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The title MnII complex, [Mn(C9H10NO2)2(H2O)4]·2H2O, is monomeric and centrosymmetric. It contains two 4-dimethyl­amino­benzoate ligands, four coordinated and two uncoordin­ated water mol­ecules, all ligands being monodentate. The four O atoms in the equatorial plane around the Mn atom form a slightly distorted square-planar arrangement, while the distorted octa­hedral coordination is completed by the two water O atoms in the axial positions. In the crystal structure, intra- and inter­molecular O—H...O hydrogen bonds link the mol­ecules into chains.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807007799/xu2210sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807007799/xu2210Isup2.hkl
Contains datablock I

CCDC reference: 640529

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.057
  • wR factor = 0.176
  • Data-to-parameter ratio = 13.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT030_ALERT_1_C _diffrn_reflns_number .LE. _reflns_number_total ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7 PLAT417_ALERT_2_C Short Inter D-H..H-D H41 .. H52 .. 2.13 Ang. PLAT417_ALERT_2_C Short Inter D-H..H-D H42 .. H52 .. 2.13 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Tetraaquabis[4-(dimethylamino)benzoato-κO]manganese(II) dihydrate top
Crystal data top
[Mn(C9H10NO2)2(H2O)4]·2H2OF(000) = 1036
Mr = 491.40Dx = 1.430 Mg m3
Orthorhombic, PbcaCu Kα radiation, λ = 1.54184 Å
Hall symbol: -P 2ac 2abCell parameters from 25 reflections
a = 7.2047 (13) Åθ = 2.6–26.3°
b = 26.101 (4) ŵ = 5.19 mm1
c = 12.141 (2) ÅT = 294 K
V = 2283.1 (7) Å3Prism, pink
Z = 40.35 × 0.25 × 0.25 mm
Data collection top
Enraf–Nonius Turbo-CAD-4
diffractometer
1438 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 74.1°, θmin = 3.3°
non–profiled ω scansh = 08
Absorption correction: ψ scan
(North et al., 1968)
k = 320
Tmin = 0.261, Tmax = 0.271l = 015
2228 measured reflections3 standard reflections every 120 min
2228 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.176H atoms treated by a mixture of independent and constrained refinement
S = 1.09 w = 1/[σ2(Fo2) + (0.0817P)2 + 2.0253P]
where P = (Fo2 + 2Fc2)/3
2228 reflections(Δ/σ)max < 0.001
168 parametersΔρmax = 0.33 e Å3
12 restraintsΔρmin = 0.59 e Å3
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
Mn0.50000.50000.50000.0350 (3)
O10.2580 (5)0.54859 (13)0.5222 (3)0.0419 (8)
O20.0570 (5)0.55012 (14)0.6609 (3)0.0447 (9)
O30.6578 (5)0.54398 (15)0.6216 (3)0.0486 (10)
H310.620 (8)0.550 (2)0.695 (3)0.08 (2)*
H320.782 (4)0.553 (3)0.619 (6)0.12 (3)*
O40.3975 (5)0.44739 (14)0.6269 (3)0.0443 (9)
H410.421 (11)0.457 (4)0.699 (3)0.14 (4)*
H420.269 (4)0.440 (3)0.624 (5)0.09 (2)*
O50.0110 (5)0.44920 (15)0.6551 (3)0.0485 (9)
H510.080 (7)0.440 (2)0.605 (5)0.08 (2)*
H520.024 (7)0.4845 (9)0.648 (5)0.051 (17)*
N10.2442 (6)0.78860 (16)0.6296 (4)0.0471 (11)
C10.1715 (6)0.57249 (19)0.5970 (4)0.0360 (11)
C20.1969 (6)0.62818 (18)0.6085 (4)0.0341 (10)
C30.1060 (6)0.6561 (2)0.6903 (4)0.0396 (11)
H30.03110.63880.74040.048*
C40.1232 (7)0.7080 (2)0.6994 (4)0.0415 (12)
H40.06250.72490.75630.050*
C50.2316 (6)0.73632 (18)0.6242 (4)0.0364 (11)
C60.3278 (7)0.7079 (2)0.5429 (5)0.0403 (12)
H60.40400.72500.49310.048*
C70.3106 (6)0.6553 (2)0.5361 (4)0.0390 (11)
H70.37620.63760.48220.047*
C80.3252 (9)0.8182 (2)0.5413 (6)0.0570 (15)
H8A0.45450.80990.53460.086*
H8B0.31210.85410.55710.086*
H8C0.26280.81030.47350.086*
C90.1468 (8)0.8165 (2)0.7152 (5)0.0569 (15)
H9A0.01540.81190.70620.085*
H9B0.17650.85220.71010.085*
H9C0.18390.80370.78600.085*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn0.0276 (5)0.0369 (5)0.0405 (5)0.0002 (5)0.0007 (5)0.0010 (5)
O10.0321 (17)0.0446 (18)0.049 (2)0.0066 (15)0.0035 (15)0.0045 (15)
O20.0356 (18)0.050 (2)0.048 (2)0.0082 (15)0.0075 (16)0.0016 (17)
O30.0327 (19)0.064 (3)0.050 (2)0.0074 (18)0.0008 (17)0.0163 (19)
O40.036 (2)0.050 (2)0.047 (2)0.0065 (17)0.0040 (16)0.0080 (18)
O50.0382 (19)0.052 (2)0.055 (2)0.0056 (19)0.0047 (19)0.0015 (18)
N10.043 (2)0.041 (2)0.057 (3)0.000 (2)0.014 (2)0.004 (2)
C10.027 (2)0.045 (3)0.036 (3)0.001 (2)0.004 (2)0.003 (2)
C20.022 (2)0.042 (3)0.038 (2)0.0036 (18)0.001 (2)0.000 (2)
C30.029 (2)0.049 (3)0.042 (3)0.000 (2)0.010 (2)0.004 (2)
C40.033 (2)0.047 (3)0.044 (3)0.001 (2)0.009 (2)0.006 (2)
C50.023 (2)0.043 (3)0.044 (3)0.0002 (19)0.0005 (19)0.002 (2)
C60.028 (2)0.048 (3)0.045 (3)0.005 (2)0.008 (2)0.003 (2)
C70.027 (2)0.048 (3)0.043 (3)0.002 (2)0.007 (2)0.001 (2)
C80.049 (3)0.043 (3)0.079 (4)0.005 (3)0.015 (3)0.004 (3)
C90.053 (3)0.053 (3)0.064 (4)0.004 (3)0.013 (3)0.010 (3)
Geometric parameters (Å, º) top
Mn—O1i2.173 (3)C1—C21.472 (6)
Mn—O12.173 (3)C2—C71.394 (6)
Mn—O32.189 (4)C2—C31.396 (6)
Mn—O3i2.189 (4)C3—C41.362 (7)
Mn—O42.192 (4)C3—H30.9300
Mn—O4i2.192 (4)C4—C51.412 (6)
O1—C11.265 (6)C4—H40.9300
O2—C11.275 (6)C5—C61.416 (7)
O3—H320.92 (2)C6—C71.381 (7)
O3—H310.95 (2)C6—H60.9300
O4—H420.94 (2)C7—H70.9300
O4—H410.93 (5)C8—H8A0.9600
O5—H520.93 (2)C8—H8B0.9600
O5—H510.93 (5)C8—H8C0.9600
N1—C51.369 (6)C9—H9A0.9600
N1—C81.445 (7)C9—H9B0.9600
N1—C91.450 (6)C9—H9C0.9600
O1i—Mn—O1180.000 (1)C7—C2—C1120.9 (4)
O1i—Mn—O388.46 (14)C3—C2—C1121.7 (4)
O1—Mn—O391.54 (14)C4—C3—C2122.3 (5)
O1i—Mn—O3i91.54 (14)C4—C3—H3118.9
O1—Mn—O3i88.46 (14)C2—C3—H3118.9
O3—Mn—O3i180.00 (18)C3—C4—C5121.2 (5)
O1i—Mn—O489.53 (13)C3—C4—H4119.4
O1—Mn—O490.47 (13)C5—C4—H4119.4
O3—Mn—O491.70 (16)N1—C5—C4121.9 (5)
O3i—Mn—O488.30 (16)N1—C5—C6121.6 (4)
O1i—Mn—O4i90.47 (13)C4—C5—C6116.5 (4)
O1—Mn—O4i89.53 (13)C7—C6—C5121.2 (5)
O3—Mn—O4i88.30 (16)C7—C6—H6119.4
O3i—Mn—O4i91.70 (16)C5—C6—H6119.4
O4—Mn—O4i180.00 (15)C6—C7—C2121.3 (5)
C5—N1—C8121.6 (4)C6—C7—H7119.3
C5—N1—C9120.2 (4)C2—C7—H7119.3
C8—N1—C9117.3 (5)N1—C8—H8A109.5
C1—O1—Mn140.5 (3)N1—C8—H8B109.5
Mn—O3—H32128 (4)H8A—C8—H8B109.5
Mn—O3—H31125 (4)N1—C8—H8C109.5
H32—O3—H31106 (4)H8A—C8—H8C109.5
Mn—O4—H42115 (4)H8B—C8—H8C109.5
Mn—O4—H41116 (6)N1—C9—H9A109.5
H42—O4—H41106 (4)N1—C9—H9B109.5
H52—O5—H51106 (4)H9A—C9—H9B109.5
O1—C1—O2122.0 (5)N1—C9—H9C109.5
O1—C1—C2119.6 (4)H9A—C9—H9C109.5
O2—C1—C2118.3 (4)H9B—C9—H9C109.5
C7—C2—C3117.3 (5)
O3—Mn—O1—C137.0 (5)C2—C3—C4—C51.5 (8)
O3i—Mn—O1—C1143.0 (5)C8—N1—C5—C4168.1 (5)
O4—Mn—O1—C154.7 (5)C9—N1—C5—C40.8 (8)
O4i—Mn—O1—C1125.3 (5)C8—N1—C5—C612.3 (8)
Mn—O1—C1—O281.3 (6)C9—N1—C5—C6178.8 (5)
Mn—O1—C1—C2101.2 (6)C3—C4—C5—N1177.3 (5)
O1—C1—C2—C71.9 (7)C3—C4—C5—C63.0 (7)
O2—C1—C2—C7175.6 (4)N1—C5—C6—C7178.3 (5)
O1—C1—C2—C3179.4 (4)C4—C5—C6—C72.1 (7)
O2—C1—C2—C33.1 (7)C5—C6—C7—C20.5 (8)
C7—C2—C3—C41.1 (7)C3—C2—C7—C62.1 (7)
C1—C2—C3—C4177.7 (5)C1—C2—C7—C6176.7 (5)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H31···O2ii0.94 (4)1.81 (4)2.743 (5)170 (5)
O3—H32···O2iii0.93 (4)2.05 (3)2.920 (5)157 (7)
O4—H41···O5ii0.93 (5)1.90 (4)2.771 (5)156 (9)
O4—H42···O50.95 (3)1.91 (3)2.806 (5)157 (6)
O5—H51···O1iv0.93 (5)2.03 (6)2.897 (5)155 (5)
O5—H52···O20.93 (2)1.74 (2)2.656 (5)169 (6)
Symmetry codes: (ii) x+1/2, y, z+3/2; (iii) x+1, y, z; (iv) x, y+1, z+1.
 

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