Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807059090/at2488sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807059090/at2488Isup2.hkl |
CCDC reference: 672717
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.043
- wR factor = 0.134
- Data-to-parameter ratio = 14.2
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 1 PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mn1 - O1 .. 28.02 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mn1 - O1W .. 15.52 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mn1 - O2 .. 30.30 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mn1 - O3 .. 11.46 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mn1 - N2 .. 10.66 su
Alert level C PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 - N1 .. 8.43 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N3 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C14 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 6 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 13 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 0 ALERT type 5 Informative message, check
For details of the DNA electrochemical biosensors of metal–phenanthroline complexes, see: Wang et al. (1996). For bond-length data, see: Allen et al. (1987).
To a solution of 2,9-dimethyl-1,10-phenanthroline (0.21 g, 1 mmol) and fumaric acid (0.058 g, 0.5 mmol) in ethanol (10 ml) was added a solution of Mn(Ac)2 (0.11 g, 1 mmol) in distilled water (10 ml). The mixture was stirred and then refluxed for 2 h. The hot solution was then filtered into another flask containing ethanol-water. Brown crystals appeared over a period of one week by slow evaporation at room temperature.
All H atoms were located in difference Fourier map. Water H atoms were refined with O1W—H1W1 and O1W—H2W1 distance restrains of 0.82 Å [1.5 Ueq(O)]. The remaining H atoms were placed in idealized positions and constrained to ride on their parent atoms, with C—H distances in the range 0.93–0.96 Å, and with Uiso(H) = 1.2 Ueq(C) and 1.5 Ueq(methyl C) H atoms.
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); 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, PARST (Nardelli, 1995) and PLATON (Spek, 2003).
[Mn2(C4H2O4)(NO3)2(C14H12N2)2(H2O)2] | F(000) = 820 |
Mr = 800.50 | Dx = 1.587 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5923 reflections |
a = 12.034 (2) Å | θ = 2.2–26.0° |
b = 9.1824 (16) Å | µ = 0.83 mm−1 |
c = 16.416 (2) Å | T = 293 K |
β = 113.532 (10)° | Block, colourless |
V = 1663.1 (4) Å3 | 0.42 × 0.33 × 0.20 mm |
Z = 2 |
Siemens SMART 1000 CCD area-detector diffractometer | 3266 independent reflections |
Radiation source: fine-focus sealed tube | 2951 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.013 |
Detector resolution: 8.33 pixels mm-1 | θmax = 26.1°, θmin = 1.9° |
ω scans | h = −14→13 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −10→11 |
Tmin = 0.723, Tmax = 0.852 | l = −20→18 |
8963 measured reflections |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.134 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0858P)2 + 1.1575P] where P = (Fo2 + 2Fc2)/3 |
3266 reflections | (Δ/σ)max = 0.001 |
230 parameters | Δρmax = 0.77 e Å−3 |
0 restraints | Δρmin = −0.86 e Å−3 |
[Mn2(C4H2O4)(NO3)2(C14H12N2)2(H2O)2] | V = 1663.1 (4) Å3 |
Mr = 800.50 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 12.034 (2) Å | µ = 0.83 mm−1 |
b = 9.1824 (16) Å | T = 293 K |
c = 16.416 (2) Å | 0.42 × 0.33 × 0.20 mm |
β = 113.532 (10)° |
Siemens SMART 1000 CCD area-detector diffractometer | 3266 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 2951 reflections with I > 2σ(I) |
Tmin = 0.723, Tmax = 0.852 | Rint = 0.013 |
8963 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 0 restraints |
wR(F2) = 0.134 | H-atom parameters constrained |
S = 1.06 | Δρmax = 0.77 e Å−3 |
3266 reflections | Δρmin = −0.86 e Å−3 |
230 parameters |
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 | 0.17583 (3) | 0.18538 (4) | 0.32962 (2) | 0.03045 (16) | |
O2 | 0.1578 (2) | 0.4355 (3) | 0.31837 (15) | 0.0611 (6) | |
C13 | 0.4425 (3) | 0.1767 (3) | 0.43220 (19) | 0.0417 (6) | |
C17 | 0.0603 (2) | 0.0233 (3) | 0.40796 (17) | 0.0428 (6) | |
N1 | 0.3457 (2) | 0.2379 (3) | 0.44183 (15) | 0.0428 (5) | |
O1 | 0.2395 (2) | 0.3349 (2) | 0.2384 (2) | 0.0683 (7) | |
O3 | 0.0941 (2) | 0.1538 (2) | 0.41663 (15) | 0.0567 (5) | |
N2 | 0.3019 (2) | 0.0450 (2) | 0.30670 (14) | 0.0397 (5) | |
N3 | 0.2067 (2) | 0.4487 (2) | 0.26373 (17) | 0.0484 (6) | |
O4 | 0.07726 (19) | −0.0591 (2) | 0.35325 (14) | 0.0544 (5) | |
C12 | 0.4195 (2) | 0.0740 (3) | 0.36088 (18) | 0.0414 (6) | |
C18 | 0.0025 (2) | −0.0354 (3) | 0.46628 (18) | 0.0441 (6) | |
H18A | −0.0319 | −0.1278 | 0.4539 | 0.066* | |
C2 | 0.3652 (3) | 0.3286 (3) | 0.5095 (2) | 0.0511 (7) | |
C8 | 0.5185 (3) | 0.0068 (3) | 0.3506 (2) | 0.0504 (7) | |
C7 | 0.6398 (3) | 0.0422 (4) | 0.4098 (3) | 0.0644 (9) | |
H7A | 0.7047 | −0.0016 | 0.4023 | 0.077* | |
C9 | 0.4917 (3) | −0.0945 (4) | 0.2813 (2) | 0.0600 (8) | |
H9A | 0.5539 | −0.1406 | 0.2713 | 0.072* | |
C5 | 0.5638 (3) | 0.2069 (3) | 0.4898 (2) | 0.0528 (7) | |
C10 | 0.3740 (3) | −0.1249 (3) | 0.2288 (2) | 0.0565 (8) | |
H10A | 0.3560 | −0.1941 | 0.1839 | 0.068* | |
C3 | 0.4854 (3) | 0.3626 (4) | 0.5702 (2) | 0.0635 (9) | |
H3A | 0.4976 | 0.4256 | 0.6174 | 0.076* | |
C14 | 0.1502 (3) | −0.0849 (4) | 0.1806 (2) | 0.0568 (7) | |
H14A | 0.0965 | −0.0275 | 0.1979 | 0.085* | |
H14B | 0.1336 | −0.1864 | 0.1843 | 0.085* | |
H14C | 0.1380 | −0.0613 | 0.1207 | 0.085* | |
C4 | 0.5817 (3) | 0.3042 (4) | 0.5597 (2) | 0.0633 (9) | |
H4A | 0.6599 | 0.3284 | 0.5989 | 0.076* | |
C11 | 0.2793 (3) | −0.0527 (3) | 0.24174 (18) | 0.0442 (6) | |
C1 | 0.2607 (4) | 0.3946 (4) | 0.5233 (2) | 0.0686 (9) | |
H1A | 0.1862 | 0.3616 | 0.4776 | 0.103* | |
H1B | 0.2652 | 0.4988 | 0.5210 | 0.103* | |
H1C | 0.2634 | 0.3657 | 0.5803 | 0.103* | |
C6 | 0.6609 (3) | 0.1381 (4) | 0.4763 (2) | 0.0626 (9) | |
H6A | 0.7404 | 0.1597 | 0.5140 | 0.075* | |
O1W | 0.0156 (2) | 0.1824 (2) | 0.21622 (17) | 0.0578 (6) | |
H1W1 | −0.0327 | 0.1265 | 0.2237 | 0.069* | |
H2W1 | −0.0054 | 0.2661 | 0.1999 | 0.087* | |
O5 | 0.2199 (2) | 0.5687 (3) | 0.23736 (19) | 0.0756 (7)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0309 (2) | 0.0322 (2) | 0.0326 (2) | −0.00011 (12) | 0.01727 (17) | 0.00015 (13) |
O2 | 0.0537 (12) | 0.0752 (16) | 0.0575 (13) | −0.0015 (11) | 0.0255 (10) | 0.0064 (11) |
C13 | 0.0423 (14) | 0.0407 (14) | 0.0415 (14) | −0.0010 (10) | 0.0162 (11) | 0.0109 (10) |
C17 | 0.0358 (12) | 0.0532 (15) | 0.0381 (13) | −0.0041 (11) | 0.0136 (10) | 0.0003 (11) |
N1 | 0.0481 (12) | 0.0426 (12) | 0.0398 (11) | −0.0047 (10) | 0.0198 (9) | 0.0004 (9) |
O1 | 0.0637 (15) | 0.0486 (13) | 0.102 (2) | 0.0047 (10) | 0.0423 (14) | −0.0012 (12) |
O3 | 0.0667 (14) | 0.0573 (12) | 0.0567 (12) | −0.0170 (10) | 0.0358 (11) | −0.0034 (10) |
N2 | 0.0453 (12) | 0.0376 (11) | 0.0415 (11) | −0.0011 (9) | 0.0228 (9) | 0.0032 (9) |
N3 | 0.0459 (12) | 0.0379 (12) | 0.0585 (14) | −0.0027 (9) | 0.0178 (11) | 0.0094 (10) |
O4 | 0.0573 (12) | 0.0651 (13) | 0.0474 (11) | 0.0009 (10) | 0.0278 (9) | −0.0037 (10) |
C12 | 0.0426 (13) | 0.0400 (13) | 0.0451 (13) | 0.0035 (10) | 0.0213 (11) | 0.0132 (11) |
C18 | 0.0422 (13) | 0.0474 (15) | 0.0442 (13) | −0.0074 (11) | 0.0189 (11) | −0.0016 (11) |
C2 | 0.0658 (19) | 0.0458 (16) | 0.0423 (15) | −0.0082 (13) | 0.0223 (14) | −0.0016 (11) |
C8 | 0.0516 (15) | 0.0492 (15) | 0.0602 (17) | 0.0110 (12) | 0.0327 (14) | 0.0188 (13) |
C7 | 0.0453 (16) | 0.074 (2) | 0.078 (2) | 0.0169 (15) | 0.0287 (15) | 0.0304 (19) |
C9 | 0.068 (2) | 0.0586 (18) | 0.070 (2) | 0.0212 (15) | 0.0448 (17) | 0.0157 (16) |
C5 | 0.0458 (15) | 0.0536 (17) | 0.0506 (16) | −0.0047 (13) | 0.0104 (13) | 0.0191 (13) |
C10 | 0.080 (2) | 0.0460 (16) | 0.0567 (17) | 0.0093 (15) | 0.0415 (17) | 0.0026 (14) |
C3 | 0.079 (2) | 0.0575 (18) | 0.0435 (16) | −0.0178 (17) | 0.0134 (15) | −0.0053 (14) |
C14 | 0.0668 (19) | 0.0561 (17) | 0.0536 (17) | −0.0095 (15) | 0.0304 (15) | −0.0129 (14) |
C4 | 0.0570 (19) | 0.064 (2) | 0.0495 (18) | −0.0160 (15) | 0.0014 (15) | 0.0098 (14) |
C11 | 0.0577 (16) | 0.0393 (13) | 0.0441 (14) | −0.0016 (12) | 0.0293 (12) | 0.0020 (11) |
C1 | 0.084 (2) | 0.070 (2) | 0.063 (2) | −0.0124 (18) | 0.0406 (19) | −0.0252 (17) |
C6 | 0.0400 (15) | 0.071 (2) | 0.068 (2) | 0.0019 (15) | 0.0119 (14) | 0.0243 (18) |
O1W | 0.0517 (12) | 0.0504 (13) | 0.0666 (14) | −0.0075 (9) | 0.0186 (11) | 0.0087 (9) |
Mn1—O3 | 2.053 (2) | C8—C9 | 1.404 (5) |
Mn1—O1W | 2.078 (2) | C8—C7 | 1.430 (5) |
Mn1—N2 | 2.136 (2) | C7—C6 | 1.345 (6) |
Mn1—N1 | 2.191 (2) | C7—H7A | 0.9300 |
Mn1—O2 | 2.307 (3) | C9—C10 | 1.361 (5) |
Mn1—O1 | 2.372 (3) | C9—H9A | 0.9300 |
O2—N3 | 1.260 (3) | C5—C4 | 1.401 (5) |
C13—N1 | 1.358 (4) | C5—C6 | 1.422 (5) |
C13—C5 | 1.415 (4) | C10—C11 | 1.406 (4) |
C13—C12 | 1.441 (4) | C10—H10A | 0.9300 |
C17—O3 | 1.255 (4) | C3—C4 | 1.349 (6) |
C17—O4 | 1.251 (3) | C3—H3A | 0.9300 |
C17—C18 | 1.491 (4) | C14—C11 | 1.505 (4) |
N1—C2 | 1.333 (4) | C14—H14A | 0.9600 |
O1—N3 | 1.246 (3) | C14—H14B | 0.9600 |
N2—C11 | 1.336 (4) | C14—H14C | 0.9600 |
N2—C12 | 1.364 (3) | C4—H4A | 0.9300 |
N3—O5 | 1.217 (4) | C1—H1A | 0.9600 |
C12—C8 | 1.411 (4) | C1—H1B | 0.9600 |
C18—C18i | 1.306 (5) | C1—H1C | 0.9600 |
C18—H18A | 0.9300 | C6—H6A | 0.9300 |
C2—C3 | 1.425 (5) | O1W—H1W1 | 0.8200 |
C2—C1 | 1.493 (5) | O1W—H2W1 | 0.8199 |
O3—Mn1—O1W | 95.18 (10) | C9—C8—C12 | 117.1 (3) |
O3—Mn1—N2 | 127.51 (9) | C9—C8—C7 | 122.9 (3) |
O1W—Mn1—N2 | 107.74 (9) | C12—C8—C7 | 120.0 (3) |
O3—Mn1—N1 | 89.52 (9) | C6—C7—C8 | 120.8 (3) |
O1W—Mn1—N1 | 167.68 (8) | C6—C7—H7A | 119.6 |
N2—Mn1—N1 | 77.92 (9) | C8—C7—H7A | 119.6 |
O3—Mn1—O2 | 98.08 (8) | C10—C9—C8 | 119.6 (3) |
O1W—Mn1—O2 | 85.28 (8) | C10—C9—H9A | 120.2 |
N2—Mn1—O2 | 129.58 (8) | C8—C9—H9A | 120.2 |
N1—Mn1—O2 | 82.78 (9) | C13—C5—C4 | 116.9 (3) |
O3—Mn1—O1 | 152.37 (9) | C13—C5—C6 | 120.1 (3) |
O1W—Mn1—O1 | 81.98 (9) | C4—C5—C6 | 123.0 (3) |
N2—Mn1—O1 | 78.87 (8) | C9—C10—C11 | 120.6 (3) |
N1—Mn1—O1 | 88.57 (9) | C9—C10—H10A | 119.7 |
O2—Mn1—O1 | 54.35 (8) | C11—C10—H10A | 119.7 |
N3—O2—Mn1 | 95.62 (18) | C4—C3—C2 | 120.5 (3) |
N1—C13—C5 | 123.0 (3) | C4—C3—H3A | 119.8 |
N1—C13—C12 | 118.1 (2) | C2—C3—H3A | 119.8 |
C5—C13—C12 | 118.9 (3) | C11—C14—H14A | 109.5 |
O3—C17—O4 | 121.4 (3) | C11—C14—H14B | 109.5 |
O3—C17—C18 | 119.0 (3) | H14A—C14—H14B | 109.5 |
O4—C17—C18 | 119.6 (3) | C11—C14—H14C | 109.5 |
C13—N1—C2 | 118.8 (3) | H14A—C14—H14C | 109.5 |
C13—N1—Mn1 | 111.50 (18) | H14B—C14—H14C | 109.5 |
C2—N1—Mn1 | 129.3 (2) | C3—C4—C5 | 119.9 (3) |
N3—O1—Mn1 | 92.88 (18) | C3—C4—H4A | 120.0 |
C17—O3—Mn1 | 106.22 (18) | C5—C4—H4A | 120.0 |
C11—N2—C12 | 118.6 (2) | N2—C11—C10 | 121.2 (3) |
C11—N2—Mn1 | 127.84 (19) | N2—C11—C14 | 119.4 (2) |
C12—N2—Mn1 | 113.10 (17) | C10—C11—C14 | 119.4 (3) |
O5—N3—O1 | 122.5 (3) | C2—C1—H1A | 109.5 |
O5—N3—O2 | 120.3 (3) | C2—C1—H1B | 109.5 |
O1—N3—O2 | 117.1 (2) | H1A—C1—H1B | 109.5 |
N2—C12—C13 | 118.0 (2) | C2—C1—H1C | 109.5 |
N2—C12—C8 | 122.9 (3) | H1A—C1—H1C | 109.5 |
C13—C12—C8 | 119.1 (3) | H1B—C1—H1C | 109.5 |
C18i—C18—C17 | 123.8 (3) | C7—C6—C5 | 121.1 (3) |
C18i—C18—H18A | 118.1 | C7—C6—H6A | 119.4 |
C17—C18—H18A | 118.1 | C5—C6—H6A | 119.4 |
N1—C2—C3 | 120.8 (3) | Mn1—O1W—H1W1 | 109.5 |
N1—C2—C1 | 120.1 (3) | Mn1—O1W—H2W1 | 109.6 |
C3—C2—C1 | 119.1 (3) | H1W1—O1W—H2W1 | 119.4 |
O3—Mn1—O2—N3 | −178.89 (17) | Mn1—O2—N3—O5 | −179.0 (2) |
O1W—Mn1—O2—N3 | −84.32 (17) | Mn1—O2—N3—O1 | 1.4 (3) |
N2—Mn1—O2—N3 | 24.9 (2) | C11—N2—C12—C13 | −178.3 (2) |
N1—Mn1—O2—N3 | 92.62 (17) | Mn1—N2—C12—C13 | 8.5 (3) |
O1—Mn1—O2—N3 | −0.82 (16) | C11—N2—C12—C8 | 0.9 (4) |
C5—C13—N1—C2 | −1.4 (4) | Mn1—N2—C12—C8 | −172.3 (2) |
C12—C13—N1—C2 | 177.4 (2) | N1—C13—C12—N2 | 0.4 (3) |
C5—C13—N1—Mn1 | 172.5 (2) | C5—C13—C12—N2 | 179.2 (2) |
C12—C13—N1—Mn1 | −8.8 (3) | N1—C13—C12—C8 | −178.8 (2) |
O3—Mn1—N1—C13 | 138.51 (18) | C5—C13—C12—C8 | 0.0 (4) |
O1W—Mn1—N1—C13 | −108.9 (4) | O3—C17—C18—C18i | −8.6 (5) |
N2—Mn1—N1—C13 | 9.86 (17) | O4—C17—C18—C18i | 169.5 (4) |
O2—Mn1—N1—C13 | −123.29 (18) | C13—N1—C2—C3 | 0.9 (4) |
O1—Mn1—N1—C13 | −69.06 (18) | Mn1—N1—C2—C3 | −171.7 (2) |
O3—Mn1—N1—C2 | −48.5 (2) | C13—N1—C2—C1 | −178.3 (3) |
O1W—Mn1—N1—C2 | 64.2 (5) | Mn1—N1—C2—C1 | 9.1 (4) |
N2—Mn1—N1—C2 | −177.1 (3) | N2—C12—C8—C9 | −0.4 (4) |
O2—Mn1—N1—C2 | 49.7 (2) | C13—C12—C8—C9 | 178.8 (2) |
O1—Mn1—N1—C2 | 104.0 (2) | N2—C12—C8—C7 | −180.0 (2) |
O3—Mn1—O1—N3 | 4.9 (3) | C13—C12—C8—C7 | −0.8 (4) |
O1W—Mn1—O1—N3 | 90.76 (19) | C9—C8—C7—C6 | −178.8 (3) |
N2—Mn1—O1—N3 | −159.3 (2) | C12—C8—C7—C6 | 0.7 (5) |
N1—Mn1—O1—N3 | −81.31 (19) | C12—C8—C9—C10 | −0.9 (4) |
O2—Mn1—O1—N3 | 0.82 (16) | C7—C8—C9—C10 | 178.6 (3) |
O4—C17—O3—Mn1 | −1.0 (3) | N1—C13—C5—C4 | 0.5 (4) |
C18—C17—O3—Mn1 | 176.98 (19) | C12—C13—C5—C4 | −178.2 (2) |
O1W—Mn1—O3—C17 | 72.8 (2) | N1—C13—C5—C6 | 179.6 (3) |
N2—Mn1—O3—C17 | −44.2 (2) | C12—C13—C5—C6 | 0.8 (4) |
N1—Mn1—O3—C17 | −118.6 (2) | C8—C9—C10—C11 | 1.8 (5) |
O2—Mn1—O3—C17 | 158.80 (19) | N1—C2—C3—C4 | 0.5 (5) |
O1—Mn1—O3—C17 | 155.4 (2) | C1—C2—C3—C4 | 179.7 (3) |
O3—Mn1—N2—C11 | 97.9 (2) | C2—C3—C4—C5 | −1.3 (5) |
O1W—Mn1—N2—C11 | −13.5 (2) | C13—C5—C4—C3 | 0.8 (5) |
N1—Mn1—N2—C11 | 177.8 (2) | C6—C5—C4—C3 | −178.2 (3) |
O2—Mn1—N2—C11 | −112.3 (2) | C12—N2—C11—C10 | 0.0 (4) |
O1—Mn1—N2—C11 | −91.3 (2) | Mn1—N2—C11—C10 | 172.1 (2) |
O3—Mn1—N2—C12 | −89.66 (18) | C12—N2—C11—C14 | −179.3 (2) |
O1W—Mn1—N2—C12 | 158.93 (16) | Mn1—N2—C11—C14 | −7.2 (4) |
N1—Mn1—N2—C12 | −9.73 (16) | C9—C10—C11—N2 | −1.4 (4) |
O2—Mn1—N2—C12 | 60.2 (2) | C9—C10—C11—C14 | 177.9 (3) |
O1—Mn1—N2—C12 | 81.19 (17) | C8—C7—C6—C5 | 0.1 (5) |
Mn1—O1—N3—O5 | 179.0 (3) | C13—C5—C6—C7 | −0.9 (5) |
Mn1—O1—N3—O2 | −1.4 (3) | C4—C5—C6—C7 | 178.1 (3) |
Symmetry code: (i) −x, −y, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2ii | 0.82 | 2.23 | 2.978 (4) | 151 |
O1W—H2W1···O4iii | 0.82 | 1.87 | 2.677 (3) | 170 |
C6—H6A···O4iv | 0.93 | 2.57 | 3.353 (4) | 142 |
C9—H9A···O1v | 0.93 | 2.56 | 3.439 (5) | 157 |
Symmetry codes: (ii) −x, y−1/2, −z+1/2; (iii) −x, y+1/2, −z+1/2; (iv) −x+1, −y, −z+1; (v) −x+1, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Mn2(C4H2O4)(NO3)2(C14H12N2)2(H2O)2] |
Mr | 800.50 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 12.034 (2), 9.1824 (16), 16.416 (2) |
β (°) | 113.532 (10) |
V (Å3) | 1663.1 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.83 |
Crystal size (mm) | 0.42 × 0.33 × 0.20 |
Data collection | |
Diffractometer | Siemens SMART 1000 CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.723, 0.852 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8963, 3266, 2951 |
Rint | 0.013 |
(sin θ/λ)max (Å−1) | 0.618 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.134, 1.06 |
No. of reflections | 3266 |
No. of parameters | 230 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.77, −0.86 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997a), SHELXTL (Sheldrick, 1997b), SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 2003).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2i | 0.82 | 2.234 | 2.978 (4) | 151.06 |
O1W—H2W1···O4ii | 0.82 | 1.866 | 2.677 (3) | 169.67 |
C6—H6A···O4iii | 0.93 | 2.569 | 3.353 (4) | 142.30 |
C9—H9A···O1iv | 0.93 | 2.564 | 3.439 (5) | 156.91 |
Symmetry codes: (i) −x, y−1/2, −z+1/2; (ii) −x, y+1/2, −z+1/2; (iii) −x+1, −y, −z+1; (iv) −x+1, y−1/2, −z+1/2. |
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Metal-phenanthroline complexes are good indicators for hydridization detection in DNA electrochemical biosensors (Wang et al., 1996). In our search for new indicators, the title complex was synthesized and its structure is presented here.
The binuclear manganese complex in (I) possesses a crystallographically imposed centre of symmetry (Fig. 1). Each MnII atom is six-coordinated by two N atoms from one 9,10-dimethyl-phennathroline ligand, one O atoms from water, one O atom from fumaric acid, and two O atom from nitrate anion in a distorted octahedral environment. The axial position is occupied by water molecule O atom and one N atom from 9,10-dimethyl-phennathroline ligand, with an O1W—Mn1—N1 bond angle of 167.68 (1)°.
In the crystal structure, the short interplanar distances between the phenanthroline moieties suggest strong π···π interactions. The distances between benzene rings are Cg1···Cg2iii = 3.826, Cg1···Cg3iii = 3.708 and Cg3···Cg3iii = 3.719 Å, where Cg1, Cg2 and Cg3 denote the centroids of N1/C2—C5/C13, N2/C8—C12 and C5—C8/C12/C13 rings, respectively, which contribure to the crystal packing [symmetry code: (i) -x + 1, -y, -z + 1]. The water molecules act as donors to form O—H···O hydrogen bonds (Table 2). Moreover, the molecules are linked into chains along the a axis by C6—H6A···O4 and C9—H9A···O1 intermolecular hydrogen bonds.