Literature DB >> 21200561

Poly[μ(2)-aqua-μ(4)-naphthalene-1,8-dicarboxyl-ato-manganese(II)].

Guo-Ying Zhang1, Xin Zhang, Gui-Sheng Yu.   

Abstract

The asymmetric unit of the title complex, [Mn(C(12)H(6)O(4))(H(2)O)](n), contains one Mn(II) ion, one 1,8-naphthalene-dicarboxyl-ate (1,8-NDC) ligand and one water mol-ecule. The Mn(II) ion is six-coordinated within a distorted octa-hedral coordination geometry, in which the equatorial sites are occupied by four carboxyl-ate O atoms from four different 1,8-NDC ligands, while the axial positions are occupied by two O atoms of two coordinated water mol-ecules. Adjacent Mn(II) centres are bridged by one coordinated water and two carboxyl-ate groups in a syn-syn mode to form infinite chains along the b axis, which are further cross-linked by the naphthalene spacers of the 1,8-NDC ligands to produce a two-dimensional extended network.

Entities:  

Year:  2007        PMID： 21200561      PMCID： PMC2915142          DOI： 10.1107/S1600536807063696

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For general background, see: Chen et al. (2005 ▶). For related literature, see: Van der Ploeg et al. (1979 ▶); Hu et al. 2006 ▶.

Experimental

Crystal data

[Mn(C12H6O4)(H2O)] M = 287.12 Monoclinic, a = 15.720 (3) Å b = 7.2167 (14) Å c = 9.837 (2) Å β = 98.87 (3)° V = 1102.6 (4) Å3 Z = 4 Mo Kα radiation μ = 1.21 mm−1 T = 294 (2) K 0.20 × 0.20 × 0.16 mm

Data collection

Rigaku R-AXIS RAPID-S diffractometer Absorption correction: multi-scan (SADABS; Bruker, 1998 ▶) T min = 0.794, T max = 0.830 9056 measured reflections 1945 independent reflections 1632 reflections with I > 2σ(I) R int = 0.058

Refinement

R[F 2 > 2σ(F 2)] = 0.040 wR(F 2) = 0.089 S = 1.09 1945 reflections 171 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.85 e Å−3 Δρmin = −0.33 e Å−3 Data collection: CrystalClear (Rigaku/MSC, 2005 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL (Bruker, 1998 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536807063696/hk2400sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536807063696/hk2400Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Mn(C12H6O4)(H2O)]F000 = 580
Mr = 287.12Dx = 1.730 Mg m−3
Monoclinic, P21/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2641 reflections
a = 15.720 (3) Åθ = 3.1–27.5º
b = 7.2167 (14) ŵ = 1.21 mm−1
c = 9.837 (2) ÅT = 294 (2) K
β = 98.87 (3)ºBlock, colourless
V = 1102.6 (4) Å30.20 × 0.20 × 0.16 mm
Z = 4
Rigaku R-AXIS RAPID-S diffractometer1945 independent reflections
Radiation source: fine-focus sealed tube1632 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.058
T = 294(2) Kθmax = 25.0º
ω scansθmin = 3.1º
Absorption correction: multi-scan(SADABS; Bruker, 1998)h = −18→18
Tmin = 0.794, Tmax = 0.830k = −8→8
9056 measured reflectionsl = −11→11
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.040H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.089  w = 1/[σ2(Fo2) + (0.0445P)2] where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
1945 reflectionsΔρmax = 0.85 e Å−3
171 parametersΔρmin = −0.33 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
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.
xyzUiso*/Ueq
Mn10.99931 (3)0.10265 (5)0.25999 (4)0.01809 (16)
O1W0.99998 (17)−0.1557 (3)0.3815 (2)0.0211 (5)
H1WA0.952 (3)−0.169 (5)0.419 (4)0.055 (13)*
H1WB1.041 (3)−0.170 (5)0.439 (4)0.045 (12)*
O10.90398 (13)0.2094 (3)0.3753 (2)0.0248 (5)
O20.89298 (12)0.5099 (3)0.3261 (2)0.0265 (5)
O31.09599 (13)0.2087 (3)0.4210 (2)0.0251 (5)
O40.89011 (12)0.0082 (3)0.1235 (2)0.0268 (5)
C10.86289 (19)0.3603 (4)0.3608 (3)0.0200 (6)
C20.76960 (19)0.3550 (4)0.3732 (3)0.0232 (7)
C30.7238 (2)0.2112 (5)0.3086 (4)0.0370 (9)
H30.75280.11190.27660.044*
C40.6336 (2)0.2110 (6)0.2897 (4)0.0509 (11)
H40.60320.11100.24690.061*
C50.5907 (2)0.3560 (6)0.3335 (4)0.0460 (10)
H50.53090.35710.31690.055*
C60.63495 (19)0.5047 (5)0.4034 (3)0.0334 (8)
C70.5903 (2)0.6559 (5)0.4497 (4)0.0437 (10)
H70.53050.65760.43230.052*
C80.6326 (2)0.7975 (6)0.5184 (4)0.0501 (10)
H80.60210.89830.54490.060*
C90.7223 (2)0.7935 (5)0.5499 (3)0.0368 (9)
H90.75080.89130.59900.044*
C100.7689 (2)0.6497 (4)0.5105 (3)0.0248 (7)
C111.13824 (19)0.3572 (4)0.4273 (3)0.0198 (6)
C120.72618 (18)0.5038 (4)0.4298 (3)0.0234 (7)
U11U22U33U12U13U23
Mn10.0187 (3)0.0169 (2)0.0185 (3)0.00005 (19)0.00249 (17)−0.00056 (18)
O1W0.0221 (13)0.0214 (11)0.0194 (12)0.0009 (9)0.0017 (10)0.0025 (8)
O10.0230 (12)0.0284 (12)0.0234 (12)0.0067 (10)0.0048 (9)−0.0014 (9)
O20.0246 (12)0.0283 (13)0.0282 (12)−0.0030 (10)0.0091 (9)0.0008 (9)
O30.0230 (12)0.0288 (12)0.0232 (12)−0.0073 (10)0.0026 (9)−0.0045 (9)
O40.0240 (12)0.0282 (13)0.0264 (12)−0.0009 (9)−0.0023 (9)−0.0033 (9)
C10.0205 (17)0.0268 (17)0.0128 (14)−0.0021 (13)0.0027 (11)−0.0038 (12)
C20.0192 (17)0.0269 (17)0.0234 (16)−0.0011 (12)0.0029 (12)−0.0009 (13)
C30.027 (2)0.034 (2)0.050 (2)−0.0056 (15)0.0051 (16)−0.0138 (16)
C40.029 (2)0.051 (3)0.070 (3)−0.0170 (18)−0.0015 (19)−0.026 (2)
C50.0181 (19)0.063 (3)0.055 (2)−0.0063 (17)0.0005 (16)−0.0129 (19)
C60.0208 (19)0.044 (2)0.035 (2)0.0001 (15)0.0018 (14)−0.0031 (16)
C70.0168 (19)0.057 (3)0.056 (2)0.0107 (16)0.0010 (16)−0.0082 (19)
C80.031 (2)0.052 (3)0.067 (3)0.0167 (19)0.0066 (19)−0.016 (2)
C90.026 (2)0.037 (2)0.046 (2)0.0074 (15)−0.0002 (15)−0.0138 (16)
C100.0203 (17)0.0282 (17)0.0251 (17)0.0016 (13)0.0010 (13)0.0008 (13)
C110.0197 (16)0.0268 (17)0.0130 (14)0.0009 (13)0.0033 (11)−0.0024 (12)
C120.0200 (17)0.0252 (17)0.0245 (17)−0.0003 (13)0.0017 (12)0.0010 (13)
Mn1—O2i2.115 (2)C6—C121.418 (4)
Mn1—O42.122 (2)C7—C81.343 (5)
Mn1—O12.156 (2)C7—H70.9300
Mn1—O32.159 (2)C8—C91.396 (5)
Mn1—O1W2.214 (2)C8—H80.9300
Mn1—O1Wii2.232 (2)C9—C101.362 (4)
C1—O21.247 (3)C9—H90.9300
C1—O11.262 (3)C10—C121.423 (4)
C1—C21.491 (4)C10—C11iii1.494 (4)
C2—C31.364 (4)C11—O4ii1.252 (3)
C2—C121.430 (4)C11—O31.257 (3)
C3—C41.401 (5)C11—C10iii1.494 (4)
C3—H30.9300O2—Mn1ii2.115 (2)
C4—C51.350 (5)O4—C11i1.252 (3)
C4—H40.9300O1W—Mn1i2.232 (2)
C5—C61.400 (5)O1W—H1WA0.89 (4)
C5—H50.9300O1W—H1WB0.80 (4)
C6—C71.410 (5)
O2i—Mn1—O4105.32 (8)C5—C6—C12119.9 (3)
O2i—Mn1—O1171.04 (8)C7—C6—C12118.9 (3)
O4—Mn1—O183.54 (8)C8—C7—C6121.3 (3)
O2i—Mn1—O383.67 (8)C8—C7—H7119.4
O4—Mn1—O3170.82 (8)C6—C7—H7119.4
O1—Mn1—O387.43 (8)C7—C8—C9120.0 (4)
O2i—Mn1—O1W90.70 (9)C7—C8—H8120.0
O4—Mn1—O1W90.40 (9)C9—C8—H8120.0
O1—Mn1—O1W87.88 (9)C10—C9—C8121.5 (3)
O3—Mn1—O1W87.61 (9)C10—C9—H9119.3
O2i—Mn1—O1Wii85.20 (9)C8—C9—H9119.3
O4—Mn1—O1Wii86.44 (9)C9—C10—C12119.6 (3)
O1—Mn1—O1Wii96.86 (8)C9—C10—C11iii116.3 (3)
O3—Mn1—O1Wii96.31 (9)C12—C10—C11iii123.4 (3)
O1W—Mn1—O1Wii173.97 (6)O4ii—C11—O3124.7 (3)
O2—C1—O1124.6 (3)O4ii—C11—C10iii117.3 (3)
O2—C1—C2117.6 (3)O3—C11—C10iii117.8 (3)
O1—C1—C2117.5 (3)C6—C12—C10118.4 (3)
C3—C2—C12120.2 (3)C6—C12—C2117.5 (3)
C3—C2—C1115.9 (3)C10—C12—C2124.0 (3)
C12—C2—C1123.2 (3)C1—O1—Mn1129.36 (18)
C2—C3—C4120.9 (3)C1—O2—Mn1ii138.1 (2)
C2—C3—H3119.6C11—O3—Mn1130.17 (19)
C4—C3—H3119.6C11i—O4—Mn1137.39 (19)
C5—C4—C3120.1 (3)Mn1—O1W—Mn1i108.74 (9)
C5—C4—H4120.0Mn1—O1W—H1WA112 (2)
C3—C4—H4120.0Mn1i—O1W—H1WA105 (2)
C4—C5—C6121.1 (3)Mn1—O1W—H1WB115 (3)
C4—C5—H5119.5Mn1i—O1W—H1WB105 (3)
C6—C5—H5119.5H1WA—O1W—H1WB110 (4)
C5—C6—C7121.2 (3)
O2—C1—C2—C3131.1 (3)C1—C2—C12—C6163.6 (3)
O1—C1—C2—C3−43.2 (4)C3—C2—C12—C10173.6 (3)
O2—C1—C2—C12−39.4 (4)C1—C2—C12—C10−16.3 (5)
O1—C1—C2—C12146.3 (3)O2—C1—O1—Mn1−35.5 (4)
C12—C2—C3—C43.5 (5)C2—C1—O1—Mn1138.5 (2)
C1—C2—C3—C4−167.3 (3)O4—Mn1—O1—C1−84.6 (2)
C2—C3—C4—C51.2 (6)O3—Mn1—O1—C197.1 (2)
C3—C4—C5—C6−2.8 (6)O1W—Mn1—O1—C1−175.2 (2)
C4—C5—C6—C7−179.8 (4)O1Wii—Mn1—O1—C11.0 (3)
C4—C5—C6—C12−0.4 (6)O1—C1—O2—Mn1ii14.5 (5)
C5—C6—C7—C8179.1 (4)C2—C1—O2—Mn1ii−159.4 (2)
C12—C6—C7—C8−0.3 (6)O4ii—C11—O3—Mn134.3 (4)
C6—C7—C8—C9−2.5 (6)C10iii—C11—O3—Mn1−140.3 (2)
C7—C8—C9—C101.2 (6)O2i—Mn1—O3—C1183.3 (2)
C8—C9—C10—C122.9 (5)O1—Mn1—O3—C11−97.7 (3)
C8—C9—C10—C11iii−168.6 (3)O1W—Mn1—O3—C11174.3 (3)
C5—C6—C12—C10−175.1 (3)O1Wii—Mn1—O3—C11−1.1 (3)
C7—C6—C12—C104.3 (5)O2i—Mn1—O4—C11i55.2 (3)
C5—C6—C12—C24.9 (5)O1—Mn1—O4—C11i−123.4 (3)
C7—C6—C12—C2−175.7 (3)O1W—Mn1—O4—C11i−35.6 (3)
C9—C10—C12—C6−5.6 (5)O1Wii—Mn1—O4—C11i139.2 (3)
C11iii—C10—C12—C6165.3 (3)O2i—Mn1—O1W—Mn1i−52.06 (11)
C9—C10—C12—C2174.4 (3)O4—Mn1—O1W—Mn1i53.27 (11)
C11iii—C10—C12—C2−14.7 (5)O1—Mn1—O1W—Mn1i136.79 (11)
C3—C2—C12—C6−6.5 (4)O3—Mn1—O1W—Mn1i−135.70 (11)
Mn1—O2i2.115 (2)
Mn1—O42.122 (2)
Mn1—O12.156 (2)
Mn1—O32.159 (2)
Mn1—O1W2.214 (2)
Mn1—O1Wii2.232 (2)
O2i—Mn1—O4105.32 (8)
O2i—Mn1—O1171.04 (8)
O4—Mn1—O183.54 (8)
O2i—Mn1—O383.67 (8)
O4—Mn1—O3170.82 (8)
O1—Mn1—O387.43 (8)
O2i—Mn1—O1W90.70 (9)
O4—Mn1—O1W90.40 (9)
O1—Mn1—O1W87.88 (9)
O3—Mn1—O1W87.61 (9)
O2i—Mn1—O1Wii85.20 (9)
O4—Mn1—O1Wii86.44 (9)
O1—Mn1—O1Wii96.86 (8)
O3—Mn1—O1Wii96.31 (9)
O1W—Mn1—O1Wii173.97 (6)

Symmetry codes: (i) ; (ii) .

  1 in total

1.  Syntheses, crystal structures, and magneto-structural correlations of novel Cu(II) complexes containing a planar [Cu(mu-L1)]2 (HL1 = 3-(2-pyridyl)pyrazole) unit: from dinuclear to tetranuclear and then to one-dimensional compounds.

Authors:  Tong-Liang Hu; Jian-Rong Li; Chun-Sen Liu; Xue-Song Shi; Jiang-Ning Zhou; Xian-He Bu; Joan Ribas
Journal:  Inorg Chem       Date:  2006-01-09       Impact factor: 5.165
  1 in total
  1 in total

1.  Poly[μ-aqua-aqua-μ4-naphthalene-1,8-dicarboxyl-ato-barium]: a layer structure.

Authors:  Dan Zhao; Fei Fei Li; Peng Liang; Jun-Ran Ren; Shen Qiu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2013-03-16
  1 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.