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The cation and anion in the title salt, C6H22N44+·2SO42-·H2O, lie on special positions of site symmetry m and the water mol­ecule on a special position of site symmetry 2/m. The cations, anions and water mol­ecules are linked by hydrogen bonds into a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805005477/bt6608sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805005477/bt6608Isup2.hkl
Contains datablock I

CCDC reference: 269394

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.006 Å
  • Disorder in main residue
  • R factor = 0.070
  • wR factor = 0.185
  • Data-to-parameter ratio = 8.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.37 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc. PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 6 PLAT430_ALERT_2_C Short Inter D...A Contact O4 .. O4 .. 2.88 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Trimethylenetetraaminium(4+) bis(sulfate) monohydrate top
Crystal data top
C6H22N44+·2SO42·H2OF(000) = 384
Mr = 360.41Dx = 1.550 Mg m3
Orthorhombic, PnnmMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2 2nCell parameters from 861 reflections
a = 6.3192 (8) Åθ = 3.4–23.5°
b = 22.253 (3) ŵ = 0.39 mm1
c = 5.4903 (7) ÅT = 295 K
V = 772.1 (2) Å3Block, yellow
Z = 20.14 × 0.14 × 0.13 mm
Data collection top
Bruker APEX area-detector
diffractometer
840 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.035
Graphite monochromatorθmax = 27.5°, θmin = 1.8°
φ and ω scansh = 83
3543 measured reflectionsk = 2528
946 independent reflectionsl = 66
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)] = 0.070Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.185H-atom parameters constrained
S = 1.14 w = 1/[σ2(Fo2) + (0.0921P)2 + 1.2465P]
where P = (Fo2 + 2Fc2)/3
946 reflections(Δ/σ)max = 0.001
113 parametersΔρmax = 0.57 e Å3
148 restraintsΔρmin = 0.51 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
S10.2004 (2)0.35894 (4)0.50000.0247 (4)
O10.360 (1)0.3110 (3)0.483 (4)0.034 (2)0.25
O20.0124 (9)0.3318 (3)0.472 (4)0.040 (3)0.25
O30.234 (3)0.4028 (5)0.306 (2)0.039 (4)0.25
O40.215 (3)0.3881 (6)0.7382 (16)0.033 (3)0.25
O50.156 (3)0.3167 (7)0.301 (2)0.027 (3)0.25
O60.4171 (9)0.3820 (3)0.474 (4)0.045 (3)0.25
O70.178 (3)0.3280 (8)0.735 (2)0.032 (4)0.25
O80.049 (1)0.4091 (2)0.488 (5)0.036 (2)0.25
O1W0.50000.50000.50000.160 (5)
N10.5074 (6)0.29452 (16)0.00000.0324 (9)
N20.8959 (6)0.42124 (15)0.00000.0302 (9)
C10.7079 (8)0.3255 (2)0.00000.044 (1)
C20.6924 (7)0.3914 (2)0.00000.039 (1)
C30.8940 (7)0.48638 (19)0.00000.039 (1)
H1W10.59460.52600.46850.192*0.25
H1W20.52690.46760.42420.192*0.25
H1N10.52880.25640.00000.039*
H1N20.43690.30440.12790.039*
H2N0.96500.40940.12620.036*
H10.78740.31310.14250.053*
H20.61350.40400.14270.047*
H30.81770.50020.14260.047*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.0245 (6)0.0217 (6)0.0278 (6)0.0004 (4)0.0000.000
O10.041 (4)0.033 (3)0.027 (6)0.013 (3)0.004 (7)0.000 (6)
O20.036 (4)0.040 (4)0.044 (8)0.006 (3)0.020 (6)0.011 (5)
O30.049 (7)0.033 (7)0.036 (6)0.005 (5)0.002 (5)0.008 (5)
O40.033 (5)0.035 (6)0.033 (6)0.002 (5)0.004 (5)0.005 (5)
O50.030 (6)0.020 (6)0.030 (6)0.010 (4)0.005 (5)0.007 (5)
O60.038 (4)0.046 (4)0.051 (8)0.013 (3)0.017 (6)0.003 (6)
O70.032 (7)0.034 (7)0.030 (6)0.001 (5)0.007 (5)0.002 (5)
O80.051 (4)0.026 (3)0.032 (5)0.012 (3)0.009 (8)0.001 (8)
O1W0.162 (8)0.120 (7)0.198 (9)0.068 (6)0.0000.000
N10.029 (2)0.021 (2)0.047 (2)0.002 (2)0.0000.000
N20.024 (2)0.022 (2)0.045 (2)0.002 (2)0.0000.000
C10.025 (2)0.025 (2)0.081 (4)0.002 (2)0.0000.000
C20.024 (2)0.023 (2)0.071 (4)0.000 (2)0.0000.000
C30.028 (2)0.020 (2)0.069 (4)0.003 (2)0.0000.000
Geometric parameters (Å, º) top
S1—O11.470 (5)C1—C21.469 (7)
S1—O21.482 (6)C3—C3i1.470 (9)
S1—O31.461 (6)O1W—H1W10.85
S1—O41.463 (6)O1W—H1W20.85
S1—O51.471 (6)N1—H1N10.86
S1—O61.469 (5)N1—H1N20.86
S1—O71.468 (7)N2—H2N0.86
S1—O81.472 (5)C1—H10.97
N1—C11.443 (6)C2—H20.97
N2—C21.448 (6)C3—H30.97
N2—C31.450 (5)
O1—S1—O2108.6 (5)N2—C2—C1113.5 (4)
O1—S1—O3109.9 (5)N2—C3—C3i113.9 (5)
O1—S1—O4109.7 (5)H1W1—O1W—H1W2109.7
O2—S1—O3109.2 (5)C1—N1—H1N1109.5
O2—S1—O4109.2 (5)C1—N1—H1N2109.5
O3—S1—O4110.3 (4)H1N1—N1—H1N2109.5
O5—S1—O6109.4 (5)C2—N2—H2N108.1
O5—S1—O7109.6 (4)C3—N2—H2N108.1
O5—S1—O8109.1 (5)N1—C1—H1108.6
O6—S1—O7109.8 (5)C2—C1—H1108.6
O6—S1—O8109.8 (5)N2—C2—H2108.9
O7—S1—O8109.7 (5)C1—C2—H2108.9
C2—N2—C3116.9 (4)N2—C3—H3108.8
N1—C1—C2114.7 (4)C3i—C3—H3108.8
C3—N2—C2—C1180.0C2—N2—C3—C3i180.0
N1—C1—C2—N2180.0
Symmetry code: (i) x+2, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O3ii0.852.292.94 (1)134
O1W—H1W1···O3iii0.852.122.94 (1)163
O1W—H1W2···O60.852.052.681 (7)131
O1W—H1W2···O6iv0.852.102.681 (7)125
O1W—H1W1···O6ii0.852.072.681 (7)128
O1W—H1W1···O6iii0.852.052.681 (7)131
N1—H1N1···O2v0.861.982.818 (8)163
N1—H1N1···O5v0.862.122.86 (2)145
N1—H1N2···O10.862.012.83 (2)159
N1—H1N2···O7iv0.861.882.65 (2)148
N2—H2N···O3vi0.861.972.75 (2)150
N2—H2N···O4vii0.861.812.58 (2)149
N2—H2N···O7vii0.862.383.10 (2)141
N2—H2N···O8vi0.862.062.86 (3)156
N2—H2N···O8vii0.862.182.98 (3)155
Symmetry codes: (ii) x+1, y+1, z+1; (iii) x+1, y+1, z; (iv) x, y, z+1; (v) x+1/2, y+1/2, z+1/2; (vi) x+1, y, z; (vii) x+1, y, z1.
 

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