trans-Tetra-aqua-bis-[bis-(pyridin-3-yl)methanone-κN]manganese(II) bis-(perchlorate).

In the title complex, [Mn(C(11)H(8)N(2)O)(2)(H(2)O)(4)](ClO(4))(2), the Mn(2+) ion is located on an inversion center with the slightly distorted N(2)O(4) octa-hedral coordination sphere comprising N-atom donors from two monodentate trans-related bis-(pyridin-3-yl)methanone ligands and four water ligands. The two perchlorate anions are linked to the mononuclear complex mol-ecule through water O-H⋯O hydrogen bonds while inter-complex water O-H⋯N(pyridine) inter-actions form an infinite chain structure extending along the b axis. The perchlorate anions also function as inter-unit links through water O-H⋯O hydrogen bonds which, together with water O-H⋯O(carbon-yl) inter-actions, give a three-dimensional framework structure.

Related literature

For background to coordination chemistry based on pyridyl­methanone derivatives, see: Huang et al. (2003 ▶); Chen et al. (2005 ▶); For transition metal complexes of bis­(pyridin-3-yl)methanone, see: Zhang (2011 ▶); Chen & Mak (2005 ▶).

Experimental

Crystal data

[Mn(C11H8N2O)2(H2O)4](ClO4)2

M = 694.29

Monoclinic,

a = 8.410 (2) Å

b = 11.962 (3) Å

c = 14.386 (4) Å

β = 95.476 (5)°

V = 1440.6 (6) Å3

Z = 2

Mo Kα radiation

μ = 0.72 mm−1

T = 296 K

0.45 × 0.32 × 0.25 mm

Data collection

Bruker APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2007 ▶) T min = 0.572, T max = 1.000

7576 measured reflections

2529 independent reflections

1853 reflections with I > 2σ(I)

R int = 0.076

Refinement

R[F 2 > 2σ(F 2)] = 0.050

wR(F 2) = 0.143

S = 1.04

2529 reflections

196 parameters

4 restraints

H-atom parameters constrained

Δρmax = 0.48 e Å−3

Δρmin = −0.51 e Å−3

Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009 ▶).

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811052184/zs2167sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811052184/zs2167Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Mn(C11H8N2O)2(H2O)4](ClO4)2	F(000) = 710
Mr = 694.29	Dx = 1.601 Mg m−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 261 reflections
a = 8.410 (2) Å	θ = 2.2–27.2°
b = 11.962 (3) Å	µ = 0.72 mm−1
c = 14.386 (4) Å	T = 296 K
β = 95.476 (5)°	Block, colorless
V = 1440.6 (6) Å3	0.45 × 0.32 × 0.25 mm
Z = 2

Bruker APEXII CCD area-detector diffractometer	2529 independent reflections
Radiation source: fine-focus sealed tube	1853 reflections with I > 2σ(I)
graphite	Rint = 0.076
ω scans	θmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −10→9
Tmin = 0.572, Tmax = 1.000	k = −13→14
7576 measured reflections	l = −8→17

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)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.143	H-atom parameters constrained
S = 1.04	w = 1/[σ2(Fo2) + (0.0816P)2] P = (Fo2 + 2Fc2)/3
2529 reflections	(Δ/σ)max < 0.001
196 parameters	Δρmax = 0.48 e Å−3
4 restraints	Δρmin = −0.51 e Å−3

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Mn1	0.5000	0.5000	0.5000	0.0230 (3)
O1	0.1206 (3)	0.9254 (2)	0.26771 (19)	0.0445 (8)
N1	0.3187 (5)	1.1514 (3)	0.4615 (3)	0.0486 (10)
N2	0.2861 (3)	0.6001 (2)	0.4305 (2)	0.0298 (7)
C1	0.3036 (6)	1.1271 (4)	0.5509 (3)	0.0560 (13)
H1A	0.3305	1.1816	0.5958	0.067*
C2	0.2504 (6)	1.0259 (4)	0.5794 (3)	0.0587 (14)
H2A	0.2426	1.0122	0.6425	0.070*
C3	0.2084 (5)	0.9447 (3)	0.5142 (3)	0.0443 (11)
H3A	0.1721	0.8753	0.5322	0.053*
C4	0.2211 (4)	0.9681 (3)	0.4213 (3)	0.0296 (9)
C5	0.2765 (5)	1.0732 (3)	0.3991 (3)	0.0428 (11)
H5A	0.2843	1.0895	0.3365	0.051*
C6	0.1683 (4)	0.8891 (3)	0.3445 (3)	0.0304 (9)
C7	0.1633 (4)	0.7661 (3)	0.3635 (2)	0.0272 (8)
C8	0.2842 (4)	0.7106 (3)	0.4172 (3)	0.0300 (9)
H8A	0.3684	0.7526	0.4455	0.036*
C9	0.1591 (4)	0.5423 (3)	0.3913 (3)	0.0391 (10)
H9A	0.1553	0.4656	0.4015	0.047*
C10	0.0360 (5)	0.5911 (3)	0.3373 (3)	0.0500 (13)
H10A	−0.0487	0.5478	0.3113	0.060*
C11	0.0373 (5)	0.7041 (3)	0.3213 (3)	0.0403 (11)
H11A	−0.0442	0.7382	0.2831	0.048*
Cl1	0.58846 (12)	0.78266 (8)	0.19059 (7)	0.0363 (3)
O2	0.4655 (4)	0.8174 (4)	0.2446 (3)	0.0884 (13)
O3	0.5324 (4)	0.7861 (3)	0.0946 (2)	0.0706 (11)
O4	0.6421 (5)	0.6736 (3)	0.2170 (2)	0.0752 (12)
O5	0.7196 (4)	0.8584 (3)	0.2095 (3)	0.0671 (10)
O1W	0.5725 (3)	0.6446 (2)	0.58278 (18)	0.0372 (7)
O2W	0.6431 (3)	0.5430 (2)	0.38484 (19)	0.0429 (7)
H1WA	0.6090	0.7146	0.5761	0.064*
H2WA	0.6821	0.4815	0.3606	0.064*
H2WB	0.6215	0.5865	0.3351	0.064*
H1WB	0.5147	0.6440	0.6352	0.064*

	U11	U22	U33	U12	U13	U23
Mn1	0.0316 (5)	0.0164 (4)	0.0206 (4)	−0.0026 (3)	0.0008 (3)	0.0006 (3)
O1	0.069 (2)	0.0323 (15)	0.0293 (16)	0.0054 (14)	−0.0088 (14)	0.0023 (13)
N1	0.075 (3)	0.0299 (19)	0.041 (2)	−0.0167 (18)	0.0046 (19)	0.0002 (16)
N2	0.0303 (17)	0.0231 (17)	0.0355 (19)	−0.0009 (13)	0.0006 (14)	−0.0005 (14)
C1	0.087 (4)	0.037 (3)	0.043 (3)	−0.017 (2)	0.001 (3)	−0.010 (2)
C2	0.107 (4)	0.043 (3)	0.027 (2)	−0.024 (3)	0.008 (3)	−0.001 (2)
C3	0.071 (3)	0.029 (2)	0.033 (2)	−0.011 (2)	0.004 (2)	0.0025 (18)
C4	0.037 (2)	0.0231 (18)	0.029 (2)	−0.0018 (16)	0.0037 (17)	−0.0006 (16)
C5	0.066 (3)	0.033 (2)	0.029 (2)	−0.007 (2)	0.004 (2)	0.0059 (18)
C6	0.035 (2)	0.025 (2)	0.031 (2)	0.0033 (16)	−0.0004 (17)	0.0002 (16)
C7	0.029 (2)	0.027 (2)	0.026 (2)	0.0007 (15)	0.0037 (16)	−0.0037 (16)
C8	0.030 (2)	0.025 (2)	0.034 (2)	−0.0047 (15)	−0.0026 (17)	−0.0045 (16)
C9	0.037 (2)	0.025 (2)	0.055 (3)	−0.0073 (18)	0.004 (2)	−0.0016 (19)
C10	0.030 (2)	0.033 (2)	0.083 (4)	−0.0073 (18)	−0.013 (2)	−0.009 (2)
C11	0.032 (2)	0.034 (2)	0.053 (3)	0.0036 (18)	−0.008 (2)	−0.005 (2)
Cl1	0.0444 (6)	0.0336 (6)	0.0316 (6)	0.0038 (4)	0.0070 (4)	0.0028 (4)
O2	0.067 (3)	0.130 (4)	0.075 (3)	0.023 (2)	0.040 (2)	0.003 (3)
O3	0.097 (3)	0.073 (2)	0.039 (2)	0.025 (2)	−0.0151 (19)	−0.0047 (17)
O4	0.123 (3)	0.0360 (18)	0.064 (3)	0.012 (2)	−0.003 (2)	0.0135 (17)
O5	0.061 (2)	0.058 (2)	0.082 (3)	−0.0116 (17)	−0.0004 (19)	0.0085 (19)
O1W	0.0595 (18)	0.0210 (13)	0.0305 (15)	−0.0106 (12)	0.0009 (13)	−0.0003 (11)
O2W	0.0547 (18)	0.0373 (16)	0.0393 (17)	−0.0002 (14)	0.0173 (14)	0.0067 (13)

Mn1—O1Wi	2.155 (2)	C5—H5A	0.9300
Mn1—O1W	2.155 (2)	C6—C7	1.499 (5)
Mn1—O2W	2.199 (3)	C7—C11	1.386 (5)
Mn1—O2Wi	2.199 (3)	C7—C8	1.386 (5)
Mn1—N2i	2.307 (3)	C8—H8A	0.9300
Mn1—N2	2.307 (3)	C9—C10	1.365 (6)
O1—C6	1.218 (4)	C9—H9A	0.9300
N1—C5	1.321 (5)	C10—C11	1.371 (6)
N1—C1	1.337 (6)	C10—H10A	0.9300
N2—C8	1.336 (4)	C11—H11A	0.9300
N2—C9	1.350 (4)	Cl1—O2	1.414 (4)
C1—C2	1.367 (6)	Cl1—O3	1.416 (3)
C1—H1A	0.9300	Cl1—O4	1.420 (3)
C2—C3	1.374 (6)	Cl1—O5	1.434 (3)
C2—H2A	0.9300	O1W—H1WA	0.9000
C3—C4	1.379 (5)	O1W—H1WB	0.9400
C3—H3A	0.9300	O2W—H2WA	0.8900
C4—C5	1.389 (5)	O2W—H2WB	0.8900
C4—C6	1.489 (5)
O1Wi—Mn1—O1W	180.00 (7)	N1—C5—H5A	118.0
O1Wi—Mn1—O2W	85.27 (10)	C4—C5—H5A	118.0
O1W—Mn1—O2W	94.73 (10)	O1—C6—C4	119.8 (3)
O1Wi—Mn1—O2Wi	94.73 (10)	O1—C6—C7	120.1 (3)
O1W—Mn1—O2Wi	85.27 (10)	C4—C6—C7	119.9 (3)
O2W—Mn1—O2Wi	180.0	C11—C7—C8	118.6 (3)
O1Wi—Mn1—N2i	89.47 (10)	C11—C7—C6	118.6 (3)
O1W—Mn1—N2i	90.53 (10)	C8—C7—C6	122.7 (3)
O2W—Mn1—N2i	89.29 (11)	N2—C8—C7	123.5 (3)
O2Wi—Mn1—N2i	90.71 (11)	N2—C8—H8A	118.2
O1Wi—Mn1—N2	90.53 (10)	C7—C8—H8A	118.2
O1W—Mn1—N2	89.47 (10)	N2—C9—C10	123.1 (4)
O2W—Mn1—N2	90.71 (11)	N2—C9—H9A	118.5
O2Wi—Mn1—N2	89.29 (11)	C10—C9—H9A	118.5
N2i—Mn1—N2	180.000 (1)	C9—C10—C11	120.0 (4)
C5—N1—C1	117.2 (4)	C9—C10—H10A	120.0
C8—N2—C9	116.6 (3)	C11—C10—H10A	120.0
C8—N2—Mn1	125.0 (2)	C10—C11—C7	118.2 (4)
C9—N2—Mn1	117.9 (2)	C10—C11—H11A	120.9
N1—C1—C2	123.0 (4)	C7—C11—H11A	120.9
N1—C1—H1A	118.5	O2—Cl1—O3	109.5 (2)
C2—C1—H1A	118.5	O2—Cl1—O4	110.7 (3)
C1—C2—C3	119.4 (4)	O3—Cl1—O4	110.8 (2)
C1—C2—H2A	120.3	O2—Cl1—O5	107.5 (2)
C3—C2—H2A	120.3	O3—Cl1—O5	110.2 (2)
C2—C3—C4	118.7 (4)	O4—Cl1—O5	108.1 (2)
C2—C3—H3A	120.6	Mn1—O1W—H1WA	140.3
C4—C3—H3A	120.6	Mn1—O1W—H1WB	107.0
C3—C4—C5	117.7 (4)	H1WA—O1W—H1WB	108
C3—C4—C6	123.1 (3)	Mn1—O2W—H2WA	110.5
C5—C4—C6	119.1 (3)	Mn1—O2W—H2WB	131.2
N1—C5—C4	124.0 (4)	H2WA—O2W—H2WB	102.9
O1Wi—Mn1—N2—C8	−150.3 (3)	C5—C4—C6—O1	−25.7 (6)
O1W—Mn1—N2—C8	29.7 (3)	C3—C4—C6—C7	−25.7 (6)
O2W—Mn1—N2—C8	−65.0 (3)	C5—C4—C6—C7	158.5 (4)
O2Wi—Mn1—N2—C8	115.0 (3)	O1—C6—C7—C11	−35.3 (5)
O1Wi—Mn1—N2—C9	22.3 (3)	C4—C6—C7—C11	140.5 (4)
O1W—Mn1—N2—C9	−157.7 (3)	O1—C6—C7—C8	141.0 (4)
O2W—Mn1—N2—C9	107.5 (3)	C4—C6—C7—C8	−43.3 (5)
O2Wi—Mn1—N2—C9	−72.5 (3)	C9—N2—C8—C7	−2.4 (6)
C5—N1—C1—C2	1.4 (8)	Mn1—N2—C8—C7	170.3 (3)
N1—C1—C2—C3	−0.7 (9)	C11—C7—C8—N2	0.1 (6)
C1—C2—C3—C4	−0.1 (8)	C6—C7—C8—N2	−176.1 (4)
C2—C3—C4—C5	0.2 (7)	C8—N2—C9—C10	2.5 (6)
C2—C3—C4—C6	−175.6 (4)	Mn1—N2—C9—C10	−170.6 (4)
C1—N1—C5—C4	−1.3 (7)	N2—C9—C10—C11	−0.4 (7)
C3—C4—C5—N1	0.5 (7)	C9—C10—C11—C7	−1.9 (7)
C6—C4—C5—N1	176.5 (4)	C8—C7—C11—C10	2.0 (6)
C3—C4—C6—O1	150.1 (4)	C6—C7—C11—C10	178.4 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···N1ii	0.90	1.82	2.704 (4)	169
O2W—H2WA···O5iii	0.89	2.01	2.889 (5)	171
O2W—H2WB···O4	0.89	2.01	2.876 (4)	162
O1W—H1WB···O1iv	0.94	2.19	2.782 (3)	120

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H1WA⋯N1i	0.90	1.82	2.704 (4)	169
O2W—H2WA⋯O5ii	0.89	2.01	2.889 (5)	171
O2W—H2WB⋯O4	0.89	2.01	2.876 (4)	162
O1W—H1WB⋯O1iii	0.94	2.19	2.782 (3)	120

Symmetry codes: (i) ; (ii) ; (iii) .