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The redetermined structure of the title compound, [Mn(C4H5NO4)(H2O)2]n, including the full hydrogen-bonding scheme, is reported; the original report was by Zhang & Lu [Acta Cryst. (2004). E60, m1189–m1190]. The structure contains polymeric chains of MnII cations bridged by imino­di­acetate (IDA) dianions. The manganese species assumes a distorted octahedral coordination geometry, formed by two IDA mol­ecules (one tridentate and one monodentate) and two water mol­ecules. The tridentate IDA chelates to the Mn atom in the facial configuration; one chelating five-membered ring is almost planar and the other adopts an envelope configuration. A significant difference of 0.118 (2) Å in Mn—Ocarboxyl bond distances is observed within the chelating IDA moiety.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804024262/hb6100sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804024262/hb6100Isup2.hkl
Contains datablock I

CCDC reference: 255403

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.021
  • wR factor = 0.051
  • Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.10 From the CIF: _reflns_number_total 1466 Count of symmetry unique reflns 893 Completeness (_total/calc) 164.17% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 573 Fraction of Friedel pairs measured 0.642 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and XP (Siemens, 1994); software used to prepare material for publication: WinGX (Farrugia, 1999).

catena-poly[[diaquamanganese(II)]-µ-iminodiacetato-κ3N,O,O'] top
Crystal data top
[Mn(C4H5NO4)(H2O)2]F(000) = 452
Mr = 222.06Dx = 1.930 Mg m3
Orthorhombic, Pca21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2acCell parameters from 3836 reflections
a = 14.5818 (15) Åθ = 3.0–26.0°
b = 5.3508 (6) ŵ = 1.72 mm1
c = 9.7958 (11) ÅT = 295 K
V = 764.31 (14) Å3Prism, colorless
Z = 40.36 × 0.32 × 0.26 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
1466 independent reflections
Radiation source: fine-focus sealed tube1440 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
Detector resolution: 10.00 pixels mm-1θmax = 27.1°, θmin = 2.8°
ω scansh = 1818
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 66
Tmin = 0.540, Tmax = 0.635l = 129
4295 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difmap (O-H and N-H) and geom (C-H)
R[F2 > 2σ(F2)] = 0.021H-atom parameters constrained
wR(F2) = 0.051 w = 1/[σ2(Fo2) + (0.0239P)2 + 0.14P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
1466 reflectionsΔρmax = 0.21 e Å3
109 parametersΔρmin = 0.19 e Å3
1 restraintAbsolute structure: Flack (1983), 573 Friedel Pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.030 (18)
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
xyzUiso*/Ueq
Mn10.558266 (18)0.63394 (5)0.50027 (4)0.02385 (9)
N10.68116 (11)0.7468 (3)0.3710 (2)0.0236 (3)
H10.70990.88110.40690.050*
O10.53536 (11)0.4775 (3)0.28685 (18)0.0316 (3)
O20.54629 (11)0.6079 (3)0.07191 (18)0.0291 (4)
O30.65804 (11)0.3480 (3)0.54612 (18)0.0337 (4)
O40.78696 (10)0.1665 (2)0.4837 (3)0.0400 (4)
O50.46108 (10)0.9330 (3)0.43057 (18)0.0303 (3)
H5A0.46291.07260.47410.050*
H5B0.40580.89360.43800.050*
O60.60267 (12)0.8983 (3)0.65723 (17)0.0362 (4)
H6A0.60971.05190.63870.050*
H6B0.56950.90320.73240.050*
C10.64496 (15)0.7964 (4)0.2340 (2)0.0278 (5)
H3B0.69430.78470.16790.033*
H3A0.62050.96500.23050.033*
C20.56952 (15)0.6107 (4)0.1966 (3)0.0241 (5)
C30.75026 (15)0.5459 (4)0.3744 (3)0.0325 (5)
H1A0.80950.61870.39580.039*
H1B0.75460.47220.28420.039*
C40.73025 (13)0.3401 (3)0.4767 (3)0.0258 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.02364 (14)0.02286 (14)0.02506 (16)0.00107 (10)0.00176 (16)0.00150 (16)
N10.0248 (8)0.0228 (8)0.0231 (8)0.0041 (7)0.0041 (7)0.0002 (7)
O10.0344 (8)0.0328 (8)0.0277 (8)0.0136 (7)0.0017 (7)0.0004 (8)
O20.0307 (8)0.0320 (8)0.0246 (9)0.0045 (6)0.0074 (6)0.0001 (7)
O30.0312 (9)0.0287 (7)0.0412 (10)0.0029 (6)0.0070 (7)0.0104 (6)
O40.0280 (7)0.0285 (7)0.0637 (13)0.0042 (6)0.0014 (10)0.0057 (10)
O50.0266 (7)0.0287 (7)0.0356 (9)0.0001 (6)0.0009 (7)0.0036 (7)
O60.0473 (11)0.0345 (9)0.0269 (10)0.0078 (8)0.0048 (8)0.0005 (7)
C10.0294 (11)0.0300 (11)0.0240 (10)0.0081 (9)0.0024 (9)0.0047 (9)
C20.0224 (10)0.0240 (10)0.0258 (12)0.0032 (8)0.0007 (8)0.0030 (8)
C30.0292 (10)0.0369 (10)0.0314 (12)0.0025 (10)0.0038 (10)0.0047 (10)
C40.0230 (9)0.0228 (8)0.0316 (15)0.0037 (7)0.0033 (9)0.0037 (9)
Geometric parameters (Å, º) top
Mn1—O12.2766 (18)O4—C41.246 (2)
Mn1—O2i2.1195 (15)O5—H5A0.8605
Mn1—O32.1585 (16)O5—H5B0.8360
Mn1—O52.2441 (16)O6—H6A0.8479
Mn1—O62.1872 (17)O6—H6B0.8815
Mn1—N12.2760 (18)C1—C21.527 (3)
N1—C11.467 (3)C1—H3B0.9700
N1—C31.474 (3)C1—H3A0.9700
N1—H10.9029C3—C41.517 (3)
O1—C21.240 (3)C3—H1A0.9700
O2—C21.268 (3)C3—H1B0.9700
O3—C41.254 (3)
O2i—Mn1—O389.03 (6)Mn1—O5—H5A116.6
O2i—Mn1—O6112.03 (6)Mn1—O5—H5B113.7
O3—Mn1—O696.46 (7)H5A—O5—H5B101.9
O2i—Mn1—O594.70 (6)Mn1—O6—H6A120.8
O3—Mn1—O5173.96 (7)Mn1—O6—H6B116.4
O6—Mn1—O586.54 (6)H6A—O6—H6B102.5
O2i—Mn1—N1155.88 (6)N1—C1—C2111.15 (18)
O3—Mn1—N176.89 (6)N1—C1—H3B109.4
O6—Mn1—N189.22 (6)C2—C1—H3B109.4
O5—Mn1—N197.97 (6)N1—C1—H3A109.4
O2i—Mn1—O188.51 (6)C2—C1—H3A109.4
O3—Mn1—O191.68 (7)H3B—C1—H3A108.0
O6—Mn1—O1157.93 (6)O1—C2—O2125.0 (2)
O5—Mn1—O183.69 (6)O1—C2—C1119.5 (2)
N1—Mn1—O172.67 (6)O2—C2—C1115.5 (2)
C1—N1—C3113.51 (18)N1—C3—C4114.39 (18)
C1—N1—Mn1105.90 (12)N1—C3—H1A108.7
C3—N1—Mn1109.39 (13)C4—C3—H1A108.7
C1—N1—H1112.3N1—C3—H1B108.7
C3—N1—H1104.7C4—C3—H1B108.7
Mn1—N1—H1111.1H1A—C3—H1B107.6
C2—O1—Mn1112.61 (14)O4—C4—O3123.5 (2)
C2—O2—Mn1ii121.22 (15)O4—C4—C3116.7 (2)
C4—O3—Mn1118.49 (14)O3—C4—C3119.68 (17)
Symmetry codes: (i) x+1, y+1, z+1/2; (ii) x+1, y+1, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O4iii0.902.042.940 (2)174
O5—H5A···O2iv0.861.962.822 (2)174
O5—H5B···O4v0.841.822.646 (2)170
O6—H6A···O3iii0.851.962.762 (2)158
O6—H6B···O5iv0.882.182.975 (2)150
Symmetry codes: (iii) x, y+1, z; (iv) x+1, y+2, z+1/2; (v) x1/2, y+1, z.
 

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