Å (Spek, 1990).

The anions are centrosymmetric, and the final cell composition is inferred from the analytical data and chemically reasonable refinement options, since the X-ray scattering of hydrogen atoms cannot be determined unambiguously in the presence of the W atoms. The atom-numbering scheme for the anion follows that in (NH4)10[H2W12O42].10H2O (Allman, 1971). A closely related six-ammonium cation (NH4)6[H6W12O42].10H2O structure has been reported by Averbuch-Pouchot et al. (1979) and a decasodium diglycine [H2W12O42]10− salt recently by Naruke et al. (2000).

The 1,6-hexanediammonium cations, which are aligned approximately along the c axial direction, can be considered to separate the anions by the length of the molecule along this axis. By contrast, the other 1,6-hexanediammonium cations, aligned along the b axis (end-on in Fig. 1), separate the anions by the width of the molecule. This pseudo-layer packing is reflected in the platey nature of the crystals.

Experimental top

The compound was prepared by the reaction of H2WO4 with diaminohexane in an ammonia (0.1 N) solution uder flowing nitrogen gas. The product was precipitated by evaporating to dryness at 353 K [Calc. N 3.96%, Found 3.71, 3.90%].

Refinement top

All non-hydrogen atoms were refined with isotropic thermal parameters. H atoms on the 1,6-hexanediammonium carbon atoms were constrained in calculated positions (C—H 0.99 Å) to ride on their parent atom, with a Uiso 1.2 times the Ueq of the parent atom. No other H atoms were located. The largest residual electron density peak was located in the vicinity of the W atom.

Computing details top

Data collection: DENZO (Otinowski & Minor, 1997); cell refinement: DENZO; data reduction: DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1]
[Figure 2]
Fig. 1. A view of the [H2W12O42]10− anion, showing atom labels (Farrugia, 1997); centrosymmetrically related atoms are not labelled. Atoms are shown with arbitrary sizes; the H atoms were not located. Fig. 2. Cell packing diagram of (I), viewed down the b axis. (Farrugia, 1997). All atoms have arbitrary radii, in reducing size order W,O,N,C. H atoms on the 1,6-hexanediammonium cations are excluded for clarity.
(I) top
Crystal data top
2(NH4)4(C6H18N2)[H2W12O42].8H2OZ = 2
Mr = 1766.66F(000) = 1582
Triclinic, P1Dx = 3.319 Mg m3
a = 10.987 (2) ÅSynchrotron radiation, λ = 0.9204 Å
b = 10.980 (2) ÅCell parameters from 340 reflections
c = 14.681 (3) Åθ = 3.8–22.5°
α = 85.99 (3)°µ = 37.82 mm1
β = 84.85 (3)°T = 100 K
γ = 87.69 (3)°Plate, colourless
V = 1758.6 (6) Å30.35 × 0.08 × 0.03 mm
Data collection top
Quantum4 CCD detector
diffractometer
3953 independent reflections
None monochromator3937 reflections with I > 2σ(I)
Detector resolution: 4000 pixels mm-1Rint = 0.066
ϕ scanθmax = 30.0°, θmin = 2.9°
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
h = 011
Tmin = 0.033, Tmax = 0.389k = 1110
3953 measured reflectionsl = 1415
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.103H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0454P)2 + 33.4374P]
where P = (Fo2 + 2Fc2)/3
3953 reflections(Δ/σ)max = 0.001
193 parametersΔρmax = 2.74 e Å3
0 restraintsΔρmin = 2.77 e Å3
Crystal data top
2(NH4)4(C6H18N2)[H2W12O42].8H2Oγ = 87.69 (3)°
Mr = 1766.66V = 1758.6 (6) Å3
Triclinic, P1Z = 2
a = 10.987 (2) ÅSynchrotron radiation, λ = 0.9204 Å
b = 10.980 (2) ŵ = 37.82 mm1
c = 14.681 (3) ÅT = 100 K
α = 85.99 (3)°0.35 × 0.08 × 0.03 mm
β = 84.85 (3)°
Data collection top
Quantum4 CCD detector
diffractometer
3953 independent reflections
Absorption correction: multi-scan
DENZO-SMN (Otwinowski & Minor, 1997)
3937 reflections with I > 2σ(I)
Tmin = 0.033, Tmax = 0.389Rint = 0.066
3953 measured reflectionsθmax = 30.0°
Refinement top
R[F2 > 2σ(F2)] = 0.0380 restraints
wR(F2) = 0.103H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0454P)2 + 33.4374P]
where P = (Fo2 + 2Fc2)/3
3953 reflectionsΔρmax = 2.74 e Å3
193 parametersΔρmin = 2.77 e Å3
Special details top

Experimental. The incomplete shell of data is all the available data accessible using the highest wavelength possible on the NSLS X9B beamline, with the CCD detector plate placed as close to the crystal as was practicable (55 cm). Crystal decay was monitored and corrected by the inter-frame analysis (DENZO: Otwinowski & Minor (1997).

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
W10.43522 (4)0.74176 (4)0.54171 (3)0.00210 (17)*
W20.67251 (4)0.75027 (4)0.38351 (3)0.00252 (17)*
W30.41623 (4)0.62649 (4)0.33707 (3)0.00217 (17)*
W40.27348 (4)0.53869 (4)0.72785 (3)0.00295 (17)*
W50.75556 (4)0.66461 (4)0.61806 (3)0.00280 (17)*
W60.52814 (4)0.66651 (4)0.77835 (3)0.00332 (17)*
O10.3635 (7)0.7476 (7)0.4258 (5)0.0037 (17)*
O20.5685 (7)0.8384 (7)0.4662 (5)0.0047 (17)*
O30.5528 (7)0.7491 (7)0.3021 (5)0.0041 (17)*
O40.3629 (7)0.8694 (7)0.5872 (5)0.0062 (18)*
O50.3295 (7)0.6781 (7)0.2469 (5)0.0067 (18)*
O60.7707 (7)0.8614 (7)0.3341 (5)0.0070 (18)*
O70.5409 (6)0.6102 (7)0.4496 (5)0.0031 (17)*
O80.3424 (7)0.6147 (7)0.5896 (5)0.0050 (17)*
O90.5601 (6)0.7070 (7)0.6248 (5)0.0018 (17)*
O100.7575 (7)0.6916 (7)0.4907 (5)0.0044 (17)*
O110.7463 (7)0.6035 (7)0.3328 (5)0.0029 (17)*
O120.5262 (7)0.5124 (7)0.2769 (5)0.0041 (17)*
O130.3241 (7)0.5141 (7)0.4007 (5)0.0024 (17)*
O140.3584 (6)0.6831 (7)0.7578 (5)0.0027 (17)*
O150.6928 (7)0.6136 (7)0.7436 (5)0.0030 (17)*
O160.7938 (7)0.8110 (7)0.6442 (5)0.0058 (17)*
O170.8960 (7)0.5803 (7)0.6205 (5)0.0040 (17)*
O180.1338 (7)0.6131 (7)0.7143 (5)0.0065 (18)*
O190.2510 (7)0.4760 (7)0.8402 (5)0.0084 (18)*
O200.5481 (7)0.8205 (7)0.7935 (5)0.0048 (17)*
O210.5196 (7)0.5992 (7)0.8901 (5)0.0051 (17)*
O1W0.2264 (8)0.1242 (8)0.1278 (6)0.018 (2)*
O2W0.0211 (7)0.1956 (7)0.2419 (5)0.0114 (19)*
O3W0.9926 (8)0.8085 (8)0.2310 (6)0.016 (2)*
O4W1.2179 (8)0.9161 (8)0.2522 (6)0.019 (2)*
N70.3966 (9)0.0094 (10)0.3721 (7)0.015 (2)*
N10.7858 (9)1.0991 (10)0.2400 (7)0.012 (2)*
C10.7729 (11)1.0442 (11)0.1514 (8)0.010 (3)*
H1A0.68621.05130.13780.012*
H1B0.79670.95620.15720.012*
C20.8531 (11)1.1074 (11)0.0712 (8)0.011 (3)*
H2A0.94021.09070.08150.013*
H2B0.83771.07090.01370.013*
C30.8305 (11)1.2435 (11)0.0594 (8)0.012 (3)*
H3A0.86121.28210.11150.014*
H3B0.74131.26130.06100.014*
C40.8929 (12)1.3005 (12)0.0311 (9)0.016 (3)*
H4A0.98261.29630.02790.019*
H4B0.87421.25210.08220.019*
C50.8512 (11)1.4340 (11)0.0512 (8)0.012 (3)*
H5A0.76271.43700.05970.014*
H5B0.86281.48050.00260.014*
C60.9192 (12)1.4956 (12)0.1355 (8)0.014 (3)*
H6A0.88751.58080.14450.017*
H6B1.00711.49780.12590.017*
N20.9046 (9)1.4289 (9)0.2201 (7)0.012 (2)*
N30.5613 (9)0.6362 (10)0.0734 (7)0.016 (2)*
C110.5691 (12)0.7707 (12)0.0708 (9)0.018 (3)*
H11A0.64060.79690.02920.022*
H11B0.58070.79580.13290.022*
C120.4544 (11)0.8318 (11)0.0380 (8)0.012 (3)*
H12A0.38350.80250.07890.015*
H12B0.44440.80640.02420.015*
C130.4525 (11)0.9708 (12)0.0349 (9)0.014 (3)*
H13A0.46620.99620.09650.017*
H13B0.37031.00250.02050.017*
N50.1151 (8)0.6115 (9)0.5068 (6)0.005 (2)*
C210.0709 (10)0.7224 (10)0.4535 (8)0.005 (3)*
H21A0.01230.70970.43590.006*
H21B0.12560.73690.39670.006*
C220.0686 (10)0.8338 (10)0.5112 (8)0.006 (3)*
H22A0.02740.81210.57260.007*
H22B0.15380.85390.51940.007*
C230.0034 (11)0.9473 (11)0.4690 (9)0.014 (3)*
H23A0.04750.97270.40940.017*
H23B0.08050.92650.45750.017*
Geometric parameters (Å, º) top
W1—O41.729 (8)W5—O92.173 (7)
W1—O81.824 (8)W5—O13i2.224 (8)
W1—O91.927 (7)W6—O201.746 (8)
W1—O11.935 (7)W6—O211.748 (7)
W1—O22.042 (8)W6—O151.914 (7)
W1—O72.263 (7)W6—O141.916 (7)
W2—O61.738 (8)W6—O92.266 (7)
W2—O31.856 (7)W6—O12i2.298 (8)
W2—O21.882 (7)O11—W4i1.880 (8)
W2—O111.940 (7)O12—W4i2.245 (7)
W2—O101.958 (7)O12—W6i2.298 (8)
W2—O72.262 (7)O13—W5i2.224 (8)
W3—O51.749 (7)N1—C11.492 (16)
W3—O131.786 (7)C1—C21.547 (16)
W3—O121.911 (7)C2—C31.506 (17)
W3—O11.961 (7)C3—C41.544 (17)
W3—O32.063 (8)C4—C51.534 (17)
W3—O72.233 (7)C5—C61.518 (17)
W4—O181.730 (7)C6—N21.509 (16)
W4—O191.742 (8)N3—C111.481 (17)
W4—O11i1.880 (8)C11—C121.506 (17)
W4—O141.967 (8)C12—C131.523 (18)
W4—O82.220 (7)C13—C13ii1.52 (2)
W4—O12i2.245 (7)N5—C211.489 (14)
W5—O161.754 (8)C21—C221.534 (16)
W5—O171.769 (7)C22—C231.533 (16)
W5—O101.871 (7)C23—C23iii1.52 (2)
W5—O151.961 (7)
O4—W1—O8104.6 (3)O16—W5—O17103.2 (3)
O4—W1—O9100.8 (3)O16—W5—O1098.7 (3)
O8—W1—O993.8 (3)O17—W5—O1097.4 (3)
O4—W1—O199.6 (3)O16—W5—O1595.0 (3)
O8—W1—O192.7 (3)O17—W5—O1595.9 (3)
O9—W1—O1156.3 (3)O10—W5—O15158.1 (3)
O4—W1—O294.2 (3)O16—W5—O994.4 (3)
O8—W1—O2161.1 (3)O17—W5—O9160.7 (3)
O9—W1—O283.7 (3)O10—W5—O987.4 (3)
O1—W1—O282.8 (3)O15—W5—O974.6 (3)
O4—W1—O7164.7 (3)O16—W5—O13i169.8 (3)
O8—W1—O788.2 (3)O17—W5—O13i85.1 (3)
O9—W1—O786.4 (3)O10—W5—O13i85.9 (3)
O1—W1—O771.0 (3)O15—W5—O13i78.1 (3)
O2—W1—O773.0 (3)O9—W5—O13i76.7 (3)
O6—W2—O3103.7 (3)O20—W6—O21103.4 (3)
O6—W2—O2102.3 (3)O20—W6—O15100.8 (3)
O3—W2—O291.9 (3)O21—W6—O1596.8 (3)
O6—W2—O11101.8 (3)O20—W6—O1496.3 (3)
O3—W2—O1189.0 (3)O21—W6—O14101.0 (3)
O2—W2—O11154.9 (3)O15—W6—O14151.7 (3)
O6—W2—O10100.9 (3)O20—W6—O989.1 (3)
O3—W2—O10155.2 (3)O21—W6—O9165.5 (3)
O2—W2—O1085.7 (3)O15—W6—O973.3 (3)
O11—W2—O1083.2 (3)O14—W6—O984.6 (3)
O6—W2—O7178.3 (3)O20—W6—O12i163.5 (3)
O3—W2—O776.1 (3)O21—W6—O12i90.9 (3)
O2—W2—O776.0 (3)O15—W6—O12i85.5 (3)
O11—W2—O780.0 (3)O14—W6—O12i72.5 (3)
O10—W2—O779.4 (3)O9—W6—O12i77.9 (3)
O5—W3—O13104.0 (3)W1—O1—W3119.6 (4)
O5—W3—O12100.4 (3)W2—O2—W1116.2 (4)
O13—W3—O1295.6 (3)W2—O3—W3115.7 (4)
O5—W3—O1100.0 (3)W3—O7—W295.2 (3)
O13—W3—O190.9 (3)W3—O7—W197.0 (3)
O12—W3—O1156.3 (3)W2—O7—W194.8 (3)
O5—W3—O394.5 (3)W1—O8—W4137.1 (4)
O13—W3—O3161.1 (3)W1—O9—W5138.4 (4)
O12—W3—O384.8 (3)W1—O9—W6125.9 (3)
O1—W3—O381.8 (3)W5—O9—W695.1 (3)
O5—W3—O7165.4 (3)W5—O10—W2149.0 (4)
O13—W3—O788.2 (3)W4i—O11—W2148.1 (4)
O12—W3—O786.2 (3)W3—O12—W4i137.2 (4)
O1—W3—O771.2 (3)W3—O12—W6i125.4 (4)
O3—W3—O772.9 (3)W4i—O12—W6i94.8 (3)
O18—W4—O19101.4 (4)W3—O13—W5i139.5 (4)
O18—W4—O11i100.2 (3)W6—O14—W4118.9 (4)
O19—W4—O11i98.2 (3)W6—O15—W5115.4 (4)
O18—W4—O1496.2 (3)N1—C1—C2111.9 (10)
O19—W4—O1495.9 (3)C3—C2—C1114.1 (10)
O11i—W4—O14155.8 (3)C2—C3—C4112.9 (10)
O18—W4—O889.5 (3)C5—C4—C3112.6 (10)
O19—W4—O8168.2 (3)C6—C5—C4113.7 (10)
O11i—W4—O884.1 (3)N2—C6—C5111.4 (11)
O14—W4—O878.4 (3)N3—C11—C12110.4 (10)
O18—W4—O12i164.4 (3)C11—C12—C13114.4 (10)
O19—W4—O12i90.9 (3)C12—C13—C13ii114.2 (14)
O11i—W4—O12i87.4 (3)N5—C21—C22110.1 (9)
O14—W4—O12i72.8 (3)C23—C22—C21113.8 (10)
O8—W4—O12i77.6 (3)C23iii—C23—C22112.0 (13)
O4—W1—O1—W3177.1 (4)O17—W5—O9—W199.9 (10)
O8—W1—O1—W377.5 (4)O10—W5—O9—W15.4 (6)
O9—W1—O1—W328.2 (10)O15—W5—O9—W1162.1 (7)
O2—W1—O1—W384.1 (4)O13i—W5—O9—W181.0 (6)
O7—W1—O1—W39.6 (4)O16—W5—O9—W685.4 (3)
O5—W3—O1—W1177.6 (4)O17—W5—O9—W670.8 (10)
O13—W3—O1—W178.1 (4)O10—W5—O9—W6176.0 (3)
O12—W3—O1—W128.3 (10)O15—W5—O9—W68.5 (3)
O3—W3—O1—W184.4 (4)O13i—W5—O9—W689.6 (3)
O7—W3—O1—W19.7 (4)O20—W6—O9—W195.0 (5)
O6—W2—O2—W1179.9 (4)O21—W6—O9—W1115.1 (12)
O3—W2—O2—W175.7 (4)O15—W6—O9—W1163.5 (5)
O11—W2—O2—W115.9 (9)O14—W6—O9—W11.5 (5)
O10—W2—O2—W179.6 (4)O12i—W6—O9—W174.6 (4)
O7—W2—O2—W10.6 (3)O20—W6—O9—W592.7 (3)
O4—W1—O2—W2172.0 (4)O21—W6—O9—W557.2 (13)
O8—W1—O2—W24.4 (12)O15—W6—O9—W58.8 (3)
O9—W1—O2—W287.6 (4)O14—W6—O9—W5170.8 (3)
O1—W1—O2—W272.8 (4)O12i—W6—O9—W597.7 (3)
O7—W1—O2—W20.6 (3)O16—W5—O10—W283.9 (9)
O6—W2—O3—W3180.0 (4)O17—W5—O10—W2171.4 (8)
O2—W2—O3—W376.8 (4)O15—W5—O10—W244.3 (14)
O11—W2—O3—W378.1 (4)O9—W5—O10—W210.2 (9)
O10—W2—O3—W36.8 (10)O13i—W5—O10—W287.0 (9)
O7—W2—O3—W31.8 (3)O6—W2—O10—W5121.9 (9)
O5—W3—O3—W2174.1 (4)O3—W2—O10—W564.9 (13)
O13—W3—O3—W26.5 (12)O2—W2—O10—W520.2 (9)
O12—W3—O3—W285.8 (4)O11—W2—O10—W5137.3 (9)
O1—W3—O3—W274.7 (4)O7—W2—O10—W556.3 (8)
O7—W3—O3—W21.9 (3)O6—W2—O11—W4i129.6 (8)
O5—W3—O7—W233.4 (13)O3—W2—O11—W4i25.8 (8)
O13—W3—O7—W2179.9 (3)O2—W2—O11—W4i66.4 (11)
O12—W3—O7—W284.3 (3)O10—W2—O11—W4i130.7 (8)
O1—W3—O7—W288.3 (3)O7—W2—O11—W4i50.2 (7)
O3—W3—O7—W21.4 (3)O5—W3—O12—W4i137.5 (6)
O5—W3—O7—W162.2 (13)O13—W3—O12—W4i117.1 (6)
O13—W3—O7—W184.3 (3)O1—W3—O12—W4i11.8 (12)
O12—W3—O7—W1179.9 (3)O3—W3—O12—W4i43.9 (5)
O1—W3—O7—W17.3 (3)O7—W3—O12—W4i29.3 (5)
O3—W3—O7—W194.2 (3)O5—W3—O12—W6i66.2 (5)
O3—W2—O7—W31.5 (3)O13—W3—O12—W6i39.2 (5)
O2—W2—O7—W397.0 (3)O1—W3—O12—W6i144.6 (6)
O11—W2—O7—W389.9 (3)O3—W3—O12—W6i159.8 (4)
O10—W2—O7—W3174.8 (3)O7—W3—O12—W6i127.0 (4)
O3—W2—O7—W196.0 (3)O5—W3—O13—W5i61.9 (6)
O2—W2—O7—W10.5 (3)O12—W3—O13—W5i40.3 (6)
O11—W2—O7—W1172.6 (3)O1—W3—O13—W5i162.5 (6)
O10—W2—O7—W187.7 (3)O3—W3—O13—W5i130.8 (8)
O4—W1—O7—W361.0 (12)O7—W3—O13—W5i126.4 (6)
O8—W1—O7—W386.1 (3)O20—W6—O14—W4176.7 (4)
O9—W1—O7—W3179.9 (3)O21—W6—O14—W478.4 (4)
O1—W1—O7—W37.4 (3)O15—W6—O14—W449.6 (8)
O2—W1—O7—W395.5 (3)O9—W6—O14—W488.1 (4)
O4—W1—O7—W234.9 (13)O12i—W6—O14—W49.1 (3)
O8—W1—O7—W2178.0 (3)O18—W4—O14—W6178.0 (4)
O9—W1—O7—W284.1 (3)O19—W4—O14—W679.9 (4)
O1—W1—O7—W288.5 (3)O11i—W4—O14—W645.5 (9)
O2—W1—O7—W20.4 (2)O8—W4—O14—W689.8 (4)
O4—W1—O8—W455.0 (6)O12i—W4—O14—W69.3 (4)
O9—W1—O8—W447.3 (6)O20—W6—O15—W575.0 (4)
O1—W1—O8—W4155.6 (6)O21—W6—O15—W5179.9 (4)
O2—W1—O8—W4128.8 (8)O14—W6—O15—W551.1 (8)
O7—W1—O8—W4133.5 (6)O9—W6—O15—W510.8 (3)
O18—W4—O8—W199.1 (6)O12i—W6—O15—W589.5 (4)
O19—W4—O8—W158.7 (18)O16—W5—O15—W682.0 (4)
O11i—W4—O8—W1160.6 (6)O17—W5—O15—W6174.1 (4)
O14—W4—O8—W12.7 (5)O10—W5—O15—W646.8 (10)
O12i—W4—O8—W172.0 (6)O9—W5—O15—W611.2 (4)
O4—W1—O9—W5132.6 (6)O13i—W5—O15—W690.4 (4)
O8—W1—O9—W5121.8 (6)N1—C1—C2—C355.3 (13)
O1—W1—O9—W516.2 (12)C1—C2—C3—C4169.1 (10)
O2—W1—O9—W539.5 (6)C2—C3—C4—C5169.6 (10)
O7—W1—O9—W533.8 (6)C3—C4—C5—C6174.9 (11)
O4—W1—O9—W659.0 (5)C4—C5—C6—N258.7 (14)
O8—W1—O9—W646.7 (5)N3—C11—C12—C13178.8 (10)
O1—W1—O9—W6152.2 (6)C11—C12—C13—C13ii65.7 (17)
O2—W1—O9—W6152.1 (5)N5—C21—C22—C23169.7 (10)
O7—W1—O9—W6134.6 (4)C21—C22—C23—C23iii176.6 (12)
O16—W5—O9—W1104.0 (6)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y+2, z; (iii) x, y+2, z+1.

Experimental details

Crystal data
Chemical formula2(NH4)4(C6H18N2)[H2W12O42].8H2O
Mr1766.66
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)10.987 (2), 10.980 (2), 14.681 (3)
α, β, γ (°)85.99 (3), 84.85 (3), 87.69 (3)
V3)1758.6 (6)
Z2
Radiation typeSynchrotron, λ = 0.9204 Å
µ (mm1)37.82
Crystal size (mm)0.35 × 0.08 × 0.03
Data collection
DiffractometerQuantum4 CCD detector
diffractometer
Absorption correctionMulti-scan
DENZO-SMN (Otwinowski & Minor, 1997)
Tmin, Tmax0.033, 0.389
No. of measured, independent and
observed [I > 2σ(I)] reflections
3953, 3953, 3937
Rint0.066
θmax (°)30.0
(sin θ/λ)max1)0.543
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.103, 1.09
No. of reflections3953
No. of parameters193
H-atom treatmentH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0454P)2 + 33.4374P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)2.74, 2.77

Computer programs: DENZO (Otinowski & Minor, 1997), DENZO, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), SHELXL97.

Selected geometric parameters (Å, º) top
W1—O41.729 (8)W1—O22.042 (8)
W1—O81.824 (8)W1—O72.263 (7)
W1—O91.927 (7)W6—O12i2.298 (8)
W1—O11.935 (7)O11—W4i1.880 (8)
O4—W1—O8104.6 (3)O4—W1—O199.6 (3)
O4—W1—O9100.8 (3)O8—W1—O192.7 (3)
O8—W1—O993.8 (3)O9—W1—O1156.3 (3)
Symmetry code: (i) x+1, y+1, z+1.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds