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In the title compound, C6H13N2+·H2AsO4·H2O, the component species inter­act by way of N—H...O, O—H...O and O—H...N hydrogen bonds, resulting in a layered structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807009178/ng2222sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807009178/ng2222Isup2.hkl
Contains datablock I

CCDC reference: 643066

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.026
  • wR factor = 0.065
  • Data-to-parameter ratio = 18.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 300 Deg.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997), and SORTAV (Blessing, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

4-Aza-1-azoniabicyclo[2.2.2]octane dihydrogenarsenate monohydrate top
Crystal data top
C6H13N2+·AsH2O4·H2OZ = 2
Mr = 272.14F(000) = 280
Triclinic, P1Dx = 1.736 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.9515 (3) ÅCell parameters from 2217 reflections
b = 9.0103 (4) Åθ = 2.9–27.5°
c = 9.2845 (4) ŵ = 3.27 mm1
α = 91.710 (3)°T = 120 K
β = 103.604 (3)°Slab, colourless
γ = 111.720 (3)°0.24 × 0.14 × 0.04 mm
V = 520.67 (4) Å3
Data collection top
Nonius KappaCCD
diffractometer
2380 independent reflections
Radiation source: fine-focus sealed tube2231 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
ω scansθmax = 27.6°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Bruker, 1999)
h = 98
Tmin = 0.508, Tmax = 0.881k = 1111
10518 measured reflectionsl = 1212
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difmap (O-H, N-H) and geom (C-H)
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0224P)2 + 0.5077P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max < 0.001
2380 reflectionsΔρmax = 0.54 e Å3
128 parametersΔρmin = 0.78 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.021 (2)
Special details top

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
As10.65267 (3)0.14830 (2)0.72146 (2)0.01423 (10)
O10.9047 (2)0.19882 (19)0.82113 (16)0.0186 (3)
O20.6216 (3)0.21008 (19)0.55540 (16)0.0205 (3)
O30.5391 (3)0.2245 (2)0.83434 (17)0.0222 (4)
H10.43790.25790.78260.027*
O40.5219 (3)0.05686 (18)0.70824 (17)0.0206 (3)
H20.48790.09520.60850.025*
O50.2508 (3)0.3304 (2)0.71010 (17)0.0222 (4)
H30.14050.29980.74710.027*
H40.20330.33380.61010.027*
N10.1288 (3)0.3163 (2)0.3963 (2)0.0167 (4)
N20.0109 (3)0.2613 (2)0.11375 (19)0.0150 (4)
H50.03270.24130.00990.018*
C10.0228 (4)0.1409 (3)0.3478 (2)0.0185 (5)
H1A0.09590.09350.39540.022*
H1B0.12740.09010.38020.022*
C20.3179 (4)0.3838 (3)0.3351 (2)0.0180 (4)
H2A0.42760.34180.38170.022*
H2B0.38200.50260.35930.022*
C30.0227 (4)0.3922 (3)0.3374 (2)0.0174 (4)
H3A0.04310.50830.37650.021*
H3B0.15420.34230.37170.021*
C40.0667 (4)0.1060 (3)0.1762 (2)0.0215 (5)
H4A0.01610.02880.13530.026*
H4B0.22560.05830.14890.026*
C50.2512 (4)0.3377 (3)0.1639 (2)0.0218 (5)
H5A0.30470.43490.11440.026*
H5B0.31310.26120.13730.026*
C60.0825 (4)0.3718 (3)0.1651 (2)0.0241 (5)
H6A0.24050.32570.12450.029*
H6B0.02410.47770.12940.029*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
As10.01670 (14)0.01544 (13)0.00860 (13)0.00522 (9)0.00178 (9)0.00091 (8)
O10.0156 (7)0.0257 (8)0.0112 (7)0.0058 (7)0.0017 (6)0.0017 (6)
O20.0307 (9)0.0160 (8)0.0107 (7)0.0064 (7)0.0022 (6)0.0008 (6)
O30.0268 (9)0.0324 (9)0.0134 (8)0.0195 (8)0.0035 (7)0.0009 (7)
O40.0297 (9)0.0137 (7)0.0117 (7)0.0028 (7)0.0025 (7)0.0003 (6)
O50.0194 (8)0.0346 (10)0.0153 (8)0.0121 (7)0.0063 (7)0.0057 (7)
N10.0197 (9)0.0177 (9)0.0124 (9)0.0069 (7)0.0046 (7)0.0015 (7)
N20.0177 (9)0.0155 (9)0.0097 (8)0.0053 (7)0.0019 (7)0.0007 (7)
C10.0227 (11)0.0155 (10)0.0166 (11)0.0065 (9)0.0055 (9)0.0033 (8)
C20.0160 (10)0.0216 (11)0.0134 (10)0.0053 (9)0.0019 (8)0.0006 (8)
C30.0213 (11)0.0189 (11)0.0116 (10)0.0077 (9)0.0042 (9)0.0000 (8)
C40.0284 (12)0.0161 (11)0.0171 (11)0.0049 (9)0.0072 (10)0.0003 (8)
C50.0169 (11)0.0289 (13)0.0142 (11)0.0030 (9)0.0043 (9)0.0003 (9)
C60.0299 (13)0.0359 (14)0.0121 (10)0.0219 (11)0.0015 (9)0.0028 (9)
Geometric parameters (Å, º) top
As1—O21.6483 (15)C1—C41.544 (3)
As1—O11.6598 (15)C1—H1A0.9900
As1—O31.7151 (15)C1—H1B0.9900
As1—O41.7172 (15)C2—C51.545 (3)
O3—H10.9068C2—H2A0.9900
O4—H20.9217C2—H2B0.9900
O5—H30.8686C3—C61.543 (3)
O5—H40.9152C3—H3A0.9900
N1—C31.470 (3)C3—H3B0.9900
N1—C11.477 (3)C4—H4A0.9900
N1—C21.483 (3)C4—H4B0.9900
N2—C41.491 (3)C5—H5A0.9900
N2—C61.495 (3)C5—H5B0.9900
N2—C51.499 (3)C6—H6A0.9900
N2—H50.9300C6—H6B0.9900
O2—As1—O1115.74 (8)N1—C2—H2B109.6
O2—As1—O3112.12 (8)C5—C2—H2B109.6
O1—As1—O3104.37 (8)H2A—C2—H2B108.1
O2—As1—O4111.19 (8)N1—C3—C6110.66 (17)
O1—As1—O4108.29 (8)N1—C3—H3A109.5
O3—As1—O4104.32 (8)C6—C3—H3A109.5
As1—O3—H1113.1N1—C3—H3B109.5
As1—O4—H2105.9C6—C3—H3B109.5
H3—O5—H4108.2H3A—C3—H3B108.1
C3—N1—C1109.10 (17)N2—C4—C1108.00 (17)
C3—N1—C2108.82 (17)N2—C4—H4A110.1
C1—N1—C2109.11 (17)C1—C4—H4A110.1
C4—N2—C6109.75 (18)N2—C4—H4B110.1
C4—N2—C5109.68 (18)C1—C4—H4B110.1
C6—N2—C5110.04 (18)H4A—C4—H4B108.4
C4—N2—H5109.1N2—C5—C2107.90 (17)
C6—N2—H5109.1N2—C5—H5A110.1
C5—N2—H5109.1C2—C5—H5A110.1
N1—C1—C4110.59 (18)N2—C5—H5B110.1
N1—C1—H1A109.5C2—C5—H5B110.1
C4—C1—H1A109.5H5A—C5—H5B108.4
N1—C1—H1B109.5N2—C6—C3108.04 (19)
C4—C1—H1B109.5N2—C6—H6A110.1
H1A—C1—H1B108.1C3—C6—H6A110.1
N1—C2—C5110.42 (17)N2—C6—H6B110.1
N1—C2—H2A109.6C3—C6—H6B110.1
C5—C2—H2A109.6H6A—C6—H6B108.4
C3—N1—C1—C454.7 (2)N1—C1—C4—N27.9 (3)
C2—N1—C1—C464.1 (2)C4—N2—C5—C265.7 (2)
C3—N1—C2—C564.9 (2)C6—N2—C5—C255.1 (2)
C1—N1—C2—C554.1 (2)N1—C2—C5—N28.7 (3)
C1—N1—C3—C663.9 (2)C4—N2—C6—C356.1 (2)
C2—N1—C3—C655.1 (2)C5—N2—C6—C364.7 (2)
C6—N2—C4—C164.9 (2)N1—C3—C6—N27.7 (3)
C5—N2—C4—C156.1 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H1···O50.911.682.579 (2)172
O4—H2···O2i0.921.662.554 (2)164
O5—H3···O1ii0.871.862.718 (2)170
O5—H4···N10.921.922.821 (2)170
N2—H5···O1iii0.931.702.627 (2)175
C2—H2A···O20.992.473.420 (3)161
C4—H4A···O1i0.992.463.330 (3)147
Symmetry codes: (i) x+1, y, z+1; (ii) x1, y, z; (iii) x1, y, z1.
 

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