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In the title compound, bis­(μ-pyridine-2,5-dicarboxyl­ato)bis­[aqua­(pyrazino[2,3-f][1,10]phenanthroline)manganese(II)] dihydrate, [Mn2(C7H3NO4)2(C14H8N4)2(H2O)2]·2H2O, each MnII atom is six-coordinated by three N atoms from one bidentate pyrazino[2,3-f][1,10]phenanthroline and one monodentate pyridine-2,5-dicarboxyl­ate ligand, and three O atoms from two monodentate pyridine-2,5-dicarboxyl­ate ligands and one water mol­ecule. The two MnII atoms are bridged by two pyridine-2,5-dicarboxyl­ate ligands, forming a centrosymmetric dinuclear molecule. Neighboring mol­ecules inter­act through π–π contacts, leading to a one-dimensional supra­molecular structure, and O—H...O hydrogen bonds complete the structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806024871/hb2098sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806024871/hb2098Isup2.hkl
Contains datablock I

CCDC reference: 618205

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.064
  • wR factor = 0.138
  • Data-to-parameter ratio = 14.2

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.

bis(µ-pyridine-2,5-dicarboxylato)bis[aqua(pyrazino[2,3-f][1,10]phenanthroline)manganese(II)] dihydrate top
Crystal data top
[Mn2(C7H3NO4)2(C14H8N4)2(H2O)2]·2H2OZ = 1
Mr = 976.64F(000) = 498
Triclinic, P1Dx = 1.671 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.3813 (15) ÅCell parameters from 6037 reflections
b = 10.044 (2) Åθ = 3.0–27.5°
c = 14.052 (3) ŵ = 0.73 mm1
α = 95.71 (3)°T = 292 K
β = 94.42 (3)°Block, pale yellow
γ = 109.47 (3)°0.33 × 0.27 × 0.21 mm
V = 970.6 (4) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
4413 independent reflections
Radiation source: rotating anode2620 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.081
Detector resolution: 10.0 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = 89
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1313
Tmin = 0.784, Tmax = 0.852l = 1818
9612 measured reflections
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)] = 0.064Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.138H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.05P)2 + 0.1792P]
where P = (Fo2 + 2Fc2)/3
4413 reflections(Δ/σ)max < 0.001
310 parametersΔρmax = 0.39 e Å3
6 restraintsΔρmin = 0.54 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
C10.1484 (6)0.0429 (5)0.2213 (3)0.0357 (10)
H10.12620.04930.15460.043*
C20.0527 (6)0.1609 (5)0.2647 (3)0.0382 (10)
H20.02940.24450.22790.046*
C30.0820 (6)0.1516 (4)0.3632 (3)0.0350 (10)
H30.01890.22850.39440.042*
C40.3004 (5)0.0859 (4)0.3667 (3)0.0244 (8)
C50.4400 (5)0.2191 (4)0.4179 (3)0.0266 (9)
C60.6651 (6)0.4382 (5)0.4113 (3)0.0403 (11)
H60.72650.50960.37540.048*
C70.7229 (7)0.4593 (5)0.5103 (3)0.0460 (12)
H70.82240.54120.53920.055*
C80.6294 (6)0.3565 (5)0.5633 (3)0.0418 (11)
H80.66210.36920.62960.050*
C90.4844 (6)0.2322 (5)0.5183 (3)0.0314 (9)
C100.2077 (6)0.0252 (4)0.4158 (3)0.0292 (9)
C110.3794 (6)0.1181 (5)0.5697 (3)0.0313 (10)
C120.2447 (6)0.0071 (5)0.5209 (3)0.0294 (9)
C130.1805 (7)0.0952 (6)0.6617 (3)0.0442 (12)
H130.11290.16590.69660.053*
C140.3181 (7)0.0289 (6)0.7110 (3)0.0474 (13)
H140.34080.03680.77770.057*
C150.2413 (5)0.2467 (4)0.0069 (3)0.0276 (9)
C160.4009 (5)0.3177 (4)0.0647 (3)0.0260 (9)
C170.5662 (6)0.2821 (5)0.0628 (3)0.0345 (10)
H170.57700.21000.02850.041*
C180.7151 (6)0.3538 (4)0.1121 (3)0.0326 (10)
H180.82600.32940.11270.039*
C190.6967 (5)0.4624 (4)0.1604 (3)0.0271 (9)
N50.5366 (4)0.4991 (3)0.1625 (2)0.0254 (7)
C210.8572 (5)0.5515 (4)0.2122 (3)0.0301 (9)
N10.5278 (4)0.3225 (4)0.3657 (2)0.0306 (8)
N20.2688 (4)0.0777 (4)0.2691 (2)0.0275 (7)
N30.1432 (5)0.1153 (4)0.5671 (3)0.0388 (9)
N40.4178 (5)0.1358 (4)0.6673 (2)0.0432 (10)
C200.3913 (5)0.4251 (4)0.1163 (3)0.0252 (8)
H200.27850.44730.11940.030*
O10.2819 (4)0.1790 (3)0.05948 (19)0.0338 (7)
O20.0819 (4)0.2597 (3)0.0247 (2)0.0410 (7)
O1W0.6746 (4)0.2682 (4)0.1776 (2)0.0414 (8)
O30.9978 (4)0.5098 (3)0.2213 (2)0.0446 (8)
O2W0.7844 (5)0.0845 (4)0.0618 (3)0.0584 (10)
O40.8387 (4)0.6606 (3)0.2406 (2)0.0376 (7)
Mn10.40163 (8)0.27795 (7)0.20439 (4)0.02762 (19)
HW120.779 (4)0.338 (3)0.194 (3)0.041*
HW220.884 (4)0.139 (3)0.042 (3)0.041*
HW110.688 (5)0.204 (3)0.140 (3)0.041*
HW210.744 (5)0.003 (2)0.028 (3)0.041*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.038 (2)0.040 (3)0.024 (2)0.008 (2)0.0028 (19)0.003 (2)
C20.043 (3)0.027 (2)0.041 (3)0.007 (2)0.005 (2)0.007 (2)
C30.036 (2)0.026 (2)0.043 (3)0.0068 (19)0.012 (2)0.011 (2)
C40.0257 (19)0.026 (2)0.025 (2)0.0116 (17)0.0032 (16)0.0063 (17)
C50.0245 (19)0.028 (2)0.030 (2)0.0115 (18)0.0055 (17)0.0073 (18)
C60.037 (2)0.032 (3)0.042 (3)0.000 (2)0.004 (2)0.004 (2)
C70.040 (3)0.040 (3)0.044 (3)0.000 (2)0.002 (2)0.003 (2)
C80.044 (3)0.047 (3)0.029 (2)0.013 (2)0.001 (2)0.004 (2)
C90.029 (2)0.039 (3)0.027 (2)0.014 (2)0.0029 (18)0.0051 (19)
C100.031 (2)0.032 (2)0.029 (2)0.0137 (19)0.0065 (18)0.0092 (18)
C110.029 (2)0.044 (3)0.027 (2)0.019 (2)0.0039 (18)0.0070 (19)
C120.029 (2)0.039 (3)0.028 (2)0.018 (2)0.0103 (18)0.0138 (19)
C130.051 (3)0.059 (3)0.039 (3)0.032 (3)0.019 (2)0.028 (2)
C140.051 (3)0.071 (4)0.031 (3)0.029 (3)0.015 (2)0.021 (3)
C150.029 (2)0.025 (2)0.026 (2)0.0082 (18)0.0009 (17)0.0018 (17)
C160.027 (2)0.024 (2)0.024 (2)0.0042 (17)0.0002 (17)0.0026 (17)
C170.038 (2)0.035 (3)0.038 (2)0.019 (2)0.0067 (19)0.016 (2)
C180.032 (2)0.028 (2)0.041 (3)0.0136 (19)0.0062 (19)0.0096 (19)
C190.025 (2)0.023 (2)0.031 (2)0.0056 (17)0.0022 (17)0.0026 (17)
N50.0218 (16)0.0272 (19)0.0265 (18)0.0066 (15)0.0034 (14)0.0061 (14)
C210.027 (2)0.025 (2)0.034 (2)0.0050 (18)0.0035 (18)0.0005 (19)
N10.0284 (18)0.028 (2)0.034 (2)0.0068 (16)0.0043 (15)0.0060 (16)
N20.0273 (17)0.031 (2)0.0222 (18)0.0081 (16)0.0000 (14)0.0050 (15)
N30.039 (2)0.049 (2)0.038 (2)0.0203 (19)0.0139 (17)0.0248 (18)
N40.050 (2)0.060 (3)0.025 (2)0.025 (2)0.0068 (17)0.0097 (19)
C200.0238 (19)0.024 (2)0.025 (2)0.0055 (17)0.0001 (16)0.0019 (17)
O10.0391 (16)0.0329 (17)0.0288 (16)0.0098 (14)0.0026 (13)0.0114 (13)
O20.0318 (16)0.048 (2)0.0452 (19)0.0125 (15)0.0057 (14)0.0188 (15)
O1W0.0326 (16)0.047 (2)0.042 (2)0.0132 (15)0.0045 (15)0.0043 (16)
O30.0307 (16)0.0361 (19)0.072 (2)0.0151 (15)0.0163 (15)0.0120 (16)
O2W0.057 (2)0.038 (2)0.078 (3)0.0086 (18)0.035 (2)0.0004 (19)
O40.0356 (16)0.0379 (18)0.0450 (18)0.0130 (14)0.0182 (14)0.0200 (15)
Mn10.0267 (3)0.0285 (4)0.0290 (4)0.0088 (3)0.0054 (3)0.0109 (3)
Geometric parameters (Å, º) top
C1—N21.317 (5)C14—H140.9300
C1—C21.389 (6)C15—C161.503 (5)
C1—H10.9300C16—C201.377 (5)
C2—C31.373 (6)C16—C171.381 (5)
C2—H20.9300C17—C181.376 (5)
C3—C101.393 (6)C17—H170.9300
C3—H30.9300C18—C191.379 (5)
C4—N21.364 (5)C18—H180.9300
C4—C101.380 (5)C19—N51.350 (4)
C4—C51.464 (5)C19—C211.513 (5)
C5—N11.346 (5)N5—C201.340 (5)
C5—C91.407 (5)N5—Mn1i2.278 (3)
C6—N11.325 (5)C20—H200.9300
C6—C71.396 (6)O1W—HW120.849 (18)
C6—H60.9300O1W—HW110.83 (4)
C7—C81.362 (6)O2W—HW220.846 (18)
C7—H70.9300O2W—HW210.851 (18)
C8—C91.397 (6)O4—Mn1i2.143 (3)
C8—H80.9300Mn1—O1W2.110 (3)
C9—C111.447 (6)Mn1—O12.156 (3)
C10—C121.463 (5)Mn1—O4i2.143 (3)
C11—N41.361 (5)Mn1—N22.241 (3)
C11—C121.389 (6)Mn1—N5i2.278 (3)
C12—N31.356 (5)Mn1—N12.324 (3)
C13—N31.317 (5)C15—O21.236 (4)
C13—C141.393 (7)C15—O11.280 (4)
C13—H130.9300C21—O41.248 (5)
C14—N41.321 (6)C21—O31.252 (4)
N2—C1—C2123.7 (4)C18—C17—C16119.7 (4)
N2—C1—H1118.1C18—C17—H17120.2
C2—C1—H1118.1C16—C17—H17120.2
C3—C2—C1118.5 (4)C17—C18—C19118.8 (3)
C3—C2—H2120.7C17—C18—H18120.6
C1—C2—H2120.7C19—C18—H18120.6
C2—C3—C10119.1 (4)N5—C19—C18122.3 (3)
C2—C3—H3120.5N5—C19—C21115.4 (3)
C10—C3—H3120.5C18—C19—C21122.3 (3)
N2—C4—C10122.3 (4)C20—N5—C19117.8 (3)
N2—C4—C5116.6 (3)C20—N5—Mn1i128.1 (2)
C10—C4—C5121.1 (3)C19—N5—Mn1i111.1 (2)
N1—C5—C9122.4 (4)O4—C21—O3126.1 (4)
N1—C5—C4118.2 (3)O4—C21—C19117.1 (3)
C9—C5—C4119.3 (4)O3—C21—C19116.8 (4)
N1—C6—C7123.8 (4)C6—N1—C5118.0 (4)
N1—C6—H6118.1C6—N1—Mn1127.9 (3)
C7—C6—H6118.1C5—N1—Mn1114.0 (3)
C8—C7—C6118.1 (4)C1—N2—C4117.7 (3)
C8—C7—H7121.0C1—N2—Mn1124.9 (3)
C6—C7—H7121.0C4—N2—Mn1117.1 (3)
C7—C8—C9120.2 (4)C13—N3—C12115.9 (4)
C7—C8—H8119.9C14—N4—C11116.0 (4)
C9—C8—H8119.9N5—C20—C16123.2 (3)
C8—C9—C5117.5 (4)N5—C20—H20118.4
C8—C9—C11123.4 (4)C16—C20—H20118.4
C5—C9—C11119.1 (4)C15—O1—Mn1123.5 (2)
C4—C10—C3118.7 (4)Mn1—O1W—HW12123 (2)
C4—C10—C12119.2 (4)Mn1—O1W—HW11123 (3)
C3—C10—C12122.1 (4)HW12—O1W—HW11113 (3)
N4—C11—C12120.7 (4)HW22—O2W—HW21111 (3)
N4—C11—C9118.2 (4)C21—O4—Mn1i119.4 (2)
C12—C11—C9121.1 (4)O1W—Mn1—O4i166.72 (12)
N3—C12—C11122.4 (4)O1W—Mn1—O190.57 (11)
N3—C12—C10117.7 (4)O4i—Mn1—O196.89 (11)
C11—C12—C10119.9 (4)O1W—Mn1—N2102.65 (12)
N3—C13—C14122.0 (4)O4i—Mn1—N287.86 (11)
N3—C13—H13119.0O1—Mn1—N293.72 (11)
C14—C13—H13119.0O1W—Mn1—N5i94.60 (12)
N4—C14—C13123.0 (4)O4i—Mn1—N5i74.22 (11)
N4—C14—H14118.5O1—Mn1—N5i92.22 (11)
C13—C14—H14118.5N2—Mn1—N5i161.67 (10)
O2—C15—O1124.4 (3)O1W—Mn1—N185.04 (12)
O2—C15—C16118.4 (3)O4i—Mn1—N190.46 (11)
O1—C15—C16117.2 (3)O1—Mn1—N1164.46 (11)
C20—C16—C17118.2 (3)N2—Mn1—N172.82 (12)
C20—C16—C15121.1 (3)N5i—Mn1—N1102.97 (12)
C17—C16—C15120.6 (3)
Symmetry code: (i) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—HW11···O2W0.83 (4)1.89 (2)2.704 (4)166 (4)
O1W—HW12···O3ii0.85 (2)1.82 (2)2.665 (4)176 (4)
O2W—HW21···O1iii0.85 (2)2.04 (2)2.874 (4)165 (4)
O2W—HW22···O2iv0.85 (2)1.93 (2)2.767 (4)170 (4)
Symmetry codes: (ii) x+2, y+1, z; (iii) x+1, y, z; (iv) x+1, y, z.
 

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