Poly[[μ-N,N'-bis-(2-hy-droxy-eth-yl)-N,N,N',N'-tetra-methyl-propane-1,3-diaminium-κ(2) O:O']tetra-μ-bromido-dibromidodimanganese(II)].

The asymmetric unit of the title three-dimensional coordination polymer, [Mn2Br6(C11H28N2O2)] n , consists of one Mn(II) cation, half of a dicationic N,N'-bis-(2-hy-droxy-eth-yl)-N,N,N',N'-tetra-methyl-propane-1,3-diaminium ligand (L) (the other half being generated by a twofold rotation axis), and three bromide ions. The Mn(II) cation is coordinated by a single L ligand via the hy-droxy O atom and by five bromide ions, resulting in a distorted octa-hedral MnBr5O coordination geometry. Four of the bromide ions are bridging to two adjacent Mn(II) atoms, thereby forming polymeric chains along the a and b axes. The L units act as links between neighbouring Mn-(μ-Br)2-Mn chains, also forming a polymeric continuum along the c axis, which completes the formation of a three-dimensional network. Classical O-H⋯Br hydrogen bonds are present. The distance between adjacent Mn(II) atoms is 4.022 (1) Å.

Related literature

For related structures of M II transition metal halide one-dimensional coordination polymers, see: Han et al. (2012 ▶); Englert & Schiffers (2006 ▶). For two-dimensional networks, see: Hu & Englert (2006 ▶); Turgunov et al. (2011 ▶). For properties of metal halides, see: Hitchcock et al. (2003 ▶); Wang et al. (2011 ▶). For ligand conformations, see: Kärnä et al. (2010 ▶).

Experimental

Crystal data

[Mn2Br6(C11H28N2O2)]

M = 809.69

Tetragonal,

a = 8.0163 (4) Å

c = 35.3103 (18) Å

V = 2269.1 (2) Å3

Z = 4

Mo Kα radiation

μ = 11.69 mm−1

T = 123 K

0.25 × 0.25 × 0.20 mm

Data collection

Bruker–NoniusKappa APEXII diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2008a ▶) T min = 0.440, T max = 0.746

5076 measured reflections

1966 independent reflections

1856 reflections with I > 2σ(I)

R int = 0.032

Refinement

R[F 2 > 2σ(F 2)] = 0.021

wR(F 2) = 0.047

S = 1.02

1966 reflections

111 parameters

1 restraint

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 0.36 e Å−3

Δρmin = −0.41 e Å−3

Absolute structure: Flack (1983 ▶), 690 Friedel pairs

Flack parameter: 0.048 (14)

Data collection: COLLECT (Bruker, 2008 ▶); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997 ▶); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b ▶); molecular graphics: Mercury (Macrae et al., 2008 ▶); software used to prepare material for publication: SHELXL97.

Click here for additional data file.

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812044765/fj2604sup1.cif

Click here for additional data file.

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812044765/fj2604Isup2.hkl

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

[Mn2Br6(C11H28N2O2)]	Dx = 2.370 Mg m−3
Mr = 809.69	Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P43212	Cell parameters from 1871 reflections
Hall symbol: P 4nw 2abw	θ = 0.4–27.9°
a = 8.0163 (4) Å	µ = 11.69 mm−1
c = 35.3103 (18) Å	T = 123 K
V = 2269.1 (2) Å3	Block, violet
Z = 4	0.25 × 0.25 × 0.20 mm
F(000) = 1536

Bruker–NoniusKappa APEXII diffractometer	1966 independent reflections
Radiation source: fine-focus sealed tube	1856 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.032
Detector resolution: 9 pixels mm-1	θmax = 25.0°, θmin = 2.8°
φ and ω scans	h = −9→9
Absorption correction: multi-scan (SADABS; Sheldrick, 2008a)	k = −4→9
Tmin = 0.440, Tmax = 0.746	l = −22→41
5076 measured reflections

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.021	H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.047	w = 1/[σ2(Fo2) + (0.P)2] where P = (Fo2 + 2Fc2)/3
S = 1.02	(Δ/σ)max = 0.001
1966 reflections	Δρmax = 0.36 e Å−3
111 parameters	Δρmin = −0.41 e Å−3
1 restraint	Absolute structure: Flack (1983), 690 Friedel pairs
Primary atom site location: structure-invariant direct methods	Flack parameter: 0.048 (14)

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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	Occ. (<1)
C2	0.8227 (5)	0.8960 (5)	0.15487 (11)	0.0158 (9)
H2A	0.8379	0.8507	0.1290	0.019*
H2B	0.7031	0.9236	0.1580	0.019*
C3	0.8705 (5)	0.7633 (5)	0.18350 (10)	0.0143 (9)
H3A	0.8340	0.6538	0.1735	0.017*
H3B	0.9937	0.7605	0.1853	0.017*
C5	0.6146 (5)	0.7687 (6)	0.22206 (11)	0.0197 (10)
H5A	0.5825	0.6644	0.2095	0.030*
H5B	0.5680	0.8634	0.2081	0.030*
H5C	0.5713	0.7693	0.2480	0.030*
C6	0.8652 (5)	0.6412 (5)	0.24628 (11)	0.0172 (10)
H6A	0.8250	0.6531	0.2724	0.026*
H6B	0.9874	0.6423	0.2461	0.026*
H6C	0.8250	0.5356	0.2357	0.026*
C7	0.8412 (5)	0.9495 (5)	0.24099 (11)	0.0116 (9)
H7A	0.7764	0.9603	0.2647	0.014*
H7B	0.8049	1.0396	0.2237	0.014*
C8	1.0268 (5)	0.9732 (5)	0.2500	0.0140 (13)
H8A	1.0594	0.9039	0.2720	0.017*	0.50
H8B	1.0961	0.9406	0.2280	0.017*	0.50
N4	0.8013 (4)	0.7825 (4)	0.22294 (9)	0.0130 (8)
O1	0.9205 (3)	1.0470 (4)	0.15874 (8)	0.0140 (6)
Br1	0.61915 (5)	1.32320 (5)	0.175357 (11)	0.01348 (10)
Br2	1.13256 (5)	1.39037 (5)	0.167113 (10)	0.01205 (10)
Br3	0.81111 (5)	1.55274 (5)	0.090982 (11)	0.01279 (11)
Mn1	0.87136 (8)	1.27065 (7)	0.124710 (17)	0.01152 (14)
H1	1.010 (3)	1.021 (5)	0.1575 (13)	0.017*

	U11	U22	U33	U12	U13	U23
C2	0.024 (2)	0.0120 (19)	0.011 (2)	−0.004 (2)	−0.003 (2)	−0.0030 (18)
C3	0.021 (2)	0.014 (2)	0.009 (2)	0.001 (2)	0.0015 (19)	0.0001 (17)
C5	0.013 (2)	0.025 (2)	0.021 (2)	−0.001 (2)	0.001 (2)	−0.006 (2)
C6	0.023 (2)	0.013 (2)	0.015 (2)	−0.0018 (19)	−0.0049 (19)	0.0016 (18)
C7	0.015 (2)	0.0074 (18)	0.012 (2)	−0.0020 (19)	−0.0027 (18)	−0.0025 (17)
C8	0.0114 (19)	0.0114 (19)	0.019 (3)	0.002 (3)	0.0015 (19)	0.0015 (19)
N4	0.0139 (16)	0.0157 (17)	0.0094 (17)	0.0011 (16)	−0.0017 (14)	0.0004 (15)
O1	0.0105 (14)	0.0137 (14)	0.0178 (15)	0.0010 (13)	0.0016 (14)	0.0026 (14)
Br1	0.01241 (19)	0.0168 (2)	0.01122 (19)	−0.00105 (19)	0.00124 (18)	−0.00200 (18)
Br2	0.01210 (19)	0.01371 (19)	0.01035 (19)	0.00068 (18)	0.00073 (16)	0.00004 (17)
Br3	0.01400 (19)	0.01200 (19)	0.0124 (2)	−0.00096 (19)	−0.00056 (18)	0.00178 (17)
Mn1	0.0117 (3)	0.0115 (3)	0.0113 (3)	−0.0001 (3)	0.0003 (3)	0.0014 (3)

C2—O1	1.449 (5)	C7—C8	1.533 (5)
C2—C3	1.517 (5)	C7—H7A	0.9900
C2—H2A	0.9900	C7—H7B	0.9900
C2—H2B	0.9900	C8—C7i	1.533 (5)
C3—N4	1.507 (4)	C8—H8A	0.9900
C3—H3A	0.9900	C8—H8B	0.9900
C3—H3B	0.9900	O1—Mn1	2.194 (3)
C5—N4	1.501 (5)	O1—H1	0.748 (19)
C5—H5A	0.9800	Br1—Mn1	2.7319 (7)
C5—H5B	0.9800	Br1—Mn1ii	2.7635 (7)
C5—H5C	0.9800	Br2—Mn1iii	2.7407 (7)
C6—N4	1.491 (5)	Br2—Mn1	2.7472 (8)
C6—H6A	0.9800	Br3—Mn1	2.6010 (7)
C6—H6B	0.9800	Mn1—Br2ii	2.7407 (7)
C6—H6C	0.9800	Mn1—Br1iii	2.7635 (7)
C7—N4	1.517 (5)
O1—C2—C3	112.7 (3)	C7i—C8—H8A	110.4
O1—C2—H2A	109.0	C7—C8—H8A	110.4
C3—C2—H2A	109.0	C7i—C8—H8B	110.4
O1—C2—H2B	109.0	C7—C8—H8B	110.4
C3—C2—H2B	109.0	H8A—C8—H8B	108.6
H2A—C2—H2B	107.8	C6—N4—C5	107.3 (3)
N4—C3—C2	116.8 (3)	C6—N4—C3	107.9 (3)
N4—C3—H3A	108.1	C5—N4—C3	109.9 (3)
C2—C3—H3A	108.1	C6—N4—C7	111.4 (3)
N4—C3—H3B	108.1	C5—N4—C7	106.5 (3)
C2—C3—H3B	108.1	C3—N4—C7	113.6 (3)
H3A—C3—H3B	107.3	C2—O1—Mn1	122.3 (2)
N4—C5—H5A	109.5	C2—O1—H1	106 (4)
N4—C5—H5B	109.5	Mn1—O1—H1	112 (4)
H5A—C5—H5B	109.5	Mn1—Br1—Mn1ii	94.082 (12)
N4—C5—H5C	109.5	Mn1iii—Br2—Mn1	94.254 (12)
H5A—C5—H5C	109.5	O1—Mn1—Br3	174.03 (8)
H5B—C5—H5C	109.5	O1—Mn1—Br1	84.28 (8)
N4—C6—H6A	109.5	Br3—Mn1—Br1	91.62 (2)
N4—C6—H6B	109.5	O1—Mn1—Br2ii	92.05 (8)
H6A—C6—H6B	109.5	Br3—Mn1—Br2ii	91.89 (2)
N4—C6—H6C	109.5	Br1—Mn1—Br2ii	84.75 (2)
H6A—C6—H6C	109.5	O1—Mn1—Br2	81.38 (8)
H6B—C6—H6C	109.5	Br3—Mn1—Br2	95.01 (2)
N4—C7—C8	113.7 (3)	Br1—Mn1—Br2	98.83 (2)
N4—C7—H7A	108.8	Br2ii—Mn1—Br2	172.12 (3)
C8—C7—H7A	108.8	O1—Mn1—Br1iii	89.94 (8)
N4—C7—H7B	108.8	Br3—Mn1—Br1iii	94.43 (2)
C8—C7—H7B	108.8	Br1—Mn1—Br1iii	173.07 (2)
H7A—C7—H7B	107.7	Br2ii—Mn1—Br1iii	91.67 (2)
C7i—C8—C7	106.5 (4)	Br2—Mn1—Br1iii	84.03 (2)
O1—C2—C3—N4	79.7 (4)	C2—O1—Mn1—Br2	179.1 (3)
N4—C7—C8—C7i	167.0 (4)	C2—O1—Mn1—Br1iii	−96.9 (3)
C2—C3—N4—C6	−179.3 (3)	Mn1ii—Br1—Mn1—O1	−105.44 (8)
C2—C3—N4—C5	64.0 (5)	Mn1ii—Br1—Mn1—Br3	78.92 (2)
C2—C3—N4—C7	−55.2 (5)	Mn1ii—Br1—Mn1—Br2ii	−12.838 (12)
C8—C7—N4—C6	54.1 (4)	Mn1ii—Br1—Mn1—Br2	174.24 (3)
C8—C7—N4—C5	170.8 (3)	Mn1iii—Br2—Mn1—O1	78.06 (8)
C8—C7—N4—C3	−68.1 (4)	Mn1iii—Br2—Mn1—Br3	−106.73 (2)
C3—C2—O1—Mn1	−175.3 (2)	Mn1iii—Br2—Mn1—Br1	160.85 (3)
C2—O1—Mn1—Br1	79.3 (3)	Mn1iii—Br2—Mn1—Br1iii	−12.785 (11)
C2—O1—Mn1—Br2ii	−5.2 (3)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···Br3iii	0.75 (2)	2.49 (2)	3.232 (3)	175 (5)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯Br3i	0.75 (2)	2.49 (2)	3.232 (3)	175 (5)

Symmetry code: (i) .