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In the title compound, [Mn(C14H8N2O6)2(H2O)4]n, each 6,6′-dihydr­oxy-3,3-diazenediyldibenzoate ligand acts as a carboxyl­ate bridge, leading to the formation of polymeric chains running in the [110] direction. The Mn atom is hexa­coordinated in a distorted octa­hedral geometry by six O atoms [Mn—O = 2.1412 (16)–2.2262 (17) Å] from two organic ligands and four water mol­ecules. The crystal packing is stabilized by π–π inter­actions and inter­molecular O—H...O and O—H...N hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807012305/cv2198sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807012305/cv2198Isup2.hkl
Contains datablock I

CCDC reference: 642953

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.029
  • wR factor = 0.070
  • Data-to-parameter ratio = 15.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn1 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8
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 28.33 From the CIF: _reflns_number_total 3620 Count of symmetry unique reflns 2410 Completeness (_total/calc) 150.21% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1210 Fraction of Friedel pairs measured 0.502 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL.

catena-Poly[[tetraaquamanganese(II)]-µ-6,6'-dihydroxy-3,3- diazenediyldibenzoato-κ2O:O'] top
Crystal data top
[Mn(C14H8N2O6)2(H2O)4]Dx = 1.758 Mg m3
Mr = 427.23Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P43212Cell parameters from 935 reflections
Hall symbol: P 4nw 2abwθ = 2.1–26°
a = 10.2694 (13) ŵ = 0.88 mm1
c = 30.611 (8) ÅT = 293 K
V = 3228.2 (10) Å3Block, orange
Z = 80.18 × 0.14 × 0.12 mm
F(000) = 1752
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
3620 independent reflections
Radiation source: fine-focus sealed tube3153 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.040
φ and ω scansθmax = 28.3°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1113
Tmin = 0.86, Tmax = 0.90k = 1112
18659 measured reflectionsl = 3839
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.029H-atom parameters constrained
wR(F2) = 0.070 w = 1/[σ2(Fo2) + (0.0368P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.13(Δ/σ)max < 0.001
3620 reflectionsΔρmax = 0.30 e Å3
239 parametersΔρmin = 0.42 e Å3
12 restraintsAbsolute structure: Flack (1983), 1210 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.003 (16)
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
Mn10.31207 (3)0.96108 (3)0.142844 (10)0.02553 (9)
O1W0.33240 (17)0.80000 (17)0.09491 (5)0.0435 (4)
H1WA0.38950.81460.07550.065*
H1WB0.26930.75770.08410.065*
O21.11938 (17)0.24608 (17)0.14725 (5)0.0405 (4)
O2W0.50673 (16)1.02057 (18)0.12576 (6)0.0462 (4)
H2WA0.54241.09320.11990.069*
H2WB0.55490.97820.14330.069*
O30.35369 (17)0.84367 (17)0.28231 (5)0.0430 (4)
H3A0.34280.87200.25750.052*
O3W0.23079 (16)1.07358 (16)0.09064 (5)0.0415 (4)
H3WA0.19251.14090.10030.062*
H3WB0.24011.07920.06320.062*
O40.39386 (15)0.86759 (16)0.19998 (5)0.0334 (4)
O4W0.12448 (17)0.85805 (19)0.15441 (5)0.0442 (4)
H4WA0.13140.80990.17690.066*
H4WB0.09080.81440.13370.066*
O50.57627 (16)0.78864 (16)0.17102 (5)0.0357 (4)
O61.18617 (17)0.06247 (16)0.26542 (5)0.0428 (4)
H6A1.22420.05490.24200.051*
N10.80204 (18)0.44061 (18)0.25395 (6)0.0302 (4)
N20.74338 (18)0.47035 (18)0.28867 (6)0.0293 (4)
O11.23776 (16)0.10721 (15)0.18662 (5)0.0341 (4)
C20.4791 (2)0.6890 (2)0.32062 (7)0.0329 (5)
H2B0.43190.70730.34580.039*
C31.0101 (2)0.1727 (2)0.29780 (7)0.0321 (5)
H3B1.02090.12220.32270.038*
C41.0720 (2)0.2238 (2)0.22317 (7)0.0262 (5)
C50.4507 (2)0.7540 (2)0.28193 (7)0.0279 (5)
C60.8987 (2)0.3420 (2)0.25912 (7)0.0273 (5)
C70.6465 (2)0.5676 (2)0.28398 (7)0.0267 (5)
C80.4969 (2)0.7982 (2)0.20195 (7)0.0270 (5)
C90.6194 (2)0.6342 (2)0.24557 (7)0.0256 (5)
H9A0.66720.61560.22050.031*
C101.0906 (2)0.1525 (2)0.26152 (7)0.0286 (5)
C110.9760 (2)0.3190 (2)0.22291 (7)0.0281 (5)
H11A0.96340.36850.19780.034*
C120.5227 (2)0.72763 (19)0.24386 (7)0.0245 (4)
C130.5760 (2)0.5984 (2)0.32171 (7)0.0309 (5)
H13A0.59560.55650.34780.037*
C140.9156 (2)0.2664 (2)0.29672 (7)0.0295 (5)
H14A0.86260.27990.32090.035*
C11.1470 (2)0.1928 (2)0.18252 (7)0.0295 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.02670 (18)0.02635 (17)0.02353 (15)0.00340 (14)0.00019 (14)0.00063 (13)
O1W0.0451 (10)0.0418 (10)0.0435 (10)0.0039 (9)0.0007 (9)0.0126 (8)
O20.0487 (10)0.0430 (10)0.0297 (8)0.0185 (8)0.0010 (8)0.0022 (8)
O2W0.0319 (9)0.0515 (11)0.0551 (10)0.0063 (8)0.0049 (8)0.0242 (9)
O30.0428 (10)0.0523 (11)0.0339 (9)0.0268 (8)0.0079 (8)0.0098 (8)
O3W0.0503 (11)0.0448 (10)0.0294 (8)0.0176 (8)0.0027 (8)0.0078 (7)
O40.0276 (9)0.0396 (9)0.0329 (8)0.0110 (7)0.0002 (7)0.0075 (7)
O4W0.0436 (11)0.0535 (12)0.0354 (9)0.0154 (8)0.0018 (8)0.0044 (8)
O50.0366 (9)0.0410 (10)0.0294 (8)0.0112 (7)0.0065 (7)0.0065 (7)
O60.0497 (11)0.0449 (10)0.0337 (9)0.0282 (9)0.0025 (8)0.0025 (8)
N10.0286 (10)0.0312 (10)0.0309 (9)0.0076 (8)0.0031 (8)0.0036 (8)
N20.0299 (10)0.0277 (10)0.0303 (10)0.0062 (8)0.0014 (8)0.0020 (8)
O10.0347 (9)0.0336 (9)0.0340 (8)0.0149 (7)0.0032 (7)0.0074 (7)
C20.0344 (12)0.0373 (12)0.0269 (11)0.0101 (11)0.0039 (9)0.0005 (10)
C30.0362 (12)0.0326 (13)0.0274 (11)0.0051 (10)0.0051 (9)0.0056 (9)
C40.0252 (11)0.0242 (11)0.0292 (11)0.0018 (8)0.0053 (9)0.0040 (9)
C50.0280 (11)0.0267 (11)0.0292 (11)0.0063 (9)0.0003 (9)0.0004 (9)
C60.0244 (11)0.0261 (12)0.0315 (12)0.0041 (9)0.0040 (9)0.0005 (9)
C70.0240 (11)0.0262 (11)0.0299 (12)0.0049 (9)0.0009 (9)0.0007 (9)
C80.0283 (11)0.0231 (11)0.0296 (11)0.0008 (9)0.0017 (9)0.0010 (9)
C90.0233 (11)0.0274 (11)0.0262 (11)0.0003 (9)0.0028 (9)0.0008 (9)
C100.0299 (12)0.0244 (12)0.0314 (12)0.0061 (9)0.0059 (9)0.0027 (9)
C110.0287 (11)0.0286 (11)0.0270 (10)0.0038 (9)0.0003 (9)0.0026 (9)
C120.0244 (11)0.0228 (11)0.0263 (11)0.0012 (8)0.0009 (9)0.0008 (8)
C130.0376 (13)0.0331 (12)0.0220 (11)0.0065 (10)0.0006 (9)0.0028 (9)
C140.0263 (11)0.0330 (12)0.0292 (11)0.0010 (9)0.0004 (9)0.0016 (10)
C10.0307 (12)0.0273 (11)0.0304 (11)0.0026 (9)0.0030 (9)0.0037 (10)
Geometric parameters (Å, º) top
Mn1—O3W2.1412 (16)N2—C71.417 (3)
Mn1—O1i2.1517 (15)O1—C11.287 (3)
Mn1—O2W2.1547 (17)O1—Mn1ii2.1517 (15)
Mn1—O42.1648 (15)C2—C131.363 (3)
Mn1—O1W2.2209 (18)C2—C51.391 (3)
Mn1—O4W2.2262 (17)C2—H2B0.9300
O1W—H1WA0.8486C3—C141.367 (3)
O1W—H1WB0.8482C3—C101.400 (3)
O2—C11.243 (3)C3—H3B0.9300
O2W—H2WA0.8499C4—C111.388 (3)
O2W—H2WB0.8498C4—C101.397 (3)
O3—C51.357 (3)C4—C11.498 (3)
O3—H3A0.8200C5—C121.407 (3)
O3W—H3WA0.8490C6—C111.384 (3)
O3W—H3WB0.8486C6—C141.399 (3)
O4—C81.277 (3)C7—C91.388 (3)
O4W—H4WA0.8500C7—C131.399 (3)
O4W—H4WB0.8500C8—C121.497 (3)
O5—C81.253 (3)C9—C121.381 (3)
O6—C101.353 (3)C9—H9A0.9300
O6—H6A0.8200C11—H11A0.9300
N1—N21.259 (3)C13—H13A0.9300
N1—C61.427 (3)C14—H14A0.9300
O3W—Mn1—O1i87.15 (6)C10—C3—H3B119.8
O3W—Mn1—O2W91.58 (7)C11—C4—C10118.2 (2)
O1i—Mn1—O2W106.40 (7)C11—C4—C1120.68 (19)
O3W—Mn1—O4173.45 (6)C10—C4—C1121.04 (19)
O1i—Mn1—O486.77 (6)O3—C5—C2118.23 (19)
O2W—Mn1—O487.81 (6)O3—C5—C12121.60 (19)
O3W—Mn1—O1W86.88 (6)C2—C5—C12120.2 (2)
O1i—Mn1—O1W164.63 (7)C11—C6—C14119.5 (2)
O2W—Mn1—O1W87.92 (7)C11—C6—N1115.57 (19)
O4—Mn1—O1W99.61 (6)C14—C6—N1124.8 (2)
O3W—Mn1—O4W92.17 (7)C9—C7—C13119.0 (2)
O1i—Mn1—O4W85.73 (7)C9—C7—N2125.02 (19)
O2W—Mn1—O4W167.47 (7)C13—C7—N2116.00 (19)
O4—Mn1—O4W89.80 (6)O5—C8—O4123.2 (2)
O1W—Mn1—O4W80.36 (6)O5—C8—C12119.60 (19)
Mn1—O1W—H1WA113.4O4—C8—C12117.21 (19)
Mn1—O1W—H1WB124.6C12—C9—C7121.22 (19)
H1WA—O1W—H1WB110.1C12—C9—H9A119.4
Mn1—O2W—H2WA134.4C7—C9—H9A119.4
Mn1—O2W—H2WB104.0O6—C10—C4122.1 (2)
H2WA—O2W—H2WB109.4O6—C10—C3117.4 (2)
C5—O3—H3A109.5C4—C10—C3120.5 (2)
Mn1—O3W—H3WA111.1C6—C11—C4121.5 (2)
Mn1—O3W—H3WB137.1C6—C11—H11A119.2
H3WA—O3W—H3WB110.0C4—C11—H11A119.2
C8—O4—Mn1127.37 (14)C9—C12—C5118.70 (19)
Mn1—O4W—H4WA109.5C9—C12—C8119.74 (19)
Mn1—O4W—H4WB118.9C5—C12—C8121.57 (18)
H4WA—O4W—H4WB109.3C2—C13—C7120.8 (2)
C10—O6—H6A109.5C2—C13—H13A119.6
N2—N1—C6114.29 (18)C7—C13—H13A119.6
N1—N2—C7114.91 (18)C3—C14—C6119.9 (2)
C1—O1—Mn1ii132.24 (14)C3—C14—H14A120.1
C13—C2—C5120.1 (2)C6—C14—H14A120.1
C13—C2—H2B119.9O2—C1—O1123.4 (2)
C5—C2—H2B119.9O2—C1—C4120.68 (19)
C14—C3—C10120.3 (2)O1—C1—C4115.89 (19)
C14—C3—H3B119.8
Symmetry codes: (i) x1, y+1, z; (ii) x+1, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O4W—H4WA···O3iii0.852.112.930 (3)162
O4W—H4WB···O5iv0.851.992.801 (2)160
O3W—H3WA···O2i0.851.952.729 (2)153
O3—H3A···O40.821.842.566 (2)147
O3W—H3WB···N1iv0.852.162.990 (3)166
O2W—H2WA···O2iv0.851.902.753 (3)176
O2W—H2WB···O50.852.132.846 (3)141
O6—H6A···O10.821.782.512 (2)147
O1W—H1WB···O5iv0.852.042.826 (3)153
O1W—H1WA···O6v0.852.322.907 (2)127
Symmetry codes: (i) x1, y+1, z; (iii) y+1, x+1, z+1/2; (iv) x1/2, y+3/2, z+1/4; (v) y+1/2, x1/2, z1/4.
 

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