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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 6| June 2011| Pages m656-m657
doi:10.1107/S1600536811015388

cis-(Aceto­nitrile-κN)aqua­bis­­(2,2′-bi­pyrimidine-κ2N1,N1′)manganese(II) cis-di­aqua­bis­­(2,2′-bi­pyrimidine-κ2N1,N1′)manganese(II) tetra­kis­(perchlorate) dihydrate

Kwang Haa*

aSchool of Applied Chemical Engineering, The Research Institute of Catalysis, Chonnam National University, Gwangju 500-757, Republic of Korea
*Correspondence e-mail: hakwang@chonnam.ac.kr

(Received 14 April 2011; accepted 24 April 2011; online 7 May 2011)

The asymmetric unit of the title compound, [Mn(CH3CN)(C8H6N4)2(H2O)][Mn(C8H6N4)2(H2O)2](ClO4)4·2H2O, contains two distinct cationic MnII complexes, four perchlorate anions and two solvent water mol­ecules. In the two complexes, both MnII ions are six-coordinated in a distorted octa­hedral environment, but one Mn ion has a cis-N5O coordination geometry defined by four N atoms of the two chelating 2,2′-bipyrimidine (bpym) ligands, one N atom of a coordinating acetonitrile mol­ecule and one O atom of a water ligand, whereas the other Mn ion has a cis-N4O2 coordination geometry defined by four N atoms of the two bpym ligands and two O atoms of water ligands. In the crystal structure, the complex mol­ecules, anions and solvent water mol­ecules are linked by inter­molecular O—H⋯O and O—H⋯N hydrogen bonds. Three of the four perchlorate anions are disordered over two sets of sites in different ratios.

Related literature

For the crystal structures of mononuclear 2,2′-bipyrimidine Mn(II) complexes, see: Hong et al. (1996[Hong, D. M., Wei, H. H., Gan, L. L., Lee, G. H. & Wang, Y. (1996). Polyhedron, 15, 2335-2340.]); Smith et al. (2001[Smith, J. A., Galán-Mascarós, J.-R., Clérac, R., Sun, J.-S., Ouyang, X. & Dunbar, K. R. (2001). Polyhedron, 20, 1727-1734.]); Ha (2011[Ha, K. (2011). Acta Cryst. E67, m474.]).

[Scheme 1]

Experimental

Crystal data

  • [Mn(C2H3N)(C8H6N4)2(H2O)][Mn(C8H6N4)2(H2O)2](ClO4)4·2H2O

  • Mr = 1271.49

  • Triclinic, [P \overline 1]

  • a = 12.0386 (5) Å

  • b = 13.1878 (6) Å

  • c = 17.5378 (8) Å

  • α = 111.201 (3)°

  • β = 104.147 (3)°

  • γ = 91.419 (2)°

  • V = 2497.37 (19) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.82 mm−1

  • T = 200 K

  • 0.24 × 0.21 × 0.13 mm
Data collection

  • Bruker SMART 1000 CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2000[Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.765, Tmax = 0.899

  • 18759 measured reflections

  • 12197 independent reflections

  • 5402 reflections with I > 2σ(I)

  • Rint = 0.052
Refinement

  • R[F2 > 2σ(F2)] = 0.082

  • wR(F2) = 0.253

  • S = 1.01

  • 12197 reflections

  • 718 parameters

  • H-atom parameters constrained

  • Δρmax = 1.01 e Å−3

  • Δρmin = −0.61 e Å−3

Table 1
Selected geometric parameters (Å, °)

Mn1—N9 2.170 (6)
Mn1—O1 2.182 (4)
Mn1—N4 2.236 (4)
Mn1—N8 2.254 (5)
Mn1—N1 2.259 (5)
Mn1—N5 2.271 (5)
Mn2—O3 2.107 (4)
Mn2—O2 2.174 (4)
Mn2—N13 2.238 (5)
Mn2—N10 2.267 (5)
Mn2—N14 2.269 (5)
Mn2—N17 2.272 (5)
N4—Mn1—N1 73.12 (18)
N8—Mn1—N5 73.27 (18)
N13—Mn2—N10 72.99 (19)
N14—Mn2—N17 72.26 (18)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O1—H1A⋯N6i 0.84 2.49 3.139 (6) 135
O1—H1A⋯N7i 0.84 2.15 2.923 (6) 152
O1—H1B⋯O21i 0.84 1.89 2.695 (7) 160
O2—H2A⋯N15ii 0.84 2.59 3.244 (7) 136
O2—H2A⋯N16ii 0.84 2.25 3.012 (7) 151
O2—H2B⋯O11Aiii 0.84 2.01 2.809 (10) 158
O3—H3A⋯O20 0.84 1.79 2.614 (6) 166
O3—H3B⋯O4iii 0.84 2.07 2.861 (6) 157
O20—H20A⋯N2iv 0.84 2.08 2.903 (7) 168
O20—H20A⋯N3iv 0.84 2.56 3.066 (7) 120
O20—H20B⋯O6 0.84 2.08 2.871 (7) 157
O21—H21A⋯O12v 0.84 2.43 3.126 (12) 141
O21—H21B⋯O16Aiv 0.84 2.07 2.904 (13) 172
Symmetry codes: (i) -x+1, -y+1, -z+1; (ii) -x+1, -y+2, -z; (iii) -x+1, -y+1, -z; (iv) x+1, y, z; (v) -x+1, -y, -z+1.

Data collection: SMART (Bruker, 2000[Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2000[Bruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]) and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811015388/om2423sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811015388/om2423Isup2.hkl

checkCIF report


Comment top

Mononuclear MnII complexes of 2,2'-bipyrimidine (bpym; C8H6N4) ligand, such as [Mn(bpym)2(H2O)2](ClO4)2.2H2O (Hong et al., 1996), [Mn(bpym)2(H2O)2](BF4)2.2H2O (Smith et al., 2001) and [MnBr2(bpym)2].CH3NO2 (Ha, 2011), have been investigated previously.

The asymmetric unit of the title compound, [Mn(bpym)2(CH3CN)(H2O)][Mn(bpym)2(H2O)2](ClO4)4.2H2O, contains two distinct cationic MnII complexes (Fig. 1), four ClO4 anions and two solvent water molecules. In the two complexes, both the MnII ions are six-coordinated in a distorted octahedral environment, but one Mn ion has a cis-N5O coordination geometry defined by four N atoms of the two chelating 2,2'-bipyrimidine ligands, one N atom of a coordinating acetonitrile molecule and one O atom of a water ligand, whereas the other Mn ion has a cis-N4O2 coordination geometry defined by four N atoms of the two bpym ligands and two O atoms of water ligands. The tight N—Mn—N chelating angles (Table 1) contribute the distortion of the octaahedron, which results in non-linear trans axes (<O1—Mn1—N1 = 163.1 (2)°, <N4—Mn1—N8 = 172.3 (2)°, <N5—Mn1—N9 = 165.5 (2)°, <O2—Mn2—N10 = 165.9 (2)°, <O3—Mn2—N14 = 162.0 (2)° and <N13—Mn2—N17 = 161.2 (2)°). The Mn—N(bpym) bond lengths are almost equivalent and slightly longer than the Mn1—N9(CH3CN) bond (Table 1). On the basis of the Mn—N bonds trans to the N and O atoms, it seems that the N and O atoms have similar trans effects. The dihedral angles between the least-squares planes of the two bpym ligands in the respective complexes are 79.7 (1)° and 70.7 (1)°. In the crystal structure, the complexes, anions and solvent water molecules are linked by intermolecular O—H···O and O—H···N hydrogen bonds (Fig. 2, Table 2). In addition, the complexes display numerous inter- and intramolecular π-π interactions between adjacent pyrimidine rings. The shortest distance between Cg1 (the centroid of ring N14—C30) and Cg2i (ring N16—C34, symmetry code i: 1 - x, 2 - y, -z) is 3.585 (4) Å, and the dihedral angle between the ring planes is 3.3 (3)°.

Related literature top

For the crystal structures of mononuclear 2,2'-bipyrimidine Mn(II) complexes, see: Hong et al. (1996); Smith et al. (2001); Ha (2011).

Experimental top

To a solution of Mn(ClO4)2.6H2O (0.3617 g, 0.999 mmol) in EtOH (20 ml) was added 2,2'-bipyrimidine (0.1586 g, 1.003 mmol) and stirred for 3 h at room temperature. The formed precipitate was separated by filtration, washed with EtOH and dried at 323 K, to give a pale yellow powder (0.2713 g). Crystals suitable for X-ray analysis were obtained by slow evaporation from a CH3CN solution.

Refinement top

H atoms were positioned geometrically and allowed to ride on their respective parent atoms [C—H = 0.95 Å (CH) or 0.98 Å (CH3), O—H = 0.84 Å and Uiso(H) = 1.2Ueq(C) or 1.5Ueq(methyl C, O)]. The ClO4- anions displayed relatively large displacement factors and low electron density peaks so that the anions appear to be highly disordered. Atoms O10 and O11 were modelled anisotropically as disordered over two sites with a site occupancy factor of 0.71 (3) for the major component. However, the seven O atoms (O13–O19) of the two ClO4- anions were refined with isotropic thermal parameters as disordered over two sites with site occupancy factors of 0.61 (1) for the atoms O13A–O15A and 0.54 (2) for the atoms O16A–O19A. The large R values are connected with the disorder of the anions and the isotropic refinement of the O atoms.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The structure of the title compound, with displacement ellipsoids drawn at the 40% probability level for non-H atoms. The four ClO4- anions and the two H2O solvent molecules have been omitted for clarity.
[Figure 2] Fig. 2. View of the unit-cell contents of the title compound. Hydrogen-bond interactions and the bonds of the disordered anions are drawn with dashed lines.
cis-(Acetonitrile-κN)aquabis(2,2'-bipyrimidine- κ2N1,N1')manganese(II) cis-diaquabis(2,2'-bipyrimidine- κ2N1,N1')manganese(II) tetrakis(perchlorate) dihydrate top
Crystal data top
[Mn(C2H3N)(C8H6N4)2(H2O)][Mn(C8H6N4)2(H2O)2](ClO4)4·2H2OZ = 2
Mr = 1271.49F(000) = 1292
Triclinic, P1Dx = 1.691 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.0386 (5) ÅCell parameters from 3208 reflections
b = 13.1878 (6) Åθ = 2.3–23.0°
c = 17.5378 (8) ŵ = 0.82 mm−1
α = 111.201 (3)°T = 200 K
β = 104.147 (3)°Block, pale yellow
γ = 91.419 (2)°0.24 × 0.21 × 0.13 mm
V = 2497.37 (19) Å3
Data collection top
Bruker SMART 1000 CCD
diffractometer		12197 independent reflections
Radiation source: fine-focus sealed tube5402 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
ϕ and ω scansθmax = 28.3°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		h = −15→16
Tmin = 0.765, Tmax = 0.899k = −17→17
18759 measured reflectionsl = −13→23
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)] = 0.082Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.253H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.1047P)2]
where P = (Fo2 + 2Fc2)/3
12197 reflections(Δ/σ)max < 0.001
718 parametersΔρmax = 1.01 e Å−3
0 restraintsΔρmin = −0.61 e Å−3
Crystal data top
[Mn(C2H3N)(C8H6N4)2(H2O)][Mn(C8H6N4)2(H2O)2](ClO4)4·2H2Oγ = 91.419 (2)°
Mr = 1271.49V = 2497.37 (19) Å3
Triclinic, P1Z = 2
a = 12.0386 (5) ÅMo Kα radiation
b = 13.1878 (6) ŵ = 0.82 mm−1
c = 17.5378 (8) ÅT = 200 K
α = 111.201 (3)°0.24 × 0.21 × 0.13 mm
β = 104.147 (3)°
Data collection top
Bruker SMART 1000 CCD
diffractometer		12197 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)		5402 reflections with I > 2σ(I)
Tmin = 0.765, Tmax = 0.899Rint = 0.052
18759 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0820 restraints
wR(F2) = 0.253H-atom parameters constrained
S = 1.01Δρmax = 1.01 e Å−3
12197 reflectionsΔρmin = −0.61 e Å−3
718 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*/UeqOcc. (<1)
Mn10.24790 (7)0.60902 (8)0.39169 (6)0.0372 (3)
O10.2664 (3)0.6133 (3)0.5198 (3)0.0432 (11)
H1A0.32050.58020.53560.065*
H1B0.27640.68120.54770.065*
N10.1739 (4)0.6075 (4)0.2598 (3)0.0364 (12)
N2−0.0030 (4)0.5887 (4)0.1555 (3)0.0441 (13)
N3−0.1202 (4)0.5380 (4)0.2547 (3)0.0396 (12)
N40.0595 (4)0.5495 (4)0.3538 (3)0.0362 (12)
N50.3165 (4)0.4446 (4)0.3495 (3)0.0368 (12)
N60.4890 (4)0.3620 (4)0.3555 (3)0.0429 (13)
N70.6126 (4)0.5630 (4)0.4485 (3)0.0393 (12)
N80.4414 (4)0.6449 (4)0.4233 (3)0.0355 (12)
N90.2262 (5)0.7817 (5)0.4347 (4)0.0513 (15)
C10.2310 (6)0.6318 (6)0.2120 (5)0.0525 (18)
H10.31270.64740.23150.063*
C20.1743 (7)0.6353 (7)0.1334 (5)0.068 (2)
H20.21590.65180.09890.081*
C30.0567 (6)0.6138 (6)0.1085 (5)0.058 (2)
H30.01590.61680.05580.069*
C40.0589 (5)0.5865 (5)0.2290 (4)0.0358 (14)
C5−0.0048 (5)0.5562 (5)0.2814 (4)0.0333 (13)
C6−0.1735 (5)0.5090 (5)0.3031 (4)0.0443 (16)
H6−0.25550.49630.28620.053*
C7−0.1166 (5)0.4966 (6)0.3754 (4)0.0546 (19)
H7−0.15600.47370.40830.065*
C80.0035 (5)0.5196 (6)0.3986 (5)0.0553 (19)
H80.04650.51320.44940.066*
C90.2540 (5)0.3463 (5)0.3085 (4)0.0438 (16)
H90.17210.34100.29270.053*
C100.3062 (6)0.2534 (6)0.2891 (4)0.0526 (18)
H100.26230.18300.25970.063*
C110.4237 (6)0.2647 (6)0.3134 (4)0.0509 (18)
H110.46110.20050.29970.061*
C120.4308 (5)0.4484 (5)0.3712 (4)0.0351 (14)
C130.4997 (5)0.5586 (5)0.4168 (4)0.0343 (14)
C140.6714 (5)0.6624 (6)0.4895 (4)0.0486 (17)
H140.75190.66860.51480.058*
C150.6210 (5)0.7575 (6)0.4973 (4)0.0464 (17)
H150.66530.82780.52430.056*
C160.5022 (6)0.7446 (5)0.4635 (4)0.0483 (17)
H160.46340.80760.46900.058*
C170.1982 (5)0.8652 (6)0.4523 (5)0.0510 (18)
C180.1624 (7)0.9751 (6)0.4753 (6)0.092 (3)
H18A0.23101.03000.50080.138*
H18B0.11690.98550.51630.138*
H18C0.11550.98350.42430.138*
Mn20.73069 (7)0.84930 (7)0.08687 (6)0.0360 (3)
O20.7368 (4)0.8748 (4)−0.0279 (3)0.0487 (12)
H2A0.69120.9070−0.05300.073*
H2B0.76460.8323−0.06520.073*
O30.7245 (4)0.6807 (3)0.0161 (3)0.0546 (13)
H3A0.73330.63970.04380.082*
H3B0.70670.6516−0.03720.082*
N100.7711 (4)0.8189 (4)0.2094 (3)0.0375 (12)
N110.9225 (5)0.8194 (4)0.3254 (4)0.0501 (15)
N121.0769 (5)0.8875 (5)0.2568 (4)0.0594 (17)
N130.9206 (4)0.8974 (4)0.1473 (3)0.0408 (13)
N140.6835 (4)1.0226 (4)0.1326 (3)0.0377 (12)
N150.5259 (5)1.1271 (5)0.1331 (4)0.0480 (14)
N160.3769 (4)0.9390 (5)0.0614 (3)0.0473 (14)
N170.5367 (4)0.8376 (4)0.0686 (3)0.0375 (12)
C190.6952 (6)0.7861 (5)0.2431 (4)0.0462 (16)
H190.61530.77610.21490.055*
C200.7279 (7)0.7664 (5)0.3158 (4)0.0513 (18)
H200.67380.74110.33840.062*
C210.8441 (7)0.7857 (5)0.3543 (4)0.0541 (19)
H210.86990.77370.40570.065*
C220.8816 (5)0.8349 (5)0.2529 (4)0.0402 (15)
C230.9659 (5)0.8756 (5)0.2170 (4)0.0399 (15)
C241.1476 (6)0.9293 (7)0.2243 (6)0.070 (2)
H241.22810.94000.25100.084*
C251.1122 (6)0.9575 (6)0.1560 (5)0.056 (2)
H251.16500.98920.13600.067*
C260.9945 (5)0.9374 (5)0.1170 (4)0.0474 (17)
H260.96600.95260.06730.057*
C270.7571 (6)1.1148 (5)0.1646 (4)0.0459 (16)
H270.83781.11040.17530.055*
C280.7185 (6)1.2159 (6)0.1824 (5)0.0538 (18)
H280.77081.28140.20460.065*
C290.6023 (7)1.2183 (6)0.1669 (5)0.061 (2)
H290.57401.28750.18060.074*
C300.5709 (5)1.0339 (5)0.1185 (4)0.0386 (14)
C310.4891 (5)0.9305 (5)0.0806 (4)0.0378 (14)
C320.3065 (6)0.8437 (6)0.0277 (4)0.0546 (19)
H320.22560.84570.01170.066*
C330.3460 (6)0.7444 (6)0.0153 (4)0.0535 (19)
H330.29420.6788−0.00600.064*
C340.4637 (5)0.7432 (5)0.0351 (4)0.0408 (15)
H340.49410.67520.02500.049*
Cl10.48977 (13)0.50530 (13)0.17253 (10)0.0410 (4)
O40.4008 (4)0.4218 (4)0.1592 (3)0.0647 (14)
O50.4494 (4)0.5679 (5)0.1233 (4)0.0745 (16)
O60.5876 (4)0.4560 (4)0.1486 (3)0.0668 (15)
O70.5234 (5)0.5730 (5)0.2605 (3)0.0773 (17)
Cl20.01877 (14)0.26540 (14)0.10338 (10)0.0466 (4)
O8−0.0134 (4)0.3198 (5)0.1779 (3)0.0739 (16)
O9−0.0433 (5)0.2906 (6)0.0345 (4)0.093 (2)
O10A−0.0218 (13)0.1481 (6)0.0770 (5)0.068 (4)0.71 (3)
O11A0.1384 (7)0.2815 (11)0.1164 (6)0.068 (5)0.71 (3)
O10B0.077 (4)0.178 (2)0.0996 (19)0.090 (18)0.29 (3)
O11B0.118 (4)0.356 (4)0.130 (3)0.144 (16)0.29 (3)
Cl30.52009 (15)0.04352 (15)0.66585 (13)0.0599 (5)
O120.4138 (6)0.0080 (8)0.6096 (6)0.166 (4)
O13A0.5402 (8)0.1556 (9)0.6816 (7)0.088 (4)*0.613 (14)
O14A0.6054 (10)0.0031 (10)0.6173 (8)0.104 (4)*0.613 (14)
O15A0.5443 (13)0.0240 (11)0.7396 (9)0.121 (5)*0.613 (14)
O13B0.5640 (15)0.1420 (16)0.7412 (14)0.104 (7)*0.387 (14)
O14B0.5893 (11)−0.0398 (11)0.6507 (9)0.061 (5)*0.387 (14)
O15B0.447 (2)0.0083 (19)0.7173 (16)0.145 (10)*0.387 (14)
Cl40.00909 (15)0.18921 (14)0.38159 (12)0.0522 (5)
O16A−0.0859 (10)0.1076 (10)0.3297 (9)0.081 (4)*0.544 (15)
O17A0.1037 (12)0.1561 (12)0.3431 (11)0.119 (6)*0.544 (15)
O18A−0.0302 (12)0.2824 (13)0.3760 (10)0.122 (6)*0.544 (15)
O19A0.0411 (15)0.1971 (17)0.4642 (12)0.162 (8)*0.544 (15)
O16B−0.0760 (10)0.0984 (10)0.3678 (9)0.060 (4)*0.456 (15)
O17B0.1208 (11)0.1573 (11)0.4020 (10)0.080 (5)*0.456 (15)
O18B0.0048 (16)0.2185 (17)0.3119 (14)0.146 (9)*0.456 (15)
O19B0.0154 (13)0.2819 (15)0.4580 (11)0.106 (6)*0.456 (15)
O200.7508 (4)0.5264 (4)0.0772 (3)0.0555 (13)
H20A0.82040.54150.10550.083*
H20B0.70800.52480.10820.083*
O210.6981 (4)0.1840 (4)0.3583 (3)0.0710 (15)
H21A0.69730.14730.38860.106*
H21B0.76190.16130.35470.106*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0292 (5)0.0412 (6)0.0418 (6)0.0069 (4)0.0078 (4)0.0175 (5)
O10.036 (2)0.055 (3)0.045 (3)0.013 (2)0.010 (2)0.027 (2)
N10.038 (3)0.041 (3)0.039 (3)0.011 (2)0.018 (2)0.021 (2)
N20.048 (3)0.056 (4)0.033 (3)0.009 (3)0.009 (3)0.025 (3)
N30.034 (3)0.042 (3)0.042 (3)0.006 (2)0.011 (2)0.015 (3)
N40.029 (3)0.047 (3)0.039 (3)−0.003 (2)0.007 (2)0.025 (3)
N50.037 (3)0.042 (3)0.031 (3)0.009 (2)0.010 (2)0.013 (2)
N60.042 (3)0.043 (3)0.049 (3)0.012 (2)0.013 (3)0.022 (3)
N70.034 (3)0.047 (3)0.038 (3)0.006 (2)0.010 (2)0.017 (3)
N80.031 (3)0.040 (3)0.037 (3)0.000 (2)0.013 (2)0.014 (2)
N90.055 (4)0.038 (3)0.054 (4)0.009 (3)0.007 (3)0.014 (3)
C10.048 (4)0.060 (5)0.061 (5)0.011 (3)0.023 (4)0.032 (4)
C20.073 (5)0.095 (6)0.058 (5)0.018 (5)0.036 (5)0.043 (5)
C30.069 (5)0.071 (5)0.041 (4)0.015 (4)0.017 (4)0.028 (4)
C40.035 (3)0.033 (3)0.038 (4)0.005 (3)0.010 (3)0.012 (3)
C50.034 (3)0.031 (3)0.031 (3)0.005 (2)0.007 (3)0.009 (3)
C60.032 (3)0.045 (4)0.054 (4)0.002 (3)0.008 (3)0.018 (3)
C70.039 (4)0.079 (5)0.049 (4)−0.005 (4)0.009 (3)0.030 (4)
C80.039 (4)0.079 (5)0.054 (5)−0.003 (3)−0.001 (3)0.042 (4)
C90.045 (4)0.042 (4)0.036 (4)−0.002 (3)0.002 (3)0.013 (3)
C100.051 (4)0.047 (4)0.049 (4)0.005 (3)0.008 (4)0.009 (3)
C110.065 (5)0.039 (4)0.051 (4)0.015 (3)0.020 (4)0.016 (3)
C120.035 (3)0.047 (4)0.036 (3)0.012 (3)0.016 (3)0.025 (3)
C130.025 (3)0.042 (4)0.041 (3)0.008 (3)0.011 (3)0.019 (3)
C140.034 (3)0.060 (5)0.049 (4)0.001 (3)0.008 (3)0.019 (4)
C150.037 (4)0.053 (4)0.048 (4)−0.004 (3)0.009 (3)0.020 (3)
C160.051 (4)0.041 (4)0.059 (5)0.007 (3)0.018 (4)0.025 (4)
C170.044 (4)0.044 (4)0.057 (5)0.004 (3)−0.001 (3)0.018 (4)
C180.087 (6)0.031 (4)0.118 (8)0.006 (4)−0.004 (6)0.001 (5)
Mn20.0334 (5)0.0383 (5)0.0356 (5)0.0089 (4)0.0071 (4)0.0145 (4)
O20.058 (3)0.061 (3)0.044 (3)0.028 (2)0.022 (2)0.032 (2)
O30.085 (3)0.037 (3)0.039 (3)0.015 (2)0.014 (3)0.013 (2)
N100.040 (3)0.035 (3)0.034 (3)0.005 (2)0.008 (2)0.012 (2)
N110.057 (4)0.044 (3)0.042 (3)0.004 (3)−0.005 (3)0.020 (3)
N120.035 (3)0.062 (4)0.067 (4)0.006 (3)−0.002 (3)0.018 (3)
N130.033 (3)0.039 (3)0.044 (3)0.003 (2)0.010 (3)0.009 (3)
N140.040 (3)0.038 (3)0.034 (3)0.004 (2)0.010 (2)0.012 (2)
N150.057 (3)0.045 (3)0.053 (4)0.021 (3)0.021 (3)0.026 (3)
N160.034 (3)0.065 (4)0.037 (3)0.014 (3)0.007 (3)0.013 (3)
N170.034 (3)0.047 (3)0.035 (3)0.003 (2)0.010 (2)0.020 (3)
C190.054 (4)0.046 (4)0.045 (4)0.006 (3)0.016 (3)0.023 (3)
C200.077 (5)0.045 (4)0.039 (4)0.006 (4)0.025 (4)0.017 (3)
C210.083 (6)0.037 (4)0.037 (4)0.006 (4)0.007 (4)0.014 (3)
C220.042 (4)0.033 (3)0.036 (4)0.012 (3)0.002 (3)0.006 (3)
C230.036 (3)0.034 (3)0.038 (4)0.005 (3)−0.002 (3)0.009 (3)
C240.031 (4)0.077 (6)0.081 (6)0.003 (4)0.004 (4)0.014 (5)
C250.050 (4)0.047 (4)0.064 (5)−0.005 (3)0.026 (4)0.006 (4)
C260.041 (4)0.049 (4)0.046 (4)0.002 (3)0.018 (3)0.008 (3)
C270.051 (4)0.042 (4)0.043 (4)0.001 (3)0.013 (3)0.016 (3)
C280.068 (5)0.041 (4)0.056 (5)0.004 (3)0.028 (4)0.016 (4)
C290.090 (6)0.041 (4)0.069 (5)0.023 (4)0.045 (5)0.023 (4)
C300.045 (4)0.039 (4)0.038 (4)0.015 (3)0.017 (3)0.017 (3)
C310.030 (3)0.049 (4)0.036 (3)0.009 (3)0.007 (3)0.020 (3)
C320.038 (4)0.072 (5)0.049 (4)0.005 (4)0.013 (3)0.016 (4)
C330.046 (4)0.059 (5)0.045 (4)−0.007 (3)0.012 (3)0.009 (4)
C340.040 (4)0.049 (4)0.036 (4)0.000 (3)0.007 (3)0.021 (3)
Cl10.0398 (8)0.0434 (9)0.0380 (9)0.0048 (7)0.0074 (7)0.0153 (7)
O40.054 (3)0.077 (4)0.057 (3)−0.021 (3)0.001 (3)0.030 (3)
O50.070 (3)0.095 (4)0.087 (4)0.027 (3)0.016 (3)0.069 (4)
O60.064 (3)0.060 (3)0.080 (4)0.020 (3)0.032 (3)0.023 (3)
O70.093 (4)0.076 (4)0.041 (3)−0.013 (3)0.018 (3)−0.003 (3)
Cl20.0461 (9)0.0512 (10)0.0397 (9)0.0108 (8)0.0107 (8)0.0143 (8)
O80.066 (3)0.088 (4)0.064 (4)0.025 (3)0.035 (3)0.012 (3)
O90.084 (4)0.128 (6)0.080 (4)0.008 (4)−0.006 (3)0.073 (4)
O10A0.089 (10)0.038 (4)0.068 (5)−0.001 (4)0.029 (5)0.007 (4)
O11A0.038 (4)0.092 (10)0.057 (5)0.008 (5)0.021 (4)0.003 (6)
O10B0.15 (4)0.07 (2)0.11 (2)0.08 (3)0.09 (3)0.065 (18)
O11B0.13 (3)0.11 (3)0.16 (3)−0.04 (2)0.02 (2)0.02 (3)
Cl30.0446 (10)0.0509 (11)0.0708 (13)0.0079 (8)0.0019 (10)0.0164 (10)
O120.081 (5)0.200 (9)0.145 (8)0.023 (5)−0.040 (5)0.028 (7)
Cl40.0525 (10)0.0490 (10)0.0529 (11)0.0070 (8)0.0066 (9)0.0217 (9)
O200.051 (3)0.064 (3)0.051 (3)0.001 (2)−0.004 (2)0.033 (3)
O210.069 (3)0.081 (4)0.061 (3)0.017 (3)0.021 (3)0.022 (3)
Geometric parameters (Å, º) top
Mn1—N92.170 (6)N11—C221.338 (8)
Mn1—O12.182 (4)N12—C231.324 (7)
Mn1—N42.236 (4)N12—C241.340 (10)
Mn1—N82.254 (5)N13—C261.328 (8)
Mn1—N12.259 (5)N13—C231.345 (8)
Mn1—N52.271 (5)N14—C271.338 (8)
O1—H1A0.8400N14—C301.339 (7)
O1—H1B0.8401N15—C301.320 (7)
N1—C11.321 (8)N15—C291.345 (9)
N1—C41.338 (7)N16—C311.327 (7)
N2—C41.332 (7)N16—C321.346 (9)
N2—C31.335 (8)N17—C311.334 (7)
N3—C61.331 (8)N17—C341.354 (7)
N3—C51.339 (7)C19—C201.359 (9)
N4—C81.302 (8)C19—H190.9500
N4—C51.351 (7)C20—C211.369 (9)
N5—C121.330 (7)C20—H200.9500
N5—C91.334 (7)C21—H210.9500
N6—C121.330 (7)C22—C231.498 (9)
N6—C111.338 (8)C24—C251.355 (11)
N7—C141.327 (8)C24—H240.9500
N7—C131.328 (7)C25—C261.387 (9)
N8—C131.336 (7)C25—H250.9500
N8—C161.339 (8)C26—H260.9500
N9—C171.115 (8)C27—C281.376 (9)
C1—C21.397 (10)C27—H270.9500
C1—H10.9500C28—C291.362 (10)
C2—C31.366 (10)C28—H280.9500
C2—H20.9500C29—H290.9500
C3—H30.9500C30—C311.493 (9)
C4—C51.478 (8)C32—C331.365 (10)
C6—C71.354 (9)C32—H320.9500
C6—H60.9500C33—C341.376 (8)
C7—C81.397 (9)C33—H330.9500
C7—H70.9500C34—H340.9500
C8—H80.9500Cl1—O51.412 (5)
C9—C101.362 (9)Cl1—O71.422 (5)
C9—H90.9500Cl1—O41.431 (5)
C10—C111.361 (9)Cl1—O61.438 (5)
C10—H100.9500Cl2—O10B1.353 (18)
C11—H110.9500Cl2—O81.399 (5)
C12—C131.488 (8)Cl2—O11A1.401 (8)
C14—C151.383 (9)Cl2—O91.411 (5)
C14—H140.9500Cl2—O10A1.476 (8)
C15—C161.387 (8)Cl2—O11B1.53 (3)
C15—H150.9500Cl3—O121.360 (7)
C16—H160.9500Cl3—O15A1.373 (14)
C17—C181.464 (10)Cl3—O14B1.383 (13)
C18—H18A0.9800Cl3—O13A1.405 (11)
C18—H18B0.9800Cl3—O13B1.45 (2)
C18—H18C0.9800Cl3—O14A1.479 (12)
Mn2—O32.107 (4)Cl3—O15B1.58 (3)
Mn2—O22.174 (4)Cl4—O18A1.356 (15)
Mn2—N132.238 (5)Cl4—O19A1.37 (2)
Mn2—N102.267 (5)Cl4—O18B1.40 (2)
Mn2—N142.269 (5)Cl4—O16A1.419 (12)
Mn2—N172.272 (5)Cl4—O17B1.420 (13)
O2—H2A0.8400Cl4—O19B1.434 (17)
O2—H2B0.8400Cl4—O17A1.459 (15)
O3—H3A0.8400Cl4—O16B1.466 (13)
O3—H3B0.8401O20—H20A0.8400
N10—C221.330 (7)O20—H20B0.8400
N10—C191.341 (8)O21—H21A0.8402
N11—C211.311 (9)O21—H21B0.8401
N9—Mn1—O190.14 (19)C30—N14—Mn2117.1 (4)
N9—Mn1—N495.16 (19)C30—N15—C29115.6 (6)
O1—Mn1—N491.18 (17)C31—N16—C32115.5 (6)
N9—Mn1—N892.58 (19)C31—N17—C34116.9 (5)
O1—Mn1—N889.07 (16)C31—N17—Mn2117.1 (4)
N4—Mn1—N8172.26 (18)C34—N17—Mn2125.3 (4)
N9—Mn1—N185.1 (2)N10—C19—C20122.8 (6)
O1—Mn1—N1163.05 (16)N10—C19—H19118.6
N4—Mn1—N173.12 (18)C20—C19—H19118.6
N8—Mn1—N1107.36 (18)C19—C20—C21115.3 (7)
N9—Mn1—N5165.5 (2)C19—C20—H20122.3
O1—Mn1—N592.60 (17)C21—C20—H20122.3
N4—Mn1—N598.99 (18)N11—C21—C20124.9 (7)
N8—Mn1—N573.27 (18)N11—C21—H21117.6
N1—Mn1—N596.08 (17)C20—C21—H21117.6
Mn1—O1—H1A113.2N10—C22—N11125.7 (7)
Mn1—O1—H1B100.7N10—C22—C23116.1 (6)
H1A—O1—H1B114.1N11—C22—C23118.2 (6)
C1—N1—C4116.4 (6)N12—C23—N13126.4 (7)
C1—N1—Mn1127.0 (4)N12—C23—C22117.3 (6)
C4—N1—Mn1116.5 (4)N13—C23—C22116.3 (5)
C4—N2—C3116.1 (6)N12—C24—C25124.5 (7)
C6—N3—C5116.4 (5)N12—C24—H24117.7
C8—N4—C5116.5 (5)C25—C24—H24117.7
C8—N4—Mn1126.6 (4)C24—C25—C26116.1 (7)
C5—N4—Mn1116.5 (4)C24—C25—H25122.0
C12—N5—C9117.7 (5)C26—C25—H25122.0
C12—N5—Mn1115.6 (4)N13—C26—C25121.7 (7)
C9—N5—Mn1126.6 (4)N13—C26—H26119.1
C12—N6—C11115.1 (5)C25—C26—H26119.1
C14—N7—C13116.3 (5)N14—C27—C28121.4 (6)
C13—N8—C16117.3 (5)N14—C27—H27119.3
C13—N8—Mn1115.7 (4)C28—C27—H27119.3
C16—N8—Mn1125.5 (4)C29—C28—C27117.2 (7)
C17—N9—Mn1169.7 (6)C29—C28—H28121.4
N1—C1—C2121.8 (7)C27—C28—H28121.4
N1—C1—H1119.1N15—C29—C28122.8 (6)
C2—C1—H1119.1N15—C29—H29118.6
C3—C2—C1117.1 (7)C28—C29—H29118.6
C3—C2—H2121.4N15—C30—N14126.3 (6)
C1—C2—H2121.4N15—C30—C31117.3 (5)
N2—C3—C2122.3 (7)N14—C30—C31116.4 (5)
N2—C3—H3118.9N16—C31—N17126.2 (6)
C2—C3—H3118.9N16—C31—C30117.7 (6)
N2—C4—N1126.4 (6)N17—C31—C30116.1 (5)
N2—C4—C5117.2 (5)N16—C32—C33123.1 (6)
N1—C4—C5116.4 (5)N16—C32—H32118.4
N3—C5—N4124.8 (6)C33—C32—H32118.4
N3—C5—C4118.7 (5)C32—C33—C34117.3 (7)
N4—C5—C4116.5 (5)C32—C33—H33121.3
N3—C6—C7123.2 (6)C34—C33—H33121.3
N3—C6—H6118.4N17—C34—C33120.9 (6)
C7—C6—H6118.4N17—C34—H34119.6
C6—C7—C8115.9 (7)C33—C34—H34119.6
C6—C7—H7122.1O5—Cl1—O7110.5 (4)
C8—C7—H7122.1O5—Cl1—O4110.4 (3)
N4—C8—C7123.2 (6)O7—Cl1—O4107.9 (3)
N4—C8—H8118.4O5—Cl1—O6108.9 (3)
C7—C8—H8118.4O7—Cl1—O6109.3 (3)
N5—C9—C10120.7 (6)O4—Cl1—O6109.8 (3)
N5—C9—H9119.6O10B—Cl2—O8117.6 (10)
C10—C9—H9119.6O10B—Cl2—O11A62.5 (17)
C11—C10—C9117.7 (6)O8—Cl2—O11A111.9 (4)
C11—C10—H10121.2O10B—Cl2—O9127.2 (13)
C9—C10—H10121.2O8—Cl2—O9112.5 (4)
N6—C11—C10123.1 (6)O11A—Cl2—O9112.5 (5)
N6—C11—H11118.4O10B—Cl2—O10A48.5 (17)
C10—C11—H11118.4O8—Cl2—O10A106.0 (5)
N5—C12—N6125.6 (6)O11A—Cl2—O10A110.6 (6)
N5—C12—C13117.2 (5)O9—Cl2—O10A102.9 (5)
N6—C12—C13117.2 (5)O10B—Cl2—O11B100.7 (18)
N7—C13—N8125.7 (6)O8—Cl2—O11B90.8 (19)
N7—C13—C12117.7 (5)O9—Cl2—O11B94.1 (17)
N8—C13—C12116.6 (5)O10A—Cl2—O11B149.0 (19)
N7—C14—C15123.1 (6)O12—Cl3—O15A119.9 (8)
N7—C14—H14118.5O12—Cl3—O14B109.7 (7)
C15—C14—H14118.5O15A—Cl3—O14B76.6 (8)
C14—C15—C16116.4 (6)O12—Cl3—O13A105.4 (6)
C14—C15—H15121.8O15A—Cl3—O13A112.1 (7)
C16—C15—H15121.8O14B—Cl3—O13A132.3 (7)
N8—C16—C15121.2 (6)O12—Cl3—O13B131.8 (8)
N8—C16—H16119.4O15A—Cl3—O13B67.0 (9)
C15—C16—H16119.4O14B—Cl3—O13B117.8 (9)
N9—C17—C18179.5 (9)O13A—Cl3—O13B45.1 (8)
C17—C18—H18A109.5O12—Cl3—O14A106.8 (6)
C17—C18—H18B109.5O15A—Cl3—O14A111.6 (7)
H18A—C18—H18B109.5O13A—Cl3—O14A98.8 (7)
C17—C18—H18C109.5O13B—Cl3—O14A113.9 (8)
H18A—C18—H18C109.5O12—Cl3—O15B76.7 (10)
H18B—C18—H18C109.5O14B—Cl3—O15B100.7 (11)
O3—Mn2—O286.66 (17)O13A—Cl3—O15B118.2 (10)
O3—Mn2—N13101.24 (18)O13B—Cl3—O15B86.9 (12)
O2—Mn2—N1393.91 (19)O14A—Cl3—O15B140.8 (10)
O3—Mn2—N1090.61 (17)O18A—Cl4—O19A111.2 (10)
O2—Mn2—N10165.85 (17)O18A—Cl4—O18B56.8 (9)
N13—Mn2—N1072.99 (19)O19A—Cl4—O18B158.0 (12)
O3—Mn2—N14162.02 (18)O18A—Cl4—O16A103.1 (8)
O2—Mn2—N1485.53 (17)O19A—Cl4—O16A113.4 (10)
N13—Mn2—N1495.43 (18)O18B—Cl4—O16A88.2 (10)
N10—Mn2—N14100.74 (18)O18A—Cl4—O17B133.9 (8)
O3—Mn2—N1793.05 (18)O19A—Cl4—O17B69.2 (9)
O2—Mn2—N1799.04 (17)O18B—Cl4—O17B104.9 (10)
N13—Mn2—N17161.24 (19)O16A—Cl4—O17B119.3 (7)
N10—Mn2—N1794.97 (18)O18A—Cl4—O19B60.7 (8)
N14—Mn2—N1772.26 (18)O19A—Cl4—O19B50.7 (9)
Mn2—O2—H2A126.8O18B—Cl4—O19B112.8 (11)
Mn2—O2—H2B123.2O16A—Cl4—O19B128.6 (8)
H2A—O2—H2B105.2O17B—Cl4—O19B100.6 (8)
Mn2—O3—H3A116.4O18A—Cl4—O17A114.3 (9)
Mn2—O3—H3B124.8O19A—Cl4—O17A109.5 (10)
H3A—O3—H3B118.5O18B—Cl4—O17A66.3 (9)
C22—N10—C19116.1 (6)O16A—Cl4—O17A105.2 (8)
C22—N10—Mn2117.0 (4)O19B—Cl4—O17A126.2 (9)
C19—N10—Mn2126.9 (4)O18A—Cl4—O16B118.0 (8)
C21—N11—C22115.2 (6)O19A—Cl4—O16B85.3 (9)
C23—N12—C24114.6 (7)O18B—Cl4—O16B116.3 (10)
C26—N13—C23116.6 (5)O17B—Cl4—O16B108.1 (8)
C26—N13—Mn2126.0 (5)O19B—Cl4—O16B112.5 (9)
C23—N13—Mn2117.1 (4)O17A—Cl4—O16B114.6 (8)
C27—N14—C30116.6 (5)H20A—O20—H20B110.5
C27—N14—Mn2125.9 (4)H21A—O21—H21B85.1
N9—Mn1—N1—C186.1 (5)O3—Mn2—N10—C2297.0 (4)
O1—Mn1—N1—C1160.2 (6)O2—Mn2—N10—C2218.3 (9)
N4—Mn1—N1—C1−177.0 (6)N13—Mn2—N10—C22−4.6 (4)
N8—Mn1—N1—C1−5.1 (6)N14—Mn2—N10—C22−97.1 (4)
N5—Mn1—N1—C1−79.4 (5)N17—Mn2—N10—C22−169.9 (4)
N9—Mn1—N1—C4−89.4 (4)O3—Mn2—N10—C19−82.9 (5)
O1—Mn1—N1—C4−15.3 (9)O2—Mn2—N10—C19−161.6 (6)
N4—Mn1—N1—C47.6 (4)N13—Mn2—N10—C19175.6 (5)
N8—Mn1—N1—C4179.5 (4)N14—Mn2—N10—C1983.1 (5)
N5—Mn1—N1—C4105.1 (4)N17—Mn2—N10—C1910.3 (5)
N9—Mn1—N4—C8−97.9 (6)O3—Mn2—N13—C2693.6 (5)
O1—Mn1—N4—C8−7.6 (6)O2—Mn2—N13—C266.3 (5)
N1—Mn1—N4—C8178.9 (6)N10—Mn2—N13—C26−179.2 (5)
N5—Mn1—N4—C885.2 (6)N14—Mn2—N13—C26−79.6 (5)
N9—Mn1—N4—C574.7 (4)N17—Mn2—N13—C26−127.4 (6)
O1—Mn1—N4—C5164.9 (4)O3—Mn2—N13—C23−80.6 (4)
N1—Mn1—N4—C5−8.6 (4)O2—Mn2—N13—C23−168.0 (4)
N5—Mn1—N4—C5−102.3 (4)N10—Mn2—N13—C236.6 (4)
N9—Mn1—N5—C1219.3 (10)N14—Mn2—N13—C23106.2 (4)
O1—Mn1—N5—C12−81.4 (4)N17—Mn2—N13—C2358.3 (8)
N4—Mn1—N5—C12−173.0 (4)O3—Mn2—N14—C27−143.7 (6)
N8—Mn1—N5—C126.8 (4)O2—Mn2—N14—C27−79.1 (5)
N1—Mn1—N5—C12113.2 (4)N13—Mn2—N14—C2714.4 (5)
N9—Mn1—N5—C9−163.2 (8)N10—Mn2—N14—C2788.1 (5)
O1—Mn1—N5—C996.1 (5)N17—Mn2—N14—C27179.9 (6)
N4—Mn1—N5—C94.5 (5)O3—Mn2—N14—C3029.2 (9)
N8—Mn1—N5—C9−175.6 (6)O2—Mn2—N14—C3093.7 (4)
N1—Mn1—N5—C9−69.3 (5)N13—Mn2—N14—C30−172.7 (5)
N9—Mn1—N8—C13172.0 (4)N10—Mn2—N14—C30−99.1 (5)
O1—Mn1—N8—C1381.9 (4)N17—Mn2—N14—C30−7.2 (4)
N1—Mn1—N8—C13−102.3 (4)O3—Mn2—N17—C31−160.4 (4)
N5—Mn1—N8—C13−11.1 (4)O2—Mn2—N17—C31−73.3 (4)
N9—Mn1—N8—C166.4 (5)N13—Mn2—N17—C3159.8 (8)
O1—Mn1—N8—C16−83.7 (5)N10—Mn2—N17—C31108.8 (4)
N1—Mn1—N8—C1692.1 (5)N14—Mn2—N17—C319.1 (4)
N5—Mn1—N8—C16−176.7 (6)O3—Mn2—N17—C349.7 (5)
O1—Mn1—N9—C17−97 (4)O2—Mn2—N17—C3496.8 (5)
N4—Mn1—N9—C17−6 (4)N13—Mn2—N17—C34−130.2 (6)
N8—Mn1—N9—C17174 (4)N10—Mn2—N17—C34−81.2 (5)
N1—Mn1—N9—C1767 (4)N14—Mn2—N17—C34179.1 (5)
N5—Mn1—N9—C17162 (3)C22—N10—C19—C20−2.0 (9)
C4—N1—C1—C2−0.1 (10)Mn2—N10—C19—C20177.8 (5)
Mn1—N1—C1—C2−175.5 (5)N10—C19—C20—C211.9 (10)
N1—C1—C2—C30.9 (11)C22—N11—C21—C200.0 (10)
C4—N2—C3—C20.5 (10)C19—C20—C21—N11−0.8 (10)
C1—C2—C3—N2−1.1 (12)C19—N10—C22—N111.1 (9)
C3—N2—C4—N10.4 (9)Mn2—N10—C22—N11−178.7 (5)
C3—N2—C4—C5−178.5 (6)C19—N10—C22—C23−177.8 (5)
C1—N1—C4—N2−0.6 (9)Mn2—N10—C22—C232.4 (7)
Mn1—N1—C4—N2175.3 (5)C21—N11—C22—N10−0.1 (9)
C1—N1—C4—C5178.3 (5)C21—N11—C22—C23178.8 (5)
Mn1—N1—C4—C5−5.8 (7)C24—N12—C23—N132.7 (10)
C6—N3—C5—N4−1.6 (9)C24—N12—C23—C22−176.8 (6)
C6—N3—C5—C4178.7 (5)C26—N13—C23—N12−1.9 (9)
C8—N4—C5—N32.3 (9)Mn2—N13—C23—N12172.9 (5)
Mn1—N4—C5—N3−171.0 (4)C26—N13—C23—C22177.5 (5)
C8—N4—C5—C4−178.0 (6)Mn2—N13—C23—C22−7.7 (7)
Mn1—N4—C5—C48.7 (7)N10—C22—C23—N12−177.0 (5)
N2—C4—C5—N3−3.2 (8)N11—C22—C23—N124.0 (8)
N1—C4—C5—N3177.8 (5)N10—C22—C23—N133.5 (8)
N2—C4—C5—N4177.1 (5)N11—C22—C23—N13−175.5 (5)
N1—C4—C5—N4−1.9 (8)C23—N12—C24—C25−0.5 (11)
C5—N3—C6—C7−0.7 (10)N12—C24—C25—C26−2.1 (12)
N3—C6—C7—C81.9 (11)C23—N13—C26—C25−1.1 (9)
C5—N4—C8—C7−0.9 (10)Mn2—N13—C26—C25−175.3 (5)
Mn1—N4—C8—C7171.6 (5)C24—C25—C26—N132.9 (10)
C6—C7—C8—N4−1.1 (11)C30—N14—C27—C280.3 (9)
C12—N5—C9—C10−0.5 (9)Mn2—N14—C27—C28173.2 (5)
Mn1—N5—C9—C10−178.0 (5)N14—C27—C28—C290.7 (11)
N5—C9—C10—C110.3 (10)C30—N15—C29—C282.4 (11)
C12—N6—C11—C10−1.1 (10)C27—C28—C29—N15−2.1 (11)
C9—C10—C11—N60.6 (11)C29—N15—C30—N14−1.3 (10)
C9—N5—C12—N6−0.1 (9)C29—N15—C30—C31−179.7 (6)
Mn1—N5—C12—N6177.7 (5)C27—N14—C30—N150.0 (10)
C9—N5—C12—C13180.0 (5)Mn2—N14—C30—N15−173.5 (5)
Mn1—N5—C12—C13−2.3 (7)C27—N14—C30—C31178.5 (5)
C11—N6—C12—N50.8 (9)Mn2—N14—C30—C314.9 (7)
C11—N6—C12—C13−179.2 (6)C32—N16—C31—N170.9 (10)
C14—N7—C13—N8−0.3 (9)C32—N16—C31—C30−179.8 (6)
C14—N7—C13—C12−179.4 (6)C34—N17—C31—N16−1.3 (9)
C16—N8—C13—N71.6 (9)Mn2—N17—C31—N16169.6 (5)
Mn1—N8—C13—N7−165.2 (5)C34—N17—C31—C30179.4 (5)
C16—N8—C13—C12−179.4 (5)Mn2—N17—C31—C30−9.7 (7)
Mn1—N8—C13—C1213.8 (7)N15—C30—C31—N162.4 (9)
N5—C12—C13—N7171.4 (5)N14—C30—C31—N16−176.2 (6)
N6—C12—C13—N7−8.6 (8)N15—C30—C31—N17−178.2 (6)
N5—C12—C13—N8−7.7 (8)N14—C30—C31—N173.2 (8)
N6—C12—C13—N8172.3 (5)C31—N16—C32—C331.4 (10)
C13—N7—C14—C15−2.3 (10)N16—C32—C33—C34−3.1 (11)
N7—C14—C15—C163.5 (10)C31—N17—C34—C33−0.6 (9)
C13—N8—C16—C15−0.2 (9)Mn2—N17—C34—C33−170.6 (5)
Mn1—N8—C16—C15165.2 (5)C32—C33—C34—N172.6 (10)
C14—C15—C16—N8−2.1 (10)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···N6i0.842.493.139 (6)135
O1—H1A···N7i0.842.152.923 (6)152
O1—H1B···O21i0.841.892.695 (7)160
O2—H2A···N15ii0.842.593.244 (7)136
O2—H2A···N16ii0.842.253.012 (7)151
O2—H2B···O11Aiii0.842.012.809 (10)158
O3—H3A···O200.841.792.614 (6)166
O3—H3B···O4iii0.842.072.861 (6)157
O20—H20A···N2iv0.842.082.903 (7)168
O20—H20A···N3iv0.842.563.066 (7)120
O20—H20B···O60.842.082.871 (7)157
O21—H21A···O12v0.842.433.126 (12)141
O21—H21B···O16Aiv0.842.072.904 (13)172
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+2, −z; (iii) −x+1, −y+1, −z; (iv) x+1, y, z; (v) −x+1, −y, −z+1.

Experimental details

Crystal data
Chemical formula[Mn(C2H3N)(C8H6N4)2(H2O)][Mn(C8H6N4)2(H2O)2](ClO4)4·2H2O
Mr1271.49
Crystal system, space groupTriclinic, P1
Temperature (K)200
a, b, c (Å)12.0386 (5), 13.1878 (6), 17.5378 (8)
α, β, γ (°)111.201 (3), 104.147 (3), 91.419 (2)
V (Å3)2497.37 (19)
Z2
Radiation typeMo Kα
µ (mm−1)0.82
Crystal size (mm)0.24 × 0.21 × 0.13
Data collection
DiffractometerBruker SMART 1000 CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.765, 0.899
No. of measured, independent and
observed [I > 2σ(I)] reflections		18759, 12197, 5402
Rint0.052
(sin θ/λ)max (Å−1)0.667
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.082, 0.253, 1.01
No. of reflections12197
No. of parameters718
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)1.01, −0.61

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009).

Selected geometric parameters (Å, º) top
Mn1—N92.170 (6)Mn2—O32.107 (4)
Mn1—O12.182 (4)Mn2—O22.174 (4)
Mn1—N42.236 (4)Mn2—N132.238 (5)
Mn1—N82.254 (5)Mn2—N102.267 (5)
Mn1—N12.259 (5)Mn2—N142.269 (5)
Mn1—N52.271 (5)Mn2—N172.272 (5)
N4—Mn1—N173.12 (18)N13—Mn2—N1072.99 (19)
N8—Mn1—N573.27 (18)N14—Mn2—N1772.26 (18)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···N6i0.842.493.139 (6)135
O1—H1A···N7i0.842.152.923 (6)152
O1—H1B···O21i0.841.892.695 (7)160
O2—H2A···N15ii0.842.593.244 (7)136
O2—H2A···N16ii0.842.253.012 (7)151
O2—H2B···O11Aiii0.842.012.809 (10)158
O3—H3A···O200.841.792.614 (6)166
O3—H3B···O4iii0.842.072.861 (6)157
O20—H20A···N2iv0.842.082.903 (7)168
O20—H20A···N3iv0.842.563.066 (7)120
O20—H20B···O60.842.082.871 (7)157
O21—H21A···O12v0.842.433.126 (12)141
O21—H21B···O16Aiv0.842.072.904 (13)172
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+2, −z; (iii) −x+1, −y+1, −z; (iv) x+1, y, z; (v) −x+1, −y, −z+1.
 

Acknowledgements

This work was supported by the Priority Research Centers Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education, Science and Technology (2010–0029626).

References

First citationBruker (2000). SADABS, SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
 First citationFarrugia, L. J. (1997). J. Appl. Cryst. 30, 565.  CrossRef IUCr Journals Google Scholar
 First citationHa, K. (2011). Acta Cryst. E67, m474.  Web of Science CSD CrossRef IUCr Journals Google Scholar
 First citationHong, D. M., Wei, H. H., Gan, L. L., Lee, G. H. & Wang, Y. (1996). Polyhedron, 15, 2335–2340.  CSD CrossRef CAS Web of Science Google Scholar
 First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
 First citationSmith, J. A., Galán-Mascarós, J.-R., Clérac, R., Sun, J.-S., Ouyang, X. & Dunbar, K. R. (2001). Polyhedron, 20, 1727–1734.  CSD CrossRef CAS Google Scholar
 First citationSpek, A. L. (2009). Acta Cryst. D65, 148–155.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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Journal logoCRYSTALLOGRAPHIC
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ISSN: 2056-9890
Volume 67| Part 6| June 2011| Pages m656-m657
doi:10.1107/S1600536811015388
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