The title compound, (C
3H
5N
2)
6[MnCl
4][MnCl
6], is composed of discrete imidazolium cations, and [MnCl
4]
2− and [MnCl
6]
4− anions. Both Mn atoms lie in positions of site symmetry
. A three-dimensional network is formed
via N—H
Cl hydrogen bonds.
Supporting information
CCDC reference: 601120
Key indicators
- Single-crystal X-ray study
- T = 223 K
- Mean (C-C) = 0.005 Å
- Disorder in main residue
- R factor = 0.036
- wR factor = 0.095
- Data-to-parameter ratio = 23.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C5
PLAT301_ALERT_3_C Main Residue Disorder ......................... 7.00 Perc.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SAINT; data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg & Berndt, 1999); software used to prepare material for publication: SHELXTL.
Hexaimidazolium tetrachloromanganese(II) hexachloromanganese(II)
top
Crystal data top
(C3H5N2)6[MnCl6][MnCl4] | Dx = 1.626 Mg m−3 |
Mr = 878.92 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41/a | Cell parameters from 24947 reflections |
Hall symbol: -I 4ad | θ = 1.9–28.4° |
a = 12.1117 (19) Å | µ = 1.48 mm−1 |
c = 24.475 (6) Å | T = 223 K |
V = 3590.3 (11) Å3 | Prism, light yellow |
Z = 4 | 0.24 × 0.20 × 0.18 mm |
F(000) = 1768 | |
Data collection top
Bruker APEX CCD area-detector diffractometer | 2253 independent reflections |
Radiation source: fine-focus sealed tube | 1690 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.069 |
ω scans | θmax = 28.4°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −16→16 |
Tmin = 0.71, Tmax = 0.77 | k = −16→16 |
24947 measured reflections | l = −32→32 |
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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0321P)2 + 6.1483P] where P = (Fo2 + 2Fc2)/3 |
2253 reflections | (Δ/σ)max = 0.001 |
96 parameters | Δρmax = 0.38 e Å−3 |
0 restraints | Δρmin = −0.42 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 | Occ. (<1) |
Mn1 | 0.5000 | 0.7500 | 0.1250 | 0.0299 (2) | |
Mn2 | 1.0000 | 0.7500 | 0.8750 | 0.02379 (18) | |
Cl1 | 0.41108 (8) | 0.62224 (7) | 0.06715 (3) | 0.0526 (2) | |
Cl2 | 0.79034 (5) | 0.76010 (5) | 0.87895 (2) | 0.02651 (15) | |
Cl3 | 1.0000 | 0.7500 | 0.98121 (3) | 0.0300 (2) | |
C1 | 0.9463 (4) | 0.7508 (4) | 0.18962 (14) | 0.102 (2) | 0.5 |
N1 | 0.9463 (4) | 0.7508 (4) | 0.18962 (14) | 0.102 (2) | 0.5 |
H1 | 0.9047 | 0.7521 | 0.2186 | 0.123* | |
N2 | 1.0000 | 0.7500 | 0.10813 (14) | 0.0504 (11) | |
H2 | 1.0000 | 0.7500 | 0.0726 | 0.060* | |
N3 | 0.1958 (2) | 1.0435 (2) | 0.03413 (11) | 0.0438 (7) | |
H3 | 0.1765 | 1.1044 | 0.0503 | 0.053* | |
N4 | 0.2104 (2) | 0.9179 (2) | −0.02475 (10) | 0.0434 (7) | |
H4 | 0.2025 | 0.8806 | −0.0549 | 0.052* | |
C5 | 0.9108 (3) | 0.7500 (3) | 0.13883 (18) | 0.0596 (10) | |
H5 | 0.8370 | 0.7495 | 0.1269 | 0.072* | |
C6 | 0.1649 (3) | 1.0129 (3) | −0.01436 (13) | 0.0414 (7) | |
H6 | 0.1179 | 1.0525 | −0.0378 | 0.050* | |
C7 | 0.2628 (3) | 0.9657 (3) | 0.05542 (14) | 0.0522 (9) | |
H7 | 0.2968 | 0.9674 | 0.0899 | 0.063* | |
C8 | 0.2716 (3) | 0.8864 (3) | 0.01851 (15) | 0.0486 (8) | |
H8 | 0.3127 | 0.8209 | 0.0218 | 0.058* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0342 (3) | 0.0342 (3) | 0.0214 (4) | 0.000 | 0.000 | 0.000 |
Mn2 | 0.0249 (2) | 0.0249 (2) | 0.0216 (4) | 0.000 | 0.000 | 0.000 |
Cl1 | 0.0736 (6) | 0.0428 (4) | 0.0414 (4) | −0.0189 (4) | −0.0125 (4) | −0.0017 (3) |
Cl2 | 0.0251 (3) | 0.0289 (3) | 0.0255 (3) | 0.0009 (2) | −0.0022 (2) | 0.0011 (2) |
Cl3 | 0.0321 (5) | 0.0394 (5) | 0.0186 (4) | −0.0011 (4) | 0.000 | 0.000 |
C1 | 0.202 (6) | 0.0510 (19) | 0.054 (2) | 0.026 (4) | 0.057 (3) | 0.015 (2) |
N1 | 0.202 (6) | 0.0510 (19) | 0.054 (2) | 0.026 (4) | 0.057 (3) | 0.015 (2) |
N2 | 0.101 (4) | 0.032 (2) | 0.0186 (15) | 0.009 (2) | 0.000 | 0.000 |
N3 | 0.0568 (17) | 0.0354 (14) | 0.0392 (14) | 0.0004 (12) | 0.0155 (13) | −0.0109 (11) |
N4 | 0.0538 (17) | 0.0415 (15) | 0.0348 (14) | −0.0161 (13) | 0.0069 (12) | −0.0140 (11) |
C5 | 0.061 (2) | 0.0394 (19) | 0.078 (3) | −0.0031 (17) | 0.005 (2) | −0.0028 (18) |
C6 | 0.0359 (16) | 0.0469 (18) | 0.0415 (17) | −0.0022 (14) | −0.0041 (13) | 0.0076 (14) |
C7 | 0.054 (2) | 0.068 (2) | 0.0345 (17) | −0.0090 (17) | −0.0137 (15) | 0.0025 (16) |
C8 | 0.0423 (18) | 0.0387 (18) | 0.065 (2) | 0.0091 (14) | 0.0069 (16) | 0.0043 (16) |
Geometric parameters (Å, º) top
Mn1—Cl1 | 2.3578 (8) | N2—C5 | 1.316 (4) |
Mn1—Cl1i | 2.3578 (8) | N2—C5vi | 1.316 (4) |
Mn1—Cl1ii | 2.3578 (8) | N2—H2 | 0.8700 |
Mn1—Cl1iii | 2.3578 (8) | N3—C6 | 1.298 (4) |
Mn2—Cl2iv | 2.5441 (7) | N3—C7 | 1.348 (4) |
Mn2—Cl2v | 2.5441 (7) | N3—H3 | 0.8700 |
Mn2—Cl2vi | 2.5441 (7) | N4—C6 | 1.301 (4) |
Mn2—Cl2 | 2.5441 (7) | N4—C8 | 1.348 (4) |
Mn2—Cl3v | 2.5994 (10) | N4—H4 | 0.8700 |
Mn2—Cl3 | 2.5994 (10) | C5—H5 | 0.9400 |
C1—C1vi | 1.300 (10) | C6—H6 | 0.9400 |
N1—N1vi | 1.300 (10) | C7—C8 | 1.322 (5) |
N1—C5 | 1.315 (6) | C7—H7 | 0.9400 |
N1—H1 | 0.8700 | C8—H8 | 0.9400 |
| | | |
Cl1—Mn1—Cl1i | 106.18 (4) | N1vi—N1—H1 | 125.5 |
Cl1—Mn1—Cl1ii | 111.14 (2) | C5—N1—H1 | 125.5 |
Cl1i—Mn1—Cl1ii | 111.14 (2) | C5—N2—C5vi | 110.3 (5) |
Cl1—Mn1—Cl1iii | 111.14 (2) | C5—N2—H2 | 124.8 |
Cl1i—Mn1—Cl1iii | 111.14 (2) | C5vi—N2—H2 | 124.8 |
Cl1ii—Mn1—Cl1iii | 106.18 (4) | C6—N3—C7 | 109.1 (3) |
Cl2iv—Mn2—Cl2v | 175.65 (3) | C6—N3—H3 | 125.4 |
Cl2iv—Mn2—Cl2vi | 90.083 (1) | C7—N3—H3 | 125.4 |
Cl2v—Mn2—Cl2vi | 90.083 (1) | C6—N4—C8 | 109.3 (3) |
Cl2iv—Mn2—Cl2 | 90.083 (1) | C6—N4—H4 | 125.4 |
Cl2v—Mn2—Cl2 | 90.083 (1) | C8—N4—H4 | 125.4 |
Cl2vi—Mn2—Cl2 | 175.65 (3) | N1—C5—N2 | 105.8 (4) |
Cl2iv—Mn2—Cl3v | 87.825 (13) | N1—C5—H5 | 127.1 |
Cl2v—Mn2—Cl3v | 87.825 (13) | N2—C5—H5 | 127.1 |
Cl2vi—Mn2—Cl3v | 92.175 (13) | N3—C6—N4 | 108.0 (3) |
Cl2—Mn2—Cl3v | 92.175 (13) | N3—C6—H6 | 126.0 |
Cl2iv—Mn2—Cl3 | 92.175 (13) | N4—C6—H6 | 126.0 |
Cl2v—Mn2—Cl3 | 92.175 (13) | C8—C7—N3 | 107.0 (3) |
Cl2vi—Mn2—Cl3 | 87.825 (13) | C8—C7—H7 | 126.5 |
Cl2—Mn2—Cl3 | 87.825 (13) | N3—C7—H7 | 126.5 |
Cl3v—Mn2—Cl3 | 180.0 | C7—C8—N4 | 106.7 (3) |
C1vi—C1—C5 | 109.1 (3) | C7—C8—H8 | 126.7 |
N1vi—N1—C5 | 109.1 (3) | N4—C8—H8 | 126.7 |
Symmetry codes: (i) −x+1, −y+3/2, z; (ii) −y+5/4, x+1/4, −z+1/4; (iii) y−1/4, −x+5/4, −z+1/4; (iv) −y+7/4, x−1/4, −z+7/4; (v) y+1/4, −x+7/4, −z+7/4; (vi) −x+2, −y+3/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···Cl1vii | 0.87 | 2.66 | 3.419 (4) | 146 |
N2—H2···Cl3viii | 0.87 | 2.24 | 3.106 (4) | 180 |
N3—H3···Cl2ix | 0.87 | 2.42 | 3.196 (3) | 149 |
N4—H4···Cl2x | 0.87 | 2.35 | 3.194 (3) | 163 |
Symmetry codes: (vii) y+1/4, −x+5/4, z+1/4; (viii) x, y, z−1; (ix) −x+1, −y+2, −z+1; (x) −x+1, −y+3/2, z−1. |