Aqua­azido­{2,2′-[o-phenylenebis(nitrilo­methyl­idyne)]diphenolato}manganese(III) hemihydrate

Zhang, X.; Wei, P.; Li, B.; Wu, C.; Hu, B.

doi:10.1107/S1600536809020200

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 7| July 2009| Page m707

doi:10.1107/S1600536809020200

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Aquaazido{2,2′-[o-phenylenebis(nitrilomethylidyne)]diphenolato}manganese(III) hemihydrate

Xiutang Zhang,^a,^b ^* Peihai Wei,^a Bin Li,^a Chunyong Wu ^c and Bo Hu ^a

^aAdvanced Material Institute of Research, Department of Chemistry and Chemical Engineering, Shandong Institute of Education, Jinan 250013, People's Republic of China, ^bCollege of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, People's Republic of China, and ^cYuncheng Normal School, Yuncheng 274700, Shandong Province, People's Republic of China
^*Correspondence e-mail: xiutangzhang@yahoo.com.cn

(Received 14 May 2009; accepted 27 May 2009; online 6 June 2009)

In the title compound, [Mn(C₂₀H₁₄N₂O₂)(N₃)(H₂O)]·0.5H₂O, the Mn^III ion is chelated by the N,N′,O,O′-tetradentate Schiff base ligand and further coordinated by one azide ion and one water molecule in trans positions, resulting in a distorted fac-MnN₃O₃ octahedral arrangement. The O atom of the uncoordinated water molecule lies on a crystallographic twofold axis. In the crystal, O—H⋯O and O—H⋯N hydrogen bonds help to establish the packing.

Related literature

For background to salicylaldehyde complexes, see: Alam et al. (2003 ); Zelewsky & von Knof (1999 ).

Experimental

Crystal data

[Mn(C₂₀H₁₄N₂O₂)(N₃)(H₂O)]·0.5H₂O
M_r = 438.33
Monoclinic, C 2/c
a = 25.100 (10) Å
b = 11.478 (5) Å
c = 12.599 (5) Å
β = 94.175 (3)°
V = 3620 (3) Å³
Z = 8
Mo Kα radiation
μ = 0.77 mm⁻¹
T = 293 K
0.12 × 0.10 × 0.08 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004 ) T_min = 0.914, T_max = 0.941
11927 measured reflections
3162 independent reflections
2371 reflections with I > 2σ(I)
R_int = 0.082

Refinement

R[F² > 2σ(F²)] = 0.037
wR(F²) = 0.086
S = 1.00
3162 reflections
280 parameters
4 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.32 e Å⁻³
Δρ_min = −0.38 e Å⁻³

Table 1
Selected bond lengths (Å)

Mn1—O1	1.8636 (18)
Mn1—O2	1.8844 (18)
Mn1—N2	1.986 (2)
Mn1—N1	1.988 (2)
Mn1—N3	2.306 (2)
Mn1—O1W	2.321 (2)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H2W⋯N3ⁱ	0.82 (2)	2.12 (2)	2.937 (3)	176 (3)
O1W—H1W⋯O2ⁱⁱ	0.820 (11)	2.076 (6)	2.885 (3)	169 (2)
O2W—H3W⋯N5	0.82 (3)	2.18 (3)	3.000 (3)	173 (4)
Symmetry codes: (i) $[x, -y, z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+2]$ .

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus; 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.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809020200/hb2977sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809020200/hb2977Isup2.hkl

checkCIF report

Comment top

The synthesis of complexes consisting of salicylaldehyde ligand has attracted continuous research interest not only because of their appealing structural and topological novelty, but also due to their unusual optical, electronic, magnetic, and catalytic properties, as well as their potential medical application (Alam et al., 2003; Zelewsky & von Knof, 1999). In the present paper, we describe the synthesis and structural characterizations of the title compound, (I),

As shown in Fig. 1, each Mn(III) atom is chelated by Schiff base ligand via two N and two O atoms and is additionally coordinated by one azide and a water molecule, forming a distorted octahedral geometry (Table 1) in which, the Schiff base lies in the equatorial plane, and the azide and aqua ligands lie in the axial coordination sites.

With O—H···O and O—H···N hydrogen bonds (Table 2), a three-dimensional network is formed as shown in Fig. 2.

Related literature top

For background to salicylaldehyde complexes, see: Alam et al. (2003); Zelewsky & von Knof (1999).

Experimental top

A mixture of manganese(III) acetylacetonate (1 mmol) and N,N'-bis(2-hydroxy-5-bromobenzyl)1,2-diaminopropane (1 mmol), and dipotassium nickel tetracyanide (1 mmol) in 20 ml methanol was refluxed for several hours. The above cooled solution was filtered and the filtrate was kept in an ice box. One week later, brown blocks of (I) were obtained with a yield of 5%. Anal. Calc. for C₄₀H₃₄Mn₂N₁₀O₇: C 54.75, H 3.88, N 15.97%; Found: C 54.71, H 3.75, N 15.82.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus (Bruker, 2004); 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 (Sheldrick, 2008).

Figures top

	Fig. 1. The molecular structure of (I), drawn with 30% probability displacement ellipsoids for the non-hydrogen atoms.
	Fig. 2. Three-dimensional network formed by hydrogen bonds (dashed lines).

Aquaazido{2,2'-[o- phenylenebis(nitrilomethylidyne)]diphenolato}manganese(III) hemihydrate top

Crystal data top

[Mn(C₂₀H₁₄N₂O₂)(N₃)(H₂O)]·0.5H₂O	F(000) = 1808
M_r = 438.33	D_x = 1.612 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71070 Å
Hall symbol: -C 2yc	Cell parameters from 3162 reflections
a = 25.10 (1) Å	θ = 3.0–25.0°
b = 11.478 (5) Å	µ = 0.77 mm⁻¹
c = 12.599 (5) Å	T = 293 K
β = 94.175 (3)°	Block, pink
V = 3620 (3) Å³	0.12 × 0.10 × 0.08 mm
Z = 8

Data collection top

Bruker APEXII CCD area-detector diffractometer	3162 independent reflections
Radiation source: fine-focus sealed tube	2371 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.082
ϕ and ω scans	θ_max = 25.0°, θ_min = 3.0°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −27→29
T_min = 0.914, T_max = 0.941	k = −13→13
11927 measured reflections	l = −14→13

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)] = 0.037	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.086	H atoms treated by a mixture of independent and constrained refinement
S = 1.00	w = 1/[σ²(F_o²) + (0.03P)²] where P = (F_o² + 2F_c²)/3
3162 reflections	(Δ/σ)_max = 0.001
280 parameters	Δρ_max = 0.32 e Å⁻³
4 restraints	Δρ_min = −0.38 e Å⁻³

Crystal data top

[Mn(C₂₀H₁₄N₂O₂)(N₃)(H₂O)]·0.5H₂O	V = 3620 (3) Å³
M_r = 438.33	Z = 8
Monoclinic, C2/c	Mo Kα radiation
a = 25.10 (1) Å	µ = 0.77 mm⁻¹
b = 11.478 (5) Å	T = 293 K
c = 12.599 (5) Å	0.12 × 0.10 × 0.08 mm
β = 94.175 (3)°

Data collection top

Bruker APEXII CCD area-detector diffractometer	3162 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2004)	2371 reflections with I > 2σ(I)
T_min = 0.914, T_max = 0.941	R_int = 0.082
11927 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.037	4 restraints
wR(F²) = 0.086	H atoms treated by a mixture of independent and constrained refinement
S = 1.00	Δρ_max = 0.32 e Å⁻³
3162 reflections	Δρ_min = −0.38 e Å⁻³
280 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	0.204685 (15)	0.09791 (3)	0.87813 (3)	0.00903 (13)
C1	0.11631 (10)	0.2543 (2)	0.90445 (18)	0.0102 (6)
C2	0.09780 (10)	0.3688 (2)	0.90882 (19)	0.0124 (6)
H2	0.1219	0.4301	0.9061	0.015*
C3	0.04451 (10)	0.3928 (2)	0.91706 (19)	0.0156 (6)
H3	0.0332	0.4699	0.9196	0.019*
C4	0.00719 (10)	0.3029 (2)	0.9217 (2)	0.0180 (6)
H4	−0.0288	0.3197	0.9260	0.022*
C5	0.02444 (10)	0.1897 (2)	0.9198 (2)	0.0161 (6)
H5	−0.0002	0.1297	0.9238	0.019*
C6	0.07880 (10)	0.1623 (2)	0.91183 (18)	0.0110 (6)
C7	0.09346 (10)	0.0426 (2)	0.91314 (18)	0.0114 (6)
H7	0.0662	−0.0115	0.9188	0.014*
C8	0.15275 (10)	−0.1198 (2)	0.91053 (18)	0.0092 (6)
C9	0.11626 (10)	−0.2052 (2)	0.93648 (19)	0.0123 (6)
H9	0.0819	−0.1844	0.9525	0.015*
C10	0.13142 (10)	−0.3207 (2)	0.93819 (18)	0.0123 (6)
H10	0.1071	−0.3777	0.9553	0.015*
C11	0.18272 (10)	−0.3529 (2)	0.91454 (18)	0.0124 (6)
H11	0.1925	−0.4311	0.9157	0.015*
C12	0.21902 (10)	−0.2690 (2)	0.88938 (18)	0.0109 (6)
H12	0.2533	−0.2906	0.8736	0.013*
C13	0.20450 (10)	−0.1518 (2)	0.88751 (18)	0.0096 (5)
C14	0.28922 (10)	−0.0719 (2)	0.84750 (19)	0.0110 (6)
H14	0.3007	−0.1480	0.8385	0.013*
C15	0.32741 (10)	0.0188 (2)	0.83746 (18)	0.0111 (6)
C16	0.38034 (10)	−0.0164 (2)	0.82023 (18)	0.0145 (6)
H16	0.3878	−0.0954	0.8143	0.017*
C17	0.42059 (10)	0.0627 (2)	0.81212 (19)	0.0155 (6)
H17	0.4548	0.0377	0.7998	0.019*
C18	0.40976 (10)	0.1809 (2)	0.82255 (18)	0.0142 (6)
H18	0.4371	0.2350	0.8181	0.017*
C19	0.35893 (10)	0.2184 (2)	0.83938 (19)	0.0136 (6)
H19	0.3525	0.2978	0.8462	0.016*
C20	0.31675 (10)	0.1395 (2)	0.84649 (18)	0.0094 (6)
N1	0.23943 (8)	−0.05699 (18)	0.86829 (15)	0.0098 (5)
N2	0.14151 (8)	0.00196 (18)	0.90708 (15)	0.0092 (5)
N3	0.17896 (8)	0.07150 (19)	0.70029 (16)	0.0131 (5)
N4	0.13255 (9)	0.05323 (19)	0.67637 (16)	0.0136 (5)
N5	0.08768 (9)	0.0341 (2)	0.65186 (17)	0.0234 (6)
O1	0.16772 (7)	0.23708 (15)	0.89293 (13)	0.0127 (4)
O2	0.26797 (6)	0.18073 (15)	0.85790 (12)	0.0113 (4)
O1W	0.23229 (7)	0.08568 (17)	1.05761 (13)	0.0138 (4)
O2W	0.0000	−0.0960 (3)	0.7500	0.0383 (8)
H1W	0.2366 (10)	0.1525 (7)	1.0796 (16)	0.023 (9)*
H2W	0.2189 (11)	0.0413 (15)	1.0991 (14)	0.037 (10)*
H3W	0.0224 (11)	−0.056 (3)	0.723 (3)	0.064 (13)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.0082 (2)	0.0069 (2)	0.0122 (2)	−0.00022 (17)	0.00244 (16)	−0.00015 (16)
C1	0.0133 (14)	0.0136 (14)	0.0037 (13)	0.0011 (11)	0.0004 (10)	0.0013 (11)
C2	0.0163 (14)	0.0085 (14)	0.0124 (14)	0.0000 (11)	0.0008 (11)	0.0017 (11)
C3	0.0190 (15)	0.0117 (15)	0.0162 (15)	0.0046 (12)	0.0017 (12)	0.0029 (11)
C4	0.0105 (14)	0.0172 (16)	0.0271 (16)	0.0050 (12)	0.0059 (12)	0.0031 (13)
C5	0.0130 (14)	0.0117 (15)	0.0239 (16)	−0.0027 (11)	0.0035 (12)	0.0033 (12)
C6	0.0149 (14)	0.0083 (14)	0.0101 (14)	0.0023 (11)	0.0031 (11)	0.0004 (11)
C7	0.0121 (14)	0.0118 (15)	0.0105 (14)	−0.0045 (11)	0.0024 (11)	−0.0004 (11)
C8	0.0129 (14)	0.0080 (14)	0.0064 (13)	−0.0001 (11)	−0.0005 (10)	−0.0019 (10)
C9	0.0119 (14)	0.0114 (15)	0.0138 (14)	−0.0013 (11)	0.0035 (11)	−0.0016 (11)
C10	0.0159 (14)	0.0119 (15)	0.0092 (14)	−0.0046 (11)	0.0014 (11)	0.0001 (11)
C11	0.0205 (15)	0.0067 (14)	0.0093 (13)	0.0021 (11)	−0.0028 (11)	0.0002 (11)
C12	0.0129 (14)	0.0145 (15)	0.0052 (13)	0.0043 (11)	0.0005 (10)	−0.0027 (10)
C13	0.0124 (14)	0.0120 (14)	0.0042 (13)	−0.0028 (11)	−0.0007 (10)	−0.0015 (11)
C14	0.0142 (14)	0.0106 (15)	0.0082 (13)	0.0035 (11)	0.0011 (11)	0.0006 (10)
C15	0.0128 (14)	0.0144 (14)	0.0062 (13)	−0.0007 (11)	0.0016 (10)	0.0010 (11)
C16	0.0170 (15)	0.0162 (15)	0.0104 (14)	0.0038 (12)	0.0021 (11)	0.0012 (11)
C17	0.0069 (14)	0.0278 (17)	0.0119 (14)	0.0028 (12)	0.0011 (11)	0.0015 (12)
C18	0.0107 (14)	0.0240 (17)	0.0077 (14)	−0.0048 (12)	−0.0008 (11)	0.0009 (12)
C19	0.0193 (15)	0.0119 (15)	0.0095 (14)	−0.0023 (12)	−0.0006 (11)	−0.0023 (11)
C20	0.0082 (13)	0.0175 (15)	0.0026 (12)	0.0006 (11)	0.0005 (10)	0.0020 (11)
N1	0.0135 (12)	0.0086 (12)	0.0073 (11)	0.0005 (9)	0.0014 (9)	0.0004 (9)
N2	0.0118 (11)	0.0070 (12)	0.0088 (11)	0.0010 (9)	0.0018 (9)	0.0002 (9)
N3	0.0097 (12)	0.0190 (14)	0.0108 (12)	−0.0020 (9)	0.0013 (9)	0.0014 (9)
N4	0.0198 (14)	0.0138 (13)	0.0078 (12)	0.0027 (10)	0.0047 (10)	0.0002 (9)
N5	0.0122 (13)	0.0395 (17)	0.0183 (13)	0.0007 (12)	−0.0002 (10)	0.0000 (11)
O1	0.0099 (9)	0.0074 (10)	0.0213 (10)	−0.0001 (7)	0.0038 (7)	−0.0005 (8)
O2	0.0114 (9)	0.0097 (10)	0.0133 (10)	−0.0007 (8)	0.0037 (7)	0.0011 (8)
O1W	0.0192 (11)	0.0090 (11)	0.0133 (10)	−0.0039 (8)	0.0027 (8)	−0.0004 (9)
O2W	0.025 (2)	0.028 (2)	0.063 (2)	0.000	0.0130 (18)	0.000

Geometric parameters (Å, º) top

Mn1—O1	1.8636 (18)	C10—H10	0.9300
Mn1—O2	1.8844 (18)	C11—C12	1.379 (3)
Mn1—N2	1.986 (2)	C11—H11	0.9300
Mn1—N1	1.988 (2)	C12—C13	1.393 (3)
Mn1—N3	2.306 (2)	C12—H12	0.9300
Mn1—O1W	2.321 (2)	C13—N1	1.430 (3)
C1—O1	1.324 (3)	C14—N1	1.307 (3)
C1—C2	1.397 (3)	C14—C15	1.427 (3)
C1—C6	1.422 (3)	C14—H14	0.9300
C2—C3	1.377 (3)	C15—C20	1.418 (4)
C2—H2	0.9300	C15—C16	1.420 (3)
C3—C4	1.398 (4)	C16—C17	1.367 (4)
C3—H3	0.9300	C16—H16	0.9300
C4—C5	1.371 (4)	C17—C18	1.392 (4)
C4—H4	0.9300	C17—H17	0.9300
C5—C6	1.411 (3)	C18—C19	1.378 (3)
C5—H5	0.9300	C18—H18	0.9300
C6—C7	1.422 (4)	C19—C20	1.401 (3)
C7—N2	1.301 (3)	C19—H19	0.9300
C7—H7	0.9300	C20—O2	1.330 (3)
C8—C9	1.397 (3)	N3—N4	1.200 (3)
C8—C13	1.401 (3)	N4—N5	1.167 (3)
C8—N2	1.425 (3)	O1W—H1W	0.820 (11)
C9—C10	1.379 (4)	O1W—H2W	0.82 (2)
C9—H9	0.9300	O2W—H3W	0.82 (3)
C10—C11	1.393 (3)

O1—Mn1—O2	90.68 (8)	C11—C10—H10	119.7
O1—Mn1—N2	92.69 (8)	C12—C11—C10	120.0 (2)
O2—Mn1—N2	175.37 (8)	C12—C11—H11	120.0
O1—Mn1—N1	175.33 (8)	C10—C11—H11	120.0
O2—Mn1—N1	93.71 (8)	C11—C12—C13	120.1 (2)
N2—Mn1—N1	82.83 (9)	C11—C12—H12	119.9
O1—Mn1—N3	95.95 (8)	C13—C12—H12	119.9
O2—Mn1—N3	96.55 (7)	C12—C13—C8	119.7 (2)
N2—Mn1—N3	86.26 (8)	C12—C13—N1	125.1 (2)
N1—Mn1—N3	85.12 (8)	C8—C13—N1	115.1 (2)
O1—Mn1—O1W	94.00 (7)	N1—C14—C15	125.5 (2)
O2—Mn1—O1W	88.14 (7)	N1—C14—H14	117.2
N2—Mn1—O1W	88.47 (7)	C15—C14—H14	117.2
N1—Mn1—O1W	84.58 (7)	C20—C15—C16	118.3 (2)
N3—Mn1—O1W	168.94 (7)	C20—C15—C14	125.0 (2)
O1—C1—C2	118.3 (2)	C16—C15—C14	116.6 (2)
O1—C1—C6	123.5 (2)	C17—C16—C15	121.8 (3)
C2—C1—C6	118.2 (2)	C17—C16—H16	119.1
C3—C2—C1	121.3 (2)	C15—C16—H16	119.1
C3—C2—H2	119.4	C16—C17—C18	119.3 (2)
C1—C2—H2	119.4	C16—C17—H17	120.3
C2—C3—C4	120.9 (3)	C18—C17—H17	120.3
C2—C3—H3	119.6	C19—C18—C17	120.6 (2)
C4—C3—H3	119.6	C19—C18—H18	119.7
C5—C4—C3	119.1 (2)	C17—C18—H18	119.7
C5—C4—H4	120.5	C18—C19—C20	121.3 (3)
C3—C4—H4	120.5	C18—C19—H19	119.3
C4—C5—C6	121.4 (2)	C20—C19—H19	119.3
C4—C5—H5	119.3	O2—C20—C19	118.9 (2)
C6—C5—H5	119.3	O2—C20—C15	122.5 (2)
C5—C6—C1	119.2 (2)	C19—C20—C15	118.6 (2)
C5—C6—C7	117.7 (2)	C14—N1—C13	122.8 (2)
C1—C6—C7	123.1 (2)	C14—N1—Mn1	124.04 (18)
N2—C7—C6	125.9 (2)	C13—N1—Mn1	113.16 (16)
N2—C7—H7	117.1	C7—N2—C8	122.2 (2)
C6—C7—H7	117.1	C7—N2—Mn1	124.61 (18)
C9—C8—C13	119.9 (2)	C8—N2—Mn1	112.96 (15)
C9—C8—N2	124.3 (2)	N4—N3—Mn1	117.69 (16)
C13—C8—N2	115.8 (2)	N5—N4—N3	178.8 (3)
C10—C9—C8	119.6 (2)	C1—O1—Mn1	129.44 (16)
C10—C9—H9	120.2	C20—O2—Mn1	128.82 (16)
C8—C9—H9	120.2	Mn1—O1W—H1W	107.2 (17)
C9—C10—C11	120.7 (2)	Mn1—O1W—H2W	123.5 (18)
C9—C10—H10	119.7	H1W—O1W—H2W	114.6 (19)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W···N3ⁱ	0.82 (2)	2.12 (2)	2.937 (3)	176 (3)
O1W—H1W···O2ⁱⁱ	0.82 (1)	2.08 (1)	2.885 (3)	169 (2)
O2W—H3W···N5	0.82 (3)	2.18 (3)	3.000 (3)	173 (4)

Symmetry codes: (i) x, −y, z+1/2; (ii) −x+1/2, −y+1/2, −z+2.

Experimental details

Crystal data
Chemical formula	[Mn(C₂₀H₁₄N₂O₂)(N₃)(H₂O)]·0.5H₂O
M_r	438.33
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	25.10 (1), 11.478 (5), 12.599 (5)
β (°)	94.175 (3)
V (Å³)	3620 (3)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	0.77
Crystal size (mm)	0.12 × 0.10 × 0.08

Data collection
Diffractometer	Bruker APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2004)
T_min, T_max	0.914, 0.941
No. of measured, independent and observed [I > 2σ(I)] reflections	11927, 3162, 2371
R_int	0.082
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.037, 0.086, 1.00
No. of reflections	3162
No. of parameters	280
No. of restraints	4
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.32, −0.38

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Mn1—O1	1.8636 (18)	Mn1—N1	1.988 (2)
Mn1—O2	1.8844 (18)	Mn1—N3	2.306 (2)
Mn1—N2	1.986 (2)	Mn1—O1W	2.321 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W···N3ⁱ	0.82 (2)	2.12 (2)	2.937 (3)	176 (3)
O1W—H1W···O2ⁱⁱ	0.820 (11)	2.076 (6)	2.885 (3)	169 (2)
O2W—H3W···N5	0.82 (3)	2.18 (3)	3.000 (3)	173 (4)

Symmetry codes: (i) x, −y, z+1/2; (ii) −x+1/2, −y+1/2, −z+2.

Acknowledgements

The authors thank the National Ministry of Science and Technology of China (grant No. 2001CB6105–07) for support.

References

Alam, M. A., Nethaji, M. & Ray, M. (2003). Angew. Chem. Int. Ed. 42, 1940–1942. Web of Science CSD CrossRef CAS Google Scholar
Bruker (2004). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Zelewsky, A. & von Knof, U. (1999). Angew. Chem. Int. Ed. 38, 302–322. Google Scholar

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Volume 65| Part 7| July 2009| Page m707

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

Aqua­azido­{2,2′-[o-phenylenebis(nitrilo­methyl­­idyne)]diphenolato}manganese(III) hemihydrate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Aquaazido{2,2′-[o-phenylenebis(nitrilomethylidyne)]diphenolato}manganese(III) hemihydrate