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The title compound, (C6H5CH2NH3)2[HAsO4]·H2O, contains a network of benzyl­ammonium cations, hydrogenarsenate anions [dav(As—O) = 1.689 (2) Å] and water mol­ecules. The crystal packing involves N—H...O [dav(H...O) = 1.91 Å, θav(N—H...O) = 167° and dav(N...O) = 2.794 (3) Å] and O—H...O [dav(H...O) = 1.83 Å, θav(O—H...O) = 173° and dav(O...O) = 2.729 (3) Å] hydrogen bonds, resulting in a layered structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803026242/su6056sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803026242/su6056Isup2.hkl
Contains datablock I

CCDC reference: 227757

Key indicators

  • Single-crystal X-ray study
  • T = 120 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.045
  • wR factor = 0.112
  • Data-to-parameter ratio = 24.3

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ..... = 5
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.122 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12 PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.02 PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 13 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.72 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.09 Ratio PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.40 PLAT301_ALERT_3_C Main Residue Disorder ......................... 21.00 Perc. PLAT757_ALERT_4_C D...A Calc 2.82305, Rep 2.823(3) ...... Senseless su N2 -O5 1.555 1.555 PLAT757_ALERT_4_C D...A Calc 2.73141, Rep 2.731(3) ...... Senseless su O5 -O3 1.555 1.455 PLAT757_ALERT_4_C D...A Calc 2.82515, Rep 2.825(2) ...... Senseless su O5 -O2 1.555 2.656 PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.12 Ratio PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.40 Deg. C9B -C8 -C9A 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 15 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 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Enraf-Nonius, 1999); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and ATOMS (Shape software, 1999); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
(C7H10N)2[HAsO4]·H2OZ = 2
Mr = 374.26F(000) = 388
Triclinic, P1Dx = 1.483 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.4400 (2) ÅCell parameters from 24435 reflections
b = 8.9128 (3) Åθ = 2.9–27.5°
c = 14.9957 (5) ŵ = 2.05 mm1
α = 99.7048 (11)°T = 120 K
β = 93.1574 (12)°Plate, colourless
γ = 97.7776 (18)°0.35 × 0.12 × 0.03 mm
V = 837.93 (5) Å3
Data collection top
Enraf-Nonius KappaCCD
diffractometer
3846 independent reflections
Radiation source: fine-focus sealed tube3538 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.122
ω and φ scansθmax = 27.5°, θmin = 2.9°
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
h = 88
Tmin = 0.534, Tmax = 0.941k = 1111
18359 measured reflectionsl = 1919
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.112 w = 1/[σ2(Fo2) + (0.0281P)2 + 2.1999P]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.001
3846 reflectionsΔρmax = 1.39 e Å3
158 parametersΔρmin = 0.69 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*/UeqOcc. (<1)
As10.79069 (5)0.27362 (3)0.455577 (19)0.01615 (13)
O10.5423 (3)0.3057 (2)0.44548 (14)0.0206 (4)
O20.8133 (3)0.0866 (2)0.43007 (14)0.0199 (4)
O30.9006 (3)0.3503 (2)0.56046 (14)0.0198 (4)
O40.9323 (4)0.3618 (3)0.37887 (14)0.0242 (5)
H10.99630.45630.40270.029*
N10.2439 (4)0.0543 (3)0.41567 (17)0.0191 (5)
H40.24820.00790.46520.023*
H50.11220.07670.40480.023*
H60.33750.14280.42610.023*
C10.3001 (5)0.0517 (4)0.3348 (2)0.0219 (6)
H100.20910.15240.32820.026*
H110.44770.06870.34470.026*
C20.2742 (5)0.0126 (3)0.2489 (2)0.0225 (6)
C30.4443 (7)0.0443 (5)0.1989 (3)0.0355 (8)
H120.58060.02920.21980.043*
C40.4147 (8)0.0988 (5)0.1177 (3)0.0438 (10)
H130.53140.11910.08320.053*
C50.2200 (8)0.1232 (5)0.0871 (2)0.0421 (10)
H140.20150.16030.03190.050*
C60.0526 (8)0.0937 (6)0.1370 (3)0.0593 (15)
H150.08270.11140.11640.071*
C70.0783 (7)0.0382 (6)0.2174 (3)0.0470 (11)
H160.03970.01750.25110.056*
N20.5536 (4)0.4647 (3)0.64221 (17)0.0208 (5)
H70.50980.52320.60270.025*
H80.45000.38550.64460.025*
H90.67080.42660.62320.025*
C80.6026 (2)0.56092 (16)0.73401 (9)0.0285 (7)
H170.47680.60710.75270.034*
H180.71670.64600.73120.034*
C9A0.6777 (2)0.47374 (16)0.80588 (9)0.023 (3)*0.50
C10A0.8731 (2)0.42391 (16)0.80400 (9)0.0350 (15)*0.596 (7)
H10A0.96190.44410.75750.042*0.596 (7)
C11A0.9386 (2)0.34449 (16)0.87007 (9)0.0428 (17)*0.596 (7)
H11A1.07220.31040.86880.051*0.596 (7)
C12A0.8088 (2)0.31491 (16)0.93803 (9)0.049 (2)*0.596 (7)
H12A0.85360.26060.98320.059*0.596 (7)
C13A0.6134 (2)0.36474 (16)0.93991 (9)0.0471 (19)*0.596 (7)
H13A0.52470.34450.98640.057*0.596 (7)
C14A0.5479 (2)0.44416 (16)0.87384 (9)0.0403 (17)*0.596 (7)
H14A0.41440.47820.87510.048*0.596 (7)
C9B0.6550 (2)0.46838 (16)0.80328 (9)0.028 (3)*0.50
C10B0.8649 (2)0.47486 (16)0.83297 (9)0.034 (2)*0.404 (7)
H10B0.97160.53400.80700.041*0.404 (7)
C11B0.9186 (2)0.39476 (16)0.90066 (9)0.033 (2)*0.404 (7)
H11B1.06210.39920.92100.040*0.404 (7)
C12B0.7625 (2)0.30818 (16)0.93865 (9)0.027 (2)*0.404 (7)
H12B0.79930.25340.98490.033*0.404 (7)
C13B0.5527 (2)0.30170 (16)0.90895 (9)0.030 (2)*0.404 (7)
H13B0.44600.24250.93490.036*0.404 (7)
C14B0.4989 (2)0.38179 (16)0.84127 (9)0.0250 (19)*0.404 (7)
H14B0.35550.37740.82100.030*0.404 (7)
O50.2125 (2)0.22976 (16)0.64252 (9)0.0247 (5)
H20.09660.26190.61140.030*
H30.20190.13370.62270.030*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
As10.02293 (19)0.00932 (18)0.01604 (18)0.00171 (11)0.00122 (11)0.00244 (11)
O10.0236 (11)0.0138 (10)0.0238 (11)0.0024 (8)0.0011 (9)0.0032 (8)
O20.0276 (11)0.0085 (9)0.0233 (11)0.0041 (8)0.0021 (9)0.0007 (8)
O30.0272 (11)0.0123 (10)0.0182 (10)0.0002 (8)0.0023 (8)0.0012 (8)
O40.0338 (13)0.0158 (10)0.0201 (11)0.0056 (9)0.0068 (9)0.0006 (8)
N10.0233 (13)0.0141 (12)0.0201 (12)0.0010 (10)0.0003 (10)0.0057 (10)
C10.0302 (16)0.0152 (14)0.0207 (15)0.0041 (12)0.0037 (12)0.0034 (11)
C20.0322 (17)0.0156 (14)0.0175 (14)0.0014 (12)0.0008 (12)0.0012 (11)
C30.047 (2)0.035 (2)0.0308 (18)0.0178 (17)0.0169 (16)0.0113 (15)
C40.069 (3)0.038 (2)0.032 (2)0.016 (2)0.026 (2)0.0133 (17)
C50.071 (3)0.030 (2)0.0209 (17)0.0076 (19)0.0081 (18)0.0076 (14)
C60.048 (3)0.077 (4)0.054 (3)0.019 (2)0.024 (2)0.044 (3)
C70.032 (2)0.066 (3)0.045 (2)0.0119 (19)0.0092 (17)0.037 (2)
N20.0300 (14)0.0135 (12)0.0196 (12)0.0052 (10)0.0020 (10)0.0031 (10)
C80.051 (2)0.0137 (15)0.0203 (15)0.0066 (14)0.0046 (14)0.0011 (12)
O50.0300 (12)0.0138 (10)0.0292 (12)0.0031 (9)0.0025 (9)0.0022 (9)
Geometric parameters (Å, º) top
As1—O11.666 (2)C8—C9A1.5252
As1—O21.675 (2)C8—H170.9900
As1—O31.681 (2)C8—H180.9900
As1—O41.732 (2)C9A—C10A1.3900
O4—H10.8919C9A—C14A1.3900
N1—C11.499 (4)C10A—C11A1.3900
N1—H40.9100C10A—H10A0.9500
N1—H50.9100C11A—C12A1.3900
N1—H60.9100C11A—H11A0.9500
C1—C21.506 (4)C12A—C13A1.3900
C1—H100.9900C12A—H12A0.9500
C1—H110.9900C13A—C14A1.3900
C2—C71.384 (5)C13A—H13A0.9500
C2—C31.385 (5)C14A—H14A0.9500
C3—C41.398 (6)C9B—C10B1.3900
C3—H120.9500C9B—C14B1.3900
C4—C51.369 (6)C10B—C11B1.3900
C4—H130.9500C10B—H10B0.9500
C5—C61.367 (7)C11B—C12B1.3900
C5—H140.9500C11B—H11B0.9500
C6—C71.389 (6)C12B—C13B1.3900
C6—H150.9500C12B—H12B0.9500
C7—H160.9500C13B—C14B1.3900
N2—C81.487 (3)C13B—H13B0.9500
N2—H70.9100C14B—H14B0.9500
N2—H80.9100O5—H20.9595
N2—H90.9100O5—H30.8499
C8—C9B1.4829
O1—As1—O2112.66 (11)N2—C8—C9A113.84 (11)
O1—As1—O3110.23 (11)C9B—C8—H17106.8
O2—As1—O3110.89 (10)N2—C8—H17109.0
O1—As1—O4109.09 (11)C9A—C8—H17110.1
O2—As1—O4105.84 (10)C9B—C8—H18112.1
O3—As1—O4107.92 (11)N2—C8—H18109.1
As1—O4—H1113.0C9A—C8—H18106.8
C1—N1—H4109.5H17—C8—H18107.8
C1—N1—H5109.5C10A—C9A—C14A120.0
H4—N1—H5109.5C10A—C9A—C8120.9
C1—N1—H6109.5C14A—C9A—C8119.1
H4—N1—H6109.5C11A—C10A—C9A120.0
H5—N1—H6109.5C11A—C10A—H10A120.0
N1—C1—C2111.8 (2)C9A—C10A—H10A120.0
N1—C1—H10109.3C10A—C11A—C12A120.0
C2—C1—H10109.3C10A—C11A—H11A120.0
N1—C1—H11109.3C12A—C11A—H11A120.0
C2—C1—H11109.3C13A—C12A—C11A120.0
H10—C1—H11107.9C13A—C12A—H12A120.0
C7—C2—C3118.8 (3)C11A—C12A—H12A120.0
C7—C2—C1120.4 (3)C14A—C13A—C12A120.0
C3—C2—C1120.9 (3)C14A—C13A—H13A120.0
C2—C3—C4119.8 (4)C12A—C13A—H13A120.0
C2—C3—H12120.1C13A—C14A—C9A120.0
C4—C3—H12120.1C13A—C14A—H14A120.0
C5—C4—C3120.9 (4)C9A—C14A—H14A120.0
C5—C4—H13119.5C10B—C9B—C14B120.0
C3—C4—H13119.5C10B—C9B—C8118.6
C6—C5—C4119.3 (4)C14B—C9B—C8121.4
C6—C5—H14120.3C9B—C10B—C11B120.0
C4—C5—H14120.3C9B—C10B—H10B120.0
C5—C6—C7120.6 (4)C11B—C10B—H10B120.0
C5—C6—H15119.7C12B—C11B—C10B120.0
C7—C6—H15119.7C12B—C11B—H11B120.0
C2—C7—C6120.6 (4)C10B—C11B—H11B120.0
C2—C7—H16119.7C13B—C12B—C11B120.0
C6—C7—H16119.7C13B—C12B—H12B120.0
C8—N2—H7109.5C11B—C12B—H12B120.0
C8—N2—H8109.5C12B—C13B—C14B120.0
H7—N2—H8109.5C12B—C13B—H13B120.0
C8—N2—H9109.5C14B—C13B—H13B120.0
H7—N2—H9109.5C13B—C14B—C9B120.0
H8—N2—H9109.5C13B—C14B—H14B120.0
C9B—C8—N2111.92 (11)C9B—C14B—H14B120.0
C9B—C8—C9A5.4H2—O5—H3104.7
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4—H1···O3i0.891.742.632 (3)173
N1—H4···O2ii0.911.942.830 (3)166
N1—H5···O2iii0.911.992.843 (3)155
N1—H6···O10.911.802.704 (3)174
N2—H7···O1iv0.911.862.731 (3)161
N2—H8···O50.911.922.823 (3)174
N2—H9···O30.911.942.835 (3)169
O5—H2···O3iii0.961.782.731 (3)171
O5—H3···O2ii0.851.982.825 (2)176
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y, z+1; (iii) x1, y, z; (iv) x+1, y+1, z+1.
 

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