Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806021039/ci2066sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806021039/ci2066Isup2.hkl |
CCDC reference: 1179714
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- R factor = 0.065
- wR factor = 0.172
- Data-to-parameter ratio = 16.4
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mn1 - O2 .. 12.14 su
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT230_ALERT_2_C Hirshfeld Test Diff for O2 - C7 .. 6.86 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 - O1 .. 6.18 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn1 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C14 H10 Mn1 O4 Atom count from _chemical_formula_moiety:
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 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 (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[Mn(C7H5O2)2] | F(000) = 302 |
Mr = 297.16 | Dx = 1.625 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 969 reflections |
a = 12.918 (2) Å | θ = 2.7–24.3° |
b = 5.831 (1) Å | µ = 1.09 mm−1 |
c = 8.101 (3) Å | T = 293 K |
β = 95.54 (3)° | Plate, brown |
V = 607.4 (3) Å3 | 0.10 × 0.10 × 0.03 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 1446 independent reflections |
Radiation source: fine-focus sealed tube | 1133 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
ω scans | θmax = 28.3°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→17 |
Tmin = 0.899, Tmax = 0.968 | k = −7→7 |
5037 measured reflections | l = −10→10 |
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)] = 0.065 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.172 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0704P)2 + 1.5184P] where P = (Fo2 + 2Fc2)/3 |
1446 reflections | (Δ/σ)max < 0.001 |
88 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.75 e Å−3 |
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 | ||
Mn1 | 0.0000 | 1.0000 | 0.5000 | 0.0274 (3) | |
O1 | 0.0959 (3) | 1.1571 (6) | 0.6383 (4) | 0.0470 (9) | |
O2 | 0.0853 (3) | 0.7514 (8) | 0.4745 (5) | 0.0638 (12) | |
C1 | 0.1919 (4) | 1.0947 (8) | 0.6849 (6) | 0.0374 (10) | |
C2 | 0.2549 (4) | 1.2490 (9) | 0.7880 (6) | 0.0429 (12) | |
H2 | 0.2271 | 1.3883 | 0.8180 | 0.052* | |
C3 | 0.3555 (4) | 1.1958 (10) | 0.8436 (6) | 0.0488 (13) | |
H3 | 0.3943 | 1.2987 | 0.9120 | 0.059* | |
C4 | 0.4012 (4) | 0.9902 (10) | 0.7998 (7) | 0.0531 (13) | |
H4 | 0.4697 | 0.9555 | 0.8380 | 0.064* | |
C5 | 0.3420 (4) | 0.8401 (10) | 0.6984 (6) | 0.0469 (12) | |
H5 | 0.3716 | 0.7033 | 0.6673 | 0.056* | |
C6 | 0.2381 (4) | 0.8889 (8) | 0.6410 (5) | 0.0352 (10) | |
C7 | 0.1814 (4) | 0.7222 (9) | 0.5388 (6) | 0.0401 (11) | |
H7 | 0.2146 | 0.5856 | 0.5168 | 0.048* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0270 (5) | 0.0246 (5) | 0.0302 (5) | 0.0040 (4) | −0.0002 (3) | −0.0075 (4) |
O1 | 0.044 (2) | 0.041 (2) | 0.054 (2) | 0.0064 (16) | −0.0039 (16) | −0.0144 (17) |
O2 | 0.066 (3) | 0.063 (3) | 0.063 (3) | 0.006 (2) | 0.006 (2) | −0.006 (2) |
C1 | 0.042 (3) | 0.036 (2) | 0.034 (2) | −0.003 (2) | 0.006 (2) | 0.003 (2) |
C2 | 0.051 (3) | 0.038 (3) | 0.038 (3) | −0.003 (2) | 0.000 (2) | −0.001 (2) |
C3 | 0.049 (3) | 0.053 (3) | 0.043 (3) | −0.014 (3) | −0.005 (2) | 0.001 (2) |
C4 | 0.043 (3) | 0.058 (3) | 0.058 (3) | −0.001 (3) | −0.002 (2) | 0.007 (3) |
C5 | 0.043 (3) | 0.049 (3) | 0.049 (3) | 0.005 (2) | 0.001 (2) | −0.001 (2) |
C6 | 0.038 (2) | 0.035 (3) | 0.033 (2) | 0.002 (2) | 0.0044 (19) | 0.0001 (19) |
C7 | 0.041 (3) | 0.041 (3) | 0.038 (2) | 0.009 (2) | 0.001 (2) | −0.002 (2) |
Mn1—O1i | 1.833 (3) | C2—H2 | 0.93 |
Mn1—O1 | 1.833 (3) | C3—C4 | 1.397 (8) |
Mn1—O2i | 1.844 (4) | C3—H3 | 0.93 |
Mn1—O2 | 1.844 (4) | C4—C5 | 1.380 (8) |
O1—C1 | 1.313 (6) | C4—H4 | 0.93 |
O2—C7 | 1.310 (6) | C5—C6 | 1.407 (7) |
C1—C6 | 1.402 (7) | C5—H5 | 0.93 |
C1—C2 | 1.427 (7) | C6—C7 | 1.432 (7) |
C2—C3 | 1.370 (7) | C7—H7 | 0.93 |
O1i—Mn1—O1 | 180 | C2—C3—H3 | 119.3 |
O1i—Mn1—O2i | 94.90 (17) | C4—C3—H3 | 119.3 |
O1—Mn1—O2i | 85.10 (17) | C5—C4—C3 | 118.1 (5) |
O1i—Mn1—O2 | 85.10 (17) | C5—C4—H4 | 120.9 |
O1—Mn1—O2 | 94.90 (17) | C3—C4—H4 | 120.9 |
O2i—Mn1—O2 | 180 | C4—C5—C6 | 121.7 (5) |
C1—O1—Mn1 | 127.0 (3) | C4—C5—H5 | 119.2 |
C7—O2—Mn1 | 127.7 (4) | C6—C5—H5 | 119.2 |
O1—C1—C6 | 125.3 (4) | C1—C6—C5 | 120.3 (4) |
O1—C1—C2 | 117.6 (5) | C1—C6—C7 | 121.4 (4) |
C6—C1—C2 | 117.1 (4) | C5—C6—C7 | 118.3 (5) |
C3—C2—C1 | 121.2 (5) | O2—C7—C6 | 123.7 (5) |
C3—C2—H2 | 119.4 | O2—C7—H7 | 118.2 |
C1—C2—H2 | 119.4 | C6—C7—H7 | 118.2 |
C2—C3—C4 | 121.5 (5) |
Symmetry code: (i) −x, −y+2, −z+1. |