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The crystal structure of the title compound, [Mn(C2H8N2)3]2[Sb2Se5], consists of discrete [Mn(en)3]2+ complex cations and [Sb2Se5]4− anions. There are two crystallographically independent cations and two crystallographically independent anions in the asymmetric unit. The cations occupy general positions whereas the anions are each located on a twofold axis. Between the Se atoms of the anions and the H atoms of the amino groups, short intermolecular distances are observed, which indicate hydrogen bonding.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803003386/bt6239sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803003386/bt6239Isup2.hkl
Contains datablock I

CCDC reference: 206742

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.009 Å
  • R factor = 0.030
  • wR factor = 0.075
  • Data-to-parameter ratio = 23.2

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.01 From the CIF: _reflns_number_total 6991 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 7542 Completeness (_total/calc) 92.69% Alert C: < 95% complete PLAT_420 Alert C D-H Without Acceptor N(4) - H(7N) ? PLAT_420 Alert C D-H Without Acceptor N(4) - H(8N) ? PLAT_420 Alert C D-H Without Acceptor N(5) - H(9N) ? PLAT_420 Alert C D-H Without Acceptor N(10) - H(20N) ? PLAT_420 Alert C D-H Without Acceptor N(11) - H(21N) ?
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
6 Alert Level C = Please check

Computing details top

Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; 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.

Bis[tris(1,2-ethanediamine-κ2N,N')manganese] pentaselenodiantimonate(III) top
Crystal data top
[Mn(C2H8N2)3]2[Sb2Se5]F(000) = 2104
Mr = 1108.80Dx = 2.137 Mg m3
Monoclinic, P2/nMo Kα radiation, λ = 0.71073 Å
a = 19.909 (3) ÅCell parameters from 7997 reflections
b = 9.041 (1) Åθ = 2–28°
c = 20.015 (3) ŵ = 7.57 mm1
β = 106.928 (17)°T = 293 K
V = 3446.5 (8) Å3Polyhedron, orange
Z = 40.11 × 0.08 × 0.06 mm
Data collection top
Stoe IPDS
diffractometer
6991 independent reflections
Radiation source: fine-focus sealed tube6407 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.055
φ scansθmax = 27.0°, θmin = 2.1°
Absorption correction: numerical
(X-SHAPE; Stoe & Cie, 1998)
h = 2525
Tmin = 0.476, Tmax = 0.625k = 1111
29806 measured reflectionsl = 2424
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)] = 0.030H-atom parameters constrained
wR(F2) = 0.075 w = 1/[σ2(Fo2) + (0.0493P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
6991 reflectionsΔρmax = 0.66 e Å3
301 parametersΔρmin = 0.96 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00151 (18)
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
Sb10.655386 (17)0.05535 (3)0.75721 (2)0.03145 (9)
Se10.75000.13853 (7)0.75000.03065 (15)
Se20.63283 (3)0.02789 (6)0.86844 (3)0.03416 (12)
Se30.54943 (3)0.03463 (9)0.66379 (3)0.05375 (19)
Sb20.246232 (17)0.57763 (3)0.654773 (17)0.02763 (9)
Se40.25000.37468 (7)0.75000.02973 (15)
Se50.36201 (3)0.54507 (6)0.63220 (3)0.03678 (13)
Se60.16176 (3)0.46609 (7)0.54806 (3)0.04270 (14)
Mn10.02795 (4)0.50839 (8)0.66504 (4)0.02794 (16)
N10.0683 (2)0.3673 (5)0.6995 (3)0.0460 (12)
H1N0.10170.40340.68180.055*
H2N0.08510.36870.74640.055*
C10.0514 (3)0.2140 (6)0.6752 (3)0.0428 (13)
H1A0.02630.16510.70390.051*
H1B0.09430.15930.67900.051*
C20.0066 (3)0.2177 (5)0.6002 (3)0.0417 (12)
H2A0.03220.26410.57140.050*
H2B0.00540.11770.58330.050*
N20.0576 (2)0.3018 (4)0.5958 (2)0.0361 (10)
H3N0.08780.24550.61050.043*
H4N0.07850.32860.55130.043*
N30.1410 (2)0.5785 (5)0.6401 (3)0.0386 (10)
H5N0.14370.67760.64300.046*
H6N0.16450.55110.59620.046*
C30.1725 (3)0.5082 (7)0.6901 (4)0.0489 (15)
H3A0.18190.40480.67790.059*
H3B0.21680.55590.68760.059*
C40.1245 (4)0.5199 (8)0.7623 (4)0.0554 (16)
H4A0.11600.62320.77510.066*
H4B0.14570.47360.79480.066*
N40.0570 (3)0.4457 (6)0.7658 (3)0.0477 (12)
H7N0.06160.34700.76830.057*
H8N0.02320.47600.80390.057*
N50.0211 (2)0.7218 (5)0.7160 (2)0.0361 (10)
H9N0.01260.78710.71740.043*
H10N0.04780.70440.75990.043*
C50.0648 (3)0.7817 (6)0.6736 (3)0.0423 (13)
H5A0.07690.88370.68680.051*
H5B0.10800.72540.68310.051*
C60.0275 (3)0.7748 (6)0.5980 (3)0.0430 (13)
H6A0.01330.83910.58760.052*
H6B0.05820.80950.57160.052*
N60.0050 (2)0.6227 (4)0.5770 (2)0.0355 (9)
H11N0.04060.57230.56830.043*
H12N0.03130.62380.53780.043*
Mn20.66301 (4)0.02505 (8)0.47260 (4)0.02940 (16)
N70.5887 (2)0.2209 (5)0.4371 (3)0.0425 (11)
H13N0.54520.18830.41480.051*
H14N0.60360.27820.40760.051*
C70.5874 (3)0.3068 (6)0.4992 (3)0.0455 (13)
H7A0.56830.40450.48520.055*
H7B0.55760.25790.52310.055*
C80.6600 (3)0.3198 (6)0.5471 (3)0.0452 (13)
H8A0.65950.37680.58800.054*
H8B0.68960.37080.52370.054*
N80.6881 (3)0.1708 (5)0.5682 (3)0.0478 (12)
H15N0.73490.17540.58780.057*
H16N0.66860.13320.59990.057*
N90.5801 (2)0.1067 (5)0.5052 (2)0.0364 (9)
H17N0.54160.11690.46840.044*
H18N0.56770.05730.53880.044*
C90.6071 (3)0.2549 (6)0.5316 (3)0.0448 (14)
H9A0.58140.29230.56250.054*
H9B0.60030.32310.49280.054*
C100.6836 (3)0.2442 (6)0.5702 (3)0.0443 (13)
H10A0.70180.34170.58600.053*
H10B0.69000.18160.61100.053*
N100.7219 (2)0.1825 (5)0.5247 (3)0.0396 (10)
H19N0.76600.15870.54980.047*
H20N0.72430.24910.49210.047*
N110.7591 (3)0.1061 (6)0.4433 (3)0.0523 (13)
H21N0.79840.08650.47810.063*
H22N0.75640.20450.43620.063*
C110.7612 (3)0.0298 (8)0.3796 (4)0.0541 (16)
H11A0.79280.08160.35880.065*
H11B0.77910.06960.39110.065*
C120.6899 (4)0.0226 (8)0.3284 (4)0.0551 (16)
H12A0.69210.03200.28740.066*
H12B0.67350.12180.31390.066*
N120.6407 (3)0.0497 (5)0.3594 (2)0.0381 (10)
H23N0.59640.02590.33520.046*
H24N0.64550.14850.35770.046*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.02897 (17)0.02431 (14)0.0420 (2)0.00189 (11)0.01182 (13)0.00511 (12)
Se10.0251 (3)0.0339 (3)0.0343 (4)0.0000.0107 (3)0.000
Se20.0313 (2)0.0391 (3)0.0333 (3)0.0014 (2)0.0114 (2)0.0070 (2)
Se30.0251 (3)0.0984 (6)0.0320 (4)0.0020 (3)0.0007 (2)0.0155 (3)
Sb20.03206 (17)0.02364 (14)0.02782 (19)0.00404 (11)0.00969 (12)0.00058 (11)
Se40.0307 (3)0.0320 (3)0.0281 (4)0.0000.0112 (3)0.000
Se50.0340 (3)0.0429 (3)0.0365 (3)0.0032 (2)0.0151 (2)0.0008 (2)
Se60.0322 (3)0.0563 (3)0.0310 (3)0.0078 (2)0.0044 (2)0.0014 (2)
Mn10.0240 (3)0.0239 (3)0.0349 (4)0.0002 (3)0.0068 (3)0.0012 (3)
N10.028 (2)0.038 (2)0.060 (3)0.0055 (18)0.005 (2)0.012 (2)
C10.033 (3)0.029 (2)0.065 (4)0.011 (2)0.013 (2)0.006 (2)
C20.054 (3)0.027 (2)0.048 (4)0.001 (2)0.019 (3)0.005 (2)
N20.039 (2)0.027 (2)0.037 (3)0.0067 (17)0.0012 (18)0.0014 (17)
N30.028 (2)0.035 (2)0.048 (3)0.0029 (17)0.0039 (18)0.0024 (19)
C30.029 (3)0.045 (3)0.076 (5)0.002 (2)0.021 (3)0.004 (3)
C40.066 (4)0.053 (4)0.059 (5)0.007 (3)0.037 (3)0.004 (3)
N40.042 (3)0.052 (3)0.047 (3)0.005 (2)0.009 (2)0.008 (2)
N50.034 (2)0.032 (2)0.039 (3)0.0000 (17)0.0058 (18)0.0101 (18)
C50.035 (3)0.034 (3)0.057 (4)0.009 (2)0.014 (2)0.015 (2)
C60.051 (3)0.030 (2)0.053 (4)0.007 (2)0.022 (3)0.002 (2)
N60.038 (2)0.032 (2)0.037 (3)0.0036 (17)0.0108 (18)0.0045 (17)
Mn20.0347 (4)0.0241 (3)0.0273 (4)0.0046 (3)0.0057 (3)0.0001 (3)
N70.039 (2)0.030 (2)0.047 (3)0.0020 (18)0.006 (2)0.0041 (19)
C70.049 (3)0.031 (3)0.058 (4)0.000 (2)0.018 (3)0.001 (2)
C80.061 (4)0.029 (2)0.045 (4)0.009 (2)0.015 (3)0.013 (2)
N80.055 (3)0.046 (3)0.033 (3)0.002 (2)0.003 (2)0.007 (2)
N90.032 (2)0.036 (2)0.039 (3)0.0043 (17)0.0061 (18)0.0012 (18)
C90.062 (4)0.029 (3)0.045 (4)0.011 (2)0.019 (3)0.003 (2)
C100.051 (3)0.042 (3)0.034 (3)0.003 (2)0.003 (2)0.011 (2)
N100.039 (2)0.034 (2)0.042 (3)0.0011 (18)0.007 (2)0.0030 (19)
N110.047 (3)0.052 (3)0.056 (4)0.024 (2)0.012 (2)0.001 (2)
C110.050 (4)0.061 (4)0.059 (5)0.018 (3)0.027 (3)0.007 (3)
C120.067 (4)0.062 (4)0.040 (4)0.009 (3)0.022 (3)0.005 (3)
N120.041 (2)0.035 (2)0.034 (3)0.0051 (18)0.0046 (19)0.0055 (18)
Geometric parameters (Å, º) top
Sb1—Se22.5113 (7)C6—H6A0.9700
Sb1—Se32.5121 (9)C6—H6B0.9700
Sb1—Se12.6077 (6)N6—H11N0.9000
Se1—Sb1i2.6077 (6)N6—H12N0.9000
Sb2—Se52.4920 (7)Mn2—N82.257 (5)
Sb2—Se62.5131 (8)Mn2—N112.279 (5)
Sb2—Se42.6309 (6)Mn2—N92.280 (4)
Se4—Sb2ii2.6309 (6)Mn2—N122.281 (5)
Mn1—N12.238 (4)Mn2—N72.284 (4)
Mn1—N32.251 (4)Mn2—N102.296 (5)
Mn1—N52.266 (4)N7—C71.471 (8)
Mn1—N62.297 (4)N7—H13N0.9000
Mn1—N22.298 (4)N7—H14N0.9000
Mn1—N42.325 (5)C7—C81.488 (9)
N1—C11.475 (7)C7—H7A0.9700
N1—H1N0.9000C7—H7B0.9700
N1—H2N0.9000C8—N81.473 (7)
C1—C21.508 (9)C8—H8A0.9700
C1—H1A0.9700C8—H8B0.9700
C1—H1B0.9700N8—H15N0.9000
C2—N21.467 (7)N8—H16N0.9000
C2—H2A0.9700N9—C91.482 (7)
C2—H2B0.9700N9—H17N0.9000
N2—H3N0.9000N9—H18N0.9000
N2—H4N0.9000C9—C101.497 (9)
N3—C31.471 (8)C9—H9A0.9700
N3—H5N0.9000C9—H9B0.9700
N3—H6N0.9000C10—N101.459 (7)
C3—C41.487 (10)C10—H10A0.9700
C3—H3A0.9700C10—H10B0.9700
C3—H3B0.9700N10—H19N0.9000
C4—N41.484 (8)N10—H20N0.9000
C4—H4A0.9700N11—C111.461 (9)
C4—H4B0.9700N11—H21N0.9000
N4—H7N0.9000N11—H22N0.9000
N4—H8N0.9000C11—C121.491 (10)
N5—C51.484 (7)C11—H11A0.9700
N5—H9N0.9000C11—H11B0.9700
N5—H10N0.9000C12—N121.456 (7)
C5—C61.480 (9)C12—H12A0.9700
C5—H5A0.9700C12—H12B0.9700
C5—H5B0.9700N12—H23N0.9000
C6—N61.469 (6)N12—H24N0.9000
Se2—Sb1—Se3103.57 (3)Mn1—N6—H11N109.8
Se2—Sb1—Se199.56 (2)C6—N6—H12N109.8
Se3—Sb1—Se1101.81 (2)Mn1—N6—H12N109.8
Sb1i—Se1—Sb195.53 (3)H11N—N6—H12N108.2
Se5—Sb2—Se6102.94 (3)N8—Mn2—N1192.0 (2)
Se5—Sb2—Se4102.48 (2)N8—Mn2—N993.57 (19)
Se6—Sb2—Se4101.93 (2)N11—Mn2—N9166.83 (19)
Sb2ii—Se4—Sb291.56 (3)N8—Mn2—N12161.18 (18)
N1—Mn1—N3160.19 (18)N11—Mn2—N1276.98 (18)
N1—Mn1—N597.39 (16)N9—Mn2—N12100.50 (16)
N3—Mn1—N597.59 (16)N8—Mn2—N776.95 (17)
N1—Mn1—N694.70 (19)N11—Mn2—N7100.8 (2)
N3—Mn1—N6101.18 (17)N9—Mn2—N792.08 (17)
N5—Mn1—N677.29 (16)N12—Mn2—N790.01 (17)
N1—Mn1—N276.64 (16)N8—Mn2—N1097.70 (17)
N3—Mn1—N291.74 (16)N11—Mn2—N1091.35 (19)
N5—Mn1—N2164.73 (17)N9—Mn2—N1076.09 (16)
N6—Mn1—N289.08 (16)N12—Mn2—N1097.77 (17)
N1—Mn1—N490.1 (2)N7—Mn2—N10166.82 (18)
N3—Mn1—N477.04 (18)C7—N7—Mn2108.4 (3)
N5—Mn1—N490.06 (18)C7—N7—H13N110.0
N6—Mn1—N4166.94 (17)Mn2—N7—H13N110.0
N2—Mn1—N4103.85 (18)C7—N7—H14N110.0
C1—N1—Mn1110.0 (3)Mn2—N7—H14N110.0
C1—N1—H1N109.7H13N—N7—H14N108.4
Mn1—N1—H1N109.7N7—C7—C8109.5 (5)
C1—N1—H2N109.7N7—C7—H7A109.8
Mn1—N1—H2N109.7C8—C7—H7A109.8
H1N—N1—H2N108.2N7—C7—H7B109.8
N1—C1—C2108.6 (4)C8—C7—H7B109.8
N1—C1—H1A110.0H7A—C7—H7B108.2
C2—C1—H1A110.0N8—C8—C7109.2 (4)
N1—C1—H1B110.0N8—C8—H8A109.8
C2—C1—H1B110.0C7—C8—H8A109.8
H1A—C1—H1B108.3N8—C8—H8B109.8
N2—C2—C1108.9 (4)C7—C8—H8B109.8
N2—C2—H2A109.9H8A—C8—H8B108.3
C1—C2—H2A109.9C8—N8—Mn2108.6 (3)
N2—C2—H2B109.9C8—N8—H15N110.0
C1—C2—H2B109.9Mn2—N8—H15N110.0
H2A—C2—H2B108.3C8—N8—H16N110.0
C2—N2—Mn1108.6 (3)Mn2—N8—H16N110.0
C2—N2—H3N110.0H15N—N8—H16N108.4
Mn1—N2—H3N110.0C9—N9—Mn2110.9 (3)
C2—N2—H4N110.0C9—N9—H17N109.5
Mn1—N2—H4N110.0Mn2—N9—H17N109.5
H3N—N2—H4N108.4C9—N9—H18N109.5
C3—N3—Mn1108.9 (3)Mn2—N9—H18N109.5
C3—N3—H5N109.9H17N—N9—H18N108.0
Mn1—N3—H5N109.9N9—C9—C10109.5 (4)
C3—N3—H6N109.9N9—C9—H9A109.8
Mn1—N3—H6N109.9C10—C9—H9A109.8
H5N—N3—H6N108.3N9—C9—H9B109.8
N3—C3—C4110.4 (5)C10—C9—H9B109.8
N3—C3—H3A109.6H9A—C9—H9B108.2
C4—C3—H3A109.6N10—C10—C9109.9 (5)
N3—C3—H3B109.6N10—C10—H10A109.7
C4—C3—H3B109.6C9—C10—H10A109.7
H3A—C3—H3B108.1N10—C10—H10B109.7
N4—C4—C3109.3 (5)C9—C10—H10B109.7
N4—C4—H4A109.8H10A—C10—H10B108.2
C3—C4—H4A109.8C10—N10—Mn2107.8 (3)
N4—C4—H4B109.8C10—N10—H19N110.2
C3—C4—H4B109.8Mn2—N10—H19N110.2
H4A—C4—H4B108.3C10—N10—H20N110.2
C4—N4—Mn1107.4 (4)Mn2—N10—H20N110.2
C4—N4—H7N110.2H19N—N10—H20N108.5
Mn1—N4—H7N110.2C11—N11—Mn2108.2 (3)
C4—N4—H8N110.2C11—N11—H21N110.1
Mn1—N4—H8N110.2Mn2—N11—H21N110.1
H7N—N4—H8N108.5C11—N11—H22N110.1
C5—N5—Mn1107.5 (3)Mn2—N11—H22N110.1
C5—N5—H9N110.2H21N—N11—H22N108.4
Mn1—N5—H9N110.2N11—C11—C12111.0 (6)
C5—N5—H10N110.2N11—C11—H11A109.4
Mn1—N5—H10N110.2C12—C11—H11A109.4
H9N—N5—H10N108.5N11—C11—H11B109.4
C6—C5—N5111.5 (4)C12—C11—H11B109.4
C6—C5—H5A109.3H11A—C11—H11B108.0
N5—C5—H5A109.3N12—C12—C11110.5 (5)
C6—C5—H5B109.3N12—C12—H12A109.6
N5—C5—H5B109.3C11—C12—H12A109.6
H5A—C5—H5B108.0N12—C12—H12B109.6
N6—C6—C5110.6 (5)C11—C12—H12B109.6
N6—C6—H6A109.5H12A—C12—H12B108.1
C5—C6—H6A109.5C12—N12—Mn2109.3 (4)
N6—C6—H6B109.5C12—N12—H23N109.8
C5—C6—H6B109.5Mn2—N12—H23N109.8
H6A—C6—H6B108.1C12—N12—H24N109.8
C6—N6—Mn1109.5 (3)Mn2—N12—H24N109.8
C6—N6—H11N109.8H23N—N12—H24N108.3
Symmetry codes: (i) x+3/2, y, z+3/2; (ii) x+1/2, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H5N···Se2iii0.902.693.568 (4)167
N5—H10N···Se5ii0.902.783.618 (5)156
N6—H11N···Se60.902.733.623 (4)170
N6—H12N···Se6iv0.902.793.619 (5)155
N7—H14N···Se5v0.902.693.503 (5)151
N9—H18N···Se30.902.763.634 (5)165
N10—H19N···Se2i0.902.773.598 (5)154
N12—H24N···Se5vi0.902.783.669 (4)168
Symmetry codes: (i) x+3/2, y, z+3/2; (ii) x+1/2, y, z+3/2; (iii) x+1/2, y+1, z+3/2; (iv) x, y+1, z+1; (v) x+1, y, z+1; (vi) x+1, y+1, z+1.
 

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