Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805032770/bt6757sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805032770/bt6757Isup2.hkl |
CCDC reference: 289654
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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.
(C3H10N)2[MnGe4Se10] | Dx = 3.081 Mg m−3 |
Mr = 1255.14 | Melting point: not measured K |
Tetragonal, I4 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: I -4 | Cell parameters from 22 reflections |
a = 9.559 (2) Å | θ = 4.9–12.9° |
c = 14.808 (6) Å | µ = 18.29 mm−1 |
V = 1353.0 (7) Å3 | T = 293 K |
Z = 2 | Tetrahedron, orange |
F(000) = 1126 | 0.16 × 0.14 × 0.12 mm |
Siemens P4 four-circle diffractometer | 790 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.025 |
Graphite monochromator | θmax = 25.0°, θmin = 2.5° |
ω scans | h = −1→11 |
Absorption correction: ψ scan (XPREP in SHELXTL-Plus; Sheldrick, 1995) | k = −1→11 |
Tmin = 0.069, Tmax = 0.117 | l = −1→17 |
945 measured reflections | 3 standard reflections every 97 reflections |
859 independent reflections | intensity decay: 0.02% |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.027 | H-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 reflections | Δρmax = 0.53 e Å−3 |
59 parameters | Δρmin = −0.59 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 242 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.00 (5) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ge | 0.17744 (8) | 0.91692 (9) | 0.91103 (5) | 0.0248 (2) | |
Se1 | 0.0000 | 1.0000 | 0.81435 (7) | 0.0338 (3) | |
Se2 | 0.09687 (9) | 0.72754 (9) | 1.00028 (7) | 0.0342 (2) | |
Se3 | 0.34837 (10) | 0.81447 (9) | 0.82588 (6) | 0.0375 (3) | |
Mn | 0.5000 | 1.0000 | 0.7500 | 0.0252 (6) | |
C1 | 0.4546 (19) | 0.6114 (17) | 1.0611 (10) | 0.073 (5) | 0.75 |
H1A | 0.4002 | 0.6786 | 1.0281 | 0.109* | 0.75 |
H1B | 0.5351 | 0.6566 | 1.0866 | 0.109* | 0.75 |
H1C | 0.3986 | 0.5721 | 1.1086 | 0.109* | 0.75 |
N1 | 0.5000 | 0.5000 | 1.0000 | 0.159 (14) | |
C2 | −0.112 (2) | 0.565 (2) | 0.801 (2) | 0.122 (10) | 0.75 |
H2A | −0.1942 | 0.5719 | 0.7643 | 0.183* | 0.75 |
H2B | −0.0835 | 0.6571 | 0.8198 | 0.183* | 0.75 |
H2C | −0.1322 | 0.5096 | 0.8537 | 0.183* | 0.75 |
N2 | 0.0000 | 0.5000 | 0.7500 | 0.28 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ge | 0.0265 (4) | 0.0242 (4) | 0.0238 (4) | 0.0012 (4) | 0.0063 (4) | −0.0014 (4) |
Se1 | 0.0406 (7) | 0.0406 (7) | 0.0204 (6) | 0.0046 (7) | 0.000 | 0.000 |
Se2 | 0.0375 (5) | 0.0259 (4) | 0.0391 (5) | 0.0051 (4) | 0.0116 (5) | 0.0051 (4) |
Se3 | 0.0435 (5) | 0.0254 (5) | 0.0437 (5) | 0.0060 (4) | 0.0232 (5) | 0.0030 (4) |
Mn | 0.0266 (8) | 0.0266 (8) | 0.0226 (14) | 0.000 | 0.000 | 0.000 |
C1 | 0.079 (11) | 0.059 (9) | 0.081 (12) | −0.002 (9) | 0.001 (10) | −0.019 (10) |
N1 | 0.122 (16) | 0.122 (16) | 0.23 (4) | 0.000 | 0.000 | 0.000 |
C2 | 0.070 (12) | 0.100 (18) | 0.20 (3) | 0.028 (14) | −0.039 (17) | 0.025 (19) |
N2 | 0.31 (6) | 0.31 (6) | 0.23 (7) | 0.000 | 0.000 | 0.000 |
Ge—Se3 | 2.2843 (12) | C1—H1B | 0.9600 |
Ge—Se2i | 2.3471 (13) | C1—H1C | 0.9600 |
Ge—Se1 | 2.3574 (11) | N1—C1vii | 1.463 (14) |
Ge—Se2 | 2.3699 (13) | N1—C1viii | 1.463 (13) |
Se1—Geii | 2.3574 (11) | N1—C1ix | 1.463 (14) |
Se2—Geiii | 2.3471 (13) | C2—N2 | 1.45 (2) |
Se3—Mn | 2.5512 (10) | C2—H2A | 0.9600 |
Mn—Se3iv | 2.5512 (10) | C2—H2B | 0.9600 |
Mn—Se3v | 2.5512 (10) | C2—H2C | 0.9600 |
Mn—Se3vi | 2.5512 (10) | N2—C2x | 1.45 (2) |
C1—N1 | 1.463 (13) | N2—C2xi | 1.45 (2) |
C1—H1A | 0.9600 | N2—C2xii | 1.45 (2) |
Se3—Ge—Se2i | 110.26 (5) | H1B—C1—H1C | 109.5 |
Se3—Ge—Se1 | 108.89 (5) | C1vii—N1—C1 | 112.5 (7) |
Se2i—Ge—Se1 | 111.80 (4) | C1vii—N1—C1viii | 112.5 (7) |
Se3—Ge—Se2 | 102.29 (5) | C1—N1—C1viii | 103.6 (14) |
Se2i—Ge—Se2 | 111.93 (4) | C1vii—N1—C1ix | 103.6 (14) |
Se1—Ge—Se2 | 111.23 (4) | C1—N1—C1ix | 112.5 (7) |
Ge—Se1—Geii | 105.21 (6) | C1viii—N1—C1ix | 112.5 (7) |
Geiii—Se2—Ge | 104.76 (5) | N2—C2—H2A | 109.5 |
Ge—Se3—Mn | 110.58 (4) | N2—C2—H2B | 109.5 |
Se3iv—Mn—Se3v | 101.19 (2) | H2A—C2—H2B | 109.5 |
Se3iv—Mn—Se3 | 127.73 (5) | N2—C2—H2C | 109.5 |
Se3v—Mn—Se3 | 101.19 (2) | H2A—C2—H2C | 109.5 |
Se3iv—Mn—Se3vi | 101.19 (2) | H2B—C2—H2C | 109.5 |
Se3v—Mn—Se3vi | 127.73 (5) | C2x—N2—C2xi | 117 (2) |
Se3—Mn—Se3vi | 101.19 (2) | C2x—N2—C2xii | 105.9 (9) |
N1—C1—H1A | 109.5 | C2xi—N2—C2xii | 105.9 (9) |
N1—C1—H1B | 109.5 | C2x—N2—C2 | 105.9 (9) |
H1A—C1—H1B | 109.5 | C2xi—N2—C2 | 105.9 (9) |
N1—C1—H1C | 109.5 | C2xii—N2—C2 | 117 (2) |
H1A—C1—H1C | 109.5 | ||
Se3—Ge—Se1—Geii | 174.85 (5) | Se2i—Ge—Se3—Mn | −46.50 (6) |
Se2i—Ge—Se1—Geii | −63.07 (4) | Se1—Ge—Se3—Mn | 76.50 (5) |
Se2—Ge—Se1—Geii | 62.87 (3) | Se2—Ge—Se3—Mn | −165.70 (4) |
Se3—Ge—Se2—Geiii | −179.05 (5) | Ge—Se3—Mn—Se3iv | 61.80 (4) |
Se2i—Ge—Se2—Geiii | 62.93 (4) | Ge—Se3—Mn—Se3v | 175.57 (5) |
Se1—Ge—Se2—Geiii | −62.94 (6) | Ge—Se3—Mn—Se3vi | −51.97 (3) |
Symmetry codes: (i) −y+1, x+1, −z+2; (ii) −x, −y+2, z; (iii) y−1, −x+1, −z+2; (iv) −x+1, −y+2, z; (v) −y+3/2, x+1/2, −z+3/2; (vi) y−1/2, −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) y−1/2, −x+1/2, −z+3/2; (xii) −x, −y+1, z. |