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Solvothermal reaction of Ge and Se with Mn(CH3COO)2·4H2O in the presence of [(CH3)3NH]Cl generates the open framework quaternary selenidogerman­ate(IV) [(CH3)3NH]2[MnGe4Se10], which contains corner-linked adamantanoid Ge4Se10 cages and MnSe4 tetra­hedra. The trimethyl­ammonium counter-cations are disordered and exhibit an S4 crystallographic site symmetry. Whereas the Ge-Se distances within the Ge4Se6 core lie in the range 2.357 (1)-2.370 (1) Å, a significantly shorter Ge-Se bond length of 2.284 (1) Å is observed for the bridging Se atom to the MnSe4 units.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805032770/bt6757sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805032770/bt6757Isup2.hkl
Contains datablock I

CCDC reference: 289654

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](e-Mn) = 0.001 Å
  • H-atom completeness 91%
  • Disorder in solvent or counterion
  • R factor = 0.027
  • wR factor = 0.066
  • Data-to-parameter ratio = 14.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 60.00 Perc. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.29 Ratio PLAT850_ALERT_2_C Check Flack Parameter Exact Value 0.00 and su .. 0.05
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:C6 H20 Ge4 Mn1 N2 Se10 Atom count from the _atom_site data: C6 H18 Ge4 Mn1 N2 Se10 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 2 From the CIF: _chemical_formula_sum C6 H20 Ge4 Mn N2 Se10 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 12.00 12.00 0.00 H 40.00 36.00 4.00 Ge 8.00 8.00 0.00 Mn 2.00 2.00 0.00 N 4.00 4.00 0.00 Se 20.00 20.00 0.00 REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 24.95 From the CIF: _reflns_number_total 859 Count of symmetry unique reflns 617 Completeness (_total/calc) 139.22% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 242 Fraction of Friedel pairs measured 0.392 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 7 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 0 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: R3m/V (Siemens, 1989); cell refinement: R3m/V; data reduction: XDISK (Siemens, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1995); software used to prepare material for publication: SHELXL97.

Bis(trimethylammonium) decaselenidotetragermanatomanganate(II) top
Crystal data top
(C3H10N)2[MnGe4Se10]Dx = 3.081 Mg m3
Mr = 1255.14Melting point: not measured K
Tetragonal, I4Mo Kα radiation, λ = 0.71073 Å
Hall symbol: I -4Cell parameters from 22 reflections
a = 9.559 (2) Åθ = 4.9–12.9°
c = 14.808 (6) ŵ = 18.29 mm1
V = 1353.0 (7) Å3T = 293 K
Z = 2Tetrahedron, orange
F(000) = 11260.16 × 0.14 × 0.12 mm
Data collection top
Siemens P4 four-circle
diffractometer
790 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.025
Graphite monochromatorθmax = 25.0°, θmin = 2.5°
ω scansh = 111
Absorption correction: ψ scan
(XPREP in SHELXTL-Plus; Sheldrick, 1995)
k = 111
Tmin = 0.069, Tmax = 0.117l = 117
945 measured reflections3 standard reflections every 97 reflections
859 independent reflections intensity decay: 0.02%
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)] = 0.027H-atom parameters constrained
wR(F2) = 0.066 w = 1/[σ2(Fo2) + (0.0368P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.002
859 reflectionsΔρmax = 0.53 e Å3
59 parametersΔρmin = 0.59 e Å3
0 restraintsAbsolute structure: Flack (1983), 242 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.00 (5)
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)
Ge0.17744 (8)0.91692 (9)0.91103 (5)0.0248 (2)
Se10.00001.00000.81435 (7)0.0338 (3)
Se20.09687 (9)0.72754 (9)1.00028 (7)0.0342 (2)
Se30.34837 (10)0.81447 (9)0.82588 (6)0.0375 (3)
Mn0.50001.00000.75000.0252 (6)
C10.4546 (19)0.6114 (17)1.0611 (10)0.073 (5)0.75
H1A0.40020.67861.02810.109*0.75
H1B0.53510.65661.08660.109*0.75
H1C0.39860.57211.10860.109*0.75
N10.50000.50001.00000.159 (14)
C20.112 (2)0.565 (2)0.801 (2)0.122 (10)0.75
H2A0.19420.57190.76430.183*0.75
H2B0.08350.65710.81980.183*0.75
H2C0.13220.50960.85370.183*0.75
N20.00000.50000.75000.28 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ge0.0265 (4)0.0242 (4)0.0238 (4)0.0012 (4)0.0063 (4)0.0014 (4)
Se10.0406 (7)0.0406 (7)0.0204 (6)0.0046 (7)0.0000.000
Se20.0375 (5)0.0259 (4)0.0391 (5)0.0051 (4)0.0116 (5)0.0051 (4)
Se30.0435 (5)0.0254 (5)0.0437 (5)0.0060 (4)0.0232 (5)0.0030 (4)
Mn0.0266 (8)0.0266 (8)0.0226 (14)0.0000.0000.000
C10.079 (11)0.059 (9)0.081 (12)0.002 (9)0.001 (10)0.019 (10)
N10.122 (16)0.122 (16)0.23 (4)0.0000.0000.000
C20.070 (12)0.100 (18)0.20 (3)0.028 (14)0.039 (17)0.025 (19)
N20.31 (6)0.31 (6)0.23 (7)0.0000.0000.000
Geometric parameters (Å, º) top
Ge—Se32.2843 (12)C1—H1B0.9600
Ge—Se2i2.3471 (13)C1—H1C0.9600
Ge—Se12.3574 (11)N1—C1vii1.463 (14)
Ge—Se22.3699 (13)N1—C1viii1.463 (13)
Se1—Geii2.3574 (11)N1—C1ix1.463 (14)
Se2—Geiii2.3471 (13)C2—N21.45 (2)
Se3—Mn2.5512 (10)C2—H2A0.9600
Mn—Se3iv2.5512 (10)C2—H2B0.9600
Mn—Se3v2.5512 (10)C2—H2C0.9600
Mn—Se3vi2.5512 (10)N2—C2x1.45 (2)
C1—N11.463 (13)N2—C2xi1.45 (2)
C1—H1A0.9600N2—C2xii1.45 (2)
Se3—Ge—Se2i110.26 (5)H1B—C1—H1C109.5
Se3—Ge—Se1108.89 (5)C1vii—N1—C1112.5 (7)
Se2i—Ge—Se1111.80 (4)C1vii—N1—C1viii112.5 (7)
Se3—Ge—Se2102.29 (5)C1—N1—C1viii103.6 (14)
Se2i—Ge—Se2111.93 (4)C1vii—N1—C1ix103.6 (14)
Se1—Ge—Se2111.23 (4)C1—N1—C1ix112.5 (7)
Ge—Se1—Geii105.21 (6)C1viii—N1—C1ix112.5 (7)
Geiii—Se2—Ge104.76 (5)N2—C2—H2A109.5
Ge—Se3—Mn110.58 (4)N2—C2—H2B109.5
Se3iv—Mn—Se3v101.19 (2)H2A—C2—H2B109.5
Se3iv—Mn—Se3127.73 (5)N2—C2—H2C109.5
Se3v—Mn—Se3101.19 (2)H2A—C2—H2C109.5
Se3iv—Mn—Se3vi101.19 (2)H2B—C2—H2C109.5
Se3v—Mn—Se3vi127.73 (5)C2x—N2—C2xi117 (2)
Se3—Mn—Se3vi101.19 (2)C2x—N2—C2xii105.9 (9)
N1—C1—H1A109.5C2xi—N2—C2xii105.9 (9)
N1—C1—H1B109.5C2x—N2—C2105.9 (9)
H1A—C1—H1B109.5C2xi—N2—C2105.9 (9)
N1—C1—H1C109.5C2xii—N2—C2117 (2)
H1A—C1—H1C109.5
Se3—Ge—Se1—Geii174.85 (5)Se2i—Ge—Se3—Mn46.50 (6)
Se2i—Ge—Se1—Geii63.07 (4)Se1—Ge—Se3—Mn76.50 (5)
Se2—Ge—Se1—Geii62.87 (3)Se2—Ge—Se3—Mn165.70 (4)
Se3—Ge—Se2—Geiii179.05 (5)Ge—Se3—Mn—Se3iv61.80 (4)
Se2i—Ge—Se2—Geiii62.93 (4)Ge—Se3—Mn—Se3v175.57 (5)
Se1—Ge—Se2—Geiii62.94 (6)Ge—Se3—Mn—Se3vi51.97 (3)
Symmetry codes: (i) y+1, x+1, z+2; (ii) x, y+2, z; (iii) y1, x+1, z+2; (iv) x+1, y+2, z; (v) y+3/2, x+1/2, z+3/2; (vi) y1/2, x+3/2, z+3/2; (vii) y+1, x, z+2; (viii) x+1, y+1, z; (ix) y, x+1, z+2; (x) y+1/2, x+1/2, z+3/2; (xi) y1/2, x+1/2, z+3/2; (xii) x, y+1, z.
 

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