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The title compound, [Mn(C30H36N6)](ClO4)2·2C3H6O·2H2O, consists of a cationic complex polymer with counter-anions and solvent mol­ecules. In the cationic polymer, Mn2+ ions are bridged by the hexa­dentate ligand N,N,N′,N′-tetra­kis(2-pyridyl­meth­yl)hexane-1,6-diamine (tphn) to form a one-dimensional chain structure along the c axis. The repeat unit of the polymer, MnII(tphn), is disposed about a twofold axis passing through the Mn atom. The coordination geometry around the Mn centre is distorted octa­hedral.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807038603/hg2266sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807038603/hg2266Isup2.hkl
Contains datablock I

CCDC reference: 660075

Key indicators

  • Single-crystal X-ray study
  • T = 243 K
  • Mean [sigma](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

Comment top

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).

Related literature top

For related literature, see: Jensen et al. (1997).

Experimental top

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.

Refinement top

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.

Structure description top

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).

Computing details top

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.

Figures top
[Figure 1] Fig. 1. The structure of the constitutional repeating unit of the title compound [Symmetry code: (a) -x, y, 1/2 - z]. Displacement ellipsoids are drawn at the 20% probability level. H atoms and the solvent molecules have been omitted for clarity.
[Figure 2] Fig. 2. View of the unit-cell contents and chain structure of the title compound. H atoms and the solvent molecules have been omitted for clarity.
[Figure 3] Fig. 3. The N,N,N',N'-tetrakis(2-pyridylmethyl)hexane-1,6-diamine ligand.
catena-Poly[[manganese(II)-µ-[N,N,N',N'-tetrakis(2-pyridylmethyl)hexane- 1,6-diamine]] diperchlorate acetone disolvate dihydrate] top
Crystal data top
[Mn(C30H36N6)](ClO4)2·2C3H6O·2H2OF(000) = 1860
Mr = 886.68Dx = 1.426 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2085 reflections
a = 18.7266 (16) Åθ = 2.2–21.0°
b = 14.5252 (12) ŵ = 0.52 mm1
c = 15.2375 (13) ÅT = 243 K
β = 94.782 (2)°Block, yellow
V = 4130.3 (6) Å30.20 × 0.18 × 0.15 mm
Z = 4
Data collection top
Bruker SMART 1000 CCD
diffractometer
4248 independent reflections
Radiation source: fine-focus sealed tube2171 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.056
φ and ω scansθmax = 26.4°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 2322
Tmin = 0.707, Tmax = 0.926k = 1818
16555 measured reflectionsl = 1912
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.073Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.227H-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 parametersΔρmax = 0.86 e Å3
0 restraintsΔρmin = 0.49 e Å3
Crystal data top
[Mn(C30H36N6)](ClO4)2·2C3H6O·2H2OV = 4130.3 (6) Å3
Mr = 886.68Z = 4
Monoclinic, C2/cMo Kα radiation
a = 18.7266 (16) ŵ = 0.52 mm1
b = 14.5252 (12) ÅT = 243 K
c = 15.2375 (13) Å0.20 × 0.18 × 0.15 mm
β = 94.782 (2)°
Data collection top
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 = 0.926Rint = 0.056
16555 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0730 restraints
wR(F2) = 0.227H-atom parameters constrained
S = 0.92Δρmax = 0.86 e Å3
4248 reflectionsΔρmin = 0.49 e Å3
230 parameters
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
xyzUiso*/Ueq
Mn0.00000.26386 (6)0.25000.0436 (3)
N10.0765 (2)0.2265 (2)0.1478 (2)0.0488 (10)
N20.0500 (2)0.3736 (2)0.3356 (3)0.0509 (10)
N30.1019 (2)0.1940 (3)0.3248 (2)0.0523 (10)
C10.0736 (3)0.2587 (3)0.0651 (3)0.0508 (12)
H10.03800.30220.04780.061*
C20.1189 (3)0.2322 (4)0.0046 (3)0.0588 (13)
H20.11380.25620.05290.071*
C30.1713 (3)0.1710 (4)0.0281 (3)0.0688 (15)
H30.20300.15140.01280.083*
C40.1773 (3)0.1378 (4)0.1134 (4)0.0661 (15)
H40.21390.09610.13180.079*
C50.1285 (3)0.1670 (3)0.1715 (3)0.0547 (13)
C60.1313 (3)0.1281 (3)0.2638 (3)0.0637 (15)
H6A0.10370.07070.26330.076*
H6B0.18110.11380.28430.076*
C70.0191 (3)0.4531 (3)0.3588 (3)0.0620 (14)
H70.02770.46570.33450.074*
C80.0512 (4)0.5154 (4)0.4146 (4)0.0718 (16)
H80.02760.57000.42850.086*
C90.1186 (4)0.4969 (4)0.4502 (4)0.087 (2)
H90.14230.53930.48910.104*
C100.1522 (3)0.4176 (5)0.4301 (4)0.0754 (17)
H100.19860.40450.45560.090*
C110.1176 (3)0.3571 (3)0.3721 (3)0.0551 (13)
C120.1520 (3)0.2711 (4)0.3387 (4)0.0605 (13)
H12A0.17220.28530.28290.073*
H12B0.19150.25250.38110.073*
C130.0935 (3)0.1483 (4)0.4109 (3)0.0632 (14)
H13A0.14110.13070.43690.076*
H13B0.07410.19360.45030.076*
C140.0467 (3)0.0653 (3)0.4084 (3)0.0650 (15)
H14A0.07230.01320.38460.078*
H14B0.00360.07680.36900.078*
C150.0251 (3)0.0406 (3)0.4997 (4)0.0738 (17)
H15A0.06850.02670.53800.089*
H15B0.00200.09410.52440.089*
Cl0.23323 (9)0.43776 (12)0.17809 (10)0.0844 (6)
O10.2592 (2)0.4928 (3)0.1128 (3)0.1020 (15)
O20.2566 (4)0.4597 (4)0.2616 (3)0.150 (3)
O30.1583 (3)0.4373 (6)0.1717 (5)0.193 (4)
O40.2472 (4)0.3424 (4)0.1612 (4)0.154 (2)
O1S0.4558 (3)0.2153 (4)0.3938 (5)0.139 (2)*
C1S0.4137 (6)0.2292 (8)0.3337 (8)0.150 (4)*
C2S0.3836 (7)0.1745 (10)0.2604 (9)0.231 (6)*
H2S10.33930.20250.23580.346*
H2S20.37380.11280.28070.346*
H2S30.41740.17140.21560.346*
C3S0.3406 (7)0.2371 (9)0.3732 (9)0.302 (10)*
H3S10.31510.29060.34880.453*
H3S20.34820.24360.43670.453*
H3S30.31250.18220.35910.453*
O1W0.4390 (7)0.3332 (9)0.2678 (9)0.416 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn0.0622 (7)0.0285 (5)0.0426 (6)0.0000.0197 (5)0.000
N10.066 (3)0.034 (2)0.048 (2)0.0046 (19)0.0172 (19)0.0045 (17)
N20.072 (3)0.034 (2)0.050 (2)0.0020 (18)0.023 (2)0.0016 (17)
N30.077 (3)0.040 (2)0.043 (2)0.013 (2)0.021 (2)0.0066 (17)
C10.069 (3)0.041 (3)0.044 (3)0.002 (2)0.015 (2)0.003 (2)
C20.077 (4)0.061 (3)0.040 (3)0.007 (3)0.016 (3)0.002 (2)
C30.083 (4)0.076 (4)0.052 (3)0.003 (3)0.029 (3)0.010 (3)
C40.078 (4)0.060 (3)0.063 (4)0.018 (3)0.027 (3)0.006 (3)
C50.074 (3)0.041 (3)0.052 (3)0.005 (2)0.023 (3)0.003 (2)
C60.091 (4)0.050 (3)0.054 (3)0.024 (3)0.026 (3)0.003 (2)
C70.090 (4)0.040 (3)0.060 (3)0.001 (3)0.025 (3)0.004 (2)
C80.120 (5)0.044 (3)0.055 (3)0.010 (3)0.025 (4)0.010 (3)
C90.142 (7)0.060 (4)0.061 (4)0.029 (4)0.018 (4)0.017 (3)
C100.084 (4)0.084 (4)0.058 (4)0.024 (3)0.004 (3)0.007 (3)
C110.073 (4)0.054 (3)0.042 (3)0.008 (3)0.020 (3)0.004 (2)
C120.065 (3)0.066 (3)0.052 (3)0.004 (3)0.014 (3)0.007 (3)
C130.090 (4)0.058 (3)0.044 (3)0.023 (3)0.020 (3)0.011 (2)
C140.109 (4)0.039 (3)0.051 (3)0.019 (3)0.030 (3)0.010 (2)
C150.128 (5)0.043 (3)0.054 (3)0.024 (3)0.031 (3)0.018 (3)
Cl0.0958 (12)0.0966 (13)0.0642 (10)0.0439 (9)0.0265 (8)0.0183 (8)
O10.112 (3)0.128 (4)0.069 (3)0.052 (3)0.022 (2)0.005 (3)
O20.236 (7)0.152 (5)0.067 (3)0.110 (5)0.034 (4)0.023 (3)
O30.101 (4)0.273 (10)0.208 (8)0.031 (5)0.041 (4)0.073 (7)
O40.240 (7)0.108 (5)0.124 (5)0.010 (5)0.079 (5)0.030 (4)
Geometric parameters (Å, º) top
Mn—N22.217 (4)C9—H90.9400
Mn—N2i2.217 (4)C10—C111.370 (7)
Mn—N1i2.267 (4)C10—H100.9400
Mn—N12.267 (4)C11—C121.514 (7)
Mn—N32.369 (4)C12—H12A0.9800
Mn—N3i2.369 (4)C12—H12B0.9800
N1—C51.331 (6)C13—C141.489 (7)
N1—C11.341 (6)C13—H13A0.9800
N2—C71.352 (6)C13—H13B0.9800
N2—C111.360 (6)C14—C151.524 (7)
N3—C121.465 (6)C14—H14A0.9800
N3—C61.472 (6)C14—H14B0.9800
N3—C131.490 (6)C15—C15ii1.509 (11)
C1—C21.360 (7)C15—H15A0.9800
C1—H10.9400C15—H15B0.9800
C2—C31.350 (7)Cl—O21.349 (5)
C2—H20.9400Cl—O11.395 (4)
C3—C41.382 (7)Cl—O31.399 (6)
C3—H30.9400Cl—O41.437 (6)
C4—C51.390 (6)O1S—C1S1.175 (11)
C4—H40.9400C1S—C2S1.446 (15)
C5—C61.513 (7)C1S—C3S1.546 (15)
C6—H6A0.9800C2S—H2S10.9700
C6—H6B0.9800C2S—H2S20.9700
C7—C81.349 (7)C2S—H2S30.9700
C7—H70.9400C3S—H3S10.9700
C8—C91.359 (8)C3S—H3S20.9700
C8—H80.9400C3S—H3S30.9700
C9—C101.359 (9)
N2—Mn—N2i88.1 (2)C8—C9—C10120.7 (6)
N2—Mn—N1i91.59 (13)C8—C9—H9119.7
N2i—Mn—N1i108.42 (14)C10—C9—H9119.7
N2—Mn—N1108.42 (14)C9—C10—C11119.0 (6)
N2i—Mn—N191.59 (13)C9—C10—H10120.5
N1i—Mn—N1152.33 (19)C11—C10—H10120.5
N2—Mn—N374.99 (14)N2—C11—C10121.7 (5)
N2i—Mn—N3151.06 (14)N2—C11—C12114.5 (4)
N1i—Mn—N395.57 (14)C10—C11—C12123.7 (5)
N1—Mn—N372.42 (13)N3—C12—C11113.2 (4)
N2—Mn—N3i151.06 (14)N3—C12—H12A108.9
N2i—Mn—N3i74.98 (14)C11—C12—H12A108.9
N1i—Mn—N3i72.42 (13)N3—C12—H12B108.9
N1—Mn—N3i95.57 (14)C11—C12—H12B108.9
N3—Mn—N3i129.2 (2)H12A—C12—H12B107.7
C5—N1—C1116.9 (4)C14—C13—N3116.3 (4)
C5—N1—Mn117.4 (3)C14—C13—H13A108.2
C1—N1—Mn125.7 (3)N3—C13—H13A108.2
C7—N2—C11116.6 (4)C14—C13—H13B108.2
C7—N2—Mn126.8 (4)N3—C13—H13B108.2
C11—N2—Mn116.6 (3)H13A—C13—H13B107.4
C12—N3—C6108.7 (4)C13—C14—C15111.6 (5)
C12—N3—C13109.1 (4)C13—C14—H14A109.3
C6—N3—C13109.8 (4)C15—C14—H14A109.3
C12—N3—Mn102.8 (3)C13—C14—H14B109.3
C6—N3—Mn107.7 (3)C15—C14—H14B109.3
C13—N3—Mn118.3 (3)H14A—C14—H14B108.0
N1—C1—C2124.1 (5)C15ii—C15—C14113.7 (6)
N1—C1—H1118.0C15ii—C15—H15A108.8
C2—C1—H1118.0C14—C15—H15A108.8
C3—C2—C1119.2 (5)C15ii—C15—H15B108.8
C3—C2—H2120.4C14—C15—H15B108.8
C1—C2—H2120.4H15A—C15—H15B107.7
C2—C3—C4118.7 (5)O2—Cl—O1115.6 (3)
C2—C3—H3120.7O2—Cl—O3108.1 (5)
C4—C3—H3120.7O1—Cl—O3111.1 (4)
C3—C4—C5119.1 (5)O2—Cl—O4110.3 (4)
C3—C4—H4120.5O1—Cl—O4110.2 (3)
C5—C4—H4120.5O3—Cl—O4100.4 (5)
N1—C5—C4122.1 (5)O1S—C1S—C2S134.4 (12)
N1—C5—C6117.6 (4)O1S—C1S—C3S105.5 (11)
C4—C5—C6120.3 (5)C2S—C1S—C3S92.3 (9)
N3—C6—C5111.0 (4)C1S—C2S—H2S1109.5
N3—C6—H6A109.4C1S—C2S—H2S2109.5
C5—C6—H6A109.4H2S1—C2S—H2S2109.5
N3—C6—H6B109.4C1S—C2S—H2S3109.5
C5—C6—H6B109.4H2S1—C2S—H2S3109.5
H6A—C6—H6B108.0H2S2—C2S—H2S3109.5
C8—C7—N2124.1 (6)C1S—C3S—H3S1109.5
C8—C7—H7118.0C1S—C3S—H3S2109.5
N2—C7—H7118.0H3S1—C3S—H3S2109.5
C7—C8—C9117.9 (6)C1S—C3S—H3S3109.5
C7—C8—H8121.0H3S1—C3S—H3S3109.5
C9—C8—H8121.0H3S2—C3S—H3S3109.5
N2—Mn—N1—C583.1 (4)Mn—N1—C1—C2177.6 (4)
N2i—Mn—N1—C5171.6 (3)N1—C1—C2—C31.2 (8)
N1i—Mn—N1—C551.2 (3)C1—C2—C3—C40.5 (8)
N3—Mn—N1—C516.1 (3)C2—C3—C4—C51.3 (8)
N3i—Mn—N1—C5113.4 (3)C1—N1—C5—C41.0 (7)
N2—Mn—N1—C197.5 (4)Mn—N1—C5—C4178.5 (4)
N2i—Mn—N1—C19.0 (4)C1—N1—C5—C6178.4 (4)
N1i—Mn—N1—C1128.2 (4)Mn—N1—C5—C61.1 (6)
N3—Mn—N1—C1164.4 (4)C3—C4—C5—N10.6 (8)
N3i—Mn—N1—C166.1 (4)C3—C4—C5—C6176.8 (5)
N2i—Mn—N2—C740.4 (3)C12—N3—C6—C570.6 (5)
N1i—Mn—N2—C767.9 (4)C13—N3—C6—C5170.2 (4)
N1—Mn—N2—C7131.5 (4)Mn—N3—C6—C540.1 (5)
N3—Mn—N2—C7163.3 (4)N1—C5—C6—N329.4 (7)
N3i—Mn—N2—C713.0 (5)C4—C5—C6—N3153.2 (5)
N2i—Mn—N2—C11143.1 (4)C11—N2—C7—C80.3 (7)
N1i—Mn—N2—C11108.5 (3)Mn—N2—C7—C8176.7 (4)
N1—Mn—N2—C1152.1 (3)N2—C7—C8—C90.4 (8)
N3—Mn—N2—C1113.1 (3)C7—C8—C9—C100.3 (9)
N3i—Mn—N2—C11163.5 (3)C8—C9—C10—C111.1 (9)
N2—Mn—N3—C1230.5 (3)C7—N2—C11—C100.6 (7)
N2i—Mn—N3—C1225.7 (4)Mn—N2—C11—C10176.2 (4)
N1i—Mn—N3—C12120.7 (3)C7—N2—C11—C12175.4 (4)
N1—Mn—N3—C1284.8 (3)Mn—N2—C11—C127.8 (5)
N3i—Mn—N3—C12167.5 (3)C9—C10—C11—N21.2 (8)
N2—Mn—N3—C6145.2 (3)C9—C10—C11—C12174.4 (5)
N2i—Mn—N3—C689.0 (4)C6—N3—C12—C11159.4 (4)
N1i—Mn—N3—C6124.7 (3)C13—N3—C12—C1180.9 (5)
N1—Mn—N3—C629.8 (3)Mn—N3—C12—C1145.5 (4)
N3i—Mn—N3—C652.8 (3)N2—C11—C12—N338.9 (6)
N2—Mn—N3—C1389.7 (3)C10—C11—C12—N3145.2 (5)
N2i—Mn—N3—C13145.9 (3)C12—N3—C13—C14177.3 (4)
N1i—Mn—N3—C130.5 (4)C6—N3—C13—C1458.3 (6)
N1—Mn—N3—C13155.0 (4)Mn—N3—C13—C1465.8 (5)
N3i—Mn—N3—C1372.3 (3)N3—C13—C14—C15164.0 (4)
C5—N1—C1—C21.9 (7)C13—C14—C15—C15ii177.3 (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
Mr886.68
Crystal system, space groupMonoclinic, C2/c
Temperature (K)243
a, b, c (Å)18.7266 (16), 14.5252 (12), 15.2375 (13)
β (°) 94.782 (2)
V3)4130.3 (6)
Z4
Radiation typeMo Kα
µ (mm1)0.52
Crystal size (mm)0.20 × 0.18 × 0.15
Data collection
DiffractometerBruker SMART 1000 CCD
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.707, 0.926
No. of measured, independent and
observed [I > 2σ(I)] reflections
16555, 4248, 2171
Rint0.056
(sin θ/λ)max1)0.626
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.073, 0.227, 0.92
No. of reflections4248
No. of parameters230
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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.

 

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