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Two new molecular metal chalcogenides, tris­(ethyl­enedi­amine-N,N′)­manganese(II) tetratelluride, [Mn(C2H8N2)3]Te4, (I), and bis­[tris­(ethyl­enedi­amine-N,N′)­iron(II)] penta­seleno­diantimonate(III), [Fe(C2H8N2)3]2(Sb2Se5), (II), containing the isolated molecular building blocks Te42− and Sb2Se54−, have been synthesized by solvothermal reactions in an ethyl­enedi­amine solution at 433 K. The anion Te42− in (I) is a zigzag oligometric chain with Te—Te bond lengths in the range 2.709–2.751 Å. There is a very short contact [3.329 (1) Å] between a pair of neighboring Te42− anions. In (II), each Sb atom is surrounded by three Se atoms to give a tripodal coordination. One of the three independent Se atoms is a μ2-bridging ligand between two Sb atoms; the other two are terminal.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100006879/da1117sup1.cif
Contains datablocks I, II, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100006879/da1117Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100006879/da1117IIsup3.hkl
Contains datablock II

CCDC references: 150771; 150772

Computing details top

For both compounds, data collection: CAD-4-PC Software (Enraf-Nonius, 1992); cell refinement: CAD-4-PC Software; data reduction: XCAD4/PC (Harms, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SCHAKAL92 (Keller, 1992) and ORTEX (McArdle, 1993); software used to prepare material for publication: SHELXL97.

(I) tri(ethylenediamino)manganous telluride top
Crystal data top
[Mn(C2H8N2)3]Te4F(000) = 1340
Mr = 745.65Dx = 2.622 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.461 (2) ÅCell parameters from 25 reflections
b = 15.653 (3) Åθ = 8.0–13.8°
c = 14.269 (3) ŵ = 6.75 mm1
β = 91.37 (3)°T = 293 K
V = 1889.2 (7) Å3Block, black
Z = 40.33 × 0.3 × 0.3 mm
Data collection top
Enraf-Nonius CAD4
diffractometer
2382 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.042
Graphite monochromatorθmax = 25.0°, θmin = 2.6°
ω–scansh = 1010
Absorption correction: ψ scan
(North et al., 1968)
k = 018
Tmin = 0.120, Tmax = 0.132l = 016
3444 measured reflections3 standard reflections every 120 min
3306 independent reflections intensity decay: 5.2%
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)] = 0.041H-atom parameters constrained
wR(F2) = 0.072Calculated w = 1/[σ2(Fo2) + (0.001P)2 + 5.0P]
where P = (Fo2 + 2Fc2)/3
S = 1.34(Δ/σ)max = 0.001
3306 reflectionsΔρmax = 1.37 e Å3
155 parametersΔρmin = 0.77 e Å3
1 restraintExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00129 (4)
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Te10.35396 (8)1.16959 (5)0.37880 (5)0.0639 (2)
Te20.37486 (9)0.99798 (5)0.40030 (5)0.0708 (2)
Te30.26166 (7)0.91945 (4)0.23989 (5)0.0549 (2)
Te40.47529 (7)0.94980 (4)0.10143 (5)0.0544 (2)
Mn10.36862 (15)0.32343 (8)0.68448 (10)0.0451 (3)
N10.3190 (9)0.1835 (4)0.6486 (5)0.057 (2)
H1A0.37460.14880.68740.100*
H1B0.34630.17220.58930.100*
N20.1023 (8)0.3228 (4)0.6625 (5)0.054 (2)
H2A0.07210.36750.62680.100*
H2B0.05470.32690.71810.100*
N30.3973 (11)0.2888 (5)0.8385 (6)0.079 (3)
H3A0.49840.27400.85110.100*
H3B0.33560.24370.85110.100*
N40.3508 (10)0.4521 (5)0.7598 (6)0.066 (2)
H4A0.25620.47620.74680.100*
H4B0.42660.48760.73980.100*
N50.3894 (8)0.3698 (5)0.5331 (5)0.059 (2)
H5A0.33010.41700.52440.100*
H5B0.35290.32920.49350.100*
N60.6308 (8)0.3190 (6)0.6567 (5)0.066 (2)
H6A0.67190.27020.68010.100*
H6B0.67930.36310.68590.100*
C10.1487 (12)0.1702 (6)0.6595 (8)0.072 (3)
H1C0.12720.16790.72520.100*
H1D0.11600.11700.63170.100*
C20.0569 (11)0.2428 (6)0.6161 (7)0.060 (3)
H2C0.08160.24650.55090.100*
H2D0.05460.23300.62080.100*
C30.3539 (14)0.3555 (7)0.8968 (7)0.084 (4)
H3C0.41490.35200.95420.100*
H3D0.24500.34760.91220.100*
C40.3693 (19)0.4414 (7)0.8583 (8)0.112 (5)
H4C0.29400.47720.88870.100*
H4D0.47250.46160.87690.100*
C50.5541 (10)0.3891 (7)0.5128 (8)0.069 (3)
H5C0.58110.44400.53850.100*
H5D0.56870.39110.44630.100*
C60.6591 (10)0.3234 (7)0.5567 (7)0.063 (3)
H6C0.63510.26890.52910.100*
H6D0.76790.33640.54540.100*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Te10.0514 (4)0.0720 (5)0.0678 (5)0.0014 (4)0.0050 (3)0.0119 (4)
Te20.0811 (5)0.0779 (5)0.0528 (4)0.0252 (4)0.0100 (4)0.0035 (4)
Te30.0449 (3)0.0515 (4)0.0685 (5)0.0040 (3)0.0019 (3)0.0035 (3)
Te40.0471 (4)0.0478 (4)0.0683 (4)0.0068 (3)0.0023 (3)0.0129 (3)
Mn10.0388 (7)0.0389 (8)0.0574 (9)0.0036 (6)0.0021 (6)0.0017 (7)
N10.058 (5)0.041 (5)0.073 (6)0.012 (4)0.003 (4)0.005 (4)
N20.038 (4)0.045 (5)0.079 (6)0.005 (4)0.002 (4)0.003 (4)
N30.119 (8)0.056 (6)0.062 (6)0.017 (6)0.008 (5)0.006 (5)
N40.075 (6)0.042 (5)0.082 (6)0.001 (4)0.013 (5)0.009 (5)
N50.045 (5)0.064 (5)0.067 (5)0.002 (4)0.007 (4)0.019 (4)
N60.044 (5)0.095 (7)0.060 (6)0.014 (5)0.004 (4)0.010 (5)
C10.070 (7)0.032 (5)0.113 (9)0.001 (5)0.006 (6)0.007 (6)
C20.044 (6)0.048 (6)0.087 (8)0.006 (5)0.006 (5)0.008 (5)
C30.084 (8)0.100 (10)0.067 (8)0.030 (8)0.008 (6)0.001 (7)
C40.196 (16)0.065 (9)0.076 (9)0.021 (9)0.048 (10)0.012 (7)
C50.046 (6)0.071 (7)0.089 (8)0.006 (5)0.007 (6)0.026 (6)
C60.038 (5)0.076 (7)0.076 (8)0.005 (5)0.001 (5)0.002 (6)
Geometric parameters (Å, º) top
Te1—Te22.7091 (12)N1—C11.468 (11)
Te2—Te32.7500 (12)N2—C21.464 (11)
Te3—Te42.7509 (12)N3—C31.389 (12)
Mn1—N62.264 (7)N4—C41.420 (13)
Mn1—N22.267 (7)N5—C51.462 (11)
Mn1—N32.271 (8)N6—C61.454 (11)
Mn1—N12.287 (7)C1—C21.502 (12)
Mn1—N52.289 (7)C3—C41.460 (8)
Mn1—N42.290 (7)C5—C61.488 (12)
Te1—Te2—Te3109.17 (3)N1—Mn1—N4159.1 (3)
Te2—Te3—Te4107.39 (3)N5—Mn1—N499.9 (3)
N6—Mn1—N2161.9 (3)C1—N1—Mn1106.7 (5)
N6—Mn1—N394.6 (3)C2—N2—Mn1108.4 (5)
N2—Mn1—N3102.4 (3)C3—N3—Mn1112.1 (6)
N6—Mn1—N196.1 (3)C4—N4—Mn1110.7 (6)
N2—Mn1—N177.8 (3)C5—N5—Mn1110.4 (6)
N3—Mn1—N190.2 (3)C6—N6—Mn1110.9 (5)
N6—Mn1—N575.3 (3)N1—C1—C2110.4 (8)
N2—Mn1—N588.3 (3)N2—C2—C1109.4 (8)
N3—Mn1—N5168.5 (3)C4—C3—N3116.1 (10)
N1—Mn1—N596.3 (3)C3—C4—N4118.1 (10)
N6—Mn1—N4100.7 (3)N5—C5—C6109.6 (8)
N2—Mn1—N489.6 (3)N6—C6—C5109.6 (8)
N3—Mn1—N476.2 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AH···AD—H···A
N1—H1B···Te1i3.01 (1)163 (1)
N2—H2A···Te4ii2.99152
N2—H2B···Te1ii2.89170
N5—H5B···Te1i2.99158
Symmetry codes: (i) x, y1, z; (ii) x1/2, y+3/2, z+1/2.
(II) di[tri(ethylenediamino)ferro] antimony selenide top
Crystal data top
[Fe(C2H8N2)3]2·Sb2Se5F(000) = 2112
Mr = 1110.62Dx = 2.184 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 25 reflections
a = 15.774 (3) Åθ = 7.5–12.0°
b = 11.739 (2) ŵ = 7.84 mm1
c = 18.239 (4) ÅT = 293 K
V = 3377.3 (11) Å3Block, brown
Z = 40.5 × 0.3 × 0.2 mm
Data collection top
Enraf-Nonius CAD4
diffractometer
1719 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.115
Graphite monochromatorθmax = 26.0°, θmin = 2.4°
ω–scansh = 1819
Absorption correction: ψ scan
(North et al,, 1968)
k = 1314
Tmin = 0.018, Tmax = 0.211l = 2221
6283 measured reflections3 standard reflections every 120 min
3321 independent reflections intensity decay: 5.0%
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)] = 0.082Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.171H-atom parameters constrained
S = 1.07Calculated w = 1/[σ2(Fo2) + (0.0556P)2 + 2.0077P]
where P = (Fo2 + 2Fc2)/3
3321 reflections(Δ/σ)max < 0.001
163 parametersΔρmax = 0.79 e Å3
0 restraintsΔρmin = 0.95 e Å3
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sb1A0.01282 (11)0.58523 (14)0.59096 (10)0.0327 (4)0.50
Sb1B0.07394 (11)0.60183 (14)0.55827 (10)0.0336 (4)0.50
Se10.06665 (17)0.4912 (2)0.53384 (15)0.0377 (6)0.50
Se20.12032 (9)0.50891 (11)0.67726 (8)0.0453 (4)
Se30.03644 (17)0.79041 (11)0.59416 (11)0.0824 (8)
Fe10.09569 (12)0.86241 (14)0.35846 (11)0.0388 (5)
N10.0019 (8)0.7559 (9)0.3055 (7)0.051 (3)
H1A0.01550.68290.30380.080*
H1B0.00970.78020.25920.080*
N20.0177 (8)0.9189 (9)0.4169 (7)0.050 (3)
H2A0.01730.99510.42200.080*
H2B0.01890.88730.46190.080*
N30.1825 (8)0.9632 (9)0.4281 (7)0.050 (3)
H3A0.15941.03180.43730.080*
H3B0.23250.97420.40550.080*
N40.1281 (10)0.7378 (10)0.4411 (7)0.066 (4)
H4A0.13910.67000.42010.080*
H4B0.08440.72900.47220.080*
N50.1962 (8)0.8039 (9)0.2840 (7)0.053 (3)
H5A0.19400.72770.27890.080*
H5B0.24750.82270.30180.080*
N60.0891 (8)0.9956 (9)0.2745 (7)0.054 (3)
H6A0.08911.06490.29560.080*
H6B0.04120.98810.24810.080*
C10.0808 (11)0.7632 (12)0.3474 (9)0.064 (5)
H1C0.08040.70930.38690.080*
H1D0.12700.74440.31540.080*
C20.0936 (9)0.8836 (12)0.3748 (10)0.060 (4)
H2C0.10300.93600.33520.080*
H2D0.14270.88480.40590.080*
C30.1950 (10)0.9043 (13)0.4984 (10)0.067 (5)
H3C0.14740.91630.53030.080*
H3D0.24470.93360.52230.080*
C40.2045 (11)0.7757 (14)0.4836 (11)0.075 (5)
H4C0.25470.76230.45530.080*
H4D0.20970.73570.52930.080*
C50.1822 (9)0.8603 (13)0.2127 (8)0.055 (4)
H5C0.13610.82450.18730.080*
H5D0.23230.85360.18310.080*
C60.1621 (10)0.9834 (12)0.2262 (9)0.059 (4)
H6C0.21011.01940.24880.080*
H6D0.15151.02090.18030.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb1A0.0325 (9)0.0304 (8)0.0351 (10)0.0035 (7)0.0008 (9)0.0040 (8)
Sb1B0.0350 (10)0.0282 (8)0.0377 (11)0.0050 (7)0.0017 (9)0.0013 (7)
Se10.0430 (15)0.0347 (12)0.0353 (16)0.0069 (12)0.0015 (13)0.0043 (12)
Se20.0513 (8)0.0394 (7)0.0452 (9)0.0012 (6)0.0129 (7)0.0017 (7)
Se30.158 (2)0.0226 (6)0.0661 (13)0.0006 (9)0.0425 (13)0.0042 (7)
Fe10.0455 (11)0.0252 (8)0.0458 (13)0.0004 (8)0.0038 (10)0.0003 (8)
N10.057 (8)0.032 (6)0.065 (9)0.006 (5)0.005 (7)0.010 (5)
N20.070 (8)0.027 (5)0.055 (8)0.003 (6)0.008 (7)0.007 (5)
N30.046 (7)0.051 (7)0.053 (9)0.008 (6)0.000 (6)0.017 (6)
N40.098 (11)0.043 (7)0.058 (10)0.002 (7)0.003 (9)0.015 (6)
N50.063 (8)0.044 (6)0.053 (9)0.010 (6)0.004 (7)0.009 (6)
N60.070 (8)0.039 (6)0.054 (8)0.009 (7)0.005 (7)0.010 (6)
C10.082 (12)0.052 (8)0.058 (12)0.031 (9)0.011 (10)0.021 (8)
C20.048 (9)0.055 (9)0.077 (12)0.012 (7)0.010 (9)0.012 (8)
C30.053 (10)0.073 (10)0.077 (13)0.011 (9)0.006 (9)0.018 (10)
C40.065 (11)0.084 (12)0.076 (14)0.017 (10)0.004 (10)0.026 (10)
C50.039 (8)0.089 (11)0.037 (9)0.008 (8)0.006 (7)0.003 (8)
C60.062 (10)0.047 (8)0.068 (12)0.012 (8)0.004 (9)0.017 (8)
Geometric parameters (Å, º) top
Sb1A—Se32.438 (2)Fe1—N12.206 (11)
Sb1A—Se22.481 (2)Fe1—N32.211 (11)
Sb1A—Se1i2.590 (3)N1—C11.463 (19)
Sb1B—Se32.383 (2)N2—C21.481 (18)
Sb1B—Se22.537 (2)N3—C31.47 (2)
Sb1B—Se12.609 (3)N4—C41.50 (2)
Se1—Sb1Ai2.590 (3)N5—C51.475 (18)
Fe1—N42.161 (12)N6—C61.456 (18)
Fe1—N22.185 (13)C1—C21.513 (19)
Fe1—N62.192 (11)C3—C41.54 (2)
Fe1—N52.198 (11)C5—C61.50 (2)
Se3—Sb1A—Se2103.72 (8)N4—Fe1—N379.4 (5)
Se3—Sb1A—Se1i108.24 (10)N2—Fe1—N393.7 (4)
Se2—Sb1A—Se1i102.03 (9)N6—Fe1—N392.8 (5)
Se3—Sb1B—Se2103.66 (9)N5—Fe1—N394.3 (5)
Se3—Sb1B—Se1107.37 (11)N1—Fe1—N3170.8 (5)
Se2—Sb1B—Se1100.20 (9)C1—N1—Fe1109.3 (9)
Sb1Ai—Se1—Sb1B92.51 (10)C2—N2—Fe1108.9 (9)
N4—Fe1—N293.4 (5)C3—N3—Fe1109.4 (9)
N4—Fe1—N6168.9 (5)C4—N4—Fe1110.5 (10)
N2—Fe1—N694.9 (4)C5—N5—Fe1107.3 (9)
N4—Fe1—N592.8 (5)C6—N6—Fe1108.4 (9)
N2—Fe1—N5170.7 (5)N1—C1—C2110.0 (12)
N6—Fe1—N579.9 (4)N2—C2—C1108.9 (13)
N4—Fe1—N195.0 (5)N3—C3—C4108.7 (13)
N2—Fe1—N179.3 (4)N4—C4—C3107.7 (13)
N6—Fe1—N193.7 (5)N5—C5—C6108.6 (12)
N5—Fe1—N193.2 (5)N6—C6—C5111.2 (12)
Symmetry code: (i) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AH···AD—H···A
N1—H1A···Se2i2.81159
N2—H2A···Se3ii2.67158
N2—H2B···Se32.68175
N3—H3A···Se3ii2.91151
N3—H3B···Se2iii2.78173
N4—H4A···Se2i2.77158
N5—H5B···Se2iii2.90150
N6—H6A···Se3ii2.76150
N6—H6B···Se2iv2.86172
Symmetry codes: (i) x, y+1, z+1; (ii) x, y+2, z+1; (iii) x+1/2, y+3/2, z+1; (iv) x, y+3/2, z1/2.
 

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