metal-organic compounds
One of the two independent Mn atoms of the polymeric title compound, [Mn3(C16H10O4)3(H2O)2]n, lies on a special position of 3 site symmetry and the other on a special position of site symmetry. One end of the 4,4'-(ethene-1,2-diyl)dibenzoate dianion bridges the two independent Mn atoms. The water-coordinated Mn atom on the threefold axis is linked to the O atoms of three dianions in a tetrahedral environment. The Mn atom is linked to the O atoms of six different dianions in an octahedral geometry.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044126/hg2119sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044126/hg2119Isup2.hkl |
CCDC reference: 627788
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: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97.
Poly[diaquatris[(E)-4,4'-(ethene-1,2-diyl)dibenzoato]trimanganese(II)] top
Crystal data top
[Mn3(C16H10O4)3(H2O)2] | Dx = 1.280 Mg m−3 |
Mr = 999.57 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3 | Cell parameters from 10113 reflections |
Hall symbol: -R 3 | θ = 3.1–27.5° |
a = 16.3366 (8) Å | µ = 0.78 mm−1 |
c = 16.8286 (7) Å | T = 293 K |
V = 3889.6 (2) Å3 | Block, yellow |
Z = 3 | 0.30 × 0.22 × 0.15 mm |
F(000) = 1527 |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 1980 independent reflections |
Radiation source: fine-focus sealed tube | 1663 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −21→21 |
Tmin = 0.661, Tmax = 0.892 | k = −21→21 |
12671 measured reflections | l = −20→21 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.069 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.251 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.1598P)2 + 8.6886P] where P = (Fo2 + 2Fc2)/3 |
1980 reflections | (Δ/σ)max = 0.001 |
96 parameters | Δρmax = 0.94 e Å−3 |
94 restraints | Δρmin = −0.58 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Mn1 | 0.0000 | 0.0000 | 0.20525 (6) | 0.0515 (4) | |
Mn2 | 0.0000 | 0.0000 | 0.0000 | 0.0352 (4) | |
O1 | −0.0113 (3) | 0.1201 (2) | 0.1910 (2) | 0.0728 (9) | |
O2 | 0.0565 (2) | 0.1213 (2) | 0.0776 (2) | 0.0644 (8) | |
O1w | 0.0000 | 0.0000 | 0.3285 (5) | 0.175 (6) | |
H1W | −0.0027 | 0.0459 | 0.3448 | 0.209* | 0.33 |
H2W | 0.0486 | 0.0027 | 0.3448 | 0.209* | 0.33 |
C1 | 0.0197 (3) | 0.1546 (3) | 0.1232 (3) | 0.0562 (10) | |
C2 | 0.0151 (10) | 0.2381 (7) | 0.0948 (8) | 0.0619 (12) | 0.50 |
C3 | −0.0557 (10) | 0.2524 (8) | 0.1254 (7) | 0.067 (3) | 0.50 |
H3 | −0.1010 | 0.2079 | 0.1593 | 0.081* | 0.50 |
C4 | −0.0589 (8) | 0.3333 (8) | 0.1052 (7) | 0.093 (2) | 0.50 |
H4 | −0.1063 | 0.3429 | 0.1256 | 0.112* | 0.50 |
C5 | 0.0088 (7) | 0.3998 (6) | 0.0544 (6) | 0.089 (2) | 0.50 |
C6 | 0.0796 (6) | 0.3854 (6) | 0.0238 (6) | 0.082 (3) | 0.50 |
H6 | 0.1249 | 0.4299 | −0.0102 | 0.098* | 0.50 |
C7 | 0.0828 (7) | 0.3046 (7) | 0.0440 (7) | 0.075 (3) | 0.50 |
H7 | 0.1302 | 0.2950 | 0.0235 | 0.090* | 0.50 |
C8 | 0.0007 (10) | 0.4825 (8) | 0.0363 (10) | 0.093 (4) | 0.50 |
H8 | −0.0345 | 0.4954 | 0.0723 | 0.111* | 0.50 |
C9 | −0.0115 (10) | 0.7608 (7) | −0.1007 (7) | 0.0619 (12) | 0.50 |
C10 | 0.0439 (11) | 0.7353 (9) | −0.1452 (6) | 0.067 (3) | 0.50 |
H10 | 0.0710 | 0.7665 | −0.1926 | 0.081* | 0.50 |
C11 | 0.0588 (9) | 0.6631 (8) | −0.1190 (7) | 0.093 (2) | 0.50 |
H11 | 0.0959 | 0.6460 | −0.1488 | 0.112* | 0.50 |
C12 | 0.0183 (6) | 0.6164 (6) | −0.0482 (6) | 0.089 (2) | 0.50 |
C13 | −0.0372 (6) | 0.6420 (6) | −0.0037 (5) | 0.082 (3) | 0.50 |
H13 | −0.0643 | 0.6108 | 0.0436 | 0.098* | 0.50 |
C14 | −0.0521 (8) | 0.7141 (7) | −0.0300 (7) | 0.075 (3) | 0.50 |
H14 | −0.0891 | 0.7312 | −0.0002 | 0.090* | 0.50 |
C15 | 0.0362 (10) | 0.5416 (8) | −0.0237 (11) | 0.093 (4) | 0.50 |
H15 | 0.0792 | 0.5344 | −0.0550 | 0.111* | 0.50 |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0517 (5) | 0.0517 (5) | 0.0511 (6) | 0.0258 (2) | 0.000 | 0.000 |
Mn2 | 0.0344 (5) | 0.0344 (5) | 0.0367 (6) | 0.0172 (2) | 0.000 | 0.000 |
O1 | 0.104 (3) | 0.0564 (17) | 0.0649 (19) | 0.0447 (18) | −0.0082 (17) | −0.0063 (14) |
O2 | 0.0582 (16) | 0.0481 (15) | 0.090 (2) | 0.0286 (13) | −0.0134 (15) | −0.0254 (14) |
O1w | 0.233 (9) | 0.233 (9) | 0.058 (5) | 0.116 (5) | 0.000 | 0.000 |
C1 | 0.061 (2) | 0.0435 (18) | 0.067 (2) | 0.0278 (17) | −0.0161 (18) | −0.0164 (17) |
C2 | 0.081 (3) | 0.053 (2) | 0.062 (3) | 0.042 (2) | 0.003 (2) | −0.0041 (18) |
C3 | 0.082 (4) | 0.062 (4) | 0.067 (6) | 0.043 (3) | 0.006 (4) | −0.008 (4) |
C4 | 0.114 (4) | 0.088 (4) | 0.108 (5) | 0.073 (3) | 0.023 (4) | 0.006 (3) |
C5 | 0.108 (6) | 0.085 (4) | 0.100 (4) | 0.067 (4) | 0.007 (4) | 0.008 (3) |
C6 | 0.101 (6) | 0.071 (5) | 0.076 (5) | 0.044 (4) | 0.008 (4) | 0.011 (4) |
C7 | 0.089 (6) | 0.076 (4) | 0.075 (4) | 0.053 (5) | 0.015 (4) | 0.003 (3) |
C8 | 0.100 (9) | 0.085 (6) | 0.111 (6) | 0.059 (6) | 0.019 (6) | 0.010 (5) |
C9 | 0.081 (3) | 0.053 (2) | 0.062 (3) | 0.042 (2) | 0.003 (2) | −0.0041 (18) |
C10 | 0.082 (4) | 0.062 (4) | 0.067 (6) | 0.043 (3) | 0.006 (4) | −0.008 (4) |
C11 | 0.114 (4) | 0.088 (4) | 0.108 (5) | 0.073 (3) | 0.023 (4) | 0.006 (3) |
C12 | 0.108 (6) | 0.085 (4) | 0.100 (4) | 0.067 (4) | 0.007 (4) | 0.008 (3) |
C13 | 0.101 (6) | 0.071 (5) | 0.076 (5) | 0.044 (4) | 0.008 (4) | 0.011 (4) |
C14 | 0.089 (6) | 0.076 (4) | 0.075 (4) | 0.053 (5) | 0.015 (4) | 0.003 (3) |
C15 | 0.100 (9) | 0.085 (6) | 0.111 (6) | 0.059 (6) | 0.019 (6) | 0.010 (5) |
Geometric parameters (Å, º) top
Mn1—O1 | 2.075 (3) | C4—H4 | 0.9300 |
Mn1—O1i | 2.075 (3) | C5—C6 | 1.3900 |
Mn1—O1ii | 2.075 (3) | C5—C8 | 1.453 (6) |
Mn1—O1w | 2.074 (9) | C6—C7 | 1.3900 |
Mn2—O2 | 2.158 (3) | C6—H6 | 0.9300 |
Mn2—O2i | 2.158 (3) | C7—H7 | 0.9300 |
Mn2—O2ii | 2.158 (3) | C8—C15 | 1.315 (8) |
Mn2—O2iii | 2.158 (3) | C8—H8 | 0.9300 |
Mn2—O2iv | 2.158 (3) | C9—C10 | 1.3900 |
Mn2—O2v | 2.158 (3) | C9—C14 | 1.3900 |
O1—C1 | 1.261 (6) | C9—C1vi | 1.502 (8) |
O2—C1 | 1.254 (5) | C10—C11 | 1.3900 |
O1w—H1W | 0.8200 | C10—H10 | 0.9300 |
O1w—H2W | 0.8200 | C11—C12 | 1.3900 |
C1—C2 | 1.482 (9) | C11—H11 | 0.9300 |
C1—C9vi | 1.502 (8) | C12—C13 | 1.3900 |
C2—C3 | 1.3900 | C12—C15 | 1.453 (6) |
C2—C7 | 1.3900 | C13—C14 | 1.3900 |
C3—C4 | 1.3900 | C13—H13 | 0.9300 |
C3—H3 | 0.9300 | C14—H14 | 0.9300 |
C4—C5 | 1.3900 | C15—H15 | 0.9300 |
O1w—Mn1—O1i | 96.64 (10) | C3—C4—C5 | 120.0 |
O1w—Mn1—O1 | 96.64 (10) | C3—C4—H4 | 120.0 |
O1i—Mn1—O1 | 118.68 (4) | C5—C4—H4 | 120.0 |
O1w—Mn1—O1ii | 96.64 (10) | C6—C5—C4 | 120.0 |
O1i—Mn1—O1ii | 118.68 (4) | C6—C5—C8 | 123.3 (5) |
O1—Mn1—O1ii | 118.68 (4) | C4—C5—C8 | 116.7 (5) |
O2—Mn2—O2iii | 180.00 (17) | C5—C6—C7 | 120.0 |
O2—Mn2—O2v | 92.85 (14) | C5—C6—H6 | 120.0 |
O2iii—Mn2—O2v | 87.15 (14) | C7—C6—H6 | 120.0 |
O2—Mn2—O2i | 87.15 (14) | C6—C7—C2 | 120.0 |
O2iii—Mn2—O2i | 92.85 (14) | C6—C7—H7 | 120.0 |
O2v—Mn2—O2i | 92.85 (14) | C2—C7—H7 | 120.0 |
O2—Mn2—O2iv | 92.85 (14) | C15—C8—C5 | 129.1 (7) |
O2iii—Mn2—O2iv | 87.15 (14) | C15—C8—H8 | 115.4 |
O2v—Mn2—O2iv | 87.15 (14) | C5—C8—H8 | 115.4 |
O2i—Mn2—O2iv | 180.0 | C10—C9—C14 | 120.0 |
O2—Mn2—O2ii | 87.15 (14) | C10—C9—C1vi | 120.8 (9) |
O2iii—Mn2—O2ii | 92.85 (14) | C14—C9—C1vi | 118.9 (9) |
O2v—Mn2—O2ii | 180.00 (17) | C11—C10—C9 | 120.0 |
O2i—Mn2—O2ii | 87.15 (14) | C11—C10—H10 | 120.0 |
O2iv—Mn2—O2ii | 92.85 (14) | C9—C10—H10 | 120.0 |
C1—O1—Mn1 | 108.7 (3) | C10—C11—C12 | 120.0 |
C1—O2—Mn2 | 133.7 (3) | C10—C11—H11 | 120.0 |
Mn1—O1w—H1W | 109.5 | C12—C11—H11 | 120.0 |
Mn1—O1w—H2W | 109.5 | C13—C12—C11 | 120.0 |
H1W—O1w—H2W | 109.5 | C13—C12—C15 | 122.4 (5) |
O2—C1—O1 | 122.2 (4) | C11—C12—C15 | 117.6 (5) |
O2—C1—C2 | 117.2 (6) | C14—C13—C12 | 120.0 |
O1—C1—C2 | 120.6 (6) | C14—C13—H13 | 120.0 |
O2—C1—C9vi | 121.8 (7) | C12—C13—H13 | 120.0 |
O1—C1—C9vi | 116.0 (6) | C13—C14—C9 | 120.0 |
C3—C2—C7 | 120.0 | C13—C14—H14 | 120.0 |
C3—C2—C1 | 117.7 (9) | C9—C14—H14 | 120.0 |
C7—C2—C1 | 122.1 (9) | C8—C15—C12 | 129.5 (8) |
C2—C3—C4 | 120.0 | C8—C15—H15 | 115.3 |
C2—C3—H3 | 120.0 | C12—C15—H15 | 115.3 |
C4—C3—H3 | 120.0 | ||
O1w—Mn1—O1—C1 | 157.2 (3) | C3—C4—C5—C6 | 0.0 |
O1i—Mn1—O1—C1 | −101.5 (3) | C3—C4—C5—C8 | −179.9 (3) |
O1ii—Mn1—O1—C1 | 55.9 (4) | C4—C5—C6—C7 | 0.0 |
O2iii—Mn2—O2—C1 | −123 (38) | C8—C5—C6—C7 | 179.8 (3) |
O2v—Mn2—O2—C1 | 66.0 (4) | C5—C6—C7—C2 | 0.0 |
O2i—Mn2—O2—C1 | −26.7 (5) | C3—C2—C7—C6 | 0.0 |
O2iv—Mn2—O2—C1 | 153.3 (5) | C1—C2—C7—C6 | −175.0 (9) |
O2ii—Mn2—O2—C1 | −114.0 (4) | C6—C5—C8—C15 | 20.6 (12) |
Mn2—O2—C1—O1 | 78.4 (6) | C4—C5—C8—C15 | −159.6 (11) |
Mn2—O2—C1—C2 | −102.4 (7) | C14—C9—C10—C11 | 0.0 |
Mn2—O2—C1—C9vi | −102.6 (7) | C1vi—C9—C10—C11 | 173.2 (9) |
Mn1—O1—C1—O2 | −4.5 (5) | C9—C10—C11—C12 | 0.0 |
Mn1—O1—C1—C2 | 176.4 (6) | C10—C11—C12—C13 | 0.0 |
Mn1—O1—C1—C9vi | 176.5 (6) | C10—C11—C12—C15 | −180.0 (3) |
O2—C1—C2—C3 | 154.0 (5) | C11—C12—C13—C14 | 0.0 |
O1—C1—C2—C3 | −26.9 (8) | C15—C12—C13—C14 | 180.0 (3) |
C9vi—C1—C2—C3 | −28 (12) | C12—C13—C14—C9 | 0.0 |
O2—C1—C2—C7 | −30.9 (9) | C10—C9—C14—C13 | 0.0 |
O1—C1—C2—C7 | 148.3 (6) | C1vi—C9—C14—C13 | −173.3 (9) |
C9vi—C1—C2—C7 | 147 (12) | C5—C8—C15—C12 | 170.6 (8) |
C7—C2—C3—C4 | 0.0 | C13—C12—C15—C8 | 6.1 (12) |
C1—C2—C3—C4 | 175.2 (9) | C11—C12—C15—C8 | −174.0 (11) |
C2—C3—C4—C5 | 0.0 |
Symmetry codes: (i) −y, x−y, z; (ii) −x+y, −x, z; (iii) −x, −y, −z; (iv) y, −x+y, −z; (v) x−y, x, −z; (vi) −x, −y+1, −z. |