Poly[propane-1,2-diammonium μ-disulfido-deca-μ-sulfido-disulfidoocta­anti­monate(III)]

In the structure of the title compound, {(C₃H₁₃N₂)[Sb₈S₁₄]}_n, SbS₃ pyramids are joined to form an [Sb₄S₇] chain. Two adjacent chains are joined via an S₂ bridge, yielding the final [Sb₈S₁₄]²⁻ anion. The structure-directing organic cations are located in the plane of large rings composed of ten S and eight Sb atoms. If Sb—S bonds longer than 3.1 Å are considered, a three-dimensional network with two types of channels is observed.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](S-S) = 0.003 Å
• Disorder in main residue
• R factor = 0.033
• wR factor = 0.094
• Data-to-parameter ratio = 21.1

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT432_ALERT_2_B Short Inter X...Y Contact  S6     ..  C3      ..       3.19 Ang.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.12 Ratio
PLAT301_ALERT_3_C Main Residue  Disorder .........................       5.00 Perc.
PLAT432_ALERT_2_C Short Inter X...Y Contact  S1     ..  C3      ..       3.25 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          6
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............          !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............          !

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  11 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   5 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
   3 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

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: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: CIFTAB in SHELXL97.

Poly[propane-1,2-diammonium µ-disulfido-deca-µ-sulfido- disulfidooctaantimonate(III)]

Crystal data

(C3H12N2)[Sb8S14]	F(000) = 1352
Mr = 1498.99	Dx = 3.474 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 97 reflections
a = 7.1404 (13) Å	θ = 2.5–25°
b = 25.522 (4) Å	µ = 8.44 mm^−1
c = 7.9316 (9) Å	T = 293 K
β = 97.558 (11)°	Block, red
V = 1432.9 (4) Å^3	0.21 × 0.1 × 0.1 mm
Z = 2

Data collection

Stoe AED2 diffractometer	2537 independent reflections
Radiation source: fine-focus sealed tube	2160 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.037
Detector resolution: n pixels mm^-1	θmax = 25.0°, θmin = 2.7°
ω/θ scans	h = −8→8
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1998)	k = −30→20
Tmin = 0.368, Tmax = 0.450	l = 0→9
4911 measured reflections

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)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.094	H-atom parameters constrained
S = 1.10	w = 1/[σ^2(Fo^2) + (0.0477P)^2 + 9.1338P] where P = (Fo^2 + 2Fc^2)/3
2537 reflections	(Δ/σ)max = 0.001
120 parameters	Δρmax = 1.50 e Å^−3
2 restraints	Δρmin = −1.18 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Sb1	0.94520 (7)	0.61319 (2)	1.50036 (7)	0.02378 (16)
Sb2	0.47556 (7)	0.67450 (2)	1.32802 (7)	0.02315 (16)
Sb3	0.08281 (7)	0.67774 (2)	0.93193 (6)	0.02318 (16)
Sb4	0.54870 (7)	0.74445 (2)	0.92448 (7)	0.02745 (17)
S1	1.0655 (3)	0.52578 (9)	1.4238 (3)	0.0374 (6)
S2	0.6114 (3)	0.59000 (9)	1.4455 (3)	0.0358 (5)
S3	0.2354 (3)	0.61942 (8)	1.1599 (3)	0.0255 (4)
S4	0.7030 (3)	0.67677 (9)	1.1195 (3)	0.0318 (5)
S5	0.3375 (3)	0.68216 (9)	0.7491 (3)	0.0309 (5)
S6	−0.0288 (4)	0.59269 (9)	0.8017 (3)	0.0375 (6)
S7	0.3177 (3)	0.77066 (9)	1.1018 (2)	0.0251 (4)
N1	0.499 (3)	0.5677 (7)	0.857 (2)	0.048 (4)*	0.50
H1N1	0.4632	0.5770	0.7477	0.072*	0.50
H2N1	0.3998	0.5704	0.9153	0.072*	0.50
H3N1	0.5922	0.5890	0.9029	0.072*	0.50
C1	0.571 (5)	0.5150 (12)	0.867 (4)	0.080 (8)*	0.50
H1A	0.6797	0.5108	0.8084	0.096*	0.50
H1B	0.4741	0.4909	0.8217	0.096*	0.50
C2	0.606 (5)	0.5106 (17)	1.039 (4)	0.110 (12)*	0.50
H2	0.5859	0.5452	1.0807	0.132*	0.50
C3	0.796 (6)	0.509 (2)	1.064 (7)	0.150 (18)*	0.50
H3A	0.8442	0.5301	0.9786	0.225*	0.50
H3B	0.8489	0.5211	1.1747	0.225*	0.50
H3C	0.8312	0.4731	1.0501	0.225*	0.50
N2	0.559 (5)	0.4778 (13)	1.177 (4)	0.107 (10)*	0.50
H1N2	0.6230	0.4885	1.2766	0.161*	0.50
H2N2	0.4344	0.4796	1.1822	0.161*	0.50
H3N2	0.5913	0.4445	1.1565	0.161*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sb1	0.0256 (3)	0.0210 (3)	0.0247 (3)	0.0013 (2)	0.0031 (2)	0.0006 (2)
Sb2	0.0211 (3)	0.0261 (3)	0.0221 (3)	0.0031 (2)	0.0025 (2)	−0.0008 (2)
Sb3	0.0212 (3)	0.0268 (3)	0.0215 (3)	0.0000 (2)	0.0026 (2)	0.0000 (2)
Sb4	0.0261 (3)	0.0300 (3)	0.0287 (3)	−0.0041 (2)	0.0125 (2)	0.0002 (2)
S1	0.0463 (13)	0.0234 (12)	0.0475 (14)	0.0066 (9)	0.0244 (11)	0.0007 (10)
S2	0.0281 (11)	0.0247 (11)	0.0506 (14)	−0.0001 (9)	−0.0102 (10)	0.0044 (10)
S3	0.0252 (9)	0.0252 (11)	0.0247 (10)	−0.0026 (8)	−0.0019 (8)	0.0031 (8)
S4	0.0233 (10)	0.0369 (13)	0.0368 (11)	0.0073 (9)	0.0103 (9)	0.0019 (10)
S5	0.0334 (11)	0.0361 (13)	0.0242 (10)	−0.0011 (9)	0.0079 (9)	−0.0043 (9)
S6	0.0569 (15)	0.0292 (12)	0.0236 (10)	−0.0111 (10)	−0.0050 (10)	0.0013 (9)
S7	0.0219 (9)	0.0301 (11)	0.0241 (9)	0.0014 (8)	0.0057 (8)	−0.0010 (9)

Geometric parameters (Å, º)

Sb1—S6^i	2.430 (2)	N1—H1N1	0.9000
Sb1—S2	2.439 (2)	N1—H2N1	0.9000
Sb1—S1	2.494 (2)	N1—H3N1	0.9000
Sb2—S4	2.466 (2)	C1—C2	1.36 (3)
Sb2—S3	2.468 (2)	C1—H1A	0.9600
Sb2—S2	2.495 (2)	C1—H1B	0.9599
Sb3—S5	2.473 (2)	C2—C3	1.35 (3)
Sb3—S3	2.481 (2)	C2—N2	1.45 (3)
Sb3—S6	2.489 (2)	C2—H2	0.9599
Sb4—S7	2.399 (2)	C3—H3A	0.9599
Sb4—S4	2.479 (2)	C3—H3B	0.9599
Sb4—S5	2.487 (2)	C3—H3C	0.9601
S1—S1^ii	2.089 (5)	N2—H1N2	0.9000
S6—Sb1^iii	2.430 (2)	N2—H2N2	0.9000
N1—C1	1.44 (3)	N2—H3N2	0.9000
S6^i—Sb1—S2	93.99 (9)	C2—C1—N1	99 (3)
S6^i—Sb1—S1	93.59 (9)	C2—C1—H1A	115.0
S2—Sb1—S1	95.70 (8)	N1—C1—H1A	112.6
S4—Sb2—S3	97.07 (8)	C2—C1—H1B	110.4
S4—Sb2—S2	90.73 (8)	N1—C1—H1B	110.1
S3—Sb2—S2	85.28 (7)	H1A—C1—H1B	109.7
S5—Sb3—S3	99.69 (8)	C3—C2—C1	101 (4)
S5—Sb3—S6	90.93 (8)	C3—C2—N2	102 (3)
S3—Sb3—S6	82.26 (7)	C1—C2—N2	141 (4)
S7—Sb4—S4	96.43 (7)	C3—C2—H2	99.9
S7—Sb4—S5	95.33 (7)	C1—C2—H2	104.5
S4—Sb4—S5	95.20 (8)	N2—C2—H2	102.4
S1^ii—S1—Sb1	103.16 (14)	C2—C3—H3A	109.1
Sb1—S2—Sb2	100.35 (8)	C2—C3—H3B	112.8
Sb2—S3—Sb3	105.03 (8)	H3A—C3—H3B	109.5
Sb2—S4—Sb4	99.03 (7)	C2—C3—H3C	106.5
Sb3—S5—Sb4	98.04 (8)	H3A—C3—H3C	109.5
Sb1^iii—S6—Sb3	101.50 (9)	H3B—C3—H3C	109.5
C1—N1—H1N1	110.9	C2—N2—H1N2	110.3
C1—N1—H2N1	110.0	C2—N2—H2N2	109.4
H1N1—N1—H2N1	109.5	H1N2—N2—H2N2	109.5
C1—N1—H3N1	107.5	C2—N2—H3N2	108.7
H1N1—N1—H3N1	109.5	H1N2—N2—H3N2	109.5
H2N1—N1—H3N1	109.5	H2N2—N2—H3N2	109.5

Symmetry codes: (i) x+1, y, z+1; (ii) −x+2, −y+1, −z+3; (iii) x−1, y, z−1.