Di-μ-acetato-κ⁴O:O′-bis­[bis­(2,2′-bipyridine-κ²N,N′)manganese(II)] bis­(perchlorate)

In the binuclear title manganese(II) complex, [Mn₂(C₂H₃O₂)₂(C₁₀H₈N₂)₄](ClO₄)₂, the Mn atoms are six-coordinate in a distorted octa­hedral coordination geometry. The two Mn atoms are bridged by two acetate groups to form a dimeric cation. The complex forms chains through π–π stacking inter­actions.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.052
• wR factor = 0.143
• Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C21
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Cl1
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          8

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

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

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Computing details

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

Di-µ-acetato-κ⁴O:O'-bis[bis(2,2'-bipyridine-κ²N,N')manganese(II)] bis(perchlorate)

Crystal data

[Mn2(C2H3O2)2(C10H8N2)4](ClO4)2	Z = 1
Mr = 1051.60	F(000) = 538
Triclinic, P1	Dx = 1.529 Mg m^−3
a = 10.436 (3) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.542 (3) Å	Cell parameters from 1539 reflections
c = 11.756 (4) Å	θ = 2.5–21.7°
α = 78.135 (4)°	µ = 0.74 mm^−1
β = 73.553 (4)°	T = 298 K
γ = 67.874 (4)°	Rod, yellow
V = 1141.8 (6) Å^3	0.39 × 0.31 × 0.25 mm

Data collection

Siemens SMART CCD area-detector diffractometer	3968 independent reflections
Radiation source: fine-focus sealed tube	2533 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.026
φ and ω scans	θmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→10
Tmin = 0.761, Tmax = 0.836	k = −12→12
6048 measured reflections	l = −13→13

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.052	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.143	H-atom parameters constrained
S = 1.00	w = 1/[σ^2(Fo^2) + (0.0676P)^2 + 0.3213P] where P = (Fo^2 + 2Fc^2)/3
3968 reflections	(Δ/σ)max < 0.001
308 parameters	Δρmax = 0.40 e Å^−3
0 restraints	Δρmin = −0.35 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Mn1	0.47384 (6)	0.86540 (6)	0.38531 (5)	0.0395 (2)
N1	0.5510 (4)	1.0038 (3)	0.2274 (3)	0.0476 (9)
N2	0.3085 (4)	0.9556 (3)	0.2607 (3)	0.0451 (9)
N3	0.5779 (3)	0.6770 (3)	0.2834 (3)	0.0397 (8)
N4	0.3579 (3)	0.7163 (3)	0.4706 (3)	0.0391 (8)
O1	0.6511 (3)	0.7987 (3)	0.4608 (3)	0.0559 (8)
O2	0.6647 (3)	0.9904 (3)	0.4963 (3)	0.0503 (8)
O3	0.7713 (5)	0.3984 (6)	0.8306 (4)	0.152 (2)
O4	0.9499 (5)	0.2990 (6)	0.9232 (4)	0.152 (2)
O5	0.9996 (6)	0.3114 (7)	0.7215 (5)	0.170 (2)
O6	0.9355 (6)	0.4977 (5)	0.8117 (6)	0.169 (3)
Cl1	0.91272 (13)	0.37528 (15)	0.82075 (11)	0.0656 (4)
C1	0.6816 (5)	1.0108 (5)	0.2027 (4)	0.0636 (14)
H1	0.7409	0.9594	0.2540	0.076*
C2	0.7327 (6)	1.0899 (6)	0.1057 (5)	0.0746 (16)
H2	0.8249	1.0906	0.0907	0.090*
C3	0.6451 (7)	1.1673 (5)	0.0320 (4)	0.0739 (16)
H3	0.6760	1.2233	−0.0338	0.089*
C4	0.5111 (6)	1.1618 (5)	0.0556 (4)	0.0684 (15)
H4	0.4505	1.2139	0.0055	0.082*
C5	0.4656 (5)	1.0786 (4)	0.1542 (4)	0.0479 (11)
C6	0.3256 (5)	1.0623 (4)	0.1805 (4)	0.0472 (11)
C7	0.2182 (6)	1.1496 (5)	0.1248 (4)	0.0661 (14)
H7	0.2305	1.2251	0.0719	0.079*
C8	0.0937 (6)	1.1232 (6)	0.1486 (5)	0.0794 (17)
H8	0.0209	1.1804	0.1116	0.095*
C9	0.0775 (5)	1.0125 (5)	0.2269 (5)	0.0706 (15)
H9	−0.0049	0.9912	0.2419	0.085*
C10	0.1844 (5)	0.9335 (5)	0.2827 (4)	0.0582 (13)
H10	0.1709	0.8607	0.3388	0.070*
C11	0.6942 (5)	0.6562 (4)	0.1957 (4)	0.0482 (11)
H11	0.7475	0.7133	0.1841	0.058*
C12	0.7402 (5)	0.5555 (5)	0.1213 (4)	0.0558 (12)
H12	0.8235	0.5429	0.0621	0.067*
C13	0.6596 (6)	0.4747 (5)	0.1371 (4)	0.0676 (14)
H13	0.6851	0.4080	0.0863	0.081*
C14	0.5404 (5)	0.4922 (5)	0.2284 (4)	0.0607 (13)
H14	0.4849	0.4372	0.2400	0.073*
C15	0.5037 (4)	0.5920 (4)	0.3029 (4)	0.0402 (10)
C16	0.3834 (4)	0.6111 (4)	0.4102 (4)	0.0387 (9)
C17	0.3055 (5)	0.5234 (4)	0.4493 (4)	0.0526 (12)
H17	0.3253	0.4499	0.4074	0.063*
C18	0.1986 (5)	0.5456 (5)	0.5508 (5)	0.0578 (13)
H18	0.1444	0.4882	0.5773	0.069*
C19	0.1726 (5)	0.6520 (5)	0.6121 (4)	0.0529 (12)
H19	0.1011	0.6682	0.6813	0.064*
C20	0.2543 (4)	0.7352 (4)	0.5698 (4)	0.0492 (11)
H20	0.2368	0.8078	0.6120	0.059*
C21	0.7065 (4)	0.8620 (4)	0.4995 (4)	0.0438 (10)
C22	0.8353 (5)	0.7771 (5)	0.5484 (5)	0.0729 (15)
H22A	0.8788	0.8368	0.5617	0.109*
H22B	0.9019	0.7151	0.4923	0.109*
H22C	0.8076	0.7253	0.6225	0.109*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.0437 (4)	0.0344 (4)	0.0435 (4)	−0.0150 (3)	−0.0134 (3)	−0.0030 (3)
N1	0.054 (2)	0.051 (2)	0.046 (2)	−0.0277 (19)	−0.0170 (18)	0.0033 (17)
N2	0.049 (2)	0.045 (2)	0.048 (2)	−0.0168 (18)	−0.0181 (17)	−0.0063 (17)
N3	0.040 (2)	0.0372 (19)	0.041 (2)	−0.0109 (16)	−0.0105 (16)	−0.0052 (15)
N4	0.040 (2)	0.0350 (18)	0.044 (2)	−0.0166 (16)	−0.0095 (16)	−0.0018 (15)
O1	0.0550 (19)	0.0398 (17)	0.082 (2)	−0.0079 (15)	−0.0366 (17)	−0.0130 (15)
O2	0.0538 (19)	0.0381 (17)	0.059 (2)	−0.0113 (15)	−0.0122 (15)	−0.0137 (14)
O3	0.076 (3)	0.254 (7)	0.128 (4)	−0.083 (4)	−0.039 (3)	0.049 (4)
O4	0.129 (4)	0.193 (5)	0.081 (3)	−0.011 (4)	−0.039 (3)	0.031 (3)
O5	0.160 (5)	0.259 (7)	0.096 (4)	−0.092 (5)	0.041 (3)	−0.088 (4)
O6	0.167 (5)	0.121 (4)	0.230 (7)	−0.093 (4)	−0.002 (5)	−0.018 (4)
Cl1	0.0609 (8)	0.0922 (10)	0.0487 (8)	−0.0400 (7)	−0.0037 (6)	−0.0040 (7)
C1	0.070 (3)	0.075 (3)	0.061 (3)	−0.046 (3)	−0.026 (3)	0.013 (3)
C2	0.085 (4)	0.098 (4)	0.063 (4)	−0.064 (4)	−0.015 (3)	0.006 (3)
C3	0.110 (5)	0.077 (4)	0.049 (3)	−0.061 (4)	−0.010 (3)	0.008 (3)
C4	0.097 (4)	0.060 (3)	0.055 (3)	−0.035 (3)	−0.030 (3)	0.014 (3)
C5	0.067 (3)	0.042 (2)	0.041 (3)	−0.023 (2)	−0.016 (2)	−0.005 (2)
C6	0.061 (3)	0.039 (2)	0.041 (3)	−0.014 (2)	−0.016 (2)	−0.005 (2)
C7	0.073 (4)	0.059 (3)	0.057 (3)	−0.012 (3)	−0.027 (3)	0.011 (2)
C8	0.062 (4)	0.089 (4)	0.078 (4)	−0.007 (3)	−0.040 (3)	0.008 (3)
C9	0.057 (3)	0.081 (4)	0.079 (4)	−0.021 (3)	−0.031 (3)	−0.004 (3)
C10	0.056 (3)	0.061 (3)	0.065 (3)	−0.024 (3)	−0.026 (3)	0.001 (2)
C11	0.046 (3)	0.048 (3)	0.047 (3)	−0.014 (2)	−0.008 (2)	−0.002 (2)
C12	0.055 (3)	0.055 (3)	0.042 (3)	−0.009 (3)	−0.003 (2)	−0.004 (2)
C13	0.080 (4)	0.057 (3)	0.057 (3)	−0.013 (3)	−0.004 (3)	−0.025 (2)
C14	0.071 (3)	0.048 (3)	0.070 (3)	−0.024 (3)	−0.015 (3)	−0.019 (2)
C15	0.041 (2)	0.036 (2)	0.043 (2)	−0.0071 (19)	−0.0157 (19)	−0.0051 (18)
C16	0.040 (2)	0.027 (2)	0.051 (3)	−0.0091 (18)	−0.020 (2)	0.0015 (18)
C17	0.054 (3)	0.038 (2)	0.072 (3)	−0.020 (2)	−0.018 (2)	−0.005 (2)
C18	0.047 (3)	0.051 (3)	0.075 (4)	−0.025 (2)	−0.017 (3)	0.012 (3)
C19	0.043 (3)	0.060 (3)	0.049 (3)	−0.019 (2)	−0.007 (2)	0.007 (2)
C20	0.050 (3)	0.046 (3)	0.047 (3)	−0.017 (2)	−0.003 (2)	−0.006 (2)
C21	0.044 (3)	0.043 (3)	0.043 (3)	−0.007 (2)	−0.012 (2)	−0.0143 (19)
C22	0.064 (3)	0.065 (3)	0.093 (4)	0.002 (3)	−0.046 (3)	−0.025 (3)

Geometric parameters (Å, º)

Mn1—O1	2.097 (3)	C6—C7	1.387 (6)
Mn1—O2^i	2.100 (3)	C7—C8	1.370 (7)
Mn1—N4	2.244 (3)	C7—H7	0.930
Mn1—N1	2.268 (3)	C8—C9	1.363 (7)
Mn1—N3	2.275 (3)	C8—H8	0.930
Mn1—N2	2.377 (3)	C9—C10	1.363 (6)
N1—C5	1.336 (5)	C9—H9	0.930
N1—C1	1.338 (5)	C10—H10	0.930
N2—C6	1.344 (5)	C11—C12	1.373 (6)
N2—C10	1.345 (5)	C11—H11	0.930
N3—C11	1.330 (5)	C12—C13	1.361 (6)
N3—C15	1.339 (5)	C12—H12	0.930
N4—C20	1.337 (5)	C13—C14	1.374 (6)
N4—C16	1.342 (5)	C13—H13	0.930
O1—C21	1.246 (5)	C14—C15	1.380 (6)
O2—C21	1.252 (4)	C14—H14	0.930
O2—Mn1^i	2.100 (3)	C15—C16	1.492 (6)
O3—Cl1	1.376 (4)	C16—C17	1.380 (5)
O4—Cl1	1.370 (4)	C17—C18	1.374 (6)
O5—Cl1	1.378 (5)	C17—H17	0.930
O6—Cl1	1.376 (5)	C18—C19	1.358 (6)
C1—C2	1.371 (6)	C18—H18	0.930
C1—H1	0.930	C19—C20	1.374 (6)
C2—C3	1.359 (7)	C19—H19	0.930
C2—H2	0.930	C20—H20	0.930
C3—C4	1.367 (7)	C21—C22	1.503 (6)
C3—H3	0.930	C22—H22A	0.960
C4—C5	1.386 (6)	C22—H22B	0.960
C4—H4	0.930	C22—H22C	0.960
C5—C6	1.473 (6)
O1—Mn1—O2^i	98.15 (11)	C7—C6—C5	122.5 (4)
O1—Mn1—N4	105.13 (12)	C8—C7—C6	119.2 (5)
O2^i—Mn1—N4	91.28 (12)	C8—C7—H7	120.4
O1—Mn1—N1	97.43 (12)	C6—C7—H7	120.4
O2^i—Mn1—N1	101.48 (12)	C9—C8—C7	119.5 (5)
N4—Mn1—N1	152.22 (12)	C9—C8—H8	120.2
O1—Mn1—N3	88.47 (11)	C7—C8—H8	120.2
O2^i—Mn1—N3	163.29 (12)	C8—C9—C10	118.8 (5)
N4—Mn1—N3	72.14 (12)	C8—C9—H9	120.6
N1—Mn1—N3	92.79 (12)	C10—C9—H9	120.6
O1—Mn1—N2	167.01 (12)	N2—C10—C9	123.3 (4)
O2^i—Mn1—N2	88.49 (11)	N2—C10—H10	118.3
N4—Mn1—N2	85.77 (12)	C9—C10—H10	118.3
N1—Mn1—N2	70.20 (12)	N3—C11—C12	123.8 (4)
N3—Mn1—N2	88.21 (11)	N3—C11—H11	118.1
C5—N1—C1	118.2 (4)	C12—C11—H11	118.1
C5—N1—Mn1	119.5 (3)	C13—C12—C11	117.6 (4)
C1—N1—Mn1	122.2 (3)	C13—C12—H12	121.2
C6—N2—C10	117.6 (4)	C11—C12—H12	121.2
C6—N2—Mn1	114.8 (3)	C12—C13—C14	119.8 (4)
C10—N2—Mn1	125.4 (3)	C12—C13—H13	120.1
C11—N3—C15	118.2 (3)	C14—C13—H13	120.1
C11—N3—Mn1	125.0 (3)	C13—C14—C15	119.4 (4)
C15—N3—Mn1	116.0 (3)	C13—C14—H14	120.3
C20—N4—C16	118.4 (3)	C15—C14—H14	120.3
C20—N4—Mn1	123.9 (3)	N3—C15—C14	121.0 (4)
C16—N4—Mn1	117.3 (3)	N3—C15—C16	115.7 (3)
C21—O1—Mn1	132.2 (3)	C14—C15—C16	123.3 (4)
C21—O2—Mn1^i	135.3 (3)	N4—C16—C17	121.2 (4)
O4—Cl1—O6	107.0 (4)	N4—C16—C15	116.0 (3)
O4—Cl1—O3	108.4 (3)	C17—C16—C15	122.8 (4)
O6—Cl1—O3	110.6 (4)	C18—C17—C16	119.4 (4)
O4—Cl1—O5	111.0 (4)	C18—C17—H17	120.3
O6—Cl1—O5	106.8 (4)	C16—C17—H17	120.3
O3—Cl1—O5	112.9 (4)	C19—C18—C17	119.6 (4)
N1—C1—C2	123.5 (4)	C19—C18—H18	120.2
N1—C1—H1	118.3	C17—C18—H18	120.2
C2—C1—H1	118.3	C18—C19—C20	118.6 (4)
C3—C2—C1	118.2 (5)	C18—C19—H19	120.7
C3—C2—H2	120.9	C20—C19—H19	120.7
C1—C2—H2	120.9	N4—C20—C19	122.9 (4)
C2—C3—C4	119.3 (5)	N4—C20—H20	118.6
C2—C3—H3	120.4	C19—C20—H20	118.6
C4—C3—H3	120.4	O1—C21—O2	124.3 (4)
C3—C4—C5	120.0 (4)	O1—C21—C22	116.9 (4)
C3—C4—H4	120.0	O2—C21—C22	118.7 (4)
C5—C4—H4	120.0	C21—C22—H22A	109.5
N1—C5—C4	120.7 (4)	C21—C22—H22B	109.5
N1—C5—C6	116.6 (4)	H22A—C22—H22B	109.5
C4—C5—C6	122.6 (4)	C21—C22—H22C	109.5
N2—C6—C7	121.6 (4)	H22A—C22—H22C	109.5
N2—C6—C5	116.0 (4)	H22B—C22—H22C	109.5

Symmetry code: (i) −x+1, −y+2, −z+1.