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In the structure of the title compound, (C3H12N2)[Sb10S16], the SbS3 pyramids are inter­connected to form a one-dimensional [Sb6S10]2− chain anion which contains 24-membered Sb12S12 rings that are inter­connected. The structure-directing cations are located above and below this ring. Accepting Sb—S distances up to 3.2 Å, a three-dimensional thio­anti­monate(III) network results.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806006738/bt2015sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806006738/bt2015Isup2.hkl
Contains datablock I

CCDC reference: 604975

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.024
  • wR factor = 0.056
  • Data-to-parameter ratio = 25.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT480_ALERT_4_B Long H...A H-Bond Reported H1C .. S10 .. 3.37 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C2 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1D ... ? PLAT481_ALERT_4_C Long D...A H-Bond Reported N1 .. S10 .. 3.90 Ang.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 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 1 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: DIF4 (Stoe & Cie, 1992); cell refinement: DIF4; data reduction: REDU4 (Stoe & Cie, 1992); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: CIFTAB in SHELXL97.

2-Ammoniopropylammonium µ-dodecasulfido-tetrasulfidodecaantimony top
Crystal data top
(C3H12N2)[Sb10S16]F(000) = 3240
Mr = 1806.61Dx = 3.745 Mg m3
Dm = n Mg m3
Dm measured by not measured
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 17.480 (3) ÅCell parameters from 92 reflections
b = 10.922 (2) Åθ = 11–20°
c = 18.030 (3) ŵ = 9.34 mm1
β = 111.415 (10)°T = 293 K
V = 3204.5 (10) Å3Block, red
Z = 40.2 × 0.1 × 0.1 mm
Data collection top
Stoe AED-II four-circle
diffractometer
6992 independent reflections
Radiation source: fine-focus sealed tube5739 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
Detector resolution: n pixels mm-1θmax = 27.0°, θmin = 2.4°
ωθ scansh = 022
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)
k = 136
Tmin = 0.345, Tmax = 0.401l = 2321
11455 measured reflections
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)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.056H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0224P)2 + 5.0622P]
where P = (Fo2 + 2Fc2)/3
6992 reflections(Δ/σ)max = 0.003
280 parametersΔρmax = 0.92 e Å3
0 restraintsΔρmin = 0.80 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Sb11.412206 (18)0.62355 (3)0.111332 (18)0.01877 (7)
Sb21.456488 (18)0.86469 (3)0.051461 (17)0.01847 (7)
Sb31.245628 (17)0.85087 (3)0.109001 (17)0.01748 (7)
Sb41.028169 (17)0.85960 (3)0.264660 (17)0.01896 (7)
Sb50.959911 (19)1.01239 (3)0.125205 (19)0.02475 (8)
Sb60.806578 (18)0.94820 (3)0.045737 (19)0.02295 (8)
Sb70.581883 (17)0.85275 (3)0.153428 (18)0.01867 (7)
Sb80.654826 (18)0.64710 (3)0.035937 (17)0.01761 (7)
Sb90.865630 (17)0.65213 (3)0.193069 (17)0.01834 (7)
Sb100.700860 (17)0.88025 (3)0.200136 (18)0.01978 (7)
S11.41676 (7)0.84261 (10)0.12516 (7)0.0191 (2)
S21.47171 (7)0.64314 (10)0.04170 (6)0.0197 (2)
S31.26256 (6)0.62939 (10)0.12057 (7)0.0189 (2)
S41.30889 (7)0.83937 (11)0.04254 (7)0.0215 (2)
S51.10046 (6)0.81489 (12)0.11902 (6)0.0233 (2)
S61.01318 (7)0.64130 (11)0.29682 (7)0.0227 (2)
S70.89314 (7)0.87887 (13)0.24672 (7)0.0265 (3)
S80.93861 (7)0.85049 (12)0.04018 (7)0.0254 (3)
S90.83685 (7)1.11761 (12)0.12197 (8)0.0279 (3)
S100.71678 (7)0.85217 (12)0.17184 (7)0.0262 (3)
S110.51176 (7)0.81046 (13)0.29719 (7)0.0249 (3)
S120.59004 (7)0.63760 (10)0.11502 (7)0.0201 (2)
S130.80123 (7)0.67173 (11)0.04206 (6)0.0209 (2)
S140.63598 (7)0.86680 (10)0.04556 (6)0.0195 (2)
S150.84821 (7)0.87393 (11)0.20742 (7)0.0201 (2)
S160.69557 (6)0.66100 (10)0.21088 (6)0.0192 (2)
C11.1854 (6)0.4301 (6)0.1499 (5)0.078 (3)
H1A1.16630.37080.10690.093*
H1B1.24350.41520.17810.093*
C21.1759 (4)0.5554 (5)0.1135 (3)0.0405 (14)
H21.18370.61680.15530.049*
C31.0954 (4)0.5793 (8)0.0463 (4)0.067 (2)
H3A1.09480.66160.02730.101*
H3B1.05100.56880.06500.101*
H3C1.08910.52280.00360.101*
N11.1441 (5)0.4070 (6)0.2031 (4)0.089 (2)
H1C1.15440.33070.22140.134*
H1D1.09020.41650.17760.134*
H1E1.16170.45930.24370.134*
N21.2422 (3)0.5689 (5)0.0810 (3)0.0542 (14)
H2A1.29070.55510.11940.081*
H2B1.24130.64450.06220.081*
H2C1.23450.51520.04180.081*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.01853 (14)0.01419 (15)0.02048 (14)0.00163 (12)0.00342 (11)0.00031 (12)
Sb20.01911 (14)0.01571 (15)0.01744 (14)0.00226 (12)0.00292 (11)0.00048 (11)
Sb30.01585 (13)0.01608 (15)0.01885 (14)0.00199 (11)0.00438 (11)0.00031 (11)
Sb40.01778 (14)0.01976 (16)0.01813 (14)0.00061 (12)0.00513 (11)0.00162 (12)
Sb50.02116 (15)0.02660 (18)0.02914 (16)0.00033 (13)0.01234 (13)0.00078 (14)
Sb60.01839 (14)0.02555 (18)0.02485 (15)0.00009 (13)0.00782 (12)0.00188 (13)
Sb70.01690 (13)0.01822 (16)0.01893 (14)0.00128 (12)0.00422 (11)0.00056 (12)
Sb80.01798 (14)0.01508 (15)0.01732 (14)0.00057 (11)0.00355 (11)0.00084 (11)
Sb90.01569 (14)0.01816 (16)0.01881 (14)0.00068 (11)0.00349 (11)0.00025 (12)
Sb100.01913 (14)0.01494 (15)0.02197 (14)0.00132 (12)0.00358 (12)0.00022 (12)
S10.0183 (5)0.0143 (5)0.0218 (5)0.0000 (4)0.0038 (4)0.0007 (4)
S20.0220 (5)0.0154 (5)0.0179 (5)0.0030 (4)0.0027 (4)0.0020 (4)
S30.0178 (5)0.0142 (5)0.0228 (5)0.0002 (4)0.0053 (4)0.0002 (4)
S40.0173 (5)0.0276 (6)0.0190 (5)0.0032 (5)0.0059 (4)0.0000 (5)
S50.0153 (5)0.0356 (7)0.0190 (5)0.0026 (5)0.0061 (4)0.0007 (5)
S60.0295 (6)0.0180 (6)0.0176 (5)0.0029 (5)0.0051 (5)0.0008 (4)
S70.0169 (5)0.0372 (7)0.0239 (6)0.0020 (5)0.0057 (4)0.0018 (5)
S80.0195 (5)0.0259 (7)0.0297 (6)0.0047 (5)0.0078 (5)0.0029 (5)
S90.0262 (6)0.0203 (6)0.0409 (7)0.0025 (5)0.0169 (5)0.0019 (5)
S100.0187 (5)0.0310 (7)0.0286 (6)0.0047 (5)0.0082 (5)0.0057 (5)
S110.0165 (5)0.0376 (7)0.0192 (5)0.0002 (5)0.0049 (4)0.0014 (5)
S120.0234 (5)0.0172 (6)0.0179 (5)0.0007 (5)0.0054 (4)0.0003 (4)
S130.0180 (5)0.0260 (6)0.0174 (5)0.0001 (5)0.0050 (4)0.0010 (5)
S140.0218 (5)0.0146 (5)0.0185 (5)0.0011 (4)0.0030 (4)0.0023 (4)
S150.0185 (5)0.0168 (6)0.0232 (5)0.0021 (4)0.0055 (4)0.0002 (5)
S160.0198 (5)0.0149 (5)0.0199 (5)0.0003 (4)0.0036 (4)0.0000 (4)
C10.145 (8)0.028 (4)0.080 (6)0.009 (5)0.065 (6)0.009 (4)
C20.060 (4)0.027 (3)0.038 (3)0.003 (3)0.021 (3)0.008 (3)
C30.057 (4)0.078 (6)0.061 (5)0.002 (4)0.015 (4)0.016 (4)
N10.152 (7)0.049 (4)0.098 (5)0.030 (5)0.082 (5)0.016 (4)
N20.055 (3)0.050 (3)0.051 (3)0.012 (3)0.012 (3)0.011 (3)
Geometric parameters (Å, º) top
Sb1—S12.4099 (12)Sb9—S152.4669 (13)
Sb1—S32.5604 (12)Sb9—S11i2.5288 (12)
Sb1—S22.5777 (12)Sb9—S132.5472 (12)
Sb2—S22.4477 (12)Sb10—S162.4070 (13)
Sb2—S42.5408 (12)Sb10—S152.5317 (12)
Sb2—S6i2.5475 (12)Sb10—S142.6014 (12)
Sb3—S32.4551 (12)S6—Sb2ii2.5475 (12)
Sb3—S52.5082 (12)S11—Sb9ii2.5288 (12)
Sb3—S42.5490 (12)C1—N11.418 (10)
Sb4—S62.4451 (13)C1—C21.500 (9)
Sb4—S72.5055 (13)C1—H1A0.9700
Sb4—S52.5115 (12)C1—H1B0.9700
Sb5—S82.4561 (13)C2—N21.486 (8)
Sb5—S92.4583 (13)C2—C31.508 (9)
Sb5—S72.5340 (13)C2—H20.9800
Sb6—S92.4747 (14)C3—H3A0.9600
Sb6—S102.4753 (13)C3—H3B0.9600
Sb6—S82.5113 (13)C3—H3C0.9600
Sb7—S122.4392 (13)N1—H1C0.8900
Sb7—S112.4727 (12)N1—H1D0.8900
Sb7—S102.4983 (13)N1—H1E0.8900
Sb8—S142.4368 (12)N2—H2A0.8900
Sb8—S132.5353 (12)N2—H2B0.8900
Sb8—S122.5397 (12)N2—H2C0.8900
S1—Sb1—S392.29 (4)Sb5—S9—Sb691.72 (4)
S1—Sb1—S290.73 (4)Sb6—S10—Sb7100.93 (5)
S3—Sb1—S294.07 (4)Sb7—S11—Sb9ii98.29 (4)
S2—Sb2—S491.28 (4)Sb7—S12—Sb8102.82 (4)
S2—Sb2—S6i92.40 (4)Sb8—S13—Sb994.74 (4)
S4—Sb2—S6i93.04 (4)Sb8—S14—Sb1096.57 (4)
S3—Sb3—S589.41 (4)Sb9—S15—Sb10100.57 (4)
S3—Sb3—S491.37 (4)N1—C1—C2117.1 (7)
S5—Sb3—S495.80 (4)N1—C1—H1A108.0
S6—Sb4—S795.06 (4)C2—C1—H1A108.0
S6—Sb4—S591.59 (4)N1—C1—H1B108.0
S7—Sb4—S591.11 (4)C2—C1—H1B108.0
S8—Sb5—S989.34 (4)H1A—C1—H1B107.3
S8—Sb5—S789.91 (5)N2—C2—C1106.6 (6)
S9—Sb5—S799.13 (4)N2—C2—C3107.4 (5)
S9—Sb6—S1089.95 (5)C1—C2—C3115.5 (7)
S9—Sb6—S887.72 (4)N2—C2—H2109.0
S10—Sb6—S897.01 (4)C1—C2—H2109.0
S12—Sb7—S1194.18 (4)C3—C2—H2109.0
S12—Sb7—S1094.30 (4)C2—C3—H3A109.5
S11—Sb7—S1089.48 (4)C2—C3—H3B109.5
S14—Sb8—S1393.03 (4)H3A—C3—H3B109.5
S14—Sb8—S1295.60 (4)C2—C3—H3C109.5
S13—Sb8—S1295.68 (4)H3A—C3—H3C109.5
S15—Sb9—S11i89.67 (4)H3B—C3—H3C109.5
S15—Sb9—S1390.36 (4)C1—N1—H1C109.5
S11i—Sb9—S1395.83 (4)C1—N1—H1D109.5
S16—Sb10—S1592.12 (4)H1C—N1—H1D109.5
S16—Sb10—S1490.89 (4)C1—N1—H1E109.5
S15—Sb10—S1495.24 (4)H1C—N1—H1E109.5
Sb2—S2—Sb198.46 (4)H1D—N1—H1E109.5
Sb3—S3—Sb199.85 (4)C2—N2—H2A109.5
Sb2—S4—Sb395.49 (4)C2—N2—H2B109.5
Sb3—S5—Sb498.88 (4)H2A—N2—H2B109.5
Sb4—S6—Sb2ii104.22 (4)C2—N2—H2C109.5
Sb4—S7—Sb590.10 (4)H2A—N2—H2C109.5
Sb5—S8—Sb690.90 (4)H2B—N2—H2C109.5
Symmetry codes: (i) x+1/2, y+3/2, z+1/2; (ii) x1/2, y+3/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···S7iii0.892.533.341 (7)151
N1—H1C···S10iii0.893.373.905 (8)121
N2—H2A···S7i0.892.533.309 (5)147
N2—H2B···S40.892.523.340 (6)153
N2—H2C···S13iii0.892.483.343 (6)163
Symmetry codes: (i) x+1/2, y+3/2, z+1/2; (iii) x+2, y+1, z.
 

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