A binuclear manganese(II) complex: di-μ-acetato-κ4O:O′-bis­[bis­(1,10-phenanthroline-κ2N,N′)manganese(II)] bis­(perchlorate)

Niu, X.-L.; Dou, J.-M.; Hu, C.-W.; Li, D.-C.; Wang, D.-Q.

doi:10.1107/S1600536805027479

Buy article online - an online subscription or single-article purchase is required to access this article.

A binuclear manganese(II) complex: di-μ-acetato-κ⁴O:O′-bis[bis(1,10-phenanthroline-κ²N,N′)manganese(II)] bis(perchlorate)

X.-L. Niu, J.-M. Dou, C.-W. Hu, D.-C. Li and D.-Q. Wang

The title binuclear manganese(II) complex, [Mn₂(C₂H₃O₂)₂(C₁₂H₈N₂)₄](ClO₄)₂, has been synthesized by the reaction of manganese(II) acetate and tetra-n-butylammonium manganate(VII) with 1,10-phenanthroline in a mixed solvent of acetic acid, ethanol and pyridine. In the centrosymmetric cation, the two Mn^II atoms are linked to each other by the four O atoms of two acetate ions. Each Mn^II atom adopts a six-coordinate geometry and the six coordinating atoms form a distorted octahedron.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805027479/is6113sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805027479/is6113Isup2.hkl Contains datablock I

CCDC reference: 268810

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.005 Å
R factor = 0.044
wR factor = 0.132
Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found





Alert level C
HYDTR01_ALERT_1_C  The hydrogen treatment should only be one of the following
            keywords
            *  refall
            *  refxyz
            *  refU
            *  noref
            *  undef
            *  constr
            *  none
            *  mixed
            Hydrogen treatment given as geom
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT230_ALERT_2_C Hirshfeld Test Diff for    C5     -   C6      ..       5.04 su
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C21
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C25
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Cl1

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

The photosystem II oxygen-evolving complex (PSII OEC) found in the chloroplast thylakoid membranes of higher plants and algae catalyzes the splitting of water. The process is generally believed to occur on four or two manganese aggregates (Arulsamy et al., 1994). Owing to their relevance to the catalytic center of the photosystem, binuclear manganese complexes have become the subjects of intensive research. Some binuclear manganese complexes have been synthesized, such as two O atoms bridge (Tan et al., 1996; Goodwin et al., 2004), O atom and Ac⁻ (CH₃COO⁻) mixed bridge (Arulsamy et al., 1994; Oberhausen et al., 1993; Sheats et al., 1987; Wieghardt et al., 1985), isophthalate bridge (Tan et al., 1997) and two Ac⁻ anions bridge binuclear manganese complexes (Oshio et al., 1993; Ishida et al., 2001; Iriller et al., 2002). We report here the title binuclear manganese(II) complex [Mn₂(µ-Ac⁻)₂(phen)₄]·(ClO₄)₂ (phen = 1,10-phenanthroline), (I).

The molecular structure and the packing diagram of (I) in are shown in Figs. 1 and 2, respectively. The manganese complex is a centrosymmetric anion with an Mn···Mn separation of 4.588 (2) Å. The two Mn^II atoms are bridged by two Ac⁻ ligends. Four N atoms of two phen ligands and two O atoms from two Ac⁻ anions coordinate each Mn^II atom to form a distorted octahedron. Atoms N1, N2, O1 and N4 form the equatorial plane, the N2—Mn1—N1, N1—Mn1—O1, O1—Mn1—N4 and N4—Mn1—N2 bond angles being 72.62 (9), 162.44 (9), 102.61 (8) and 163.76 (9)°, respectively. Atoms N3 and O2 lie in the axial positions with an N3—Mn1—O2 angle of 166.39 (8)°.

Experimental top

Mn(Ac⁻)₂·4H₂O (0.815 mmol) was dissolved in a mixed solvent (3 ml pyridine, 12 ml acetic acid, 20 ml EtOH); fresh (C₄H₉)₄NMnO₄ (0.315 mmol) was added slowly with continuous stirring and then NaClO₄ (0.565 mmol) was added. After 1 h, solid phen (2.0 mmol) was added to the reaction solution with continuous stirring. The final mixture was filtered, and the filtrate was allowed to layer with ether. After three weeks, a red pole-shaped [yellow block?] crystal of (I) was obtained. M.p. >573 K. Analysis calculated for C₅₂H₃₈Cl₂Mn₂N₈O₁₂: C 54.37, H 3.31, N 9.76%; found: C 54.23, H 3.25, N 9.71%. Selected FT–IR (KBr, cm⁻¹): υ 3072 (m), 3000 (s), 1625 (m), 1567 (s), 1516 (s), 1494 (m), 1094 (s), 865 (w), 848 (s), 770 (w), 728 (s).

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Figures top

	Fig. 1. The title complex, with the atomic numbering scheme and displacement ellipsoids at the 30% probability level. H atoms have been omitted for clarity.
	Fig. 2. The packing of the title complex viewed along the a axis. H atoms have been omitted.

di-µ-acetato-κ⁴O:O'-bis[bis(1,10-phenanthroline-κ²N,N')manganese(II)] bis(perchlorate) top

Crystal data top

[Mn₂(C₂H₃O₂)₂(C₁₂H₈N₂)₄](ClO₄)₂	D_x = 1.506 Mg m⁻³
M_r = 1147.68	Melting point > 300 K
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 9.5474 (12) Å	Cell parameters from 5713 reflections
b = 14.1858 (18) Å	θ = 2.6–27.6°
c = 18.802 (2) Å	µ = 0.68 mm⁻¹
β = 96.224 (2)°	T = 293 K
V = 2531.5 (5) Å³	Block, yellow
Z = 2	0.45 × 0.38 × 0.31 mm
F(000) = 1172

Data collection top

Siemens SMART CCD area-detector diffractometer	4444 independent reflections
Radiation source: fine-focus sealed tube	3681 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.031
ϕ and ω scans	θ_max = 25.0°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→11
T_min = 0.751, T_max = 0.818	k = −16→13
12909 measured reflections	l = −22→22

Refinement top

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)] = 0.044	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.132	H-atom parameters constrained
S = 1.01	w = 1/[σ²(F_o²) + (0.0794P)² + 1.191P] where P = (F_o² + 2F_c²)/3
4444 reflections	(Δ/σ)_max < 0.001
344 parameters	Δρ_max = 0.64 e Å⁻³
0 restraints	Δρ_min = −0.33 e Å⁻³

Crystal data top

[Mn₂(C₂H₃O₂)₂(C₁₂H₈N₂)₄](ClO₄)₂	V = 2531.5 (5) Å³
M_r = 1147.68	Z = 2
Monoclinic, P2₁/c	Mo Kα radiation
a = 9.5474 (12) Å	µ = 0.68 mm⁻¹
b = 14.1858 (18) Å	T = 293 K
c = 18.802 (2) Å	0.45 × 0.38 × 0.31 mm
β = 96.224 (2)°

Data collection top

Siemens SMART CCD area-detector diffractometer	4444 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3681 reflections with I > 2σ(I)
T_min = 0.751, T_max = 0.818	R_int = 0.031
12909 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.044	0 restraints
wR(F²) = 0.132	H-atom parameters constrained
S = 1.01	Δρ_max = 0.64 e Å⁻³
4444 reflections	Δρ_min = −0.33 e Å⁻³
344 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

	x	y	z	U_iso*/U_eq
Mn1	0.48252 (4)	0.15506 (3)	0.032485 (19)	0.04150 (16)
Cl1	0.03229 (9)	0.37814 (6)	0.17235 (5)	0.0707 (3)
N1	0.3818 (3)	0.29822 (16)	0.00123 (12)	0.0525 (6)
N2	0.6458 (3)	0.24196 (16)	−0.01692 (12)	0.0538 (6)
N3	0.5281 (2)	0.21402 (15)	0.14617 (11)	0.0438 (5)
N4	0.3037 (3)	0.10828 (17)	0.09445 (12)	0.0540 (6)
O1	0.6298 (2)	0.04504 (13)	0.05213 (10)	0.0516 (5)
O2	0.3895 (2)	0.10793 (13)	−0.06989 (9)	0.0572 (5)
O3	−0.0446 (4)	0.3325 (3)	0.1156 (2)	0.1570 (17)
O4	0.1779 (3)	0.35989 (19)	0.17173 (15)	0.0811 (7)
O5	−0.0092 (4)	0.3485 (3)	0.2389 (2)	0.1319 (14)
O6	0.0119 (4)	0.4779 (2)	0.1681 (2)	0.1208 (11)
C1	0.2537 (4)	0.3264 (2)	0.01140 (19)	0.0703 (9)
H1	0.2001	0.2892	0.0389	0.084*
C2	0.1952 (5)	0.4109 (3)	−0.0179 (2)	0.0918 (14)
H2	0.1045	0.4289	−0.0100	0.110*
C3	0.2732 (6)	0.4653 (3)	−0.0576 (2)	0.0958 (15)
H3	0.2355	0.5212	−0.0772	0.115*
C4	0.4084 (5)	0.4390 (2)	−0.06941 (18)	0.0786 (12)
C5	0.4606 (4)	0.35334 (18)	−0.03781 (15)	0.0570 (8)
C6	0.5988 (4)	0.3231 (2)	−0.04834 (15)	0.0547 (7)
C7	0.6839 (5)	0.3771 (2)	−0.09080 (17)	0.0759 (11)
C8	0.8167 (5)	0.3440 (3)	−0.0992 (2)	0.0936 (14)
H8	0.8746	0.3776	−0.1269	0.112*
C9	0.8632 (4)	0.2624 (4)	−0.0672 (2)	0.0960 (13)
H9	0.9525	0.2393	−0.0729	0.115*
C10	0.7755 (4)	0.2142 (3)	−0.0261 (2)	0.0720 (9)
H10	0.8092	0.1591	−0.0035	0.086*
C11	0.4992 (7)	0.4902 (3)	−0.1130 (2)	0.0986 (17)
H11	0.4657	0.5457	−0.1350	0.118*
C12	0.6265 (7)	0.4619 (3)	−0.1227 (2)	0.0975 (16)
H12	0.6804	0.4977	−0.1509	0.117*
C13	0.6391 (3)	0.2643 (2)	0.17166 (15)	0.0522 (7)
H13	0.7111	0.2737	0.1428	0.063*
C14	0.6526 (3)	0.3038 (2)	0.23998 (16)	0.0602 (8)
H14	0.7326	0.3382	0.2562	0.072*
C15	0.5490 (3)	0.2917 (2)	0.28235 (15)	0.0581 (8)
H15	0.5565	0.3188	0.3276	0.070*
C16	0.4295 (3)	0.23786 (19)	0.25805 (13)	0.0476 (6)
C17	0.4250 (3)	0.20005 (17)	0.18895 (13)	0.0410 (6)
C18	0.3074 (3)	0.14250 (18)	0.16192 (14)	0.0454 (6)
C19	0.2001 (3)	0.1237 (2)	0.20575 (16)	0.0563 (7)
C20	0.0901 (4)	0.0656 (3)	0.1780 (2)	0.0811 (11)
H20	0.0188	0.0498	0.2057	0.097*
C21	0.0874 (4)	0.0321 (3)	0.1100 (2)	0.0965 (14)
H21	0.0127	−0.0051	0.0906	0.116*
C22	0.1962 (4)	0.0539 (3)	0.07023 (19)	0.0801 (11)
H22	0.1940	0.0292	0.0243	0.096*
C23	0.3173 (3)	0.2200 (2)	0.29973 (14)	0.0568 (7)
H23	0.3190	0.2472	0.3448	0.068*
C24	0.2096 (4)	0.1650 (2)	0.27562 (16)	0.0630 (8)
H24	0.1389	0.1532	0.3048	0.076*
C25	0.6348 (3)	−0.02586 (18)	0.09172 (13)	0.0446 (6)
C26	0.6739 (4)	−0.0126 (2)	0.17081 (16)	0.0753 (10)
H26A	0.5900	−0.0027	0.1938	0.113*
H26B	0.7346	0.0411	0.1787	0.113*
H26C	0.7218	−0.0678	0.1904	0.113*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.0545 (3)	0.0347 (2)	0.0354 (2)	−0.00482 (16)	0.00554 (17)	0.00263 (15)
Cl1	0.0550 (5)	0.0691 (5)	0.0876 (6)	0.0028 (4)	0.0054 (4)	0.0115 (4)
N1	0.0657 (15)	0.0389 (12)	0.0498 (13)	0.0029 (11)	−0.0076 (11)	−0.0070 (10)
N2	0.0643 (16)	0.0470 (13)	0.0497 (13)	−0.0127 (11)	0.0045 (11)	0.0060 (11)
N3	0.0512 (13)	0.0391 (11)	0.0405 (11)	−0.0021 (9)	0.0023 (9)	0.0014 (9)
N4	0.0601 (14)	0.0561 (14)	0.0467 (13)	−0.0170 (12)	0.0095 (11)	−0.0075 (11)
O1	0.0663 (12)	0.0409 (10)	0.0479 (10)	0.0019 (9)	0.0079 (9)	0.0083 (8)
O2	0.0910 (15)	0.0383 (11)	0.0386 (10)	−0.0012 (10)	−0.0096 (9)	0.0019 (8)
O3	0.104 (3)	0.202 (4)	0.160 (4)	−0.051 (3)	−0.008 (2)	−0.056 (3)
O4	0.0597 (14)	0.0900 (18)	0.0942 (18)	0.0091 (12)	0.0109 (13)	0.0184 (14)
O5	0.096 (2)	0.165 (4)	0.143 (3)	0.015 (2)	0.051 (2)	0.057 (3)
O6	0.127 (3)	0.082 (2)	0.156 (3)	0.0319 (18)	0.026 (2)	0.019 (2)
C1	0.074 (2)	0.061 (2)	0.071 (2)	0.0090 (17)	−0.0110 (17)	−0.0186 (16)
C2	0.087 (3)	0.073 (3)	0.106 (3)	0.029 (2)	−0.035 (2)	−0.031 (2)
C3	0.131 (4)	0.049 (2)	0.092 (3)	0.016 (2)	−0.055 (3)	−0.011 (2)
C4	0.128 (3)	0.0372 (16)	0.0594 (19)	0.0003 (19)	−0.040 (2)	−0.0032 (14)
C5	0.092 (2)	0.0329 (14)	0.0408 (14)	−0.0097 (14)	−0.0183 (14)	0.0004 (11)
C6	0.079 (2)	0.0409 (15)	0.0418 (14)	−0.0196 (14)	−0.0043 (14)	0.0009 (12)
C7	0.117 (3)	0.059 (2)	0.0482 (17)	−0.043 (2)	−0.0051 (19)	0.0080 (15)
C8	0.101 (3)	0.103 (3)	0.080 (3)	−0.050 (3)	0.023 (2)	0.007 (2)
C9	0.074 (3)	0.114 (4)	0.102 (3)	−0.030 (2)	0.023 (2)	0.005 (3)
C10	0.062 (2)	0.074 (2)	0.081 (2)	−0.0114 (17)	0.0158 (17)	0.0067 (18)
C11	0.180 (5)	0.0388 (19)	0.066 (2)	−0.026 (3)	−0.040 (3)	0.0239 (17)
C12	0.159 (5)	0.065 (3)	0.064 (2)	−0.046 (3)	−0.012 (3)	0.0191 (19)
C13	0.0530 (16)	0.0508 (16)	0.0525 (16)	−0.0042 (13)	0.0038 (13)	0.0004 (13)
C14	0.0620 (19)	0.0602 (19)	0.0548 (17)	−0.0080 (15)	−0.0098 (14)	−0.0076 (15)
C15	0.071 (2)	0.0590 (18)	0.0408 (14)	0.0046 (15)	−0.0075 (14)	−0.0056 (13)
C16	0.0613 (17)	0.0445 (15)	0.0356 (13)	0.0111 (13)	−0.0013 (12)	0.0038 (11)
C17	0.0500 (15)	0.0354 (13)	0.0369 (12)	0.0040 (11)	0.0016 (11)	0.0054 (10)
C18	0.0557 (16)	0.0427 (14)	0.0387 (13)	0.0000 (11)	0.0085 (11)	0.0051 (11)
C19	0.0629 (18)	0.0588 (17)	0.0487 (16)	−0.0061 (14)	0.0132 (13)	0.0070 (13)
C20	0.074 (2)	0.100 (3)	0.074 (2)	−0.033 (2)	0.0283 (18)	−0.004 (2)
C21	0.089 (3)	0.117 (3)	0.088 (3)	−0.059 (3)	0.028 (2)	−0.029 (2)
C22	0.086 (2)	0.090 (3)	0.067 (2)	−0.040 (2)	0.0233 (18)	−0.0246 (19)
C23	0.074 (2)	0.0631 (18)	0.0338 (13)	0.0098 (16)	0.0059 (13)	0.0042 (13)
C24	0.072 (2)	0.075 (2)	0.0445 (16)	0.0077 (17)	0.0201 (15)	0.0118 (15)
C25	0.0535 (16)	0.0412 (15)	0.0380 (13)	0.0013 (12)	0.0001 (11)	0.0028 (11)
C26	0.120 (3)	0.0570 (19)	0.0439 (16)	−0.0063 (19)	−0.0151 (17)	−0.0021 (14)

Geometric parameters (Å, º) top

Mn1—O1	2.1061 (19)	C8—H8	0.9300
Mn1—O2	2.1376 (18)	C9—C10	1.381 (5)
Mn1—N2	2.264 (2)	C9—H9	0.9300
Mn1—N4	2.268 (2)	C10—H10	0.9300
Mn1—N3	2.293 (2)	C11—C12	1.312 (7)
Mn1—N1	2.296 (2)	C11—H11	0.9300
Cl1—O3	1.388 (4)	C12—H12	0.9300
Cl1—O4	1.416 (3)	C13—C14	1.394 (4)
Cl1—O5	1.417 (3)	C13—H13	0.9300
Cl1—O6	1.430 (3)	C14—C15	1.346 (4)
N1—C1	1.320 (4)	C14—H14	0.9300
N1—C5	1.355 (4)	C15—C16	1.407 (4)
N2—C10	1.329 (4)	C15—H15	0.9300
N2—C6	1.348 (4)	C16—C17	1.402 (4)
N3—C13	1.324 (3)	C16—C23	1.417 (4)
N3—C17	1.351 (3)	C17—C18	1.436 (4)
N4—C22	1.325 (4)	C18—C19	1.408 (4)
N4—C18	1.355 (3)	C19—C20	1.391 (5)
O1—C25	1.249 (3)	C19—C24	1.432 (4)
O2—C25ⁱ	1.248 (3)	C20—C21	1.361 (5)
C1—C2	1.409 (5)	C20—H20	0.9300
C1—H1	0.9300	C21—C22	1.379 (5)
C2—C3	1.352 (6)	C21—H21	0.9300
C2—H2	0.9300	C22—H22	0.9300
C3—C4	1.385 (7)	C23—C24	1.330 (5)
C3—H3	0.9300	C23—H23	0.9300
C4—C5	1.419 (4)	C24—H24	0.9300
C4—C11	1.451 (7)	C25—O2ⁱ	1.248 (3)
C5—C6	1.422 (5)	C25—C26	1.505 (4)
C6—C7	1.423 (5)	C26—H26A	0.9600
C7—C8	1.377 (6)	C26—H26B	0.9600
C7—C12	1.426 (6)	C26—H26C	0.9600
C8—C9	1.358 (6)

O1—Mn1—O2	97.49 (8)	C7—C8—H8	120.0
O1—Mn1—N2	89.96 (8)	C8—C9—C10	118.8 (4)
O2—Mn1—N2	92.18 (8)	C8—C9—H9	120.6
O1—Mn1—N4	102.61 (8)	C10—C9—H9	120.6
O2—Mn1—N4	96.25 (8)	N2—C10—C9	123.8 (4)
N2—Mn1—N4	163.76 (9)	N2—C10—H10	118.1
O1—Mn1—N3	92.94 (7)	C9—C10—H10	118.1
O2—Mn1—N3	166.39 (8)	C12—C11—C4	123.0 (4)
N2—Mn1—N3	96.57 (8)	C12—C11—H11	118.5
N4—Mn1—N3	72.84 (8)	C4—C11—H11	118.5
O1—Mn1—N1	162.44 (9)	C11—C12—C7	121.3 (4)
O2—Mn1—N1	85.68 (7)	C11—C12—H12	119.3
N2—Mn1—N1	72.62 (9)	C7—C12—H12	119.3
N4—Mn1—N1	94.16 (9)	N3—C13—C14	122.7 (3)
N3—Mn1—N1	87.00 (8)	N3—C13—H13	118.7
O3—Cl1—O4	110.3 (2)	C14—C13—H13	118.7
O3—Cl1—O5	111.4 (3)	C15—C14—C13	119.6 (3)
O4—Cl1—O5	108.78 (19)	C15—C14—H14	120.2
O3—Cl1—O6	111.2 (3)	C13—C14—H14	120.2
O4—Cl1—O6	107.97 (19)	C14—C15—C16	119.9 (3)
O5—Cl1—O6	107.1 (2)	C14—C15—H15	120.0
C1—N1—C5	118.7 (3)	C16—C15—H15	120.0
C1—N1—Mn1	126.9 (2)	C17—C16—C15	116.8 (3)
C5—N1—Mn1	114.0 (2)	C17—C16—C23	119.7 (3)
C10—N2—C6	117.8 (3)	C15—C16—C23	123.5 (3)
C10—N2—Mn1	125.8 (2)	N3—C17—C16	123.0 (2)
C6—N2—Mn1	115.7 (2)	N3—C17—C18	117.7 (2)
C13—N3—C17	118.0 (2)	C16—C17—C18	119.3 (2)
C13—N3—Mn1	126.70 (18)	N4—C18—C19	122.2 (3)
C17—N3—Mn1	115.14 (16)	N4—C18—C17	118.3 (2)
C22—N4—C18	118.1 (3)	C19—C18—C17	119.4 (2)
C22—N4—Mn1	126.3 (2)	C20—C19—C18	117.4 (3)
C18—N4—Mn1	115.58 (18)	C20—C19—C24	123.8 (3)
C25—O1—Mn1	133.10 (18)	C18—C19—C24	118.8 (3)
C25ⁱ—O2—Mn1	129.23 (16)	C21—C20—C19	119.8 (3)
N1—C1—C2	122.4 (4)	C21—C20—H20	120.1
N1—C1—H1	118.8	C19—C20—H20	120.1
C2—C1—H1	118.8	C20—C21—C22	119.5 (3)
C3—C2—C1	118.9 (4)	C20—C21—H21	120.3
C3—C2—H2	120.6	C22—C21—H21	120.3
C1—C2—H2	120.6	N4—C22—C21	123.0 (3)
C2—C3—C4	120.8 (4)	N4—C22—H22	118.5
C2—C3—H3	119.6	C21—C22—H22	118.5
C4—C3—H3	119.6	C24—C23—C16	121.3 (3)
C3—C4—C5	117.1 (4)	C24—C23—H23	119.4
C3—C4—C11	125.4 (4)	C16—C23—H23	119.4
C5—C4—C11	117.5 (4)	C23—C24—C19	121.5 (3)
N1—C5—C4	122.0 (4)	C23—C24—H24	119.3
N1—C5—C6	118.7 (2)	C19—C24—H24	119.3
C4—C5—C6	119.3 (3)	O2ⁱ—C25—O1	124.1 (2)
N2—C6—C5	117.8 (3)	O2ⁱ—C25—C26	117.3 (2)
N2—C6—C7	121.5 (3)	O1—C25—C26	118.5 (2)
C5—C6—C7	120.7 (3)	C25—C26—H26A	109.5
C8—C7—C6	118.0 (4)	C25—C26—H26B	109.5
C8—C7—C12	123.8 (4)	H26A—C26—H26B	109.5
C6—C7—C12	118.2 (4)	C25—C26—H26C	109.5
C9—C8—C7	120.1 (4)	H26A—C26—H26C	109.5
C9—C8—H8	120.0	H26B—C26—H26C	109.5

Symmetry code: (i) −x+1, −y, −z.

Experimental details

Crystal data
Chemical formula	[Mn₂(C₂H₃O₂)₂(C₁₂H₈N₂)₄](ClO₄)₂
M_r	1147.68
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	9.5474 (12), 14.1858 (18), 18.802 (2)
β (°)	96.224 (2)
V (Å³)	2531.5 (5)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.68
Crystal size (mm)	0.45 × 0.38 × 0.31

Data collection
Diffractometer	Siemens SMART CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.751, 0.818
No. of measured, independent and observed [I > 2σ(I)] reflections	12909, 4444, 3681
R_int	0.031
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.044, 0.132, 1.01
No. of reflections	4444
No. of parameters	344
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.64, −0.33

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.

E-mail address*
Repeat e-mail address* (for error checking)

Format*	PDF (US $40)
	HTML (US $40)
	PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number (non-UK EC countries only)
Country*

Terms and conditions of use
Contact us

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page