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Yellow crystals of the title compound, [Mn(dien)2][Sb4S7]·0.5H2O (dien = diethyl­enetri­amine = C4H13N3) were synthesized under solvothermal conditions by reacting MnSb2S4 with pure dien. The Mn2+ ion is in an octahedral environment of six N atoms of the tridentate dien mol­ecules. The [Sb4S7]2- units, and anions are joined together to form two-dimensional layers. In the layered anion, Sb2S2, Sb4S4 and Sb8S8 hetero-rings are found.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803027983/hg6011sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803027983/hg6011Isup2.hkl
Contains datablock I

CCDC reference: 234802

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • H-atom completeness 97%
  • Disorder in solvent or counterion
  • R factor = 0.028
  • wR factor = 0.083
  • Data-to-parameter ratio = 26.6

checkCIF/PLATON results

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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 ............ 0.25 Ratio PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT420_ALERT_2_C D-H Without Acceptor N3 - H2N3 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N5 - H2N5 ... ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C8 H27 Mn1 N6 O0.5 S7 Sb4 Atom count from the _atom_site data: C8 H26 Mn1 N6 O0.5 S7 Sb4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C8 H27 Mn N6 O0.5 S7 Sb4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 32.00 32.00 0.00 H 108.00 104.00 4.00 Mn 4.00 4.00 0.00 N 24.00 24.00 0.00 O 2.00 2.00 0.00 S 28.00 28.00 0.00 Sb 16.00 16.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 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: DIAMOND (Crystal Impact, 1999); software used to prepare material for publication: CIFTAB in SHELXL97.

[tris(2-aminoethyl)amine]manganese(II) tetraantimony heptasulfide hemihydrate, [Mn(dien)2][Sb4S7]·0.5H20 top
Crystal data top
[Mn(C4H13N3)2][Sb4S7]·0.5H20F(000) = 1844
Mr = 980.71Dx = 2.400 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 8000 reflections
a = 9.7216 (19) Åθ = 2.5–28°
b = 16.113 (3) ŵ = 4.93 mm1
c = 17.339 (4) ÅT = 293 K
β = 91.88 (3)°Polyhedra, yellow
V = 2714.6 (9) Å30.2 × 0.2 × 0.1 mm
Z = 4
Data collection top
Stoe IPDS
diffractometer
6508 independent reflections
Radiation source: fine-focus sealed tube5824 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
φ scansθmax = 28.0°, θmin = 2.5°
Absorption correction: numerical
[X-SHAPE (Stoe & Cie, 1998)and X-RED (Stoe & Cie, 1998)]
h = 1212
Tmin = 0.390, Tmax = 0.609k = 2121
31130 measured reflectionsl = 2222
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)] = 0.028H-atom parameters constrained
wR(F2) = 0.083 w = 1/[σ2(Fo2) + (0.0547P)2 + 3.6221P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
6508 reflectionsΔρmax = 1.25 e Å3
245 parametersΔρmin = 1.12 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00169 (13)
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*/UeqOcc. (<1)
Mn0.60094 (6)0.72629 (4)0.49237 (3)0.02702 (13)
Sb10.02292 (2)0.878909 (15)0.743886 (14)0.02171 (8)
Sb20.00953 (2)0.640658 (15)0.760134 (14)0.02201 (8)
Sb30.33220 (3)0.523731 (15)0.776720 (15)0.02592 (8)
Sb40.70681 (3)0.484698 (16)0.756691 (16)0.02626 (8)
S10.06567 (10)0.97071 (6)0.64786 (5)0.02589 (19)
S20.26679 (9)0.87910 (6)0.70261 (7)0.0300 (2)
S30.02577 (10)0.75440 (6)0.66536 (6)0.02764 (19)
S40.24192 (10)0.63188 (6)0.73701 (7)0.0330 (2)
S50.10328 (11)0.54262 (6)0.67292 (5)0.02722 (19)
S60.47357 (10)0.51326 (7)0.66700 (6)0.0279 (2)
S70.55817 (11)0.48663 (8)0.86381 (6)0.0338 (2)
N10.3699 (4)0.7394 (2)0.4727 (2)0.0344 (8)
H1N10.34760.79420.47240.041*
N20.5209 (4)0.7268 (2)0.61302 (19)0.0323 (7)
H1N20.54430.67890.63670.039*
H2N20.56050.76870.64000.039*
N30.5700 (5)0.7161 (3)0.3595 (2)0.0440 (10)
H1N30.62720.75150.33630.053*
H2N30.59000.66430.34410.053*
N40.8302 (4)0.7126 (3)0.5034 (2)0.0353 (8)
H1N40.85620.71780.55400.042*
N50.6752 (5)0.8591 (3)0.4887 (3)0.0484 (11)
H1N50.64100.88390.44570.058*
H2N50.64450.88690.52970.058*
N60.6385 (4)0.5839 (2)0.5000 (2)0.0404 (9)
H1N60.58850.56240.53790.049*
H2N60.61090.55990.45530.049*
C10.3070 (4)0.6994 (4)0.5388 (3)0.0421 (11)
H1A0.32380.64010.53760.051*
H1B0.20830.70850.53670.051*
C20.3700 (5)0.7366 (3)0.6128 (3)0.0387 (10)
H2A0.34660.79500.61580.046*
H2B0.33350.70870.65720.046*
C30.3309 (5)0.7030 (4)0.3969 (3)0.0484 (12)
H3A0.23630.71720.38300.058*
H3B0.33840.64300.39930.058*
C40.4253 (6)0.7364 (3)0.3369 (3)0.0501 (13)
H4A0.40180.71190.28710.060*
H4B0.41430.79600.33270.060*
C50.8881 (6)0.7827 (4)0.4606 (3)0.0508 (13)
H5A0.86570.77670.40600.061*
H5B0.98750.78320.46760.061*
C60.8302 (6)0.8619 (4)0.4894 (3)0.0551 (15)
H6A0.85970.90740.45720.066*
H6B0.86510.87210.54160.066*
C70.8704 (6)0.6294 (4)0.4768 (3)0.0524 (13)
H7A0.96720.61990.48900.063*
H7B0.85600.62530.42130.063*
C80.7857 (6)0.5659 (3)0.5157 (3)0.0505 (13)
H8A0.80770.51100.49660.061*
H8B0.80570.56690.57090.061*
O0.2287 (9)0.9120 (4)0.4739 (4)0.0513 (19)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn0.0255 (3)0.0309 (3)0.0247 (3)0.0044 (2)0.0019 (2)0.0010 (2)
Sb10.01879 (12)0.02100 (13)0.02533 (13)0.00158 (8)0.00089 (9)0.00326 (8)
Sb20.01717 (12)0.02230 (13)0.02644 (13)0.00324 (8)0.00115 (9)0.00453 (9)
Sb30.02609 (14)0.01968 (13)0.03232 (14)0.00045 (9)0.00612 (10)0.00277 (9)
Sb40.02345 (14)0.02348 (14)0.03193 (14)0.00115 (9)0.00196 (10)0.00429 (9)
S10.0288 (5)0.0228 (4)0.0261 (4)0.0084 (3)0.0013 (4)0.0024 (3)
S20.0163 (4)0.0249 (4)0.0490 (6)0.0016 (3)0.0031 (4)0.0140 (4)
S30.0301 (5)0.0190 (4)0.0344 (5)0.0039 (3)0.0097 (4)0.0003 (3)
S40.0166 (4)0.0280 (5)0.0541 (6)0.0013 (3)0.0018 (4)0.0122 (4)
S50.0348 (5)0.0206 (4)0.0264 (4)0.0085 (4)0.0032 (4)0.0002 (3)
S60.0203 (4)0.0389 (5)0.0246 (4)0.0053 (4)0.0017 (3)0.0040 (4)
S70.0218 (5)0.0524 (7)0.0271 (5)0.0061 (4)0.0007 (4)0.0058 (4)
N10.0334 (18)0.040 (2)0.0293 (17)0.0078 (15)0.0049 (14)0.0066 (14)
N20.0289 (17)0.042 (2)0.0261 (15)0.0044 (15)0.0011 (13)0.0004 (14)
N30.057 (3)0.050 (2)0.0258 (17)0.004 (2)0.0060 (17)0.0025 (16)
N40.0315 (18)0.043 (2)0.0313 (17)0.0065 (16)0.0030 (14)0.0007 (15)
N50.065 (3)0.031 (2)0.049 (2)0.0066 (19)0.008 (2)0.0079 (17)
N60.055 (2)0.033 (2)0.0336 (18)0.0110 (18)0.0054 (17)0.0027 (15)
C10.023 (2)0.065 (3)0.039 (2)0.004 (2)0.0020 (17)0.010 (2)
C20.030 (2)0.056 (3)0.0300 (19)0.001 (2)0.0044 (16)0.0071 (19)
C30.040 (3)0.069 (4)0.036 (2)0.006 (2)0.013 (2)0.010 (2)
C40.074 (4)0.049 (3)0.027 (2)0.008 (3)0.010 (2)0.0030 (19)
C50.040 (3)0.068 (4)0.045 (3)0.019 (3)0.008 (2)0.012 (3)
C60.070 (4)0.048 (3)0.047 (3)0.031 (3)0.001 (3)0.013 (2)
C70.042 (3)0.057 (3)0.059 (3)0.006 (2)0.012 (2)0.012 (3)
C80.067 (3)0.038 (3)0.047 (3)0.012 (2)0.001 (2)0.004 (2)
O0.088 (6)0.039 (4)0.027 (3)0.024 (4)0.012 (3)0.013 (3)
Geometric parameters (Å, º) top
Mn—N42.241 (4)N3—H2N30.9000
Mn—N22.256 (4)N4—C51.473 (6)
Mn—N52.259 (4)N4—C71.476 (7)
Mn—N12.270 (4)N4—H1N40.9100
Mn—N32.320 (4)N5—C61.507 (8)
Mn—N62.326 (4)N5—H1N50.9000
Sb1—S12.4076 (10)N5—H2N50.9000
Sb1—S22.4539 (11)N6—C81.477 (7)
Sb1—S32.4790 (10)N6—H1N60.9000
Sb2—S52.3883 (10)N6—H2N60.9000
Sb2—S42.4682 (11)C1—C21.526 (6)
Sb2—S32.4701 (10)C1—H1A0.9700
Sb3—S62.3893 (12)C1—H1B0.9700
Sb3—S2i2.4451 (11)C2—H2A0.9700
Sb3—S72.6917 (13)C2—H2B0.9700
Sb3—S52.8322 (13)C3—C41.507 (8)
Sb4—S72.3907 (13)C3—H3A0.9700
Sb4—S4ii2.4495 (11)C3—H3B0.9700
Sb4—S1iii2.7279 (13)C4—H4A0.9700
Sb4—S62.7459 (13)C4—H4B0.9700
S1—Sb4iv2.7279 (13)C5—C61.487 (9)
S2—Sb3v2.4451 (11)C5—H5A0.9700
S4—Sb4vi2.4495 (11)C5—H5B0.9700
N1—C11.466 (6)C6—H6A0.9700
N1—C31.479 (5)C6—H6B0.9700
N1—H1N10.9100C7—C81.489 (8)
N2—C21.475 (6)C7—H7A0.9700
N2—H1N20.9000C7—H7B0.9700
N2—H2N20.9000C8—H8A0.9700
N3—C41.484 (7)C8—H8B0.9700
N3—H1N30.9000
N4—Mn—N2107.09 (13)C7—N4—H1N4108.5
N4—Mn—N577.15 (16)Mn—N4—H1N4108.5
N2—Mn—N598.22 (16)C6—N5—Mn110.4 (3)
N4—Mn—N1176.26 (13)C6—N5—H1N5109.6
N2—Mn—N176.64 (13)Mn—N5—H1N5109.6
N5—Mn—N1102.89 (16)C6—N5—H2N5109.6
N4—Mn—N3100.00 (15)Mn—N5—H2N5109.6
N2—Mn—N3152.13 (15)H1N5—N5—H2N5108.1
N5—Mn—N393.99 (16)C8—N6—Mn110.8 (3)
N1—Mn—N376.26 (15)C8—N6—H1N6109.5
N4—Mn—N675.19 (15)Mn—N6—H1N6109.5
N2—Mn—N690.53 (14)C8—N6—H2N6109.5
N5—Mn—N6152.33 (17)Mn—N6—H2N6109.5
N1—Mn—N6104.66 (15)H1N6—N6—H2N6108.1
N3—Mn—N690.12 (15)N1—C1—C2108.5 (4)
S1—Sb1—S299.30 (4)N1—C1—H1A110.0
S1—Sb1—S392.19 (4)C2—C1—H1A110.0
S2—Sb1—S392.35 (4)N1—C1—H1B110.0
S5—Sb2—S4104.82 (4)C2—C1—H1B110.0
S5—Sb2—S392.03 (4)H1A—C1—H1B108.4
S4—Sb2—S391.09 (4)N2—C2—C1109.4 (4)
S6—Sb3—S2i102.04 (4)N2—C2—H2A109.8
S6—Sb3—S787.18 (4)C1—C2—H2A109.8
S2i—Sb3—S785.27 (4)N2—C2—H2B109.8
S6—Sb3—S587.83 (4)C1—C2—H2B109.8
S2i—Sb3—S589.59 (3)H2A—C2—H2B108.2
S7—Sb3—S5171.94 (3)N1—C3—C4109.1 (4)
S7—Sb4—S4ii103.10 (4)N1—C3—H3A109.9
S7—Sb4—S1iii91.63 (4)C4—C3—H3A109.9
S4ii—Sb4—S1iii89.99 (3)N1—C3—H3B109.9
S7—Sb4—S685.92 (4)C4—C3—H3B109.9
S4ii—Sb4—S685.80 (3)H3A—C3—H3B108.3
S1iii—Sb4—S6174.53 (3)N3—C4—C3109.5 (4)
Sb1—S1—Sb4iv86.13 (3)N3—C4—H4A109.8
Sb3v—S2—Sb1102.23 (3)C3—C4—H4A109.8
Sb2—S3—Sb1102.56 (4)N3—C4—H4B109.8
Sb4vi—S4—Sb2103.76 (4)C3—C4—H4B109.8
Sb2—S5—Sb388.68 (3)H4A—C4—H4B108.2
Sb3—S6—Sb492.68 (4)N4—C5—C6109.5 (4)
Sb4—S7—Sb394.02 (4)N4—C5—H5A109.8
C1—N1—C3114.8 (4)C6—C5—H5A109.8
C1—N1—Mn106.2 (3)N4—C5—H5B109.8
C3—N1—Mn108.7 (3)C6—C5—H5B109.8
C1—N1—H1N1109.0H5A—C5—H5B108.2
C3—N1—H1N1109.0C5—C6—N5111.1 (4)
Mn—N1—H1N1109.0C5—C6—H6A109.4
C2—N2—Mn111.8 (2)N5—C6—H6A109.4
C2—N2—H1N2109.3C5—C6—H6B109.4
Mn—N2—H1N2109.3N5—C6—H6B109.4
C2—N2—H2N2109.3H6A—C6—H6B108.0
Mn—N2—H2N2109.3N4—C7—C8109.1 (4)
H1N2—N2—H2N2107.9N4—C7—H7A109.9
C4—N3—Mn109.7 (3)C8—C7—H7A109.9
C4—N3—H1N3109.7N4—C7—H7B109.9
Mn—N3—H1N3109.7C8—C7—H7B109.9
C4—N3—H2N3109.7H7A—C7—H7B108.3
Mn—N3—H2N3109.7N6—C8—C7109.1 (4)
H1N3—N3—H2N3108.2N6—C8—H8A109.9
C5—N4—C7115.5 (4)C7—C8—H8A109.9
C5—N4—Mn106.1 (3)N6—C8—H8B109.9
C7—N4—Mn109.6 (3)C7—C8—H8B109.9
C5—N4—H1N4108.5H8A—C8—H8B108.3
Symmetry codes: (i) x, y1/2, z+3/2; (ii) x+1, y, z; (iii) x+1, y1/2, z+3/2; (iv) x+1, y+1/2, z+3/2; (v) x, y+1/2, z+3/2; (vi) x1, y, z.
 

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