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The crystal structure of the title compound, (C2H10N2)(C2H9N2)2[Sn2S6], consists of discrete [Sn2S6]4− anions and mono- as well as diprotonated ethyl­enediamine mol­ecules. The anion and the monoprotonated cation occupy general positions, whereas the dications are located on centres of inversion. In the crystal structure, the anions and cations are connected via N—H...S and N—H...N hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805010871/bt6643sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805010871/bt6643Isup2.hkl
Contains datablock I

CCDC reference: 271820

Key indicators

  • Single-crystal X-ray study
  • T = 170 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.029
  • wR factor = 0.076
  • Data-to-parameter ratio = 25.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.94
Alert level C REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 27.99 From the CIF: _diffrn_reflns_theta_full 27.99 From the CIF: _reflns_number_total 4820 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 5109 Completeness (_total/calc) 94.34% PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 16
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 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 0 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

Computing details top

Data collection: IPDS (Stoe & Cie, 1998); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXL97.

Bis(2-aminoethylammonium)(ethylenediammonium)(di-µ-sulfido- κ2S:S)bis[disulfidotin(IV)] top
Crystal data top
(C2H10N2)(C2H9N2)2[Sn2S6]Z = 2
Mr = 614.08F(000) = 604
Triclinic, P1Dx = 1.927 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.7638 (7) ÅCell parameters from 8000 reflections
b = 10.7287 (10) Åθ = 2.5–28°
c = 12.2216 (10) ŵ = 2.95 mm1
α = 74.845 (10)°T = 170 K
β = 72.997 (10)°Block, colourless
γ = 88.978 (10)°0.09 × 0.09 × 0.08 mm
V = 1058.54 (16) Å3
Data collection top
Stoe IPDS-1
diffractometer
3926 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.044
Graphite monochromatorθmax = 28.0°, θmin = 2.3°
φ scansh = 1111
11088 measured reflectionsk = 1414
4820 independent reflectionsl = 1616
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)] = 0.029H-atom parameters constrained
wR(F2) = 0.077 w = 1/[σ2(Fo2) + (0.0472P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.97(Δ/σ)max = 0.001
4820 reflectionsΔρmax = 0.91 e Å3
186 parametersΔρmin = 1.80 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0039 (5)
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
Sn10.34747 (2)0.63752 (2)0.154153 (17)0.00856 (8)
Sn20.13770 (2)0.36405 (2)0.334696 (17)0.00832 (8)
S10.58686 (9)0.70422 (8)0.17769 (7)0.01206 (16)
S20.25563 (9)0.77505 (8)0.00775 (7)0.01272 (16)
S30.34584 (9)0.41326 (8)0.14064 (6)0.01217 (16)
S40.12997 (9)0.58798 (8)0.34600 (7)0.01226 (16)
S50.24852 (9)0.22744 (8)0.47117 (7)0.01222 (16)
S60.10768 (9)0.28440 (8)0.32975 (7)0.01187 (16)
N10.4617 (3)0.1191 (3)0.2382 (3)0.0172 (6)
H1N10.39190.08760.20800.026*
H2N10.53560.17580.17850.026*
H3N10.40750.16030.29280.026*
C10.5430 (4)0.0112 (4)0.2955 (3)0.0185 (7)
H1A0.62890.04650.31860.022*
H1B0.59310.03870.23800.022*
C20.4283 (4)0.0776 (4)0.4039 (3)0.0183 (7)
H2A0.48700.14810.44050.022*
H2B0.38130.02870.46280.022*
N20.3002 (3)0.1333 (3)0.3732 (3)0.0196 (6)
H1N20.24090.19420.43830.029*
H2N20.34520.17360.31560.029*
N30.0231 (4)0.0186 (3)0.3250 (3)0.0209 (7)
H1N30.12250.03890.33000.031*
H2N30.05150.07370.38560.031*
H3N30.00690.06410.32980.031*
C30.0089 (4)0.0303 (4)0.2093 (4)0.0257 (9)
H3A0.10390.02290.20960.031*
H3B0.04110.11650.19930.031*
C40.1134 (5)0.0740 (5)0.1061 (3)0.0277 (9)
H4A0.09490.06830.03140.033*
H4B0.08370.16020.11740.033*
N40.2832 (4)0.0595 (3)0.0970 (3)0.0220 (7)
H1N40.34530.12110.03400.033*
H2N40.30990.01950.08570.033*
N50.7907 (3)0.4613 (3)1.1043 (2)0.0136 (6)
H1N50.75910.41191.06360.020*
H2N50.71140.51311.12790.020*
H3N50.81180.40891.16930.020*
C50.9384 (4)0.5432 (3)1.0258 (3)0.0148 (7)
H5A0.98130.58881.07230.018*
H5B0.91280.60880.96100.018*
N60.2903 (3)0.4523 (3)0.6009 (2)0.0140 (6)
H1N60.26490.39740.56260.021*
H2N60.20550.50000.62300.021*
H3N60.31510.40590.66660.021*
C60.4303 (4)0.5403 (3)0.5202 (3)0.0146 (7)
H6A0.46070.59860.56220.018*
H6B0.40240.59410.45040.018*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.00919 (11)0.00736 (13)0.00709 (11)0.00105 (8)0.00028 (8)0.00094 (8)
Sn20.00882 (11)0.00705 (13)0.00717 (11)0.00145 (8)0.00073 (8)0.00059 (8)
S10.0114 (3)0.0132 (4)0.0111 (3)0.0007 (3)0.0031 (3)0.0027 (3)
S20.0154 (3)0.0103 (4)0.0109 (3)0.0033 (3)0.0034 (3)0.0009 (3)
S30.0157 (3)0.0084 (4)0.0084 (3)0.0032 (3)0.0022 (3)0.0023 (3)
S40.0129 (3)0.0090 (4)0.0113 (3)0.0014 (3)0.0026 (3)0.0037 (3)
S50.0131 (3)0.0111 (4)0.0111 (3)0.0034 (3)0.0037 (3)0.0006 (3)
S60.0110 (3)0.0122 (4)0.0119 (3)0.0011 (3)0.0034 (3)0.0023 (3)
N10.0174 (13)0.0142 (16)0.0152 (13)0.0001 (12)0.0006 (11)0.0020 (11)
C10.0149 (14)0.0149 (18)0.0227 (16)0.0011 (13)0.0016 (13)0.0048 (14)
C20.0248 (16)0.0134 (18)0.0191 (16)0.0030 (14)0.0121 (14)0.0025 (13)
N20.0201 (13)0.0183 (17)0.0160 (13)0.0050 (12)0.0016 (11)0.0011 (11)
N30.0186 (13)0.0189 (17)0.0201 (14)0.0010 (12)0.0005 (12)0.0033 (12)
C30.0174 (15)0.033 (2)0.0276 (19)0.0012 (16)0.0036 (15)0.0136 (17)
C40.0314 (19)0.032 (2)0.0181 (16)0.0119 (18)0.0081 (16)0.0031 (16)
N40.0256 (14)0.0187 (17)0.0160 (13)0.0057 (13)0.0009 (12)0.0005 (12)
N50.0144 (12)0.0154 (15)0.0104 (11)0.0033 (11)0.0028 (10)0.0037 (10)
C50.0136 (14)0.0108 (17)0.0186 (15)0.0036 (13)0.0032 (13)0.0037 (13)
N60.0120 (11)0.0198 (16)0.0086 (11)0.0032 (11)0.0003 (10)0.0046 (11)
C60.0121 (13)0.0138 (18)0.0159 (15)0.0050 (13)0.0017 (12)0.0037 (13)
Geometric parameters (Å, º) top
Sn1—S22.3337 (9)N3—H3N30.9100
Sn1—S12.3474 (8)C3—C41.517 (6)
Sn1—S32.4549 (9)C3—H3A0.9900
Sn1—S42.4868 (8)C3—H3B0.9900
Sn2—S52.3434 (9)C4—N41.468 (5)
Sn2—S62.3509 (8)C4—H4A0.9900
Sn2—S42.4409 (9)C4—H4B0.9900
Sn2—S32.4659 (8)N4—H1N40.9100
N1—C11.475 (5)N4—H2N40.9100
N1—H1N10.9100N5—C51.497 (4)
N1—H2N10.9100N5—H1N50.9100
N1—H3N10.9100N5—H2N50.9100
C1—C21.507 (5)N5—H3N50.9100
C1—H1A0.9900C5—C5i1.514 (7)
C1—H1B0.9900C5—H5A0.9900
C2—N21.465 (4)C5—H5B0.9900
C2—H2A0.9900N6—C61.489 (4)
C2—H2B0.9900N6—H1N60.9100
N2—H1N20.9100N6—H2N60.9100
N2—H2N20.9100N6—H3N60.9100
N3—C31.491 (5)C6—C6ii1.521 (6)
N3—H1N30.9100C6—H6A0.9900
N3—H2N30.9100C6—H6B0.9900
S2—Sn1—S1117.06 (3)H2N3—N3—H3N3109.5
S2—Sn1—S3111.51 (3)N3—C3—C4111.2 (3)
S1—Sn1—S3112.48 (3)N3—C3—H3A109.4
S2—Sn1—S4109.00 (3)C4—C3—H3A109.4
S1—Sn1—S4110.79 (3)N3—C3—H3B109.4
S3—Sn1—S493.46 (3)C4—C3—H3B109.4
S5—Sn2—S6114.80 (3)H3A—C3—H3B108.0
S5—Sn2—S4113.84 (3)N4—C4—C3110.9 (3)
S6—Sn2—S4112.12 (3)N4—C4—H4A109.5
S5—Sn2—S3106.50 (3)C3—C4—H4A109.5
S6—Sn2—S3113.35 (3)N4—C4—H4B109.5
S4—Sn2—S394.34 (3)C3—C4—H4B109.5
Sn1—S3—Sn286.14 (3)H4A—C4—H4B108.0
Sn2—S4—Sn185.98 (3)C4—N4—H1N4110.5
C1—N1—H1N1109.5C4—N4—H2N4108.9
C1—N1—H2N1109.5H1N4—N4—H2N4108.3
H1N1—N1—H2N1109.5C5—N5—H1N5109.5
C1—N1—H3N1109.5C5—N5—H2N5109.5
H1N1—N1—H3N1109.5H1N5—N5—H2N5109.5
H2N1—N1—H3N1109.5C5—N5—H3N5109.5
N1—C1—C2111.6 (3)H1N5—N5—H3N5109.5
N1—C1—H1A109.3H2N5—N5—H3N5109.5
C2—C1—H1A109.3N5—C5—C5i108.8 (3)
N1—C1—H1B109.3N5—C5—H5A109.9
C2—C1—H1B109.3C5i—C5—H5A109.9
H1A—C1—H1B108.0N5—C5—H5B109.9
N2—C2—C1111.0 (3)C5i—C5—H5B109.9
N2—C2—H2A109.4H5A—C5—H5B108.3
C1—C2—H2A109.4C6—N6—H1N6109.5
N2—C2—H2B109.4C6—N6—H2N6109.5
C1—C2—H2B109.4H1N6—N6—H2N6109.5
H2A—C2—H2B108.0C6—N6—H3N6109.5
C2—N2—H1N2108.8H1N6—N6—H3N6109.5
C2—N2—H2N2108.6H2N6—N6—H3N6109.5
H1N2—N2—H2N2107.9N6—C6—C6ii109.1 (4)
C3—N3—H1N3109.5N6—C6—H6A109.9
C3—N3—H2N3109.5C6ii—C6—H6A109.9
H1N3—N3—H2N3109.5N6—C6—H6B109.9
C3—N3—H3N3109.5C6ii—C6—H6B109.9
H1N3—N3—H3N3109.5H6A—C6—H6B108.3
Symmetry codes: (i) x+2, y+1, z+2; (ii) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N1···N40.911.952.833 (4)162
N1—H2N1···S2iii0.912.403.228 (3)151
N1—H3N1···S50.912.493.390 (3)168
N2—H1N2···S6iv0.912.653.477 (3)152
N2—H2N2···S1v0.912.833.683 (3)157
N3—H1N3···N20.911.972.849 (5)162
N3—H2N3···S5iv0.912.363.271 (3)174
N3—H3N3···S60.912.553.436 (4)164
N4—H1N4···S1iii0.912.683.523 (3)155
N4—H2N4···S2v0.912.723.533 (3)150
N5—H1N5···S2ii0.912.413.263 (3)157
N5—H2N5···S1vi0.912.443.303 (3)159
N5—H3N5···S6vii0.912.353.260 (3)174
N6—H1N6···S50.912.403.293 (3)167
N6—H2N6···S6viii0.912.603.399 (3)147
N6—H3N6···S1ii0.912.353.250 (3)173
Symmetry codes: (ii) x+1, y+1, z+1; (iii) x+1, y+1, z; (iv) x, y, z+1; (v) x, y1, z; (vi) x, y, z+1; (vii) x+1, y, z+1; (viii) x, y+1, z+1.
 

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