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
Key indicators
- Single-crystal X-ray study
- T = 243 K
- Mean (C-C) = 0.009 Å
- H-atom completeness 93%
- R factor = 0.073
- wR factor = 0.227
- Data-to-parameter ratio = 18.5
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W PLAT432_ALERT_2_A Short Inter X...Y Contact O1W .. C1S .. 1.90 Ang. PLAT432_ALERT_2_A Short Inter X...Y Contact O1W .. C2S .. 2.53 Ang.
Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O1S .. O1W .. 2.57 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O1W .. C3S .. 2.90 Ang.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.707 0.926 Tmin(prime) and Tmax expected: 0.900 0.926 RR(prime) = 0.786 Please check that your absorption correction is appropriate. PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.78 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 1 PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 5 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1S PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.10 PLAT321_ALERT_2_C Check Hybridisation of C1S in Solvent/Ion .. ? PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C36 H52 Cl2 Mn1 N6 O12 Atom count from the _atom_site data: C36 H48 Cl2 Mn1 N6 O12 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C36 H52 Cl2 Mn N6 O12 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 144.00 144.00 0.00 H 208.00 192.00 16.00 Cl 8.00 8.00 0.00 Mn 4.00 4.00 0.00 N 24.00 24.00 0.00 O 48.00 48.00 0.00 PLAT793_ALERT_1_G Check the Absolute Configuration of N3 = ... R PLAT794_ALERT_5_G Check Predicted Bond Valency for Mn (2) 1.88
3 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 8 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
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.
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
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).