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The zwitterionic title compound, [Mn(C10H8O5)(C12H8N2)(H2O)3]·H2O, has the Mn atom in an octa­hedral geometry that comprises the O atom of the 2-(4-carboxyl­atophen­oxy)­propionate group, two N atoms of the 1,10-phenanthroline ligand and three water mol­ecules. Extensive hydrogen-bonding and π–π stacking inter­actions lead to a three-dimensional supra­molecular network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807021101/ng2262sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807021101/ng2262Isup2.hkl
Contains datablock I

CCDC reference: 650537

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.038
  • wR factor = 0.100
  • Data-to-parameter ratio = 15.9

checkCIF/PLATON results

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Alert level C PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 3000 Deg. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H2 O
Alert level G PLAT793_ALERT_1_G Check the Absolute Configuration of C8 = ... R PLAT794_ALERT_5_G Check Predicted Bond Valency for Mn1 (2) 2.06
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 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 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

Our studies have addressed the metal derivatives of carboxyphenoxypropionic acids for the construction of supramolecular architectures. ecently, we have reported the structures of cobalt(II) and nickel(II) derivatives of 2-(4-carboxylatophenoxy)propionic acid (Deng et al., 2007a,b). In the title Mn complex (I) (Fig. 1), the 2-(p-CPOP)2- anion coordinates in a monodentate fashion to the Mn atom through the carboxylate group. The Mn atom is chelated by the phenanthroline and is also linked to three water molecules. A three-dimensional supramolecular network is constructed from π-π stacking between the 1,10-phenanthroline rings (centroid-centroid distance being 3.689 (5) and 3.869 (5) Å) and hydrogen-bonding interactions (Table 2).

Related literature top

For the cobalt(II) and nickel(II) complexes of the title carboxylic acid, see: Deng et al. (2007a,b).

Experimental top

The title complex was prepared by the addition of MnCl2.4H2O (10 mmol) and 1,10-phenanthroline (10 mmol) to a solution of 2-(p-CPOPH2) (15 mmol) in H2O/MeOH (V/V = 1:1) solution. The pH value was adjusted to 5 with NaOH (0.2 M) solution. Colorless crystals were obtained from the filtered solution at room temperature over several days. CH&N analysis. Calc. for C22H24N2O9Mn: C 51.27, H 4.69, N 5.43. Found: C 51.26, H 4.67, N 5.46%.

Refinement top

The H atoms were placed in calculated positions with C—H = 0.93 or 0.97 Å and Uiso(H) = 1.2Ueq (C) and were included in the refinement in the riding model approximation. The H atoms of water molecules and hydroxyl groups were located in difference Fourier maps and refined with the O—H distance restrained to 0.85 (1) Å and Uiso(H) = 1.5Ueq(O).

Structure description top

Our studies have addressed the metal derivatives of carboxyphenoxypropionic acids for the construction of supramolecular architectures. ecently, we have reported the structures of cobalt(II) and nickel(II) derivatives of 2-(4-carboxylatophenoxy)propionic acid (Deng et al., 2007a,b). In the title Mn complex (I) (Fig. 1), the 2-(p-CPOP)2- anion coordinates in a monodentate fashion to the Mn atom through the carboxylate group. The Mn atom is chelated by the phenanthroline and is also linked to three water molecules. A three-dimensional supramolecular network is constructed from π-π stacking between the 1,10-phenanthroline rings (centroid-centroid distance being 3.689 (5) and 3.869 (5) Å) and hydrogen-bonding interactions (Table 2).

For the cobalt(II) and nickel(II) complexes of the title carboxylic acid, see: Deng et al. (2007a,b).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. Molecular structure of the title compound with 30% probability ellipsoid for the non-H atoms. Dashed lines indicate O—H···O hydrogen bonds.
Triaqua[2-(4-carboxylatophenoxy)propionato-κO](1,10-phenanthroline- κ2N,N')manganese(II) monohydrate top
Crystal data top
[Mn(C10H8O5)(C12H8N2)(H2O)3]·H2OZ = 2
Mr = 515.37F(000) = 534
Triclinic, P1Dx = 1.469 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.5457 (15) ÅCell parameters from 7678 reflections
b = 11.073 (2) Åθ = 3.3–27.5°
c = 15.372 (3) ŵ = 0.62 mm1
α = 106.16 (3)°T = 295 K
β = 99.53 (3)°Prism, colourless
γ = 103.14 (3)°0.38 × 0.25 × 0.17 mm
V = 1164.8 (5) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
5280 independent reflections
Radiation source: fine-focus sealed tube3105 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
Detector resolution: 10.000 pixels mm-1θmax = 27.5°, θmin = 3.3°
ω scansh = 99
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1414
Tmin = 0.826, Tmax = 0.893l = 1919
11565 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)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.100H atoms treated by a mixture of independent and constrained refinement
S = 1.12 w = 1/[σ2(Fo2) + (0.0275P)2 + 0.6167P]
where P = (Fo2 + 2Fc2)/3
5280 reflections(Δ/σ)max = 0.001
332 parametersΔρmax = 0.56 e Å3
0 restraintsΔρmin = 0.73 e Å3
Crystal data top
[Mn(C10H8O5)(C12H8N2)(H2O)3]·H2Oγ = 103.14 (3)°
Mr = 515.37V = 1164.8 (5) Å3
Triclinic, P1Z = 2
a = 7.5457 (15) ÅMo Kα radiation
b = 11.073 (2) ŵ = 0.62 mm1
c = 15.372 (3) ÅT = 295 K
α = 106.16 (3)°0.38 × 0.25 × 0.17 mm
β = 99.53 (3)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
5280 independent reflections
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
3105 reflections with I > 2σ(I)
Tmin = 0.826, Tmax = 0.893Rint = 0.036
11565 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0380 restraints
wR(F2) = 0.100H atoms treated by a mixture of independent and constrained refinement
S = 1.12Δρmax = 0.56 e Å3
5280 reflectionsΔρmin = 0.73 e Å3
332 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn10.27669 (6)0.37228 (4)0.71204 (3)0.03294 (13)
O1W0.5797 (3)0.4182 (2)0.75865 (16)0.0471 (5)
H1W10.624 (5)0.362 (3)0.774 (2)0.071*
H1W20.633 (5)0.493 (4)0.796 (3)0.071*
O2W0.2654 (3)0.3051 (2)0.83041 (14)0.0432 (5)
H2W10.353 (5)0.286 (3)0.859 (2)0.065*
H2W20.170 (5)0.286 (3)0.857 (2)0.065*
O3W0.0264 (3)0.34586 (19)0.69778 (14)0.0385 (5)
H3W10.086 (4)0.309 (3)0.734 (2)0.058*
H3W20.026 (5)0.426 (3)0.717 (2)0.058*
O4W0.1908 (3)0.6600 (2)0.88034 (17)0.0560 (6)
H4W10.098 (6)0.649 (4)0.851 (3)0.084*
H4W20.146 (6)0.686 (4)0.939 (3)0.084*
O10.3311 (3)0.58037 (17)0.75925 (14)0.0424 (5)
O20.0499 (3)0.60400 (18)0.76959 (15)0.0479 (5)
O30.5231 (3)1.20164 (16)0.92263 (13)0.0364 (4)
O41.0045 (3)1.2598 (2)0.92143 (14)0.0485 (5)
O50.7683 (3)1.25399 (18)0.81085 (13)0.0425 (5)
N10.2598 (3)0.1668 (2)0.61862 (15)0.0386 (6)
N20.2602 (3)0.3778 (2)0.56302 (16)0.0424 (6)
C10.2238 (4)0.6494 (2)0.78069 (18)0.0343 (6)
C20.3088 (4)0.7955 (2)0.82068 (18)0.0334 (6)
C30.5007 (4)0.8509 (2)0.84896 (18)0.0355 (6)
H30.57890.79670.84430.043*
C40.5795 (4)0.9867 (3)0.88444 (19)0.0366 (6)
H40.70911.02290.90280.044*
C50.4628 (4)1.0666 (2)0.89205 (17)0.0306 (6)
C60.2693 (4)1.0124 (3)0.8677 (2)0.0382 (7)
H60.19111.06650.87540.046*
C70.1938 (4)0.8781 (3)0.8321 (2)0.0382 (7)
H70.06410.84200.81530.046*
C80.7194 (4)1.2660 (2)0.96311 (18)0.0332 (6)
H80.76541.22791.00960.040*
C90.7334 (4)1.4088 (3)1.0117 (2)0.0434 (7)
H9A0.69281.44720.96610.065*
H9B0.86121.45591.04480.065*
H9C0.65491.41351.05500.065*
C100.8382 (4)1.2573 (2)0.89161 (19)0.0332 (6)
C110.2577 (5)0.4808 (3)0.5357 (2)0.0569 (9)
H110.25520.55770.57900.068*
C120.2588 (5)0.4788 (4)0.4442 (3)0.0722 (11)
H120.25870.55330.42750.087*
C130.2601 (5)0.3666 (4)0.3804 (2)0.0705 (11)
H130.26110.36400.31950.085*
C140.2599 (5)0.2548 (4)0.4058 (2)0.0551 (9)
C150.2562 (5)0.1317 (5)0.3425 (2)0.0727 (11)
H150.25680.12490.28090.087*
C160.2517 (6)0.0256 (4)0.3689 (2)0.0722 (11)
H160.24920.05290.32560.087*
C170.2506 (5)0.0323 (3)0.4632 (2)0.0529 (8)
C180.2449 (5)0.0746 (3)0.4952 (3)0.0653 (10)
H180.23900.15590.45430.078*
C190.2480 (5)0.0595 (3)0.5858 (3)0.0641 (10)
H190.24520.12980.60790.077*
C200.2553 (5)0.0628 (3)0.6457 (2)0.0523 (8)
H200.25720.07200.70790.063*
C210.2571 (4)0.1526 (3)0.52810 (18)0.0395 (7)
C220.2592 (4)0.2654 (3)0.49881 (19)0.0407 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0368 (3)0.0277 (2)0.0340 (2)0.00985 (18)0.00952 (18)0.00888 (18)
O1W0.0373 (13)0.0414 (12)0.0608 (14)0.0123 (10)0.0063 (11)0.0165 (11)
O2W0.0430 (14)0.0543 (13)0.0474 (12)0.0224 (11)0.0180 (10)0.0291 (11)
O3W0.0381 (12)0.0318 (10)0.0457 (12)0.0092 (9)0.0120 (9)0.0123 (10)
O4W0.0417 (15)0.0607 (15)0.0568 (14)0.0119 (12)0.0060 (12)0.0115 (13)
O10.0402 (12)0.0265 (10)0.0585 (13)0.0100 (9)0.0148 (10)0.0090 (9)
O20.0359 (13)0.0308 (10)0.0685 (14)0.0059 (9)0.0089 (11)0.0086 (10)
O30.0350 (11)0.0247 (9)0.0492 (11)0.0085 (8)0.0103 (9)0.0118 (9)
O40.0355 (13)0.0656 (14)0.0499 (12)0.0150 (11)0.0133 (10)0.0253 (11)
O50.0472 (13)0.0460 (11)0.0385 (11)0.0160 (10)0.0134 (10)0.0166 (10)
N10.0442 (15)0.0344 (13)0.0342 (12)0.0113 (11)0.0091 (11)0.0070 (11)
N20.0449 (16)0.0479 (15)0.0378 (13)0.0128 (12)0.0085 (11)0.0207 (13)
C10.0390 (17)0.0281 (14)0.0371 (15)0.0102 (13)0.0097 (13)0.0123 (12)
C20.0384 (17)0.0299 (14)0.0348 (14)0.0086 (12)0.0111 (13)0.0149 (12)
C30.0361 (17)0.0294 (14)0.0440 (16)0.0115 (12)0.0142 (13)0.0127 (13)
C40.0306 (16)0.0316 (14)0.0488 (16)0.0079 (12)0.0121 (13)0.0145 (13)
C50.0367 (16)0.0245 (13)0.0331 (14)0.0088 (12)0.0126 (12)0.0112 (12)
C60.0366 (17)0.0301 (14)0.0541 (17)0.0143 (13)0.0159 (14)0.0166 (14)
C70.0299 (16)0.0311 (14)0.0542 (18)0.0077 (12)0.0072 (13)0.0180 (14)
C80.0320 (16)0.0276 (13)0.0355 (14)0.0048 (12)0.0055 (12)0.0080 (12)
C90.050 (2)0.0333 (15)0.0421 (16)0.0116 (14)0.0123 (14)0.0056 (13)
C100.0365 (17)0.0235 (13)0.0372 (15)0.0057 (12)0.0081 (13)0.0091 (12)
C110.065 (2)0.059 (2)0.0528 (19)0.0197 (18)0.0097 (17)0.0297 (18)
C120.076 (3)0.084 (3)0.068 (2)0.019 (2)0.006 (2)0.052 (2)
C130.062 (3)0.107 (3)0.044 (2)0.015 (2)0.0071 (18)0.036 (2)
C140.046 (2)0.082 (2)0.0347 (16)0.0144 (18)0.0073 (15)0.0201 (18)
C150.065 (3)0.108 (3)0.0323 (18)0.022 (2)0.0141 (17)0.006 (2)
C160.074 (3)0.081 (3)0.044 (2)0.028 (2)0.0130 (19)0.010 (2)
C170.044 (2)0.058 (2)0.0418 (17)0.0126 (16)0.0072 (15)0.0031 (16)
C180.066 (3)0.045 (2)0.069 (2)0.0215 (18)0.009 (2)0.0064 (19)
C190.075 (3)0.0363 (18)0.075 (2)0.0192 (17)0.010 (2)0.0101 (18)
C200.071 (2)0.0362 (17)0.0478 (18)0.0167 (16)0.0122 (17)0.0106 (15)
C210.0330 (17)0.0440 (16)0.0319 (15)0.0068 (13)0.0059 (12)0.0024 (14)
C220.0306 (16)0.0554 (19)0.0320 (14)0.0091 (14)0.0082 (12)0.0105 (14)
Geometric parameters (Å, º) top
Mn1—O12.1318 (19)C5—C61.389 (4)
Mn1—O2W2.156 (2)C6—C71.376 (4)
Mn1—O1W2.174 (2)C6—H60.9300
Mn1—O3W2.204 (2)C7—H70.9300
Mn1—N12.290 (2)C8—C91.521 (4)
Mn1—N22.292 (2)C8—C101.526 (4)
O1W—H1W10.84 (4)C8—H80.9800
O1W—H1W20.83 (4)C9—H9A0.9600
O2W—H2W10.83 (4)C9—H9B0.9600
O2W—H2W20.90 (4)C9—H9C0.9600
O3W—H3W10.90 (3)C11—C121.402 (5)
O3W—H3W20.85 (3)C11—H110.9300
O4W—H4W10.91 (4)C12—C131.354 (5)
O4W—H4W20.85 (4)C12—H120.9300
O1—C11.256 (3)C13—C141.398 (5)
O2—C11.257 (3)C13—H130.9300
O3—C51.375 (3)C14—C221.403 (4)
O3—C81.435 (3)C14—C151.429 (5)
O4—C101.253 (3)C15—C161.340 (5)
O5—C101.253 (3)C15—H150.9300
N1—C201.324 (3)C16—C171.432 (5)
N1—C211.352 (3)C16—H160.9300
N2—C111.322 (4)C17—C181.397 (5)
N2—C221.354 (4)C17—C211.410 (4)
C1—C21.501 (4)C18—C191.352 (5)
C2—C31.379 (4)C18—H180.9300
C2—C71.393 (4)C19—C201.393 (4)
C3—C41.393 (4)C19—H190.9300
C3—H30.9300C20—H200.9300
C4—C51.380 (4)C21—C221.439 (4)
C4—H40.9300
O1—Mn1—O2W108.33 (8)C2—C7—H7119.5
O1—Mn1—O1W83.81 (9)O3—C8—C9105.4 (2)
O2W—Mn1—O1W85.84 (9)O3—C8—C10113.6 (2)
O1—Mn1—O3W90.70 (8)C9—C8—C10109.8 (2)
O2W—Mn1—O3W85.06 (9)O3—C8—H8109.3
O1W—Mn1—O3W167.32 (8)C9—C8—H8109.3
O1—Mn1—N1159.22 (8)C10—C8—H8109.3
O2W—Mn1—N191.18 (8)C8—C9—H9A109.5
O1W—Mn1—N190.74 (10)C8—C9—H9B109.5
O3W—Mn1—N198.24 (9)H9A—C9—H9B109.5
O1—Mn1—N288.65 (9)C8—C9—H9C109.5
O2W—Mn1—N2162.90 (8)H9A—C9—H9C109.5
O1W—Mn1—N298.30 (9)H9B—C9—H9C109.5
O3W—Mn1—N292.97 (9)O5—C10—O4125.3 (3)
N1—Mn1—N272.27 (9)O5—C10—C8119.3 (3)
Mn1—O1W—H1W1118 (2)O4—C10—C8115.4 (2)
Mn1—O1W—H1W2115 (3)N2—C11—C12122.7 (3)
H1W1—O1W—H1W2111 (4)N2—C11—H11118.6
Mn1—O2W—H2W1124 (2)C12—C11—H11118.6
Mn1—O2W—H2W2130 (2)C13—C12—C11119.0 (3)
H2W1—O2W—H2W2105 (3)C13—C12—H12120.5
Mn1—O3W—H3W1120 (2)C11—C12—H12120.5
Mn1—O3W—H3W2100 (2)C12—C13—C14120.3 (3)
H3W1—O3W—H3W2105 (3)C12—C13—H13119.9
H4W1—O4W—H4W2110 (4)C14—C13—H13119.9
C1—O1—Mn1130.21 (18)C13—C14—C22117.0 (3)
C5—O3—C8118.4 (2)C13—C14—C15124.0 (3)
C20—N1—C21117.9 (2)C22—C14—C15119.0 (3)
C20—N1—Mn1125.92 (19)C16—C15—C14122.3 (3)
C21—N1—Mn1116.17 (18)C16—C15—H15118.9
C11—N2—C22118.1 (3)C14—C15—H15118.9
C11—N2—Mn1126.1 (2)C15—C16—C17120.5 (3)
C22—N2—Mn1115.78 (17)C15—C16—H16119.8
O1—C1—O2124.3 (2)C17—C16—H16119.8
O1—C1—C2117.6 (3)C18—C17—C21117.6 (3)
O2—C1—C2118.1 (2)C18—C17—C16123.5 (3)
C3—C2—C7118.6 (2)C21—C17—C16119.0 (3)
C3—C2—C1121.2 (3)C19—C18—C17119.8 (3)
C7—C2—C1120.2 (3)C19—C18—H18120.1
C2—C3—C4121.1 (3)C17—C18—H18120.1
C2—C3—H3119.4C18—C19—C20119.1 (3)
C4—C3—H3119.4C18—C19—H19120.4
C5—C4—C3119.2 (3)C20—C19—H19120.4
C5—C4—H4120.4N1—C20—C19123.4 (3)
C3—C4—H4120.4N1—C20—H20118.3
O3—C5—C4124.8 (2)C19—C20—H20118.3
O3—C5—C6114.9 (2)N1—C21—C17122.3 (3)
C4—C5—C6120.4 (2)N1—C21—C22117.6 (2)
C7—C6—C5119.6 (3)C17—C21—C22120.1 (3)
C7—C6—H6120.2N2—C22—C14122.8 (3)
C5—C6—H6120.2N2—C22—C21118.0 (2)
C6—C7—C2121.0 (3)C14—C22—C21119.2 (3)
C6—C7—H7119.5
O2W—Mn1—O1—C176.5 (2)C5—O3—C8—C9165.6 (2)
O1W—Mn1—O1—C1160.0 (2)C5—O3—C8—C1074.1 (3)
O3W—Mn1—O1—C18.5 (2)O3—C8—C10—O531.7 (3)
N1—Mn1—O1—C1124.4 (3)C9—C8—C10—O586.1 (3)
N2—Mn1—O1—C1101.5 (2)O3—C8—C10—O4151.2 (2)
O1—Mn1—N1—C20157.5 (3)C9—C8—C10—O491.0 (3)
O2W—Mn1—N1—C202.7 (3)C22—N2—C11—C121.6 (5)
O1W—Mn1—N1—C2083.2 (3)Mn1—N2—C11—C12176.0 (3)
O3W—Mn1—N1—C2087.9 (3)N2—C11—C12—C130.8 (6)
N2—Mn1—N1—C20178.4 (3)C11—C12—C13—C140.1 (6)
O1—Mn1—N1—C2121.4 (4)C12—C13—C14—C220.3 (5)
O2W—Mn1—N1—C21178.4 (2)C12—C13—C14—C15178.3 (4)
O1W—Mn1—N1—C2195.8 (2)C13—C14—C15—C16178.4 (4)
O3W—Mn1—N1—C2193.2 (2)C22—C14—C15—C160.1 (6)
N2—Mn1—N1—C212.71 (19)C14—C15—C16—C170.0 (6)
O1—Mn1—N2—C119.4 (3)C15—C16—C17—C18179.6 (4)
O2W—Mn1—N2—C11164.1 (3)C15—C16—C17—C210.9 (5)
O1W—Mn1—N2—C1192.9 (3)C21—C17—C18—C190.8 (5)
O3W—Mn1—N2—C1181.3 (3)C16—C17—C18—C19178.7 (4)
N1—Mn1—N2—C11179.0 (3)C17—C18—C19—C200.5 (6)
O1—Mn1—N2—C22168.3 (2)C21—N1—C20—C190.0 (5)
O2W—Mn1—N2—C2218.2 (4)Mn1—N1—C20—C19178.9 (3)
O1W—Mn1—N2—C2284.8 (2)C18—C19—C20—N10.1 (6)
O3W—Mn1—N2—C22101.0 (2)C20—N1—C21—C170.3 (4)
N1—Mn1—N2—C223.33 (19)Mn1—N1—C21—C17178.7 (2)
Mn1—O1—C1—O26.8 (4)C20—N1—C21—C22179.1 (3)
Mn1—O1—C1—C2174.23 (16)Mn1—N1—C21—C221.9 (3)
O1—C1—C2—C311.7 (4)C18—C17—C21—N10.7 (5)
O2—C1—C2—C3169.3 (2)C16—C17—C21—N1178.8 (3)
O1—C1—C2—C7169.9 (2)C18—C17—C21—C22178.7 (3)
O2—C1—C2—C79.1 (4)C16—C17—C21—C221.8 (5)
C7—C2—C3—C42.8 (4)C11—N2—C22—C141.4 (4)
C1—C2—C3—C4178.8 (2)Mn1—N2—C22—C14176.4 (2)
C2—C3—C4—C50.6 (4)C11—N2—C22—C21178.5 (3)
C8—O3—C5—C410.1 (4)Mn1—N2—C22—C213.7 (3)
C8—O3—C5—C6170.2 (2)C13—C14—C22—N20.5 (5)
C3—C4—C5—O3177.5 (2)C15—C14—C22—N2179.1 (3)
C3—C4—C5—C62.2 (4)C13—C14—C22—C21179.4 (3)
O3—C5—C6—C7177.0 (2)C15—C14—C22—C210.8 (5)
C4—C5—C6—C72.8 (4)N1—C21—C22—N21.2 (4)
C5—C6—C7—C20.5 (4)C17—C21—C22—N2178.2 (3)
C3—C2—C7—C62.3 (4)N1—C21—C22—C14178.9 (3)
C1—C2—C7—C6179.3 (2)C17—C21—C22—C141.7 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O5i0.84 (4)1.92 (4)2.754 (3)170 (3)
O1W—H1W2···O4Wii0.83 (4)1.96 (4)2.774 (4)168 (4)
O2W—H2W1···O3i0.83 (4)2.03 (4)2.847 (3)167 (3)
O2W—H2W2···O4iii0.90 (4)1.73 (4)2.634 (3)173 (3)
O3W—H3W1···O5iii0.90 (3)1.87 (3)2.759 (3)170 (3)
O3W—H3W2···O20.85 (3)1.82 (3)2.647 (3)163 (3)
O4W—H4W1···O20.91 (4)1.85 (4)2.744 (3)168 (4)
O4W—H4W2···O4iv0.85 (4)2.08 (4)2.925 (3)171 (4)
Symmetry codes: (i) x, y1, z; (ii) x+1, y, z; (iii) x1, y1, z; (iv) x+1, y+2, z+2.

Experimental details

Crystal data
Chemical formula[Mn(C10H8O5)(C12H8N2)(H2O)3]·H2O
Mr515.37
Crystal system, space groupTriclinic, P1
Temperature (K)295
a, b, c (Å)7.5457 (15), 11.073 (2), 15.372 (3)
α, β, γ (°)106.16 (3), 99.53 (3), 103.14 (3)
V3)1164.8 (5)
Z2
Radiation typeMo Kα
µ (mm1)0.62
Crystal size (mm)0.38 × 0.25 × 0.17
Data collection
DiffractometerRigaku R-AXIS RAPID
Absorption correctionMulti-scan
(ABSCOR; Higashi, 1995)
Tmin, Tmax0.826, 0.893
No. of measured, independent and
observed [I > 2σ(I)] reflections
11565, 5280, 3105
Rint0.036
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.038, 0.100, 1.12
No. of reflections5280
No. of parameters332
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.56, 0.73

Computer programs: RAPID-AUTO (Rigaku, 1998), RAPID-AUTO, CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.

Selected geometric parameters (Å, º) top
Mn1—O12.1318 (19)Mn1—O3W2.204 (2)
Mn1—O2W2.156 (2)Mn1—N12.290 (2)
Mn1—O1W2.174 (2)Mn1—N22.292 (2)
O1—Mn1—O2W108.33 (8)O1W—Mn1—N190.74 (10)
O1—Mn1—O1W83.81 (9)O3W—Mn1—N198.24 (9)
O2W—Mn1—O1W85.84 (9)O1—Mn1—N288.65 (9)
O1—Mn1—O3W90.70 (8)O2W—Mn1—N2162.90 (8)
O2W—Mn1—O3W85.06 (9)O1W—Mn1—N298.30 (9)
O1W—Mn1—O3W167.32 (8)O3W—Mn1—N292.97 (9)
O1—Mn1—N1159.22 (8)N1—Mn1—N272.27 (9)
O2W—Mn1—N191.18 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O5i0.84 (4)1.92 (4)2.754 (3)170 (3)
O1W—H1W2···O4Wii0.83 (4)1.96 (4)2.774 (4)168 (4)
O2W—H2W1···O3i0.83 (4)2.03 (4)2.847 (3)167 (3)
O2W—H2W2···O4iii0.90 (4)1.73 (4)2.634 (3)173 (3)
O3W—H3W1···O5iii0.90 (3)1.87 (3)2.759 (3)170 (3)
O3W—H3W2···O20.85 (3)1.82 (3)2.647 (3)163 (3)
O4W—H4W1···O20.91 (4)1.85 (4)2.744 (3)168 (4)
O4W—H4W2···O4iv0.85 (4)2.08 (4)2.925 (3)171 (4)
Symmetry codes: (i) x, y1, z; (ii) x+1, y, z; (iii) x1, y1, z; (iv) x+1, y+2, z+2.
 

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