Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807038603/hg2266sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807038603/hg2266Isup2.hkl |
CCDC reference: 660075
To a solution of N,N,N',N'-tetrakis(2-pyridylmethyl)-1,6-diaminohexane (0.50 g, 1.04 mmol) in EtOH (15 ml) was added Mn(ClO4)2.6H2O (0.38 g, 1.05 mmol) and stirred for 1 h at room temparature. The formed precipitate was separated by filtration and washed with EtOH and dried, to give a dark yellow powder (0.48 g). Crystals suitable for X-ray analysis were obtained by slow evaporation from a acetone/H2O(1:1) solution.
H atoms were positioned geometrically and allowed to ride on their respective carrier atoms [C—H = 0.94 (aromatic), 0.98 (CH2) or 0.97 Å (CH3) and Uiso(H) = 1.2Ueq or 1.5Ueq(methyl C)]. The solvent molecules were highly disordered, and then the atoms of acetone and water were refined with isotropic thermal parameters, as a result it reflects on large value of the R factor. The H atoms of the solvent H2O molecules could neither be located from Fourier difference maps nor added geometrically.
The title compound consists of cationic complex polymer with counter anions (ClO4) and solvents (acetone and water). In the cation polymer, Mn2+ ions are bridged by the hexadentate ligand, N,N,N',N'-tetrakis(2-pyridylmethyl)-1,6-diaminohexane (tphn), and the constitutional repeating unit of the polymer, MnII(tphn), is disposed about a twofold axis passing through the Mn atom (Fig. 1). The Mn ion is six-coordinated in a distorted octahedral structure by three N atoms from one tphn ligand and three N atoms from another tphn ligand in the facial positions, respectively. The Mn—N(pyridyl) bond lengths (2.267 (4) and 2.217 (4) Å) are slightly longer than the Mn—N(amine) bond length (2.369 (4) Å). The polymer reveals a one-dimensional chain structure along the c axis (Fig. 2).
For related literature, see: Jensen et al. (1997).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.
[Mn(C30H36N6)](ClO4)2·2C3H6O·2H2O | F(000) = 1860 |
Mr = 886.68 | Dx = 1.426 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2085 reflections |
a = 18.7266 (16) Å | θ = 2.2–21.0° |
b = 14.5252 (12) Å | µ = 0.52 mm−1 |
c = 15.2375 (13) Å | T = 243 K |
β = 94.782 (2)° | Block, yellow |
V = 4130.3 (6) Å3 | 0.20 × 0.18 × 0.15 mm |
Z = 4 |
Bruker SMART 1000 CCD diffractometer | 4248 independent reflections |
Radiation source: fine-focus sealed tube | 2171 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
φ and ω scans | θmax = 26.4°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −23→22 |
Tmin = 0.707, Tmax = 0.926 | k = −18→18 |
16555 measured reflections | l = −19→12 |
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)] = 0.073 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.227 | H-atom parameters constrained |
S = 0.92 | w = 1/[σ2(Fo2) + (0.132P)2] where P = (Fo2 + 2Fc2)/3 |
4248 reflections | (Δ/σ)max < 0.001 |
230 parameters | Δρmax = 0.86 e Å−3 |
0 restraints | Δρmin = −0.49 e Å−3 |
[Mn(C30H36N6)](ClO4)2·2C3H6O·2H2O | V = 4130.3 (6) Å3 |
Mr = 886.68 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 18.7266 (16) Å | µ = 0.52 mm−1 |
b = 14.5252 (12) Å | T = 243 K |
c = 15.2375 (13) Å | 0.20 × 0.18 × 0.15 mm |
β = 94.782 (2)° |
Bruker SMART 1000 CCD diffractometer | 4248 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | 2171 reflections with I > 2σ(I) |
Tmin = 0.707, Tmax = 0.926 | Rint = 0.056 |
16555 measured reflections |
R[F2 > 2σ(F2)] = 0.073 | 0 restraints |
wR(F2) = 0.227 | H-atom parameters constrained |
S = 0.92 | Δρmax = 0.86 e Å−3 |
4248 reflections | Δρmin = −0.49 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 | ||
Mn | 0.0000 | 0.26386 (6) | 0.2500 | 0.0436 (3) | |
N1 | 0.0765 (2) | 0.2265 (2) | 0.1478 (2) | 0.0488 (10) | |
N2 | 0.0500 (2) | 0.3736 (2) | 0.3356 (3) | 0.0509 (10) | |
N3 | 0.1019 (2) | 0.1940 (3) | 0.3248 (2) | 0.0523 (10) | |
C1 | 0.0736 (3) | 0.2587 (3) | 0.0651 (3) | 0.0508 (12) | |
H1 | 0.0380 | 0.3022 | 0.0478 | 0.061* | |
C2 | 0.1189 (3) | 0.2322 (4) | 0.0046 (3) | 0.0588 (13) | |
H2 | 0.1138 | 0.2562 | −0.0529 | 0.071* | |
C3 | 0.1713 (3) | 0.1710 (4) | 0.0281 (3) | 0.0688 (15) | |
H3 | 0.2030 | 0.1514 | −0.0128 | 0.083* | |
C4 | 0.1773 (3) | 0.1378 (4) | 0.1134 (4) | 0.0661 (15) | |
H4 | 0.2139 | 0.0961 | 0.1318 | 0.079* | |
C5 | 0.1285 (3) | 0.1670 (3) | 0.1715 (3) | 0.0547 (13) | |
C6 | 0.1313 (3) | 0.1281 (3) | 0.2638 (3) | 0.0637 (15) | |
H6A | 0.1037 | 0.0707 | 0.2633 | 0.076* | |
H6B | 0.1811 | 0.1138 | 0.2843 | 0.076* | |
C7 | 0.0191 (3) | 0.4531 (3) | 0.3588 (3) | 0.0620 (14) | |
H7 | −0.0277 | 0.4657 | 0.3345 | 0.074* | |
C8 | 0.0512 (4) | 0.5154 (4) | 0.4146 (4) | 0.0718 (16) | |
H8 | 0.0276 | 0.5700 | 0.4285 | 0.086* | |
C9 | 0.1186 (4) | 0.4969 (4) | 0.4502 (4) | 0.087 (2) | |
H9 | 0.1423 | 0.5393 | 0.4891 | 0.104* | |
C10 | 0.1522 (3) | 0.4176 (5) | 0.4301 (4) | 0.0754 (17) | |
H10 | 0.1986 | 0.4045 | 0.4556 | 0.090* | |
C11 | 0.1176 (3) | 0.3571 (3) | 0.3721 (3) | 0.0551 (13) | |
C12 | 0.1520 (3) | 0.2711 (4) | 0.3387 (4) | 0.0605 (13) | |
H12A | 0.1722 | 0.2853 | 0.2829 | 0.073* | |
H12B | 0.1915 | 0.2525 | 0.3811 | 0.073* | |
C13 | 0.0935 (3) | 0.1483 (4) | 0.4109 (3) | 0.0632 (14) | |
H13A | 0.1411 | 0.1307 | 0.4369 | 0.076* | |
H13B | 0.0741 | 0.1936 | 0.4503 | 0.076* | |
C14 | 0.0467 (3) | 0.0653 (3) | 0.4084 (3) | 0.0650 (15) | |
H14A | 0.0723 | 0.0132 | 0.3846 | 0.078* | |
H14B | 0.0036 | 0.0768 | 0.3690 | 0.078* | |
C15 | 0.0251 (3) | 0.0406 (3) | 0.4997 (4) | 0.0738 (17) | |
H15A | 0.0685 | 0.0267 | 0.5380 | 0.089* | |
H15B | 0.0020 | 0.0941 | 0.5244 | 0.089* | |
Cl | 0.23323 (9) | 0.43776 (12) | 0.17809 (10) | 0.0844 (6) | |
O1 | 0.2592 (2) | 0.4928 (3) | 0.1128 (3) | 0.1020 (15) | |
O2 | 0.2566 (4) | 0.4597 (4) | 0.2616 (3) | 0.150 (3) | |
O3 | 0.1583 (3) | 0.4373 (6) | 0.1717 (5) | 0.193 (4) | |
O4 | 0.2472 (4) | 0.3424 (4) | 0.1612 (4) | 0.154 (2) | |
O1S | 0.4558 (3) | 0.2153 (4) | 0.3938 (5) | 0.139 (2)* | |
C1S | 0.4137 (6) | 0.2292 (8) | 0.3337 (8) | 0.150 (4)* | |
C2S | 0.3836 (7) | 0.1745 (10) | 0.2604 (9) | 0.231 (6)* | |
H2S1 | 0.3393 | 0.2025 | 0.2358 | 0.346* | |
H2S2 | 0.3738 | 0.1128 | 0.2807 | 0.346* | |
H2S3 | 0.4174 | 0.1714 | 0.2156 | 0.346* | |
C3S | 0.3406 (7) | 0.2371 (9) | 0.3732 (9) | 0.302 (10)* | |
H3S1 | 0.3151 | 0.2906 | 0.3488 | 0.453* | |
H3S2 | 0.3482 | 0.2436 | 0.4367 | 0.453* | |
H3S3 | 0.3125 | 0.1822 | 0.3591 | 0.453* | |
O1W | 0.4390 (7) | 0.3332 (9) | 0.2678 (9) | 0.416 (9)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn | 0.0622 (7) | 0.0285 (5) | 0.0426 (6) | 0.000 | 0.0197 (5) | 0.000 |
N1 | 0.066 (3) | 0.034 (2) | 0.048 (2) | 0.0046 (19) | 0.0172 (19) | 0.0045 (17) |
N2 | 0.072 (3) | 0.034 (2) | 0.050 (2) | −0.0020 (18) | 0.023 (2) | −0.0016 (17) |
N3 | 0.077 (3) | 0.040 (2) | 0.043 (2) | 0.013 (2) | 0.021 (2) | 0.0066 (17) |
C1 | 0.069 (3) | 0.041 (3) | 0.044 (3) | −0.002 (2) | 0.015 (2) | 0.003 (2) |
C2 | 0.077 (4) | 0.061 (3) | 0.040 (3) | −0.007 (3) | 0.016 (3) | −0.002 (2) |
C3 | 0.083 (4) | 0.076 (4) | 0.052 (3) | 0.003 (3) | 0.029 (3) | −0.010 (3) |
C4 | 0.078 (4) | 0.060 (3) | 0.063 (4) | 0.018 (3) | 0.027 (3) | −0.006 (3) |
C5 | 0.074 (3) | 0.041 (3) | 0.052 (3) | 0.005 (2) | 0.023 (3) | −0.003 (2) |
C6 | 0.091 (4) | 0.050 (3) | 0.054 (3) | 0.024 (3) | 0.026 (3) | 0.003 (2) |
C7 | 0.090 (4) | 0.040 (3) | 0.060 (3) | 0.001 (3) | 0.025 (3) | −0.004 (2) |
C8 | 0.120 (5) | 0.044 (3) | 0.055 (3) | −0.010 (3) | 0.025 (4) | −0.010 (3) |
C9 | 0.142 (7) | 0.060 (4) | 0.061 (4) | −0.029 (4) | 0.018 (4) | −0.017 (3) |
C10 | 0.084 (4) | 0.084 (4) | 0.058 (4) | −0.024 (3) | 0.004 (3) | −0.007 (3) |
C11 | 0.073 (4) | 0.054 (3) | 0.042 (3) | −0.008 (3) | 0.020 (3) | 0.004 (2) |
C12 | 0.065 (3) | 0.066 (3) | 0.052 (3) | 0.004 (3) | 0.014 (3) | 0.007 (3) |
C13 | 0.090 (4) | 0.058 (3) | 0.044 (3) | 0.023 (3) | 0.020 (3) | 0.011 (2) |
C14 | 0.109 (4) | 0.039 (3) | 0.051 (3) | 0.019 (3) | 0.030 (3) | 0.010 (2) |
C15 | 0.128 (5) | 0.043 (3) | 0.054 (3) | 0.024 (3) | 0.031 (3) | 0.018 (3) |
Cl | 0.0958 (12) | 0.0966 (13) | 0.0642 (10) | −0.0439 (9) | 0.0265 (8) | −0.0183 (8) |
O1 | 0.112 (3) | 0.128 (4) | 0.069 (3) | −0.052 (3) | 0.022 (2) | −0.005 (3) |
O2 | 0.236 (7) | 0.152 (5) | 0.067 (3) | −0.110 (5) | 0.034 (4) | −0.023 (3) |
O3 | 0.101 (4) | 0.273 (10) | 0.208 (8) | −0.031 (5) | 0.041 (4) | 0.073 (7) |
O4 | 0.240 (7) | 0.108 (5) | 0.124 (5) | −0.010 (5) | 0.079 (5) | −0.030 (4) |
Mn—N2 | 2.217 (4) | C9—H9 | 0.9400 |
Mn—N2i | 2.217 (4) | C10—C11 | 1.370 (7) |
Mn—N1i | 2.267 (4) | C10—H10 | 0.9400 |
Mn—N1 | 2.267 (4) | C11—C12 | 1.514 (7) |
Mn—N3 | 2.369 (4) | C12—H12A | 0.9800 |
Mn—N3i | 2.369 (4) | C12—H12B | 0.9800 |
N1—C5 | 1.331 (6) | C13—C14 | 1.489 (7) |
N1—C1 | 1.341 (6) | C13—H13A | 0.9800 |
N2—C7 | 1.352 (6) | C13—H13B | 0.9800 |
N2—C11 | 1.360 (6) | C14—C15 | 1.524 (7) |
N3—C12 | 1.465 (6) | C14—H14A | 0.9800 |
N3—C6 | 1.472 (6) | C14—H14B | 0.9800 |
N3—C13 | 1.490 (6) | C15—C15ii | 1.509 (11) |
C1—C2 | 1.360 (7) | C15—H15A | 0.9800 |
C1—H1 | 0.9400 | C15—H15B | 0.9800 |
C2—C3 | 1.350 (7) | Cl—O2 | 1.349 (5) |
C2—H2 | 0.9400 | Cl—O1 | 1.395 (4) |
C3—C4 | 1.382 (7) | Cl—O3 | 1.399 (6) |
C3—H3 | 0.9400 | Cl—O4 | 1.437 (6) |
C4—C5 | 1.390 (6) | O1S—C1S | 1.175 (11) |
C4—H4 | 0.9400 | C1S—C2S | 1.446 (15) |
C5—C6 | 1.513 (7) | C1S—C3S | 1.546 (15) |
C6—H6A | 0.9800 | C2S—H2S1 | 0.9700 |
C6—H6B | 0.9800 | C2S—H2S2 | 0.9700 |
C7—C8 | 1.349 (7) | C2S—H2S3 | 0.9700 |
C7—H7 | 0.9400 | C3S—H3S1 | 0.9700 |
C8—C9 | 1.359 (8) | C3S—H3S2 | 0.9700 |
C8—H8 | 0.9400 | C3S—H3S3 | 0.9700 |
C9—C10 | 1.359 (9) | ||
N2—Mn—N2i | 88.1 (2) | C8—C9—C10 | 120.7 (6) |
N2—Mn—N1i | 91.59 (13) | C8—C9—H9 | 119.7 |
N2i—Mn—N1i | 108.42 (14) | C10—C9—H9 | 119.7 |
N2—Mn—N1 | 108.42 (14) | C9—C10—C11 | 119.0 (6) |
N2i—Mn—N1 | 91.59 (13) | C9—C10—H10 | 120.5 |
N1i—Mn—N1 | 152.33 (19) | C11—C10—H10 | 120.5 |
N2—Mn—N3 | 74.99 (14) | N2—C11—C10 | 121.7 (5) |
N2i—Mn—N3 | 151.06 (14) | N2—C11—C12 | 114.5 (4) |
N1i—Mn—N3 | 95.57 (14) | C10—C11—C12 | 123.7 (5) |
N1—Mn—N3 | 72.42 (13) | N3—C12—C11 | 113.2 (4) |
N2—Mn—N3i | 151.06 (14) | N3—C12—H12A | 108.9 |
N2i—Mn—N3i | 74.98 (14) | C11—C12—H12A | 108.9 |
N1i—Mn—N3i | 72.42 (13) | N3—C12—H12B | 108.9 |
N1—Mn—N3i | 95.57 (14) | C11—C12—H12B | 108.9 |
N3—Mn—N3i | 129.2 (2) | H12A—C12—H12B | 107.7 |
C5—N1—C1 | 116.9 (4) | C14—C13—N3 | 116.3 (4) |
C5—N1—Mn | 117.4 (3) | C14—C13—H13A | 108.2 |
C1—N1—Mn | 125.7 (3) | N3—C13—H13A | 108.2 |
C7—N2—C11 | 116.6 (4) | C14—C13—H13B | 108.2 |
C7—N2—Mn | 126.8 (4) | N3—C13—H13B | 108.2 |
C11—N2—Mn | 116.6 (3) | H13A—C13—H13B | 107.4 |
C12—N3—C6 | 108.7 (4) | C13—C14—C15 | 111.6 (5) |
C12—N3—C13 | 109.1 (4) | C13—C14—H14A | 109.3 |
C6—N3—C13 | 109.8 (4) | C15—C14—H14A | 109.3 |
C12—N3—Mn | 102.8 (3) | C13—C14—H14B | 109.3 |
C6—N3—Mn | 107.7 (3) | C15—C14—H14B | 109.3 |
C13—N3—Mn | 118.3 (3) | H14A—C14—H14B | 108.0 |
N1—C1—C2 | 124.1 (5) | C15ii—C15—C14 | 113.7 (6) |
N1—C1—H1 | 118.0 | C15ii—C15—H15A | 108.8 |
C2—C1—H1 | 118.0 | C14—C15—H15A | 108.8 |
C3—C2—C1 | 119.2 (5) | C15ii—C15—H15B | 108.8 |
C3—C2—H2 | 120.4 | C14—C15—H15B | 108.8 |
C1—C2—H2 | 120.4 | H15A—C15—H15B | 107.7 |
C2—C3—C4 | 118.7 (5) | O2—Cl—O1 | 115.6 (3) |
C2—C3—H3 | 120.7 | O2—Cl—O3 | 108.1 (5) |
C4—C3—H3 | 120.7 | O1—Cl—O3 | 111.1 (4) |
C3—C4—C5 | 119.1 (5) | O2—Cl—O4 | 110.3 (4) |
C3—C4—H4 | 120.5 | O1—Cl—O4 | 110.2 (3) |
C5—C4—H4 | 120.5 | O3—Cl—O4 | 100.4 (5) |
N1—C5—C4 | 122.1 (5) | O1S—C1S—C2S | 134.4 (12) |
N1—C5—C6 | 117.6 (4) | O1S—C1S—C3S | 105.5 (11) |
C4—C5—C6 | 120.3 (5) | C2S—C1S—C3S | 92.3 (9) |
N3—C6—C5 | 111.0 (4) | C1S—C2S—H2S1 | 109.5 |
N3—C6—H6A | 109.4 | C1S—C2S—H2S2 | 109.5 |
C5—C6—H6A | 109.4 | H2S1—C2S—H2S2 | 109.5 |
N3—C6—H6B | 109.4 | C1S—C2S—H2S3 | 109.5 |
C5—C6—H6B | 109.4 | H2S1—C2S—H2S3 | 109.5 |
H6A—C6—H6B | 108.0 | H2S2—C2S—H2S3 | 109.5 |
C8—C7—N2 | 124.1 (6) | C1S—C3S—H3S1 | 109.5 |
C8—C7—H7 | 118.0 | C1S—C3S—H3S2 | 109.5 |
N2—C7—H7 | 118.0 | H3S1—C3S—H3S2 | 109.5 |
C7—C8—C9 | 117.9 (6) | C1S—C3S—H3S3 | 109.5 |
C7—C8—H8 | 121.0 | H3S1—C3S—H3S3 | 109.5 |
C9—C8—H8 | 121.0 | H3S2—C3S—H3S3 | 109.5 |
N2—Mn—N1—C5 | 83.1 (4) | Mn—N1—C1—C2 | −177.6 (4) |
N2i—Mn—N1—C5 | 171.6 (3) | N1—C1—C2—C3 | −1.2 (8) |
N1i—Mn—N1—C5 | −51.2 (3) | C1—C2—C3—C4 | −0.5 (8) |
N3—Mn—N1—C5 | 16.1 (3) | C2—C3—C4—C5 | 1.3 (8) |
N3i—Mn—N1—C5 | −113.4 (3) | C1—N1—C5—C4 | −1.0 (7) |
N2—Mn—N1—C1 | −97.5 (4) | Mn—N1—C5—C4 | 178.5 (4) |
N2i—Mn—N1—C1 | −9.0 (4) | C1—N1—C5—C6 | −178.4 (4) |
N1i—Mn—N1—C1 | 128.2 (4) | Mn—N1—C5—C6 | 1.1 (6) |
N3—Mn—N1—C1 | −164.4 (4) | C3—C4—C5—N1 | −0.6 (8) |
N3i—Mn—N1—C1 | 66.1 (4) | C3—C4—C5—C6 | 176.8 (5) |
N2i—Mn—N2—C7 | 40.4 (3) | C12—N3—C6—C5 | −70.6 (5) |
N1i—Mn—N2—C7 | −67.9 (4) | C13—N3—C6—C5 | 170.2 (4) |
N1—Mn—N2—C7 | 131.5 (4) | Mn—N3—C6—C5 | 40.1 (5) |
N3—Mn—N2—C7 | −163.3 (4) | N1—C5—C6—N3 | −29.4 (7) |
N3i—Mn—N2—C7 | −13.0 (5) | C4—C5—C6—N3 | 153.2 (5) |
N2i—Mn—N2—C11 | −143.1 (4) | C11—N2—C7—C8 | 0.3 (7) |
N1i—Mn—N2—C11 | 108.5 (3) | Mn—N2—C7—C8 | 176.7 (4) |
N1—Mn—N2—C11 | −52.1 (3) | N2—C7—C8—C9 | −0.4 (8) |
N3—Mn—N2—C11 | 13.1 (3) | C7—C8—C9—C10 | −0.3 (9) |
N3i—Mn—N2—C11 | 163.5 (3) | C8—C9—C10—C11 | 1.1 (9) |
N2—Mn—N3—C12 | −30.5 (3) | C7—N2—C11—C10 | 0.6 (7) |
N2i—Mn—N3—C12 | 25.7 (4) | Mn—N2—C11—C10 | −176.2 (4) |
N1i—Mn—N3—C12 | −120.7 (3) | C7—N2—C11—C12 | −175.4 (4) |
N1—Mn—N3—C12 | 84.8 (3) | Mn—N2—C11—C12 | 7.8 (5) |
N3i—Mn—N3—C12 | 167.5 (3) | C9—C10—C11—N2 | −1.2 (8) |
N2—Mn—N3—C6 | −145.2 (3) | C9—C10—C11—C12 | 174.4 (5) |
N2i—Mn—N3—C6 | −89.0 (4) | C6—N3—C12—C11 | 159.4 (4) |
N1i—Mn—N3—C6 | 124.7 (3) | C13—N3—C12—C11 | −80.9 (5) |
N1—Mn—N3—C6 | −29.8 (3) | Mn—N3—C12—C11 | 45.5 (4) |
N3i—Mn—N3—C6 | 52.8 (3) | N2—C11—C12—N3 | −38.9 (6) |
N2—Mn—N3—C13 | 89.7 (3) | C10—C11—C12—N3 | 145.2 (5) |
N2i—Mn—N3—C13 | 145.9 (3) | C12—N3—C13—C14 | −177.3 (4) |
N1i—Mn—N3—C13 | −0.5 (4) | C6—N3—C13—C14 | −58.3 (6) |
N1—Mn—N3—C13 | −155.0 (4) | Mn—N3—C13—C14 | 65.8 (5) |
N3i—Mn—N3—C13 | −72.3 (3) | N3—C13—C14—C15 | −164.0 (4) |
C5—N1—C1—C2 | 1.9 (7) | C13—C14—C15—C15ii | 177.3 (6) |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Mn(C30H36N6)](ClO4)2·2C3H6O·2H2O |
Mr | 886.68 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 243 |
a, b, c (Å) | 18.7266 (16), 14.5252 (12), 15.2375 (13) |
β (°) | 94.782 (2) |
V (Å3) | 4130.3 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.52 |
Crystal size (mm) | 0.20 × 0.18 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART 1000 CCD |
Absorption correction | Multi-scan (SADABS; Bruker, 2000) |
Tmin, Tmax | 0.707, 0.926 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 16555, 4248, 2171 |
Rint | 0.056 |
(sin θ/λ)max (Å−1) | 0.626 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.073, 0.227, 0.92 |
No. of reflections | 4248 |
No. of parameters | 230 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.86, −0.49 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003), SHELXL97.
The title compound consists of cationic complex polymer with counter anions (ClO4) and solvents (acetone and water). In the cation polymer, Mn2+ ions are bridged by the hexadentate ligand, N,N,N',N'-tetrakis(2-pyridylmethyl)-1,6-diaminohexane (tphn), and the constitutional repeating unit of the polymer, MnII(tphn), is disposed about a twofold axis passing through the Mn atom (Fig. 1). The Mn ion is six-coordinated in a distorted octahedral structure by three N atoms from one tphn ligand and three N atoms from another tphn ligand in the facial positions, respectively. The Mn—N(pyridyl) bond lengths (2.267 (4) and 2.217 (4) Å) are slightly longer than the Mn—N(amine) bond length (2.369 (4) Å). The polymer reveals a one-dimensional chain structure along the c axis (Fig. 2).