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Yellow crystals of [Mn(pn)3]2[Sb4S8]·2H2O (pn = 1,2-di­amino­propane) were synthesized under solvothermal conditions by reacting elemental Mn, Sb and S in an aqueous solution of 1,2-di­amino­propane. The structure is composed of cyclic [Sb4S8]4- anions and octahedral [Mn(pn)3]2+ cations, both stacked in a rod-like manner along the a axis. The anion sits on a centre of symmetry. Between the anions and the cations there is an extended hydrogen-bonding network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803011036/bt6281sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803011036/bt6281Isup2.hkl
Contains datablock I

CCDC reference: 214795

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.032
  • wR factor = 0.092
  • Data-to-parameter ratio = 30.5

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
PLAT_735 Alert B D-H Calc 0.85(5), Rep 0.848(10) .... 5.00 su-Ratio O1 -H1O 1.555 1.555 PLAT_735 Alert B D-H Calc 0.84(7), Rep 0.849(10) .... 7.00 su-Ratio O1 -H2O 1.555 1.555
Yellow Alert Alert Level C:
WEIGH_01 Alert C Extra text has been found in the _refine_ls_weighting_scheme field. This should be in the _refine_ls_weighting_details field. Weighting scheme given as calc w = 1/[\s^2^(Fo^2^)+(0.0455P)^2^+2.987 Weighting scheme identified as calc PLAT_420 Alert C D-H Without Acceptor N(1) - H(1A) ? PLAT_420 Alert C D-H Without Acceptor N(1) - H(1B) ? PLAT_420 Alert C D-H Without Acceptor N(2) - H(2A) ? PLAT_420 Alert C D-H Without Acceptor N(3) - H(3B) ? PLAT_420 Alert C D-H Without Acceptor N(4) - H(4A) ? PLAT_420 Alert C D-H Without Acceptor N(6) - H(6B) ?
0 Alert Level A = Potentially serious problem
2 Alert Level B = Potential problem
7 Alert Level C = Please check

Comment top

During the last few years, a large number of thioantimonates(III) were reported demonstrating the rich structural diversity of this class of compounds. In the structures, the primary SbS3 trigonal pyramid is often interconnected forming so-called secondary building units (SBU) like Sb2S2, Sb3S3, Sb4S4 hetero-rings or the Sb3S4 semicube. Until now only a few thioantimonates(III) have been reported containing isolated SbS anions. The isolated [SbS3]3− anion is found in M3SbS3 (M = Ag, Cu, Tl; Wattenberg & Hellner, 1966; Pfitzner, 1994; Rey et al., 1984). Using a cut-off for the Sb—S distance of 3 Å isolated SbS3 and Sb2S4 units co-exist in Ca2Sb2S5 (Cordier & Schäfer, 1981). In Ba8Sb6S17 and in BaSb2S4, chain-like Sb3S8 anions and isolated SbS3 pyramids were observed (Dörrscheidt & Schäfer, 1986; Cordier et al., 1984). The isolated Sb2S54− anion is found in Sr2Sb2S5.15H2O (Cordier et al., 1985). It should be noted that besides these isolated anions only one compound with an isolated ring anion was reported so far (Bensch et al., 2001). In the anion of the title compound, (I), four pyramidal SbS3 units sharing common corners form a Sb4S4 hetero-ring that adopts a chair conformation. Each Sb atom has a terminal S atom to form the [Sb4S8]4− ring anion (Fig. 1). The bridging Sb—S distances are between 2.4598 (10) and 2.4919 (10) Å (Table 1). As expected, the terminal Sb—S bonds (Sb1—S2 and Sb2—S4) are significantly shorter with values of 2.3322 (11) and 2.3442 (10) Å. The S—Sb—S angles vary between 92.33 (4) and 104.37 (3)°. The terminal Sb—S distances in the recently reported compound [Ni[C4H13N3)2]2Sb4S8 are between 2.315 (3) and 2.337 (2) Å, and the bond lengths within the Sb4S4 ring range from 2.426 (2) to 2.497 (2) Å. The S—Sb—S angles scatter over a larger range than in the title compound [87.92 (7)–107.53 (8)°; Bensch et al., 2001]. The differences of the geometrical parameters in the two compounds demonstrate the high flexibility of the Sb—S bonds and S—Sb—S angles to accomodate an optimal arrangement of cations and anions in the structure. The Mn2+ cation is in an octahedral environment of six N atoms of three bidentate amine molecules (Fig. 1). The Mn—N distances are between 2.258 (3) and 2.322 (3) Å (Table 1) and are in accordance with literature data (Laskowski & Hendrickson, 1978; Wendland et al., 2000). The N—Mn—N angles vary from 76.37 (11) to 171.97 (12)°, indicative of a relatively strong distorted octahedral environment. The three-dimensional interconnection of anions and cations is achieved by ten N—H···S interactions. Only three of the four unique S atoms are involved and the N—H···S distances range between 2.62 and 3.03 Å, with corresponding angles ranging from 136.0 to 172.0° (Table 2). We note that in [Ni[C4H13N3)2]2Sb4S8 the H···S contacts are signficantly shorter (2.513–2.837 Å), which may have an influence on the geometrical parameters of the anions, as mentioned above. The water molecule acts as a hydrogen-bond donor and acceptor. Two short contacts are observed to S2 and S4 and on to N5 (Table 2). Cations and anions form separate stacks parallel to the a and c axes. A view of the arrangement of the cations and anions with view along [100] is displayed in Fig. 2. The disordered water molecule is situated between the cations.

Experimental top

The title compound was prepared by solvothermal synthesis of elemental Mn (54.94 mg, 1 mmol), Sb (121.75 mg, 1 mmol) and S (80.15 mg, 2.5 mmol) in a 70% aqueous solution of 1,2-diaminopropane (5 ml). The mixture was heated for 7 d in a Teflon-lined steel autoclave at 383 K. The yield was about 60% based on Mn after washing with water and acetone.

Refinement top

The positions of the H atoms were located from difference maps. H atoms bound to C atoms were positioned with idealized geometry and refined with fixed isotropic displacement parameters [Uiso(H) = 1.2UeqC] using a riding model with the parameters C—H(tertiary) = 0.98 Å, C—H(secondary) = 0.97 Å and C—H(primary) = 0.96 Å. The positions of the H atoms of the NH2 groups were idealized, with N—H distances of 0.90 Å, then refined as rigid groups allowed to rotate but not tip. These H atoms were refined using fixed isotropic displacement parameters [Uiso(H) = 1.5UeqN]. The H atoms of H2O were refined with restraints setting the distances for O—H to 0.84 (1) Å and for H···H to 1.40 (1) Å. The isotropic displacement parameters were fixed [Uiso(H) = 1.5UeqO].

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: XP in SHELXTL (Bruker, 1998); software used to prepare material for publication: CIFTAB in SHELXTL.

Figures top
[Figure 1] Fig. 1. The cation (top) and the anion (bottom) in the title compound. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry code: (') 1 − x, −y, 1 − z.]
[Figure 2] Fig. 2. The crystal structure of the title compound, viewed in the direction of the crystallographic a axis. O atoms have been omitted and hydrogen bonding is shown as dashed lines.
(I) top
Crystal data top
[Mn(C3H10N2)3]2[Sb4S8]·2H2OF(000) = 1308
Mr = 1334.17Dx = 1.897 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 9.4773 (19) ÅCell parameters from 126 reflections
b = 19.579 (4) Åθ = 12–19°
c = 12.592 (3) ŵ = 3.20 mm1
β = 91.56 (3)°T = 293 K
V = 2335.6 (8) Å3Polyhedra, yellow
Z = 20.22 × 0.19 × 0.16 mm
Data collection top
Philips PW1100
diffractometer
5895 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.016
Graphite monochromatorθmax = 30.0°, θmin = 2.6°
ω scansh = 012
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)
k = 271
Tmin = 0.495, Tmax = 0.641l = 1717
7248 measured reflections3 standard reflections every 120 min
6515 independent reflections intensity decay: none
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H atoms treated by a mixture of independent and constrained refinement
S = 1.18Calculated w = 1/[σ2(Fo2) + (0.0455P)2 + 2.9874P]
where P = (Fo2 + 2Fc2)/3
6518 reflections(Δ/σ)max = 0.002
214 parametersΔρmax = 1.69 e Å3
3 restraintsΔρmin = 1.06 e Å3
Crystal data top
[Mn(C3H10N2)3]2[Sb4S8]·2H2OV = 2335.6 (8) Å3
Mr = 1334.17Z = 2
Monoclinic, P21/nMo Kα radiation
a = 9.4773 (19) ŵ = 3.20 mm1
b = 19.579 (4) ÅT = 293 K
c = 12.592 (3) Å0.22 × 0.19 × 0.16 mm
β = 91.56 (3)°
Data collection top
Philips PW1100
diffractometer
5895 reflections with I > 2σ(I)
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)
Rint = 0.016
Tmin = 0.495, Tmax = 0.6413 standard reflections every 120 min
7248 measured reflections intensity decay: none
6515 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0323 restraints
wR(F2) = 0.092H atoms treated by a mixture of independent and constrained refinement
S = 1.18Δρmax = 1.69 e Å3
6518 reflectionsΔρmin = 1.06 e Å3
214 parameters
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
Mn10.89270 (6)0.21041 (3)0.46332 (4)0.03759 (12)
N11.0165 (3)0.18843 (18)0.3102 (3)0.0444 (7)
H1A1.00930.22430.26560.053*
H1B1.10850.18180.32680.053*
N20.7544 (4)0.1342 (2)0.3751 (3)0.0487 (8)
H2A0.76190.09290.40630.058*
H2B0.66360.14750.37650.058*
N30.7623 (3)0.21612 (15)0.6156 (2)0.0389 (6)
H3A0.77860.25610.64890.047*
H3B0.66960.21360.59850.047*
N40.9987 (4)0.13341 (18)0.5731 (3)0.0450 (7)
H4A0.97200.09100.55400.054*
H4B1.09300.13640.56760.054*
N50.7914 (4)0.30858 (18)0.4008 (2)0.0452 (7)
H5A0.79480.30960.32950.054*
H5B0.70020.31010.41890.054*
N61.0509 (4)0.29247 (17)0.5146 (3)0.0464 (7)
H6A1.04110.30250.58370.056*
H6B1.13950.27740.50550.056*
C10.9571 (5)0.1274 (2)0.2588 (3)0.0513 (9)
H10.98890.08800.30120.062*
C20.8006 (5)0.1298 (3)0.2637 (4)0.0572 (11)
H2C0.76550.16920.22440.069*
H2D0.76080.08910.23060.069*
C31.0051 (5)0.1158 (3)0.1466 (3)0.0546 (10)
H3C1.10630.11450.14630.066*
H3D0.97140.15230.10180.066*
H3E0.96800.07310.12050.066*
C40.9598 (4)0.14625 (19)0.6841 (3)0.0390 (7)
H41.00820.18800.70820.047*
C50.8031 (4)0.1590 (2)0.6867 (3)0.0458 (8)
H5C0.75270.11810.66460.055*
H5D0.77680.16970.75880.055*
C61.0044 (5)0.0882 (2)0.7588 (4)0.0568 (11)
H6C1.10440.08110.75510.068*
H6D0.95580.04710.73810.068*
H6E0.98110.09990.83020.068*
C71.0243 (5)0.3541 (2)0.4487 (3)0.0481 (9)
H71.05210.34390.37610.058*
C80.8678 (5)0.3682 (2)0.4465 (3)0.0480 (9)
H8A0.83660.37680.51800.058*
H8B0.84770.40840.40380.058*
C91.1098 (7)0.4156 (3)0.4877 (4)0.0699 (14)
H9A1.20850.40460.48780.084*
H9B1.08300.42720.55840.084*
H9C1.09180.45370.44130.084*
Sb10.44836 (2)0.092969 (10)0.550951 (16)0.03000 (6)
Sb20.33911 (2)0.042109 (12)0.274505 (16)0.03448 (7)
S10.25047 (9)0.03300 (5)0.45579 (7)0.03606 (17)
S20.34266 (11)0.18915 (4)0.62605 (7)0.04116 (19)
S30.43326 (10)0.01756 (5)0.70648 (7)0.04195 (19)
S40.41252 (12)0.15576 (5)0.27104 (8)0.0478 (2)
O10.4653 (9)0.2783 (3)0.4355 (4)0.119 (2)
H1O0.438 (10)0.267 (5)0.497 (3)0.179*
H2O0.417 (9)0.258 (5)0.388 (5)0.179*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0369 (3)0.0400 (3)0.0359 (2)0.0023 (2)0.0006 (2)0.0025 (2)
N10.0346 (15)0.0499 (17)0.0489 (17)0.0041 (13)0.0064 (13)0.0067 (14)
N20.0394 (17)0.065 (2)0.0423 (16)0.0146 (15)0.0067 (13)0.0068 (15)
N30.0331 (14)0.0375 (14)0.0460 (16)0.0028 (11)0.0003 (12)0.0064 (12)
N40.0418 (17)0.0499 (18)0.0432 (16)0.0131 (14)0.0022 (13)0.0042 (13)
N50.0468 (18)0.0534 (18)0.0350 (14)0.0090 (14)0.0029 (12)0.0035 (13)
N60.0417 (17)0.0470 (17)0.0503 (18)0.0018 (13)0.0049 (14)0.0022 (14)
C10.052 (2)0.057 (2)0.045 (2)0.0043 (19)0.0074 (17)0.0075 (17)
C20.053 (2)0.071 (3)0.047 (2)0.011 (2)0.0023 (18)0.004 (2)
C30.055 (2)0.064 (3)0.045 (2)0.008 (2)0.0094 (18)0.0034 (19)
C40.0376 (18)0.0408 (17)0.0384 (16)0.0020 (13)0.0020 (13)0.0015 (13)
C50.0365 (18)0.050 (2)0.051 (2)0.0035 (15)0.0068 (15)0.0040 (16)
C60.055 (3)0.056 (2)0.058 (2)0.0012 (19)0.011 (2)0.0125 (19)
C70.058 (2)0.050 (2)0.0356 (17)0.0070 (18)0.0048 (16)0.0040 (15)
C80.064 (3)0.0398 (18)0.0401 (18)0.0077 (17)0.0041 (17)0.0063 (14)
C90.086 (4)0.061 (3)0.062 (3)0.027 (3)0.008 (3)0.012 (2)
Sb10.02437 (11)0.03266 (11)0.03318 (11)0.00047 (7)0.00439 (7)0.00220 (7)
Sb20.03559 (12)0.03858 (12)0.02891 (10)0.00252 (8)0.00602 (8)0.00381 (8)
S10.0287 (4)0.0413 (4)0.0384 (4)0.0011 (3)0.0037 (3)0.0065 (3)
S20.0496 (5)0.0324 (4)0.0416 (4)0.0029 (3)0.0052 (4)0.0073 (3)
S30.0410 (5)0.0471 (5)0.0383 (4)0.0105 (4)0.0108 (3)0.0079 (3)
S40.0558 (6)0.0371 (4)0.0503 (5)0.0015 (4)0.0027 (4)0.0083 (4)
O10.209 (7)0.081 (3)0.069 (3)0.054 (4)0.030 (4)0.010 (2)
Geometric parameters (Å, º) top
Sb1—S22.3442 (10)N1—C11.463 (5)
Sb1—S32.4598 (10)N2—C21.483 (5)
Sb1—S12.4919 (10)N3—C51.477 (5)
Sb2—S42.3322 (11)N4—C41.477 (5)
Sb2—S3i2.4593 (10)N5—C81.482 (6)
Sb2—S12.4602 (11)N6—C71.481 (5)
S3—Sb2i2.4593 (10)C1—C21.487 (6)
Mn1—N22.258 (3)C1—C31.513 (6)
Mn1—N42.262 (3)C4—C51.507 (5)
Mn1—N62.279 (3)C4—C61.528 (6)
Mn1—N52.279 (3)C7—C81.508 (6)
Mn1—N32.312 (3)C7—C91.526 (6)
Mn1—N12.322 (3)
N2—Mn1—N495.87 (14)N1—C1—C2109.2 (4)
N2—Mn1—N6166.85 (13)N1—C1—C3114.4 (4)
N4—Mn1—N691.09 (13)C2—C1—C3111.6 (4)
N2—Mn1—N598.86 (14)N2—C2—C1111.2 (4)
N4—Mn1—N5161.64 (12)N4—C4—C5108.7 (3)
N6—Mn1—N576.76 (12)N4—C4—C6112.6 (3)
N2—Mn1—N397.10 (11)C5—C4—C6111.5 (3)
N4—Mn1—N376.37 (11)N3—C5—C4110.7 (3)
N6—Mn1—N395.37 (12)N6—C7—C8108.2 (3)
N5—Mn1—N390.92 (12)N6—C7—C9112.5 (4)
N2—Mn1—N176.64 (12)C8—C7—C9112.0 (4)
N4—Mn1—N199.05 (12)N5—C8—C7109.4 (3)
N6—Mn1—N191.28 (13)S2—Sb1—S397.25 (4)
N5—Mn1—N194.99 (13)S2—Sb1—S1104.37 (3)
N3—Mn1—N1171.97 (12)S3—Sb1—S192.33 (4)
C1—N1—Mn1108.7 (2)S4—Sb2—S3i101.17 (4)
C2—N2—Mn1108.7 (3)S4—Sb2—S1101.31 (4)
C5—N3—Mn1109.2 (2)S3i—Sb2—S1101.30 (4)
C4—N4—Mn1110.3 (2)Sb2—S1—Sb198.07 (4)
C8—N5—Mn1109.4 (2)Sb2i—S3—Sb1107.02 (4)
C7—N6—Mn1108.4 (2)
Symmetry code: (i) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2B···S40.902.703.487 (4)147
N1—H1A···S2ii0.902.883.692 (4)150
N1—H1B···S4iii0.903.033.853 (4)153
N2—H2A···S1i0.903.023.906 (4)168
N3—H3A···S4iv0.902.623.464 (3)157
N4—H4B···S2iii0.902.673.484 (4)152
N4—H4B···S1iii0.902.903.454 (3)121
N5—H5A···S2ii0.902.613.506 (3)172
N5—H5B···O10.902.333.188 (8)160
N6—H6A···S4iv0.902.813.662 (4)159
N6—H6B···S2iii0.902.973.674 (4)136
O1—H1O···S20.85 (1)2.43 (5)3.211 (5)154 (9)
O1—H2O···S40.85 (1)2.48 (7)3.199 (5)143 (10)
Symmetry codes: (i) x+1, y, z+1; (ii) x+1/2, y+1/2, z1/2; (iii) x+1, y, z; (iv) x+1/2, y+1/2, z+1/2.

Experimental details

Crystal data
Chemical formula[Mn(C3H10N2)3]2[Sb4S8]·2H2O
Mr1334.17
Crystal system, space groupMonoclinic, P21/n
Temperature (K)293
a, b, c (Å)9.4773 (19), 19.579 (4), 12.592 (3)
β (°) 91.56 (3)
V3)2335.6 (8)
Z2
Radiation typeMo Kα
µ (mm1)3.20
Crystal size (mm)0.22 × 0.19 × 0.16
Data collection
DiffractometerPhilips PW1100
diffractometer
Absorption correctionNumerical
(X-SHAPE; Stoe & Cie, 1998)
Tmin, Tmax0.495, 0.641
No. of measured, independent and
observed [I > 2σ(I)] reflections
7248, 6515, 5895
Rint0.016
(sin θ/λ)max1)0.704
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.092, 1.18
No. of reflections6518
No. of parameters214
No. of restraints3
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.69, 1.06

Computer programs: DIF4 (Stoe & Cie, 1992), DIF4, REDU4 (Stoe & Cie, 1992), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP in SHELXTL (Bruker, 1998), CIFTAB in SHELXTL.

Selected bond lengths (Å) top
Sb1—S22.3442 (10)Mn1—N22.258 (3)
Sb1—S32.4598 (10)Mn1—N42.262 (3)
Sb1—S12.4919 (10)Mn1—N62.279 (3)
Sb2—S42.3322 (11)Mn1—N52.279 (3)
Sb2—S3i2.4593 (10)Mn1—N32.312 (3)
Sb2—S12.4602 (11)Mn1—N12.322 (3)
S3—Sb2i2.4593 (10)
Symmetry code: (i) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2B···S40.902.703.487 (4)147
N1—H1A···S2ii0.902.883.692 (4)150
N1—H1B···S4iii0.903.033.853 (4)153
N2—H2A···S1i0.903.023.906 (4)168
N3—H3A···S4iv0.902.623.464 (3)157
N4—H4B···S2iii0.902.673.484 (4)152
N4—H4B···S1iii0.902.903.454 (3)121
N5—H5A···S2ii0.902.613.506 (3)172
N5—H5B···O10.902.333.188 (8)160
N6—H6A···S4iv0.902.813.662 (4)159
N6—H6B···S2iii0.902.973.674 (4)136
O1—H1O···S20.848 (10)2.43 (5)3.211 (5)154 (9)
O1—H2O···S40.849 (10)2.48 (7)3.199 (5)143 (10)
Symmetry codes: (i) x+1, y, z+1; (ii) x+1/2, y+1/2, z1/2; (iii) x+1, y, z; (iv) x+1/2, y+1/2, z+1/2.
 

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