Bis[diethyl­enetriaminium(3+)] tris­(sulfate) monohydrate

The cations, anions and water mol­ecules in the title compound, 2C₄H₁₆N₃³⁺·3SO₄^2-·H₂O, are linked by hydrogen bonds into a three-dimensional network structure. The water mol­ecule and one sulfate anion lie on special positions of site symmetry 2; one of the sulfate anions is disordered.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.004 Å
• Disorder in main residue
• R factor = 0.058
• wR factor = 0.154
• Data-to-parameter ratio = 15.9

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT242_ALERT_2_B Check Low       Ueq as Compared to Neighbors for         S2

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 ....          ?
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         S1
PLAT301_ALERT_3_C Main Residue  Disorder .........................      18.00 Perc.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          9

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
   5 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
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

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.

Bis[diethylenetriaminium(3+)] tris(sulfate) monohydrate

Crystal data

2C4H16N3^3+·3SO4^2^−·H2O	F(000) = 1104
Mr = 518.59	Dx = 1.566 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1515 reflections
a = 10.249 (1) Å	θ = 2.5–27.1°
b = 13.648 (1) Å	µ = 0.41 mm^−1
c = 16.082 (2) Å	T = 295 K
β = 102.045 (2)°	Block, yellow
V = 2199.9 (4) Å^3	0.15 × 0.13 × 0.12 mm
Z = 4

Data collection

Bruker APEX area-detector diffractometer	1971 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.033
Graphite monochromator	θmax = 27.5°, θmin = 2.5°
φ and ω scans	h = −10→13
6500 measured reflections	k = −17→17
2468 independent reflections	l = −16→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.058	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.154	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0814P)^2 + 3.1409P] where P = (Fo^2 + 2Fc^2)/3
2468 reflections	(Δ/σ)max = 0.001
155 parameters	Δρmax = 0.52 e Å^−3
6 restraints	Δρmin = −0.37 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
S1	−0.02979 (8)	0.30927 (5)	0.53962 (5)	0.0325 (2)
S2	0.5000	0.46114 (7)	0.7500	0.0282 (3)
O1	0.1158 (2)	0.3145 (2)	0.5720 (2)	0.0476 (6)
O2	−0.0955 (2)	0.3729 (2)	0.5922 (2)	0.0482 (7)
O3	−0.0618 (2)	0.3480 (2)	0.4522 (2)	0.0484 (7)
O4	−0.0736 (3)	0.2083 (2)	0.5432 (2)	0.0521 (7)
O5	0.4522 (6)	0.5410 (3)	0.6899 (3)	0.056 (2)	0.50
O6	0.4621 (7)	0.3675 (3)	0.7073 (4)	0.073 (2)	0.50
O7	0.6473 (4)	0.4659 (4)	0.7594 (4)	0.053 (1)	0.50
O8	0.4654 (7)	0.4725 (5)	0.8317 (3)	0.076 (2)	0.50
O1w	0.0000	0.4740 (4)	0.7500	0.139 (3)
N1	0.2490 (3)	0.4872 (2)	0.5531 (2)	0.0374 (7)
N2	0.3032 (2)	0.3691 (2)	0.3524 (2)	0.0277 (5)
N3	0.2069 (3)	0.2139 (2)	0.1576 (2)	0.0380 (6)
C1	0.3239 (3)	0.4580 (2)	0.4881 (2)	0.0345 (7)
C2	0.2300 (3)	0.4143 (2)	0.4122 (2)	0.0354 (7)
C3	0.2146 (3)	0.3227 (2)	0.2790 (2)	0.0331 (7)
C4	0.2948 (3)	0.2662 (2)	0.2271 (2)	0.0355 (7)
H1w1	−0.0261	0.4368	0.7068	0.167*
H1n1	0.3031	0.5119	0.5961	0.045*
H1n2	0.2107	0.4366	0.5690	0.045*
H1n3	0.1898	0.5300	0.5320	0.045*
H2n1	0.3502	0.4134	0.3342	0.033*
H2n2	0.3571	0.3257	0.3789	0.033*
H3n1	0.2544	0.1819	0.1286	0.046*
H3n2	0.1574	0.2553	0.1251	0.046*
H3n3	0.1574	0.1737	0.1783	0.046*
H1a	0.3916	0.4103	0.5119	0.041*
H1b	0.3681	0.5148	0.4704	0.041*
H2a	0.1747	0.3652	0.4316	0.043*
H2b	0.1717	0.4652	0.3832	0.043*
H3a	0.1627	0.3726	0.2439	0.040*
H3b	0.1532	0.2788	0.2989	0.040*
H4a	0.3515	0.3108	0.2038	0.043*
H4b	0.3516	0.2196	0.2633	0.043*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.0352 (4)	0.0303 (4)	0.0330 (4)	0.0067 (3)	0.0095 (3)	0.0096 (3)
S2	0.0310 (6)	0.0247 (5)	0.0267 (5)	0.000	0.0012 (4)	0.000
O1	0.035 (1)	0.058 (2)	0.047 (2)	0.010 (1)	0.003 (1)	0.020 (1)
O2	0.051 (2)	0.035 (1)	0.064 (2)	0.004 (1)	0.024 (1)	−0.005 (1)
O3	0.042 (1)	0.060 (2)	0.041 (1)	−0.003 (1)	0.002 (1)	0.021 (1)
O4	0.074 (2)	0.029 (1)	0.059 (2)	0.003 (1)	0.026 (1)	0.005 (1)
O5	0.073 (4)	0.036 (3)	0.044 (3)	0.004 (2)	−0.021 (3)	0.007 (2)
O6	0.079 (4)	0.031 (3)	0.097 (5)	−0.013 (3)	−0.011 (3)	−0.010 (3)
O7	0.031 (3)	0.065 (4)	0.064 (3)	−0.004 (2)	0.013 (2)	0.013 (3)
O8	0.084 (5)	0.106 (6)	0.049 (3)	0.034 (4)	0.039 (3)	0.018 (3)
O1w	0.239 (8)	0.055 (3)	0.083 (4)	0.000	−0.059 (5)	0.000
N1	0.040 (2)	0.038 (2)	0.031 (1)	0.015 (1)	−0.003 (1)	−0.006 (1)
N2	0.027 (1)	0.027 (1)	0.030 (1)	0.002 (1)	0.007 (1)	0.002 (1)
N3	0.046 (2)	0.036 (2)	0.035 (2)	−0.010 (1)	0.017 (1)	−0.005 (1)
C1	0.028 (2)	0.036 (2)	0.037 (2)	0.002 (1)	0.003 (1)	−0.005 (1)
C2	0.028 (2)	0.044 (2)	0.035 (2)	0.002 (1)	0.007 (1)	−0.009 (1)
C3	0.029 (2)	0.035 (2)	0.035 (2)	−0.001 (1)	0.006 (1)	−0.005 (1)
C4	0.034 (2)	0.037 (2)	0.036 (2)	0.002 (1)	0.007 (1)	−0.005 (1)

Geometric parameters (Å, º)

S1—O1	1.476 (2)	N1—H1n2	0.86
S1—O2	1.470 (2)	N1—H1n3	0.86
S1—O3	1.473 (2)	N2—H2n1	0.86
S1—O4	1.455 (2)	N2—H2n2	0.86
S2—O5	1.471 (3)	N3—H3n1	0.86
S2—O6	1.465 (4)	N3—H3n2	0.86
S2—O7	1.486 (3)	N3—H3n3	0.86
S2—O8	1.439 (4)	C1—H1a	0.97
N1—C1	1.474 (4)	C1—H1b	0.97
N2—C3	1.474 (4)	C2—H2a	0.97
N2—C2	1.474 (4)	C2—H2b	0.97
N3—C4	1.466 (4)	C3—H3a	0.97
C1—C2	1.510 (4)	C3—H3b	0.97
C3—C4	1.500 (4)	C4—H4a	0.97
O1w—H1w1	0.86	C4—H4b	0.97
N1—H1n1	0.86
O1—S1—O2	108.6 (2)	H2n1—N2—H2n2	107.8
O1—S1—O3	109.1 (1)	C4—N3—H3n1	109.5
O1—S1—O4	109.2 (2)	C4—N3—H3n2	109.5
O2—S1—O3	107.4 (2)	H3n1—N3—H3n2	109.5
O2—S1—O4	110.8 (1)	C4—N3—H3n3	109.5
O3—S1—O4	111.7 (2)	H3n1—N3—H3n3	109.5
O5—S2—O6	108.6 (3)	H3n2—N3—H3n3	109.5
O5—S2—O7	103.1 (3)	N1—C1—H1a	109.7
O5—S2—O8	114.1 (4)	C2—C1—H1a	109.7
O6—S2—O7	104.5 (4)	N1—C1—H1b	109.7
O6—S2—O8	115.5 (4)	C2—C1—H1b	109.7
O7—S2—O8	109.9 (4)	H1a—C1—H1b	108.2
C3—N2—C2	113.0 (2)	N2—C2—H2a	109.3
N1—C1—C2	109.9 (2)	C1—C2—H2a	109.3
N2—C2—C1	111.5 (2)	N2—C2—H2b	109.3
N2—C3—C4	110.4 (2)	C1—C2—H2b	109.3
N3—C4—C3	110.7 (3)	H2a—C2—H2b	108.0
C1—N1—H1n1	109.5	N2—C3—H3a	109.6
C1—N1—H1n2	109.5	C4—C3—H3a	109.6
H1n1—N1—H1n2	109.5	N2—C3—H3b	109.6
C1—N1—H1n3	109.5	C4—C3—H3b	109.6
H1n1—N1—H1n3	109.5	H3a—C3—H3b	108.1
H1n2—N1—H1n3	109.5	N3—C4—H4a	109.5
C3—N2—H2n1	109.0	C3—C4—H4a	109.5
C2—N2—H2n1	109.0	N3—C4—H4b	109.5
C3—N2—H2n2	109.0	C3—C4—H4b	109.5
C2—N2—H2n2	109.0	H4a—C4—H4b	108.1
C3—N2—C2—C1	178.0 (3)	C2—N2—C3—C4	−172.1 (3)
N1—C1—C2—N2	−170.3 (2)	N2—C3—C4—N3	175.8 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1w—H1w1···O2	0.86	2.03	2.875 (4)	169
N1—H1n2···O1	0.86	1.93	2.772 (4)	164
N1—H1n1···O5	0.86	1.95	2.793 (5)	166
N1—H1n3···O3^i	0.86	2.17	2.946 (4)	151
N2—H2n2···O1^ii	0.86	2.07	2.833 (3)	148
N2—H2n1···O8^iii	0.86	1.96	2.788 (6)	161
N3—H3n1···O2^iv	0.86	1.91	2.738 (4)	162
N3—H3n3···O6^v	0.86	2.22	3.001 (7)	151
N3—H3n3···O7^v	0.86	2.32	3.080 (6)	147
N3—H3n3···O8^ii	0.86	2.35	3.122 (8)	150
N3—H3n2···O3^vi	0.86	1.90	2.755 (4)	174

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1/2, −y+1/2, −z+1; (iii) x, −y+1, z−1/2; (iv) x+1/2, −y+1/2, z−1/2; (v) x−1/2, −y+1/2, z−1/2; (vi) −x, y, −z+1/2.