The title compound, [Mn(C2H8N2)3]2[Sn2Te6], contains [Mn(en)3]2+ (en is ethylenediamine) complex cations and crystallographically centrosymmetric [Sn2Te6]4− anions in its monoclinic crystal structure. The five-membered chelate rings of symmetry-related cations exhibit either λλλ or δδδ conformations. Two SnTe4 tetrahedra edge-share to afford the hexatelluridodistannate(IV) anions, whose terminal Sn—Te bonds are significantly shorter than the bridging Sn—Te bonds.
Supporting information
CCDC reference: 289649
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.014 Å
- R factor = 0.036
- wR factor = 0.106
- Data-to-parameter ratio = 23.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT480_ALERT_4_B Long H...A H-Bond Reported H9A .. TE2 .. 3.60 Ang.
PLAT480_ALERT_4_B Long H...A H-Bond Reported H9B .. TE2 .. 3.61 Ang.
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 ............ 2.00 Ratio
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 14
PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1A ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1B ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N4 - H4A ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N4 - H4B ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N5 - H5A ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N5 - H5B ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N8 - H8A ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N8 - H8B ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N9 - H9A ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N9 - H9B ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N12 - H12A ... ?
PLAT420_ALERT_2_C D-H Without Acceptor N12 - H12B ... ?
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1A .. TE1 .. 3.34 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1B .. TE3 .. 3.31 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H8A .. TE3 .. 3.19 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H9A .. TE1 .. 3.19 Ang.
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 44.00 A 3
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
25 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
14 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
6 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 (Sheldrick, 1995); software used to prepare material for publication: SHELXL97.
Bis[tris(ethylenediamine)manganese(II)]
di-µ-tellurido-bis[ditelluridostannate(IV)]
top
Crystal data top
[Mn(C2H8N2)3]2[Sn2T6] | F(000) = 1332 |
Mr = 1473.44 | Dx = 2.359 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 20 reflections |
a = 9.1006 (18) Å | θ = 12.4–32.1° |
b = 18.019 (4) Å | µ = 5.94 mm−1 |
c = 12.701 (3) Å | T = 293 K |
β = 95.23 (3)° | Block, dark-red |
V = 2074.1 (7) Å3 | 0.5 × 0.4 × 0.3 mm |
Z = 2 | |
Data collection top
Siemens P4 four-circle diffractometer | 3055 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.028 |
Graphite monochromator | θmax = 25.0°, θmin = 2.3° |
ω scans | h = −10→10 |
Absorption correction: ψ scan (XPREP in SHELXTL; Sheldrick, 1995) | k = 0→21 |
Tmin = 0.067, Tmax = 0.169 | l = 0→15 |
3807 measured reflections | 3 standard reflections every 100 reflections |
3639 independent reflections | intensity decay: 1% |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.106 | H-atom parameters constrained |
S = 1.38 | w = 1/[σ2(Fo2) + (0.0494P)2] where P = (Fo2 + 2Fc2)/3 |
3639 reflections | (Δ/σ)max < 0.001 |
154 parameters | Δρmax = 0.95 e Å−3 |
0 restraints | Δρmin = −1.03 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Sn | 0.49729 (6) | 0.09053 (3) | 0.07648 (4) | 0.04450 (15) | |
Te3 | 0.51030 (6) | 0.22599 (3) | −0.01342 (4) | 0.05234 (16) | |
Te2 | 0.27227 (6) | 0.00041 (3) | −0.02084 (4) | 0.05066 (16) | |
Te1 | 0.47692 (8) | 0.10152 (3) | 0.28637 (4) | 0.0706 (2) | |
Mn | 1.01169 (12) | 0.32129 (6) | 0.12714 (9) | 0.0520 (3) | |
N5 | 0.8779 (8) | 0.4230 (4) | 0.0684 (6) | 0.0675 (19) | |
H5A | 0.9187 | 0.4642 | 0.0983 | 0.081* | |
H5B | 0.8789 | 0.4271 | −0.0022 | 0.081* | |
N12 | 1.2126 (8) | 0.3610 (4) | 0.0449 (5) | 0.072 (2) | |
H12A | 1.2717 | 0.3223 | 0.0335 | 0.087* | |
H12B | 1.1828 | 0.3817 | −0.0179 | 0.087* | |
N4 | 0.9414 (8) | 0.2427 (4) | −0.0100 (6) | 0.0710 (19) | |
H4A | 0.8434 | 0.2348 | −0.0136 | 0.085* | |
H4B | 0.9633 | 0.2627 | −0.0715 | 0.085* | |
N9 | 1.1439 (8) | 0.3863 (4) | 0.2558 (5) | 0.0671 (18) | |
H9A | 1.1045 | 0.4318 | 0.2616 | 0.081* | |
H9B | 1.1417 | 0.3629 | 0.3182 | 0.081* | |
N8 | 0.8018 (8) | 0.3094 (5) | 0.2095 (5) | 0.076 (2) | |
H8A | 0.7431 | 0.2745 | 0.1773 | 0.091* | |
H8B | 0.8236 | 0.2960 | 0.2774 | 0.091* | |
C11 | 1.2927 (10) | 0.4154 (5) | 0.1133 (7) | 0.072 (2) | |
H11A | 1.2447 | 0.4633 | 0.1040 | 0.086* | |
H11B | 1.3924 | 0.4203 | 0.0928 | 0.086* | |
C10 | 1.2989 (9) | 0.3929 (6) | 0.2286 (7) | 0.074 (2) | |
H10A | 1.3497 | 0.3459 | 0.2396 | 0.088* | |
H10B | 1.3512 | 0.4301 | 0.2727 | 0.088* | |
N1 | 1.0999 (9) | 0.2092 (4) | 0.1884 (6) | 0.085 (2) | |
H1A | 1.1980 | 0.2068 | 0.1842 | 0.102* | |
H1B | 1.0822 | 0.2034 | 0.2565 | 0.102* | |
C7 | 0.7247 (11) | 0.3842 (6) | 0.2037 (8) | 0.084 (3) | |
H7A | 0.6235 | 0.3784 | 0.2205 | 0.101* | |
H7B | 0.7743 | 0.4179 | 0.2549 | 0.101* | |
C6 | 0.7270 (10) | 0.4156 (5) | 0.0953 (9) | 0.081 (3) | |
H6A | 0.6725 | 0.3833 | 0.0447 | 0.097* | |
H6B | 0.6795 | 0.4639 | 0.0921 | 0.097* | |
C3 | 1.0207 (11) | 0.1723 (5) | 0.0087 (8) | 0.081 (3) | |
H3A | 1.1206 | 0.1773 | −0.0113 | 0.097* | |
H3B | 0.9719 | 0.1336 | −0.0347 | 0.097* | |
C2 | 1.0252 (12) | 0.1507 (5) | 0.1233 (8) | 0.089 (3) | |
H2A | 0.9256 | 0.1440 | 0.1430 | 0.106* | |
H2B | 1.0778 | 0.1041 | 0.1348 | 0.106* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn | 0.0568 (3) | 0.0393 (3) | 0.0369 (3) | 0.0009 (2) | 0.0018 (2) | −0.00226 (19) |
Te3 | 0.0618 (3) | 0.0392 (3) | 0.0559 (3) | 0.0012 (2) | 0.0049 (2) | 0.0012 (2) |
Te2 | 0.0527 (3) | 0.0450 (3) | 0.0533 (3) | 0.0012 (2) | −0.0003 (2) | −0.0038 (2) |
Te1 | 0.1057 (5) | 0.0699 (4) | 0.0355 (3) | 0.0077 (3) | 0.0027 (3) | −0.0045 (2) |
Mn | 0.0504 (6) | 0.0542 (7) | 0.0509 (6) | 0.0037 (5) | 0.0016 (5) | −0.0088 (5) |
N5 | 0.068 (5) | 0.072 (5) | 0.063 (4) | 0.009 (4) | 0.011 (3) | −0.002 (4) |
N12 | 0.067 (5) | 0.090 (5) | 0.059 (4) | 0.007 (4) | 0.001 (3) | −0.005 (4) |
N4 | 0.075 (5) | 0.075 (5) | 0.064 (4) | −0.004 (4) | 0.011 (4) | −0.016 (4) |
N9 | 0.078 (5) | 0.074 (5) | 0.050 (4) | −0.007 (4) | 0.010 (3) | −0.005 (3) |
N8 | 0.063 (4) | 0.112 (7) | 0.055 (4) | 0.000 (4) | 0.009 (3) | 0.003 (4) |
C11 | 0.057 (5) | 0.079 (6) | 0.080 (6) | −0.004 (4) | 0.010 (4) | 0.006 (5) |
C10 | 0.062 (5) | 0.095 (7) | 0.062 (5) | −0.010 (5) | −0.004 (4) | −0.006 (5) |
N1 | 0.086 (6) | 0.088 (6) | 0.078 (5) | 0.025 (5) | −0.009 (4) | −0.004 (4) |
C7 | 0.069 (6) | 0.108 (8) | 0.077 (6) | 0.009 (6) | 0.018 (5) | −0.023 (6) |
C6 | 0.059 (6) | 0.073 (6) | 0.109 (8) | 0.014 (5) | −0.008 (5) | −0.001 (6) |
C3 | 0.093 (7) | 0.063 (6) | 0.085 (7) | 0.012 (5) | 0.005 (5) | −0.028 (5) |
C2 | 0.098 (8) | 0.060 (6) | 0.101 (8) | 0.007 (5) | −0.029 (6) | −0.014 (6) |
Geometric parameters (Å, º) top
Sn—Te1 | 2.6965 (8) | N9—H9B | 0.9000 |
Sn—Te3 | 2.7018 (8) | N8—C7 | 1.518 (12) |
Sn—Te2i | 2.8022 (8) | N8—H8A | 0.9000 |
Sn—Te2 | 2.8102 (9) | N8—H8B | 0.9000 |
Te2—Sni | 2.8022 (8) | C11—C10 | 1.516 (12) |
Mn—N9 | 2.266 (7) | C11—H11A | 0.9700 |
Mn—N8 | 2.270 (7) | C11—H11B | 0.9700 |
Mn—N1 | 2.283 (8) | C10—H10A | 0.9700 |
Mn—N5 | 2.287 (7) | C10—H10B | 0.9700 |
Mn—N4 | 2.291 (7) | N1—C2 | 1.468 (11) |
Mn—N12 | 2.301 (7) | N1—H1A | 0.9000 |
N5—C6 | 1.452 (11) | N1—H1B | 0.9000 |
N5—H5A | 0.9000 | C7—C6 | 1.490 (14) |
N5—H5B | 0.9000 | C7—H7A | 0.9700 |
N12—C11 | 1.459 (11) | C7—H7B | 0.9700 |
N12—H12A | 0.9000 | C6—H6A | 0.9700 |
N12—H12B | 0.9000 | C6—H6B | 0.9700 |
N4—C3 | 1.469 (11) | C3—C2 | 1.504 (14) |
N4—H4A | 0.9000 | C3—H3A | 0.9700 |
N4—H4B | 0.9000 | C3—H3B | 0.9700 |
N9—C10 | 1.487 (10) | C2—H2A | 0.9700 |
N9—H9A | 0.9000 | C2—H2B | 0.9700 |
| | | |
Te1—Sn—Te3 | 111.17 (2) | C7—N8—H8A | 110.2 |
Te1—Sn—Te2i | 114.38 (3) | Mn—N8—H8A | 110.2 |
Te3—Sn—Te2i | 111.04 (3) | C7—N8—H8B | 110.2 |
Te1—Sn—Te2 | 111.36 (3) | Mn—N8—H8B | 110.2 |
Te3—Sn—Te2 | 113.23 (3) | H8A—N8—H8B | 108.5 |
Te2i—Sn—Te2 | 94.78 (2) | N12—C11—C10 | 111.6 (7) |
Sni—Te2—Sn | 85.22 (2) | N12—C11—H11A | 109.3 |
N9—Mn—N8 | 97.5 (3) | C10—C11—H11A | 109.3 |
N9—Mn—N1 | 93.7 (3) | N12—C11—H11B | 109.3 |
N8—Mn—N1 | 92.5 (3) | C10—C11—H11B | 109.3 |
N9—Mn—N5 | 93.0 (3) | H11A—C11—H11B | 108.0 |
N8—Mn—N5 | 77.3 (3) | N9—C10—C11 | 107.1 (7) |
N1—Mn—N5 | 168.5 (3) | N9—C10—H10A | 110.3 |
N9—Mn—N4 | 164.1 (3) | C11—C10—H10A | 110.3 |
N8—Mn—N4 | 96.0 (3) | N9—C10—H10B | 110.3 |
N1—Mn—N4 | 77.1 (3) | C11—C10—H10B | 110.3 |
N5—Mn—N4 | 98.3 (3) | H10A—C10—H10B | 108.6 |
N9—Mn—N12 | 77.0 (2) | C2—N1—Mn | 108.2 (6) |
N8—Mn—N12 | 167.3 (3) | C2—N1—H1A | 110.0 |
N1—Mn—N12 | 99.2 (3) | Mn—N1—H1A | 110.0 |
N5—Mn—N12 | 91.4 (3) | C2—N1—H1B | 110.0 |
N4—Mn—N12 | 91.5 (3) | Mn—N1—H1B | 110.0 |
C6—N5—Mn | 109.7 (5) | H1A—N1—H1B | 108.4 |
C6—N5—H5A | 109.7 | C6—C7—N8 | 109.7 (7) |
Mn—N5—H5A | 109.7 | C6—C7—H7A | 109.7 |
C6—N5—H5B | 109.7 | N8—C7—H7A | 109.7 |
Mn—N5—H5B | 109.7 | C6—C7—H7B | 109.7 |
H5A—N5—H5B | 108.2 | N8—C7—H7B | 109.7 |
C11—N12—Mn | 108.3 (5) | H7A—C7—H7B | 108.2 |
C11—N12—H12A | 110.0 | N5—C6—C7 | 110.2 (8) |
Mn—N12—H12A | 110.0 | N5—C6—H6A | 109.6 |
C11—N12—H12B | 110.0 | C7—C6—H6A | 109.6 |
Mn—N12—H12B | 110.0 | N5—C6—H6B | 109.6 |
H12A—N12—H12B | 108.4 | C7—C6—H6B | 109.6 |
C3—N4—Mn | 108.2 (5) | H6A—C6—H6B | 108.1 |
C3—N4—H4A | 110.1 | N4—C3—C2 | 110.4 (7) |
Mn—N4—H4A | 110.1 | N4—C3—H3A | 109.6 |
C3—N4—H4B | 110.1 | C2—C3—H3A | 109.6 |
Mn—N4—H4B | 110.1 | N4—C3—H3B | 109.6 |
H4A—N4—H4B | 108.4 | C2—C3—H3B | 109.6 |
C10—N9—Mn | 109.1 (5) | H3A—C3—H3B | 108.1 |
C10—N9—H9A | 109.9 | N1—C2—C3 | 109.3 (9) |
Mn—N9—H9A | 109.9 | N1—C2—H2A | 109.8 |
C10—N9—H9B | 109.9 | C3—C2—H2A | 109.8 |
Mn—N9—H9B | 109.9 | N1—C2—H2B | 109.8 |
H9A—N9—H9B | 108.3 | C3—C2—H2B | 109.8 |
C7—N8—Mn | 107.4 (5) | H2A—C2—H2B | 108.3 |
| | | |
Te1—Sn—Te2—Sni | −118.52 (3) | N4—Mn—N9—C10 | 24.7 (13) |
Te3—Sn—Te2—Sni | 115.34 (3) | N12—Mn—N9—C10 | −19.8 (6) |
Te2i—Sn—Te2—Sni | 0.0 | N9—Mn—N8—C7 | 74.7 (6) |
N9—Mn—N5—C6 | −109.3 (6) | N1—Mn—N8—C7 | 168.8 (6) |
N8—Mn—N5—C6 | −12.3 (6) | N5—Mn—N8—C7 | −16.8 (6) |
N1—Mn—N5—C6 | 16.5 (17) | N4—Mn—N8—C7 | −113.9 (6) |
N4—Mn—N5—C6 | 82.0 (6) | N12—Mn—N8—C7 | 11.5 (14) |
N12—Mn—N5—C6 | 173.7 (6) | Mn—N12—C11—C10 | 40.0 (9) |
N9—Mn—N12—C11 | −10.6 (6) | Mn—N9—C10—C11 | 46.2 (8) |
N8—Mn—N12—C11 | 54.7 (13) | N12—C11—C10—N9 | −59.1 (10) |
N1—Mn—N12—C11 | −102.3 (6) | N9—Mn—N1—C2 | 176.3 (7) |
N5—Mn—N12—C11 | 82.2 (6) | N8—Mn—N1—C2 | 78.6 (7) |
N4—Mn—N12—C11 | −179.5 (6) | N5—Mn—N1—C2 | 50.5 (17) |
N9—Mn—N4—C3 | 43.0 (13) | N4—Mn—N1—C2 | −16.9 (7) |
N8—Mn—N4—C3 | −104.3 (6) | N12—Mn—N1—C2 | −106.3 (7) |
N1—Mn—N4—C3 | −13.1 (6) | Mn—N8—C7—C6 | 44.1 (9) |
N5—Mn—N4—C3 | 177.6 (6) | Mn—N5—C6—C7 | 40.6 (9) |
N12—Mn—N4—C3 | 86.0 (6) | N8—C7—C6—N5 | −58.1 (11) |
N8—Mn—N9—C10 | 171.9 (6) | Mn—N4—C3—C2 | 41.6 (9) |
N1—Mn—N9—C10 | 78.8 (6) | Mn—N1—C2—C3 | 44.5 (9) |
N5—Mn—N9—C10 | −110.5 (6) | N4—C3—C2—N1 | −59.5 (11) |
Symmetry code: (i) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Te1ii | 0.90 | 3.34 | 4.039 (8) | 137 |
N1—H1B···Te3iii | 0.90 | 3.31 | 4.115 (8) | 151 |
N4—H4A···Te3 | 0.90 | 3.04 | 3.931 (7) | 173 |
N4—H4B···Te1iv | 0.90 | 3.05 | 3.851 (8) | 149 |
N5—H5A···Te1v | 0.90 | 2.99 | 3.880 (7) | 173 |
N5—H5B···Te1iv | 0.90 | 2.95 | 3.798 (7) | 157 |
N8—H8A···Te3 | 0.90 | 3.19 | 3.994 (8) | 150 |
N8—H8B···Te3iii | 0.90 | 3.05 | 3.895 (7) | 158 |
N9—H9A···Te1v | 0.90 | 3.19 | 4.052 (8) | 161 |
N9—H9B···Te3iii | 0.90 | 3.01 | 3.849 (7) | 157 |
N12—H12A···Te3ii | 0.90 | 2.88 | 3.764 (7) | 166 |
N12—H12B···Te1iv | 0.90 | 2.99 | 3.816 (7) | 154 |
N9—H9A···Te2v | 0.90 | 3.60 | 3.959 (7) | 107 |
N9—H9B···Te2v | 0.90 | 3.61 | 3.959 (7) | 107 |
Symmetry codes: (ii) x+1, y, z; (iii) x+1/2, −y+1/2, z+1/2; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+3/2, y+1/2, −z+1/2. |