Tris(ethyl­enediamine)manganese(II) sulfate

Lu, J.

doi:10.1107/S1600536809034874

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 10| October 2009| Page m1187

doi:10.1107/S1600536809034874

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RETRACTED ARTICLE

This article has been retracted. To view the retraction notice, click here.

Retracted: Tris(ethylenediamine)manganese(II) sulfate

Jing Lu ^a ^*

^aSchool of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, People's Republic of China
^*Correspondence e-mail: lujing@lcu.edu.cn

(Received 21 August 2009; accepted 31 August 2009; online 9 September 2009)

In the title compound, [Mn(C₂H₈N₂)₃]SO₄, the metal atom (site symmetry 3.2) is coordinated by six N atoms from three ethylenediamine (en) ligands in a slightly distorted octahedral geometry. The en ligands are generated from one half-molecule in the asymmetric unit. The O atoms of the sulfate anion (S site symmetry 3.2) are disordered over four orientations in a 0.220 (12):0.210 (13):0.203 (14):0.10 (2) ratio, with one of the O atoms having site symmetry 3. In the crystal, the ions are connected by N—H⋯O hydrogen bonds, forming a three-dimensional network.

Related literature

For a structure containing Mn^II and aromatic amine ligands, see: Shang et al. (2009 ). For other compounds containing transition metals coordinated by ethylenediamine, see: Cullen & Lingafelter (1970 ); Daniels et al. (1995 ); Jameson et al. (1982 ).

Experimental

Crystal data

[Mn(C₂H₈N₂)₃]SO₄
M_r = 331.31
Trigonal, $[P \overline 31c ]$
a = 8.9460 (13) Å
c = 9.6230 (19) Å
V = 666.96 (19) Å³
Z = 2
Mo Kα radiation
μ = 1.17 mm⁻¹
T = 293 K
0.35 × 0.30 × 0.28 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2003 ) T_min = 0.686, T_max = 0.736
2640 measured reflections
402 independent reflections
386 reflections with I > 2σ(I)
R_int = 0.031

Refinement

R[F² > 2σ(F²)] = 0.058
wR(F²) = 0.159
S = 1.55
402 reflections
44 parameters
2 restraints
H-atom parameters constrained
Δρ_max = 0.72 e Å⁻³
Δρ_min = −0.63 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Mn1—N1	2.125 (6)

N1ⁱ—Mn1—N1	81.6 (3)
Symmetry code: (i) $[-x+y, y, -z+{\script{3\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯O1ⁱⁱ	0.90	2.28	3.16 (3)	166
N1—H1A⋯O1ⁱⁱⁱ	0.90	2.43	3.15 (3)	138
N1—H1B⋯O1^iv	0.90	2.17	3.06 (2)	170
N1—H1B⋯O2^iv	0.90	2.11	3.00 (2)	167
N1—H1A⋯O2^v	0.90	2.14	2.95 (5)	148
N1—H1A⋯O3ⁱⁱ	0.90	1.92	2.80 (3)	166
N1—H1B⋯O3^iv	0.90	2.15	2.96 (3)	150
N1—H1B⋯O3^vi	0.90	2.36	3.18 (3)	152
N1—H1B⋯O4^vii	0.90	2.15	2.94 (7)	146
Symmetry codes: (ii) x-y+1, x, -z+1; (iii) $[-x+1, -x+y, z+{\script{1\over 2}}]$ ; (iv) -x+y, -x+1, z+1; (v) -x+1, -y+1, -z+1; (vi) -y+1, x-y+1, z+1; (vii) x, y, z+1.

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); 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.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809034874/hb5060sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809034874/hb5060Isup2.hkl

checkCIF report

Comment top

Ethylenediamine (en) ligand has been seen in a number of coordination compound (Cullen et al., 1970; Daniels et al., 1995 and Jameson et al., 1982), because it can not only chelate metal center by two nitrogen atoms, but also offer hydrogen atoms to form N—H···X hydrogen bonds. In this paper, we report the structure of the title compound, (I).

In the title compound (Fig. 1), [Mn(C₂H₈N₂)₃]SO₄, the cation and anion are situated on a sixfold rotation axis. The Mn(II) is coordinated by six N atoms from three en ligands in a distorted octahedral geometry. The Mn—N bond length is 2.129 Å, which is shorter than the distance between Mn(II) and aromatic nitrogen atom (Shang et al., 2009). The O atoms of the sulfate anions are disordered. The disordered anions hydrogen bond with the coordination cations by N—H···O hydrogen bonds, forming three-dimensional supramolecular network. The hydrogen bond is listed in table 1.

Related literature top

For a structure contaiing Mn(II) and aromatic amine ligands, see: Shang et al. (2009). For other compounds containing transition metals coordinated by ethylenediamine, see: Cullen & Lingafelter (1970); Daniels et al. (1995); Jameson et al. (1982).

Experimental top

Manganese sulfate (0.2 mmol) and malic acid (0.4 mmol) were added to water (15 ml). The pH value was adjusted to 9 by en. Violet blocks of (I) were obtained after several days in 30% yield. Elemental analysis, Found:C, 21.73; H, 7.24; N, 25.35%. Calc. for C₆H₂₄N₆MnSO₄: C, 21.20; H, 7.00; N, 24.93%.

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXS97 (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) with 50% probability displacement ellipsoids. The symmetry codes for N and C atoms: A -y+1, x-y+1, z; B -x+y, -x+1, z; C -y+1, -x+1, -z+3/2; D -x+y, y, -z+3/2; E x, x-y+1, -z+3/2.

Tris(ethylenediamine)manganese(II) sulfate top

Crystal data top

[Mn(C₂H₈N₂)₃]SO₄	D_x = 1.650 Mg m⁻³
M_r = 331.31	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P31c	Cell parameters from 2640 reflections
a = 8.9460 (13) Å	θ = 2.6–25.0°
c = 9.6230 (19) Å	µ = 1.17 mm⁻¹
V = 666.96 (19) Å³	T = 293 K
Z = 2	Block, violet
F(000) = 350	0.35 × 0.30 × 0.28 mm

Data collection top

Bruker SMART CCD diffractometer	402 independent reflections
Radiation source: fine-focus sealed tube	386 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.031
ω scans	θ_max = 25.0°, θ_min = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2003)	h = −8→10
T_min = 0.686, T_max = 0.736	k = −10→4
2640 measured reflections	l = −11→11

Refinement top

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)] = 0.058	H-atom parameters constrained
wR(F²) = 0.159	w = 1/[σ²(F_o²) + (0.0637P)² + 1.2291P] where P = (F_o² + 2F_c²)/3
S = 1.55	(Δ/σ)_max = 0.001
402 reflections	Δρ_max = 0.72 e Å⁻³
44 parameters	Δρ_min = −0.63 e Å⁻³
2 restraints	Extinction correction: SHELXS97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.051 (15)

Crystal data top

[Mn(C₂H₈N₂)₃]SO₄	Z = 2
M_r = 331.31	Mo Kα radiation
Trigonal, P31c	µ = 1.17 mm⁻¹
a = 8.9460 (13) Å	T = 293 K
c = 9.6230 (19) Å	0.35 × 0.30 × 0.28 mm
V = 666.96 (19) Å³

Data collection top

Bruker SMART CCD diffractometer	402 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2003)	386 reflections with I > 2σ(I)
T_min = 0.686, T_max = 0.736	R_int = 0.031
2640 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.058	2 restraints
wR(F²) = 0.159	H-atom parameters constrained
S = 1.55	Δρ_max = 0.72 e Å⁻³
402 reflections	Δρ_min = −0.63 e Å⁻³
44 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	Occ. (<1)
Mn1	0.3333	0.6667	0.7500	0.0200 (8)
S1	0.3333	0.6667	0.2500	0.0332 (10)
O1	0.489 (3)	0.813 (4)	0.186 (2)	0.051 (4)	0.220 (12)
O2	0.489 (3)	0.721 (6)	0.163 (3)	0.051 (4)	0.210 (13)
O3	0.373 (6)	0.799 (3)	0.146 (3)	0.051 (4)	0.203 (14)
O4	0.3333	0.6667	0.114 (9)	0.051 (4)	0.10 (2)
N1	0.3136 (7)	0.4590 (8)	0.8712 (6)	0.0427 (14)
H1A	0.4072	0.4479	0.8581	0.051*
H1B	0.3070	0.4791	0.9621	0.051*
C1	0.1570 (9)	0.3007 (9)	0.8275 (8)	0.0491 (18)
H1C	0.0561	0.2960	0.8692	0.059*
H1D	0.1626	0.2002	0.8578	0.059*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mn1	0.0208 (9)	0.0208 (9)	0.0184 (12)	0.0104 (5)	0.000	0.000
S1	0.0327 (13)	0.0327 (13)	0.034 (2)	0.0163 (7)	0.000	0.000
O1	0.045 (8)	0.042 (12)	0.047 (7)	0.008 (10)	0.007 (6)	0.000 (8)
O2	0.045 (8)	0.042 (12)	0.047 (7)	0.008 (10)	0.007 (6)	0.000 (8)
O3	0.045 (8)	0.042 (12)	0.047 (7)	0.008 (10)	0.007 (6)	0.000 (8)
O4	0.045 (8)	0.042 (12)	0.047 (7)	0.008 (10)	0.007 (6)	0.000 (8)
N1	0.041 (3)	0.051 (3)	0.040 (3)	0.026 (3)	0.008 (2)	0.000 (2)
C1	0.051 (4)	0.053 (4)	0.054 (4)	0.035 (3)	0.002 (3)	−0.006 (3)

Geometric parameters (Å, º) top

Mn1—N1ⁱ	2.125 (6)	S1—O2ⁱⁱⁱ	1.48 (3)
Mn1—N1ⁱⁱ	2.125 (6)	S1—O2^vii	1.48 (3)
Mn1—N1ⁱⁱⁱ	2.125 (6)	S1—O2^viii	1.48 (3)
Mn1—N1^iv	2.125 (6)	S1—O2ⁱⁱ	1.48 (3)
Mn1—N1^v	2.125 (6)	O1—O1^viii	1.74 (5)
Mn1—N1	2.125 (6)	O2—O2^viii	1.72 (6)
S1—O4	1.30 (9)	O3—O3ⁱⁱⁱ	1.82 (4)
S1—O4^vi	1.30 (9)	O3—O3ⁱⁱ	1.82 (4)
S1—O3^vii	1.45 (3)	N1—C1	1.471 (9)
S1—O3ⁱⁱⁱ	1.45 (3)	N1—H1A	0.9000
S1—O3	1.45 (3)	N1—H1B	0.9000
S1—O3^vi	1.45 (3)	C1—C1^iv	1.496 (15)
S1—O3ⁱⁱ	1.45 (3)	C1—H1C	0.9700
S1—O3^viii	1.45 (3)	C1—H1D	0.9700

N1ⁱ—Mn1—N1ⁱⁱ	81.6 (3)	O3ⁱⁱ—S1—O2ⁱⁱⁱ	99.3 (13)
N1ⁱ—Mn1—N1ⁱⁱⁱ	93.5 (3)	O3^viii—S1—O2ⁱⁱⁱ	170.3 (17)
N1ⁱⁱ—Mn1—N1ⁱⁱⁱ	92.7 (2)	O4—S1—O2^vii	124.3 (10)
N1ⁱ—Mn1—N1^iv	92.7 (2)	O4^vi—S1—O2^vii	55.7 (10)
N1ⁱⁱ—Mn1—N1^iv	93.5 (3)	O3^vii—S1—O2^vii	62.4 (15)
N1ⁱⁱⁱ—Mn1—N1^iv	171.8 (3)	O3ⁱⁱⁱ—S1—O2^vii	97 (2)
N1ⁱ—Mn1—N1^v	92.7 (2)	O3—S1—O2^vii	94 (3)
N1ⁱⁱ—Mn1—N1^v	171.8 (3)	O3^vi—S1—O2^vii	30.1 (12)
N1ⁱⁱⁱ—Mn1—N1^v	81.6 (3)	O3ⁱⁱ—S1—O2^vii	170.3 (17)
N1^iv—Mn1—N1^v	92.7 (2)	O3^viii—S1—O2^vii	99.3 (13)
N1ⁱ—Mn1—N1	171.8 (3)	O2ⁱⁱⁱ—S1—O2^vii	71 (2)
N1ⁱⁱ—Mn1—N1	92.7 (2)	O4—S1—O2^viii	124.3 (11)
N1ⁱⁱⁱ—Mn1—N1	92.7 (2)	O4^vi—S1—O2^viii	55.7 (10)
N1^iv—Mn1—N1	81.6 (3)	O3^vii—S1—O2^viii	30.1 (12)
N1^v—Mn1—N1	93.5 (3)	O3ⁱⁱⁱ—S1—O2^viii	170.3 (18)
O4—S1—O4^vi	180.000 (19)	O3—S1—O2^viii	97 (2)
O4—S1—O3^vii	133.7 (10)	O3^vi—S1—O2^viii	99.3 (13)
O4^vi—S1—O3^vii	46.3 (10)	O3ⁱⁱ—S1—O2^viii	94 (3)
O4—S1—O3ⁱⁱⁱ	46.3 (10)	O3^viii—S1—O2^viii	62.4 (15)
O4^vi—S1—O3ⁱⁱⁱ	133.7 (10)	O2ⁱⁱⁱ—S1—O2^viii	116 (3)
O3^vii—S1—O3ⁱⁱⁱ	156 (4)	O2^vii—S1—O2^viii	91.3 (15)
O4—S1—O3	46.3 (10)	O4—S1—O2ⁱⁱ	55.7 (10)
O4^vi—S1—O3	133.7 (10)	O4^vi—S1—O2ⁱⁱ	124.3 (10)
O3^vii—S1—O3	90 (2)	O3^vii—S1—O2ⁱⁱ	170.3 (17)
O3ⁱⁱⁱ—S1—O3	77.5 (15)	O3ⁱⁱⁱ—S1—O2ⁱⁱ	30.1 (12)
O4—S1—O3^vi	133.7 (10)	O3—S1—O2ⁱⁱ	99.3 (13)
O4^vi—S1—O3^vi	46.3 (10)	O3^vi—S1—O2ⁱⁱ	97 (2)
O3^vii—S1—O3^vi	77.5 (15)	O3ⁱⁱ—S1—O2ⁱⁱ	62.4 (15)
O3ⁱⁱⁱ—S1—O3^vi	90 (2)	O3^viii—S1—O2ⁱⁱ	94 (3)
O3—S1—O3^vi	121 (3)	O2ⁱⁱⁱ—S1—O2ⁱⁱ	91.3 (15)
O4—S1—O3ⁱⁱ	46.3 (10)	O2^vii—S1—O2ⁱⁱ	116 (3)
O4^vi—S1—O3ⁱⁱ	133.7 (10)	O2^viii—S1—O2ⁱⁱ	147 (4)
O3^vii—S1—O3ⁱⁱ	121 (3)	S1—O1—O1^viii	54.1 (11)
O3ⁱⁱⁱ—S1—O3ⁱⁱ	77.5 (15)	S1—O2—O2^viii	54.5 (12)
O3—S1—O3ⁱⁱ	77.5 (15)	S1—O3—O3ⁱⁱⁱ	51.2 (7)
O3^vi—S1—O3ⁱⁱ	156 (4)	S1—O3—O3ⁱⁱ	51.2 (7)
O4—S1—O3^viii	133.7 (10)	O3ⁱⁱⁱ—O3—O3ⁱⁱ	60.000 (1)
O4^vi—S1—O3^viii	46.3 (10)	C1—N1—Mn1	107.9 (4)
O3^vii—S1—O3^viii	77.5 (15)	C1—N1—H1A	110.1
O3ⁱⁱⁱ—S1—O3^viii	121 (3)	Mn1—N1—H1A	110.1
O3—S1—O3^viii	156 (4)	C1—N1—H1B	110.1
O3^vi—S1—O3^viii	77.5 (15)	Mn1—N1—H1B	110.1
O3ⁱⁱ—S1—O3^viii	90 (2)	H1A—N1—H1B	108.4
O4—S1—O2ⁱⁱⁱ	55.7 (10)	N1—C1—C1^iv	108.9 (5)
O4^vi—S1—O2ⁱⁱⁱ	124.3 (10)	N1—C1—H1C	109.9
O3^vii—S1—O2ⁱⁱⁱ	97 (2)	C1^iv—C1—H1C	109.9
O3ⁱⁱⁱ—S1—O2ⁱⁱⁱ	62.4 (15)	N1—C1—H1D	109.9
O3—S1—O2ⁱⁱⁱ	30.1 (12)	C1^iv—C1—H1D	109.9
O3^vi—S1—O2ⁱⁱⁱ	94 (3)	H1C—C1—H1D	108.3

O4—S1—O1—O1^viii	−129 (2)	O3^vii—S1—O3—O3ⁱⁱⁱ	−159 (3)
O4^vi—S1—O1—O1^viii	51 (2)	O3^vi—S1—O3—O3ⁱⁱⁱ	−83 (2)
O3^vii—S1—O1—O1^viii	65.8 (19)	O3ⁱⁱ—S1—O3—O3ⁱⁱⁱ	79.8 (10)
O3ⁱⁱⁱ—S1—O1—O1^viii	−140 (3)	O3^viii—S1—O3—O3ⁱⁱⁱ	141.8 (18)
O3—S1—O1—O1^viii	179 (3)	O2ⁱⁱⁱ—S1—O3—O3ⁱⁱⁱ	−55 (3)
O3^vi—S1—O1—O1^viii	100 (3)	O2^vii—S1—O3—O3ⁱⁱⁱ	−96 (3)
O3ⁱⁱ—S1—O1—O1^viii	−77 (2)	O2^viii—S1—O3—O3ⁱⁱⁱ	172 (3)
O3^viii—S1—O1—O1^viii	0 (2)	O2ⁱⁱ—S1—O3—O3ⁱⁱⁱ	20.9 (16)
O2ⁱⁱⁱ—S1—O1—O1^viii	171 (2)	O4—S1—O3—O3ⁱⁱ	−39.9 (5)
O2^vii—S1—O1—O1^viii	112.2 (18)	O4^vi—S1—O3—O3ⁱⁱ	140.1 (5)
O2^viii—S1—O1—O1^viii	34.5 (19)	O3^vii—S1—O3—O3ⁱⁱ	122 (4)
O2ⁱⁱ—S1—O1—O1^viii	−108 (3)	O3ⁱⁱⁱ—S1—O3—O3ⁱⁱ	−79.8 (10)
O4—S1—O2—O2^viii	163 (4)	O3^vi—S1—O3—O3ⁱⁱ	−163 (2)
O4^vi—S1—O2—O2^viii	−17 (4)	O3^viii—S1—O3—O3ⁱⁱ	62 (2)
O3^vii—S1—O2—O2^viii	20 (2)	O2ⁱⁱⁱ—S1—O3—O3ⁱⁱ	−135 (3)
O3ⁱⁱⁱ—S1—O2—O2^viii	179 (4)	O2^vii—S1—O3—O3ⁱⁱ	−176 (3)
O3—S1—O2—O2^viii	109 (4)	O2^viii—S1—O3—O3ⁱⁱ	92 (3)
O3^vi—S1—O2—O2^viii	−3 (22)	O2ⁱⁱ—S1—O3—O3ⁱⁱ	−58.9 (16)
O3ⁱⁱ—S1—O2—O2^viii	−136 (5)	N1ⁱ—Mn1—N1—C1	32.2 (4)
O3^viii—S1—O2—O2^viii	−58 (2)	N1ⁱⁱ—Mn1—N1—C1	78.5 (5)
O2ⁱⁱⁱ—S1—O2—O2^viii	117 (4)	N1ⁱⁱⁱ—Mn1—N1—C1	171.4 (4)
O2^vii—S1—O2—O2^viii	61 (2)	N1^iv—Mn1—N1—C1	−14.7 (3)
O2ⁱⁱ—S1—O2—O2^viii	−151 (4)	N1^v—Mn1—N1—C1	−106.9 (4)
O4—S1—O3—O3ⁱⁱⁱ	39.9 (5)	Mn1—N1—C1—C1^iv	41.5 (7)
O4^vi—S1—O3—O3ⁱⁱⁱ	−140.1 (5)

Symmetry codes: (i) x, x−y+1, −z+3/2; (ii) −x+y, −x+1, z; (iii) −y+1, x−y+1, z; (iv) −x+y, y, −z+3/2; (v) −y+1, −x+1, −z+3/2; (vi) −y+1, −x+1, −z+1/2; (vii) −x+y, y, −z+1/2; (viii) x, x−y+1, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O1^ix	0.90	2.28	3.16 (3)	166
N1—H1A···O1^x	0.90	2.43	3.15 (3)	138
N1—H1B···O1^xi	0.90	2.17	3.06 (2)	170
N1—H1B···O2^xi	0.90	2.11	3.00 (2)	167
N1—H1A···O2^xii	0.90	2.14	2.95 (5)	148
N1—H1A···O3^ix	0.90	1.92	2.80 (3)	166
N1—H1B···O3^xi	0.90	2.15	2.96 (3)	150
N1—H1B···O3^xiii	0.90	2.36	3.18 (3)	152
N1—H1B···O4^xiv	0.90	2.15	2.94 (7)	146

Symmetry codes: (ix) x−y+1, x, −z+1; (x) −x+1, −x+y, z+1/2; (xi) −x+y, −x+1, z+1; (xii) −x+1, −y+1, −z+1; (xiii) −y+1, x−y+1, z+1; (xiv) x, y, z+1.

Experimental details

Crystal data
Chemical formula	[Mn(C₂H₈N₂)₃]SO₄
M_r	331.31
Crystal system, space group	Trigonal, P31c
Temperature (K)	293
a, c (Å)	8.9460 (13), 9.6230 (19)
V (Å³)	666.96 (19)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.17
Crystal size (mm)	0.35 × 0.30 × 0.28

Data collection
Diffractometer	Bruker SMART CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2003)
T_min, T_max	0.686, 0.736
No. of measured, independent and observed [I > 2σ(I)] reflections	2640, 402, 386
R_int	0.031
(sin θ/λ)_max (Å⁻¹)	0.594

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.058, 0.159, 1.55
No. of reflections	402
No. of parameters	44
No. of restraints	2
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.72, −0.63

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SHELXS97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected geometric parameters (Å, º) top

Mn1—N1	2.125 (6)

N1ⁱ—Mn1—N1	81.6 (3)

Symmetry code: (i) −x+y, y, −z+3/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O1ⁱⁱ	0.90	2.28	3.16 (3)	166
N1—H1A···O1ⁱⁱⁱ	0.90	2.43	3.15 (3)	138
N1—H1B···O1^iv	0.90	2.17	3.06 (2)	170
N1—H1B···O2^iv	0.90	2.11	3.00 (2)	167
N1—H1A···O2^v	0.90	2.14	2.95 (5)	148
N1—H1A···O3ⁱⁱ	0.90	1.92	2.80 (3)	166
N1—H1B···O3^iv	0.90	2.15	2.96 (3)	150
N1—H1B···O3^vi	0.90	2.36	3.18 (3)	152
N1—H1B···O4^vii	0.90	2.15	2.94 (7)	146

Symmetry codes: (ii) x−y+1, x, −z+1; (iii) −x+1, −x+y, z+1/2; (iv) −x+y, −x+1, z+1; (v) −x+1, −y+1, −z+1; (vi) −y+1, x−y+1, z+1; (vii) x, y, z+1.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. 20671048) and the Doctoral Foundation of Liaocheng University (No. 31805).

References

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