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A new linear bismuth(III) coordination polymer,
catena-poly[[chloridobismuth(III)]-μ
3-1,10-phenanthroline-2,9-dicarboxylato-κ
6O2:
O2,
N1,
N10,
O9:
O9], [Bi(C
14H
6N
2O
4)Cl]
n, has been obtained by an ionothermal method and characterized by elemental analysis, energy-dispersive X-ray spectroscopy, IR spectroscopy, thermal stability studies and single-crystal X-ray diffraction. The structure is constructed by Bi(C
14H
6N
2O
4)Cl fragments in which each Bi
III centre is seven-coordinated by one Cl atom, four O atoms and two N atoms. The coordination geometry of the Bi
III cation is distorted pentagonal–bipyramidal (BiO
4N
2Cl), with one bridging carboxylate O atom and one Cl atom located in the axial positions. The Bi(C
14H
6N
2O
4)Cl fragments are further extended into a one-dimensional linear polymeric structure
via subsequent but different centres of symmetry (bridging carboxylate O atoms). Neighbouring linear chains are assembled
via weak C—H
O and C—H
Cl hydrogen bonds, forming a three-dimensional supramolecular architecture. Intermolecular π–π stacking interactions are observed, with centroid-to-centroid distances of 3.678 (4) Å, which further stabilize the structure. In addition, the solid-state fluorescence properties of the title coordination polymer were investigated.
Supporting information
CCDC reference: 1411303
Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXT (Sheldrick, 2015); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).
catena-Poly[[chloridobismuth(III)]-µ
3-1,10-phenanthroline-2,9-dicarboxylato-
κ5O2:
N1,
N10,
O9:
O9]
top
Crystal data top
[Bi(C14H6N2O4)Cl] | Z = 2 |
Mr = 510.64 | F(000) = 472 |
Triclinic, P1 | Dx = 2.533 Mg m−3 |
a = 8.887 (6) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.118 (5) Å | Cell parameters from 2502 reflections |
c = 10.099 (4) Å | θ = 2.5–28.0° |
α = 111.034 (13)° | µ = 13.39 mm−1 |
β = 115.407 (9)° | T = 296 K |
γ = 92.872 (13)° | Block, colourless |
V = 669.4 (6) Å3 | 0.26 × 0.24 × 0.21 mm |
Data collection top
Bruker APEXII CCD area-detector diffractometer | 2586 independent reflections |
Radiation source: fine-focus sealed tube | 2387 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
φ and ω scans | θmax = 26.0°, θmin = 2.5° |
Absorption correction: multi-scan (SADABS; Bruker, 2008) | h = −10→6 |
Tmin = 0.369, Tmax = 0.746 | k = −9→11 |
3659 measured reflections | l = −12→12 |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.068 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.035P)2] where P = (Fo2 + 2Fc2)/3 |
2586 reflections | (Δ/σ)max = 0.001 |
199 parameters | Δρmax = 1.64 e Å−3 |
0 restraints | Δρmin = −1.74 e Å−3 |
Special details top
Experimental. Absorption correction:
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1239 before and 0.0333 after correction.
The Ratio of minimum to maximum transmission is 0.4948.
The λ/2 correction factor is Not present. |
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 | x | y | z | Uiso*/Ueq | |
Bi1 | 0.37660 (2) | 0.18971 (2) | 0.47993 (2) | 0.02700 (10) | |
C1 | 0.2339 (8) | −0.2145 (7) | 0.2427 (7) | 0.0295 (13) | |
C2 | 0.0755 (7) | −0.1553 (6) | 0.1718 (7) | 0.0266 (12) | |
C3 | −0.0805 (8) | −0.2614 (7) | 0.0398 (7) | 0.0331 (14) | |
H3 | −0.0902 | −0.3725 | −0.0042 | 0.040* | |
C4 | −0.2189 (7) | −0.1981 (7) | −0.0232 (7) | 0.0350 (14) | |
H4 | −0.3233 | −0.2668 | −0.1088 | 0.042* | |
C5 | −0.2012 (7) | −0.0290 (7) | 0.0425 (7) | 0.0300 (13) | |
C6 | −0.0394 (7) | 0.0683 (7) | 0.1772 (7) | 0.0256 (12) | |
C7 | −0.0135 (7) | 0.2434 (7) | 0.2483 (7) | 0.0265 (12) | |
C8 | −0.1445 (7) | 0.3167 (7) | 0.1845 (7) | 0.0289 (12) | |
C9 | −0.3073 (8) | 0.2168 (8) | 0.0481 (7) | 0.0360 (14) | |
H9 | −0.3952 | 0.2649 | 0.0064 | 0.043* | |
C10 | −0.3346 (8) | 0.0491 (8) | −0.0218 (8) | 0.0353 (14) | |
H10 | −0.4398 | −0.0134 | −0.1109 | 0.042* | |
C11 | −0.1062 (7) | 0.4881 (7) | 0.2561 (7) | 0.0315 (13) | |
H11 | −0.1901 | 0.5417 | 0.2188 | 0.038* | |
C12 | 0.0553 (8) | 0.5753 (7) | 0.3807 (8) | 0.0331 (13) | |
H12 | 0.0826 | 0.6879 | 0.4258 | 0.040* | |
C13 | 0.1807 (8) | 0.4902 (7) | 0.4401 (8) | 0.0304 (13) | |
C14 | 0.3633 (8) | 0.5742 (7) | 0.5774 (7) | 0.0323 (13) | |
Cl1 | 0.2559 (3) | 0.1457 (2) | 0.6498 (2) | 0.0523 (4) | |
N1 | 0.0938 (6) | 0.0057 (5) | 0.2395 (5) | 0.0250 (10) | |
N2 | 0.1448 (6) | 0.3289 (5) | 0.3759 (6) | 0.0274 (10) | |
O1 | 0.3694 (5) | −0.1018 (5) | 0.3640 (5) | 0.0352 (10) | |
O2 | 0.2340 (6) | −0.3587 (5) | 0.1865 (6) | 0.0471 (12) | |
O3 | 0.4525 (5) | 0.4849 (5) | 0.6327 (5) | 0.0409 (11) | |
O4 | 0.4130 (6) | 0.7228 (5) | 0.6221 (6) | 0.0420 (11) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Bi1 | 0.02535 (13) | 0.01731 (13) | 0.03377 (15) | 0.00634 (8) | 0.01205 (10) | 0.00850 (9) |
C1 | 0.036 (3) | 0.018 (3) | 0.030 (3) | 0.005 (2) | 0.016 (2) | 0.005 (2) |
C2 | 0.028 (3) | 0.021 (3) | 0.027 (3) | 0.005 (2) | 0.013 (2) | 0.007 (2) |
C3 | 0.037 (3) | 0.021 (3) | 0.030 (3) | 0.003 (2) | 0.014 (3) | 0.002 (2) |
C4 | 0.027 (3) | 0.031 (3) | 0.035 (3) | 0.000 (2) | 0.012 (3) | 0.006 (3) |
C5 | 0.023 (3) | 0.035 (3) | 0.027 (3) | 0.003 (2) | 0.012 (2) | 0.009 (2) |
C6 | 0.029 (3) | 0.022 (3) | 0.029 (3) | 0.009 (2) | 0.017 (2) | 0.009 (2) |
C7 | 0.027 (3) | 0.026 (3) | 0.029 (3) | 0.009 (2) | 0.016 (2) | 0.011 (2) |
C8 | 0.027 (3) | 0.033 (3) | 0.034 (3) | 0.012 (2) | 0.019 (2) | 0.015 (3) |
C9 | 0.027 (3) | 0.047 (4) | 0.036 (3) | 0.015 (3) | 0.016 (3) | 0.018 (3) |
C10 | 0.026 (3) | 0.041 (4) | 0.034 (3) | 0.005 (2) | 0.014 (2) | 0.011 (3) |
C11 | 0.031 (3) | 0.031 (3) | 0.043 (4) | 0.018 (2) | 0.024 (3) | 0.018 (3) |
C12 | 0.038 (3) | 0.026 (3) | 0.047 (4) | 0.017 (2) | 0.025 (3) | 0.020 (3) |
C13 | 0.033 (3) | 0.024 (3) | 0.041 (3) | 0.012 (2) | 0.023 (3) | 0.015 (3) |
C14 | 0.037 (3) | 0.024 (3) | 0.034 (3) | 0.009 (2) | 0.018 (3) | 0.009 (3) |
Cl1 | 0.0674 (12) | 0.0526 (11) | 0.0564 (11) | 0.0276 (9) | 0.0407 (10) | 0.0278 (9) |
N1 | 0.026 (2) | 0.018 (2) | 0.027 (2) | 0.0056 (18) | 0.0120 (19) | 0.0053 (19) |
N2 | 0.027 (2) | 0.021 (2) | 0.030 (3) | 0.0050 (18) | 0.014 (2) | 0.0058 (19) |
O1 | 0.028 (2) | 0.025 (2) | 0.035 (2) | 0.0092 (17) | 0.0059 (18) | 0.0056 (18) |
O2 | 0.048 (3) | 0.025 (2) | 0.055 (3) | 0.014 (2) | 0.019 (2) | 0.009 (2) |
O3 | 0.039 (2) | 0.022 (2) | 0.041 (3) | 0.0078 (18) | 0.006 (2) | 0.0071 (19) |
O4 | 0.047 (3) | 0.020 (2) | 0.048 (3) | 0.0037 (18) | 0.020 (2) | 0.008 (2) |
Geometric parameters (Å, º) top
Bi1—Cl1 | 2.508 (2) | C6—N1 | 1.345 (7) |
Bi1—N1 | 2.538 (5) | C7—C8 | 1.401 (8) |
Bi1—N2 | 2.514 (5) | C7—N2 | 1.364 (7) |
Bi1—O1i | 2.502 (4) | C8—C9 | 1.441 (8) |
Bi1—O1 | 2.474 (4) | C8—C11 | 1.415 (8) |
Bi1—O3 | 2.454 (4) | C9—H9 | 0.9300 |
Bi1—O4ii | 2.700 (5) | C9—C10 | 1.391 (9) |
C1—C2 | 1.508 (8) | C10—H10 | 0.9300 |
C1—O1 | 1.309 (7) | C11—H11 | 0.9300 |
C1—O2 | 1.231 (7) | C11—C12 | 1.376 (9) |
C2—C3 | 1.410 (8) | C12—H12 | 0.9300 |
C2—N1 | 1.345 (7) | C12—C13 | 1.432 (8) |
C3—H3 | 0.9300 | C13—C14 | 1.525 (8) |
C3—C4 | 1.384 (9) | C13—N2 | 1.333 (7) |
C4—H4 | 0.9300 | C14—O3 | 1.271 (7) |
C4—C5 | 1.412 (8) | C14—O4 | 1.250 (7) |
C5—C6 | 1.426 (8) | O1—Bi1i | 2.502 (4) |
C5—C10 | 1.446 (9) | O4—Bi1ii | 2.700 (5) |
C6—C7 | 1.454 (8) | | |
| | | |
Cl1—Bi1—N1 | 85.68 (12) | N1—C6—C5 | 122.8 (5) |
Cl1—Bi1—N2 | 89.79 (12) | N1—C6—C7 | 117.9 (5) |
Cl1—Bi1—O4ii | 163.92 (11) | C8—C7—C6 | 120.7 (5) |
N1—Bi1—O4ii | 110.21 (15) | N2—C7—C6 | 116.1 (5) |
N2—Bi1—N1 | 64.18 (15) | N2—C7—C8 | 123.1 (5) |
N2—Bi1—O4ii | 99.23 (15) | C7—C8—C9 | 119.3 (6) |
O1—Bi1—Cl1 | 90.38 (12) | C7—C8—C11 | 117.2 (5) |
O1i—Bi1—Cl1 | 86.41 (13) | C11—C8—C9 | 123.5 (6) |
O1i—Bi1—N1 | 126.35 (14) | C8—C9—H9 | 119.6 |
O1—Bi1—N1 | 63.81 (14) | C10—C9—C8 | 120.8 (6) |
O1—Bi1—N2 | 127.81 (14) | C10—C9—H9 | 119.6 |
O1i—Bi1—N2 | 168.36 (14) | C5—C10—H10 | 119.6 |
O1—Bi1—O1i | 63.29 (15) | C9—C10—C5 | 120.7 (6) |
O1i—Bi1—O4ii | 82.12 (16) | C9—C10—H10 | 119.6 |
O1—Bi1—O4ii | 94.45 (14) | C8—C11—H11 | 120.0 |
O3—Bi1—Cl1 | 92.05 (13) | C12—C11—C8 | 120.0 (5) |
O3—Bi1—N1 | 129.00 (15) | C12—C11—H11 | 120.0 |
O3—Bi1—N2 | 64.87 (14) | C11—C12—H12 | 120.5 |
O3—Bi1—O1 | 167.12 (14) | C11—C12—C13 | 119.1 (6) |
O3—Bi1—O1i | 104.24 (14) | C13—C12—H12 | 120.5 |
O3—Bi1—O4ii | 79.97 (15) | C12—C13—C14 | 123.6 (5) |
O1—C1—C2 | 115.2 (5) | N2—C13—C12 | 121.4 (6) |
O2—C1—C2 | 121.4 (5) | N2—C13—C14 | 115.0 (5) |
O2—C1—O1 | 123.4 (6) | O3—C14—C13 | 116.5 (5) |
C3—C2—C1 | 122.1 (5) | O4—C14—C13 | 117.4 (5) |
N1—C2—C1 | 115.7 (5) | O4—C14—O3 | 126.1 (6) |
N1—C2—C3 | 122.1 (5) | C2—N1—Bi1 | 120.5 (4) |
C2—C3—H3 | 120.5 | C2—N1—C6 | 119.1 (5) |
C4—C3—C2 | 119.1 (5) | C6—N1—Bi1 | 120.3 (4) |
C4—C3—H3 | 120.5 | C7—N2—Bi1 | 121.5 (4) |
C3—C4—H4 | 120.1 | C13—N2—Bi1 | 119.2 (4) |
C3—C4—C5 | 119.9 (5) | C13—N2—C7 | 119.2 (5) |
C5—C4—H4 | 120.1 | Bi1—O1—Bi1i | 116.71 (15) |
C4—C5—C6 | 117.0 (5) | C1—O1—Bi1 | 124.6 (4) |
C4—C5—C10 | 123.9 (5) | C1—O1—Bi1i | 117.8 (4) |
C6—C5—C10 | 119.1 (5) | C14—O3—Bi1 | 121.9 (4) |
C5—C6—C7 | 119.3 (5) | C14—O4—Bi1ii | 116.4 (4) |
| | | |
C1—C2—C3—C4 | −177.5 (6) | N1—Bi1—N2—C7 | 0.7 (4) |
C1—C2—N1—Bi1 | −2.8 (7) | N1—Bi1—N2—C13 | −175.1 (5) |
C1—C2—N1—C6 | 176.5 (5) | N1—Bi1—O1—Bi1i | −170.8 (3) |
C2—C1—O1—Bi1i | 169.9 (4) | N1—Bi1—O1—C1 | −1.7 (4) |
C2—C1—O1—Bi1 | 1.0 (7) | N1—Bi1—O3—C14 | −16.8 (6) |
C2—C3—C4—C5 | 1.4 (9) | N1—C2—C3—C4 | 0.6 (9) |
C3—C2—N1—Bi1 | 179.0 (4) | N1—C6—C7—C8 | 177.2 (5) |
C3—C2—N1—C6 | −1.7 (8) | N1—C6—C7—N2 | −1.3 (8) |
C3—C4—C5—C6 | −2.2 (9) | N2—Bi1—N1—C2 | 177.9 (5) |
C3—C4—C5—C10 | 175.8 (6) | N2—Bi1—N1—C6 | −1.4 (4) |
C4—C5—C6—C7 | 179.2 (5) | N2—Bi1—O1—Bi1i | −175.83 (15) |
C4—C5—C6—N1 | 1.1 (9) | N2—Bi1—O1—C1 | −6.7 (6) |
C4—C5—C10—C9 | −179.2 (6) | N2—Bi1—O3—C14 | −14.1 (4) |
C5—C6—C7—C8 | −1.0 (8) | N2—C7—C8—C9 | 179.2 (5) |
C5—C6—C7—N2 | −179.5 (5) | N2—C7—C8—C11 | 1.3 (8) |
C5—C6—N1—Bi1 | −179.9 (4) | N2—C13—C14—O3 | −10.7 (8) |
C5—C6—N1—C2 | 0.8 (8) | N2—C13—C14—O4 | 167.5 (5) |
C6—C5—C10—C9 | −1.3 (9) | O1—Bi1—N1—C2 | 2.3 (4) |
C6—C7—C8—C9 | 0.8 (8) | O1i—Bi1—N1—C2 | −7.9 (5) |
C6—C7—C8—C11 | −177.1 (5) | O1i—Bi1—N1—C6 | 172.8 (4) |
C6—C7—N2—Bi1 | 0.0 (7) | O1—Bi1—N1—C6 | −177.0 (5) |
C6—C7—N2—C13 | 175.8 (5) | O1i—Bi1—N2—C7 | −155.5 (6) |
C7—C6—N1—Bi1 | 2.0 (7) | O1—Bi1—N2—C7 | 5.7 (5) |
C7—C6—N1—C2 | −177.3 (5) | O1i—Bi1—N2—C13 | 28.7 (9) |
C7—C8—C9—C10 | −0.9 (9) | O1—Bi1—N2—C13 | −170.1 (4) |
C7—C8—C11—C12 | 1.2 (8) | O1i—Bi1—O1—Bi1i | 0.0 |
C8—C7—N2—Bi1 | −178.5 (4) | O1i—Bi1—O1—C1 | 169.1 (6) |
C8—C7—N2—C13 | −2.7 (8) | O1i—Bi1—O3—C14 | 170.3 (4) |
C8—C9—C10—C5 | 1.1 (9) | O1—Bi1—O3—C14 | 156.3 (6) |
C8—C11—C12—C13 | −2.3 (9) | O1—C1—C2—C3 | 179.5 (5) |
C9—C8—C11—C12 | −176.6 (6) | O1—C1—C2—N1 | 1.3 (8) |
C10—C5—C6—C7 | 1.2 (8) | O2—C1—C2—C3 | 0.9 (9) |
C10—C5—C6—N1 | −176.9 (5) | O2—C1—C2—N1 | −177.3 (6) |
C11—C8—C9—C10 | 176.9 (6) | O2—C1—O1—Bi1i | −11.5 (8) |
C11—C12—C13—C14 | 179.9 (6) | O2—C1—O1—Bi1 | 179.5 (5) |
C11—C12—C13—N2 | 0.9 (9) | O3—Bi1—N1—C2 | −179.4 (4) |
C12—C13—C14—O3 | 170.2 (6) | O3—Bi1—N1—C6 | 1.3 (5) |
C12—C13—C14—O4 | −11.6 (9) | O3—Bi1—N2—C7 | −177.0 (5) |
C12—C13—N2—Bi1 | 177.4 (4) | O3—Bi1—N2—C13 | 7.2 (4) |
C12—C13—N2—C7 | 1.5 (8) | O3—Bi1—O1—Bi1i | 15.1 (8) |
C13—C14—O3—Bi1 | 18.7 (7) | O3—Bi1—O1—C1 | −175.8 (6) |
C13—C14—O4—Bi1ii | −102.9 (5) | O3—C14—O4—Bi1ii | 75.1 (7) |
C14—C13—N2—Bi1 | −1.7 (7) | O4ii—Bi1—N1—C2 | 87.2 (4) |
C14—C13—N2—C7 | −177.5 (5) | O4ii—Bi1—N1—C6 | −92.1 (4) |
Cl1—Bi1—N1—C2 | −90.2 (4) | O4ii—Bi1—N2—C7 | 108.7 (4) |
Cl1—Bi1—N1—C6 | 90.5 (4) | O4ii—Bi1—N2—C13 | −67.0 (4) |
Cl1—Bi1—N2—C7 | −84.6 (4) | O4ii—Bi1—O1—Bi1i | 78.9 (2) |
Cl1—Bi1—N2—C13 | 99.6 (4) | O4ii—Bi1—O1—C1 | −112.1 (5) |
Cl1—Bi1—O1—Bi1i | −85.79 (19) | O4ii—Bi1—O3—C14 | 91.1 (5) |
Cl1—Bi1—O1—C1 | 83.3 (5) | O4—C14—O3—Bi1 | −159.4 (5) |
Cl1—Bi1—O3—C14 | −102.9 (5) | | |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H3···O2iii | 0.93 | 2.34 | 3.201 (7) | 155 |
C4—H4···O3iv | 0.93 | 2.60 | 3.492 (7) | 161 |
C11—H11···Cl1v | 0.93 | 2.89 | 3.616 (6) | 136 |
Symmetry codes: (iii) −x, −y−1, −z; (iv) x−1, y−1, z−1; (v) −x, −y+1, −z+1. |
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