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metal-organic compounds
The cystal structure of the title compound, [Mn(C10H8N2)(H2O)4]n[Mn(C9H6O5)2(H2O)2]n·2nH2O, is an unusual example of a compound displaying separated chain motifs for both the cationic and anionic portions. The cations are bridged into chains by the N-heterocycle, while the anions are bridged by pairs of dicarboxylate groups. In the cationic chain, the Mn atom and the N-heterocycle lie on centers of inversion. The cationic and anionic chains interact via a three-dimensional network of O—HO hydrogen bonds, which involve the uncoordinated water molecules.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805031910/cv6586sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805031910/cv6586Isup2.hkl |
CCDC reference: 289704
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.005 Å
- R factor = 0.052
- wR factor = 0.136
- Data-to-parameter ratio = 13.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C3 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.97 PLAT417_ALERT_2_C Short Inter D-H..H-D H3W2 .. H4W1 .. 2.12 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8 PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
checkCIF publication errors
Alert level A PUBL023_ALERT_1_A There is a mismatched ^ on line 154 the cationic {[Mn(C~10~H~8~N~2~)(H~2~O)~4~Mn]^2+}~n~ chain, the Mn atom and the If you require a ^ then it should be escaped with a \, i.e. \^ Otherwise there must be a matching closing ~, e.g. ^12^C
1 ALERT level A = Data missing that is essential or data in wrong format 0 ALERT level G = General alerts. Data that may be required is missing
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.
catena-Poly[tetraaquamanganese(II)-µ-4,4'-bipyridine]
catena-poly[diaquamanganate(II)-di-µ-4-carboxyphenoxyacetato]
dihydrate top
Crystal data top
[Mn(C10H8N2)(H2O)4][Mn(C9H6O5)2(H2O)2]·2H2O | Z = 1 |
Mr = 798.47 | F(000) = 412 |
Triclinic, P1 | Dx = 1.638 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.688 (2) Å | Cell parameters from 6308 reflections |
b = 10.163 (2) Å | θ = 3.1–27.5° |
c = 10.797 (2) Å | µ = 0.87 mm−1 |
α = 94.08 (3)° | T = 295 K |
β = 101.01 (3)° | Prism, colorless |
γ = 100.46 (3)° | 0.34 × 0.26 × 0.18 mm |
V = 809.4 (3) Å3 |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 3581 independent reflections |
Radiation source: fine-focus sealed tube | 2567 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
ω scans | h = −9→9 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −13→13 |
Tmin = 0.757, Tmax = 0.860 | l = 0→14 |
6804 measured reflections |
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)] = 0.052 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.136 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0602P)2 + 0.8256P] where P = (Fo2 + 2Fc2)/3 |
3581 reflections | (Δ/σ)max = 0.001 |
261 parameters | Δρmax = 0.49 e Å−3 |
8 restraints | Δρmin = −0.67 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.5000 | 0.5000 | 0.5000 | 0.0280 (2) | |
Mn2 | 0.0000 | 0.5000 | 1.0000 | 0.0285 (2) | |
O1 | −0.0672 (3) | 0.6088 (2) | 0.8310 (2) | 0.0350 (6) | |
O2 | 0.0333 (3) | 0.6016 (3) | 0.6519 (2) | 0.0410 (6) | |
O3 | 0.4536 (3) | 1.1873 (2) | 0.8933 (2) | 0.0406 (6) | |
O4 | 0.6383 (3) | 1.4624 (2) | 1.1312 (2) | 0.0368 (6) | |
O5 | 0.7252 (3) | 1.3919 (2) | 0.9574 (2) | 0.0341 (6) | |
O1w | 0.2471 (3) | 0.5801 (3) | 0.4818 (3) | 0.0351 (6) | |
O2w | 0.4249 (3) | 0.4573 (3) | 0.2964 (3) | 0.0419 (7) | |
O3w | −0.0676 (4) | 0.6567 (3) | 1.1214 (3) | 0.0386 (6) | |
O4w | 0.2645 (4) | 0.7645 (3) | 0.2788 (3) | 0.0482 (7) | |
N1 | 0.3337 (4) | 0.2953 (3) | 0.5123 (3) | 0.0335 (7) | |
C1 | 0.2211 (6) | 0.2843 (4) | 0.5917 (4) | 0.047 (1) | |
C2 | 0.0897 (6) | 0.1716 (4) | 0.5893 (4) | 0.046 (1) | |
C3 | 0.0704 (4) | 0.0615 (3) | 0.5025 (3) | 0.031 (1) | |
C4 | 0.1906 (5) | 0.0706 (4) | 0.4220 (4) | 0.048 (1) | |
C5 | 0.3166 (5) | 0.1880 (4) | 0.4301 (4) | 0.046 (1) | |
C6 | 0.0305 (4) | 0.6601 (3) | 0.7577 (3) | 0.029 (1) | |
C7 | 0.1435 (4) | 0.7992 (3) | 0.7976 (3) | 0.029 (1) | |
C8 | 0.1346 (5) | 0.8729 (3) | 0.9076 (3) | 0.034 (1) | |
C9 | 0.2351 (5) | 1.0034 (4) | 0.9445 (4) | 0.035 (1) | |
C10 | 0.3492 (4) | 1.0607 (3) | 0.8686 (3) | 0.033 (1) | |
C11 | 0.3616 (5) | 0.9874 (4) | 0.7586 (4) | 0.038 (1) | |
C12 | 0.2582 (5) | 0.8581 (4) | 0.7223 (4) | 0.036 (1) | |
C13 | 0.4641 (4) | 1.2628 (3) | 1.0114 (3) | 0.033 (1) | |
C14 | 0.6207 (4) | 1.3827 (3) | 1.0338 (3) | 0.028 (1) | |
H1w1 | 0.213 (6) | 0.599 (5) | 0.550 (3) | 0.06 (2)* | |
H1w2 | 0.163 (4) | 0.523 (3) | 0.433 (3) | 0.05 (1)* | |
H2w1 | 0.314 (2) | 0.445 (5) | 0.259 (4) | 0.07 (2)* | |
H2w2 | 0.493 (6) | 0.456 (5) | 0.243 (4) | 0.08 (2)* | |
H3w1 | −0.155 (5) | 0.612 (5) | 1.148 (5) | 0.09 (2)* | |
H3w2 | 0.021 (4) | 0.682 (5) | 1.184 (3) | 0.07 (2)* | |
H4w1 | 0.306 (8) | 0.742 (6) | 0.214 (4) | 0.10 (2)* | |
H4w2 | 0.284 (9) | 0.718 (6) | 0.340 (5) | 0.12 (3)* | |
H1 | 0.2314 | 0.3566 | 0.6523 | 0.056* | |
H2 | 0.0136 | 0.1699 | 0.6468 | 0.055* | |
H4 | 0.1867 | −0.0016 | 0.3630 | 0.057* | |
H5 | 0.3951 | 0.1922 | 0.3741 | 0.055* | |
H8 | 0.0592 | 0.8345 | 0.9588 | 0.041* | |
H9 | 0.2260 | 1.0513 | 1.0189 | 0.043* | |
H11 | 0.4395 | 1.0247 | 0.7086 | 0.045* | |
H12 | 0.2657 | 0.8106 | 0.6473 | 0.043* | |
H13a | 0.4814 | 1.2062 | 1.0795 | 0.040* | |
H13b | 0.3519 | 1.2939 | 1.0110 | 0.040* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0233 (3) | 0.0270 (4) | 0.0320 (4) | −0.0052 (3) | 0.0100 (3) | 0.0053 (3) |
Mn2 | 0.0234 (3) | 0.0297 (4) | 0.0313 (4) | −0.0020 (3) | 0.0100 (3) | 0.0037 (3) |
O1 | 0.028 (1) | 0.038 (1) | 0.036 (1) | −0.006 (1) | 0.010 (1) | 0.009 (1) |
O2 | 0.038 (1) | 0.045 (2) | 0.034 (2) | −0.010 (1) | 0.013 (1) | −0.002 (1) |
O3 | 0.044 (1) | 0.033 (1) | 0.041 (2) | −0.013 (1) | 0.016 (1) | 0.000 (1) |
O4 | 0.031 (1) | 0.039 (1) | 0.037 (1) | −0.006 (1) | 0.014 (1) | −0.002 (1) |
O5 | 0.026 (1) | 0.038 (1) | 0.036 (1) | −0.005 (1) | 0.013 (1) | 0.003 (1) |
O1w | 0.028 (1) | 0.035 (1) | 0.041 (2) | −0.004 (1) | 0.013 (1) | −0.002 (1) |
O2w | 0.027 (1) | 0.065 (2) | 0.030 (1) | −0.003 (1) | 0.011 (1) | 0.003 (1) |
O3w | 0.035 (1) | 0.041 (2) | 0.040 (2) | 0.004 (1) | 0.013 (1) | 0.000 (1) |
O4w | 0.045 (2) | 0.049 (2) | 0.050 (2) | 0.005 (1) | 0.014 (2) | 0.004 (2) |
N1 | 0.030 (1) | 0.032 (2) | 0.038 (2) | −0.003 (1) | 0.013 (1) | 0.007 (1) |
C1 | 0.056 (2) | 0.034 (2) | 0.048 (2) | −0.014 (2) | 0.029 (2) | −0.007 (2) |
C2 | 0.053 (2) | 0.032 (2) | 0.053 (3) | −0.012 (2) | 0.032 (2) | −0.005 (2) |
C3 | 0.029 (2) | 0.027 (2) | 0.034 (2) | −0.003 (1) | 0.009 (1) | 0.006 (1) |
C4 | 0.051 (2) | 0.030 (2) | 0.062 (3) | −0.011 (2) | 0.033 (2) | −0.007 (2) |
C5 | 0.041 (2) | 0.036 (2) | 0.062 (3) | −0.005 (2) | 0.034 (2) | −0.002 (2) |
C6 | 0.020 (1) | 0.034 (2) | 0.031 (2) | 0.002 (1) | 0.003 (1) | 0.008 (2) |
C7 | 0.024 (2) | 0.029 (2) | 0.031 (2) | 0.002 (1) | 0.004 (1) | 0.008 (1) |
C8 | 0.030 (2) | 0.033 (2) | 0.039 (2) | −0.001 (2) | 0.014 (2) | 0.007 (2) |
C9 | 0.032 (2) | 0.034 (2) | 0.041 (2) | −0.001 (2) | 0.014 (2) | 0.004 (2) |
C10 | 0.029 (2) | 0.026 (2) | 0.039 (2) | −0.004 (1) | 0.007 (2) | 0.005 (1) |
C11 | 0.038 (2) | 0.038 (2) | 0.037 (2) | −0.003 (2) | 0.015 (2) | 0.008 (2) |
C12 | 0.035 (2) | 0.037 (2) | 0.035 (2) | 0.000 (2) | 0.010 (2) | 0.005 (2) |
C13 | 0.029 (2) | 0.030 (2) | 0.040 (2) | −0.003 (1) | 0.013 (2) | 0.007 (2) |
C14 | 0.022 (2) | 0.029 (2) | 0.034 (2) | 0.003 (1) | 0.005 (1) | 0.009 (1) |
Geometric parameters (Å, º) top
Mn1—O1w | 2.221 (3) | C7—C8 | 1.378 (5) |
Mn1—O1wi | 2.221 (3) | C7—C12 | 1.396 (5) |
Mn1—O2w | 2.155 (3) | C8—C9 | 1.397 (5) |
Mn1—O2wi | 2.155 (3) | C9—C10 | 1.393 (5) |
Mn1—N1 | 2.262 (3) | C10—C11 | 1.384 (5) |
Mn1—N1i | 2.262 (3) | C11—C12 | 1.393 (5) |
Mn2—O1 | 2.226 (2) | C13—C14 | 1.519 (4) |
Mn2—O1ii | 2.226 (2) | O1w—H1w1 | 0.85 (3) |
Mn2—O5iii | 2.144 (2) | O1w—H1w2 | 0.85 (3) |
Mn2—O5iv | 2.144 (2) | O2w—H2w1 | 0.85 (5) |
Mn2—O3w | 2.188 (3) | O2w—H2w2 | 0.84 (5) |
Mn2—O3wii | 2.188 (3) | O3w—H3w1 | 0.84 (5) |
O1—C6 | 1.268 (4) | O3w—H3w2 | 0.84 (5) |
O2—C6 | 1.255 (4) | O4w—H4w1 | 0.85 (5) |
O3—C10 | 1.365 (4) | O4w—H4w2 | 0.85 (5) |
O3—C13 | 1.421 (4) | C1—H1 | 0.93 |
O4—C14 | 1.251 (4) | C2—H2 | 0.93 |
O5—C14 | 1.254 (4) | C4—H4 | 0.93 |
N1—C5 | 1.326 (5) | C5—H5 | 0.93 |
N1—C1 | 1.326 (5) | C8—H8 | 0.93 |
C1—C2 | 1.378 (5) | C9—H9 | 0.93 |
C2—C3 | 1.374 (5) | C11—H11 | 0.93 |
C3—C4 | 1.380 (5) | C12—H12 | 0.93 |
C3—C3v | 1.488 (6) | C13—H13a | 0.97 |
C4—C5 | 1.379 (5) | C13—H13b | 0.97 |
C6—C7 | 1.504 (5) | ||
O1w—Mn1—O1wi | 180 | C8—C7—C12 | 118.2 (3) |
O1w—Mn1—O2w | 85.0 (1) | C8—C7—C6 | 121.3 (3) |
O1w—Mn1—O2wi | 95.0 (1) | C12—C7—C6 | 120.5 (3) |
O1w—Mn1—N1 | 87.9 (1) | C7—C8—C9 | 122.1 (3) |
O1w—Mn1—N1i | 92.1 (1) | C10—C9—C8 | 119.1 (3) |
O1wi—Mn1—O2w | 95.0 (1) | O3—C10—C11 | 115.5 (3) |
O1wi—Mn1—O2wi | 85.0 (1) | O3—C10—C9 | 124.9 (3) |
O1wi—Mn1—N1 | 92.1 (1) | C11—C10—C9 | 119.5 (3) |
O1wi—Mn1—N1i | 87.9 (1) | C10—C11—C12 | 120.6 (3) |
O2w—Mn1—O2wi | 180 | C11—C12—C7 | 120.6 (4) |
O2w—Mn1—N1 | 87.8 (1) | O3—C13—C14 | 109.9 (3) |
O2w—Mn1—N1i | 92.2 (1) | O4—C14—O5 | 125.2 (3) |
O2wi—Mn1—N1 | 92.2 (1) | O4—C14—C13 | 116.4 (3) |
O2wi—Mn1—N1i | 87.8 (1) | O5—C14—C13 | 118.4 (3) |
N1—Mn1—N1i | 180 | Mn1—O1w—H1w1 | 117 (3) |
O1—Mn2—O1ii | 180 | Mn1—O1w—H1w2 | 108 (3) |
O1—Mn2—O5iii | 88.2 (1) | H1w1—O1w—H1w2 | 109 (4) |
O1—Mn2—O5iv | 91.79 (9) | Mn1—O2w—H2w1 | 120 (3) |
O1—Mn2—O3w | 90.7 (1) | Mn1—O2w—H2w2 | 129 (4) |
O1—Mn2—O3wii | 89.3 (1) | H2w1—O2w—H2w2 | 111 (5) |
O1ii—Mn2—O5iv | 88.2 (1) | Mn2—O3w—H3w1 | 101 (4) |
O1ii—Mn2—O5iii | 91.8 (1) | Mn2—O3w—H3w2 | 108 (3) |
O1ii—Mn2—O3w | 89.3 (1) | H3w1—O3w—H3w2 | 108 (5) |
O1ii—Mn2—O3wii | 90.7 (1) | H4w1—O4w—H4w2 | 115 (6) |
O5iii—Mn2—O5iv | 180 | N1—C1—H1 | 118.2 |
O5iii—Mn2—O3w | 91.4 (1) | C2—C1—H1 | 118.2 |
O5iii—Mn2—O3wii | 88.6 (1) | C3—C2—H2 | 119.8 |
O5iv—Mn2—O3w | 88.6 (1) | C1—C2—H2 | 119.8 |
O5iv—Mn2—O3wii | 91.4 (1) | C5—C4—H4 | 120.3 |
O3w—Mn2—O3wii | 180 | C3—C4—H4 | 120.3 |
C6—O1—Mn2 | 130.8 (2) | N1—C5—H5 | 117.7 |
C10—O3—C13 | 118.7 (3) | C4—C5—H5 | 117.7 |
C14—O5—Mn2vi | 125.1 (2) | C7—C8—H8 | 119.0 |
C5—N1—C1 | 115.8 (3) | C9—C8—H8 | 119.0 |
C5—N1—Mn1 | 124.1 (2) | C10—C9—H9 | 120.5 |
C1—N1—Mn1 | 119.1 (3) | C8—C9—H9 | 120.5 |
N1—C1—C2 | 123.6 (4) | C10—C11—H11 | 119.7 |
C3—C2—C1 | 120.4 (3) | C12—C11—H11 | 119.7 |
C2—C3—C4 | 116.3 (3) | C11—C12—H12 | 119.7 |
C2—C3—C3v | 121.6 (4) | C7—C12—H12 | 119.7 |
C4—C3—C3v | 122.0 (4) | O3—C13—H13a | 109.7 |
C5—C4—C3 | 119.3 (4) | C14—C13—H13a | 109.7 |
N1—C5—C4 | 124.5 (3) | O3—C13—H13b | 109.7 |
O2—C6—O1 | 122.9 (3) | C14—C13—H13b | 109.7 |
O2—C6—C7 | 118.7 (3) | H13a—C13—H13b | 108.2 |
O1—C6—C7 | 118.4 (3) | ||
O5iv—Mn2—O1—C6 | 28.9 (3) | Mn2—O1—C6—C7 | −83.3 (4) |
O5iii—Mn2—O1—C6 | −151.1 (3) | O2—C6—C7—C8 | 174.5 (3) |
O3wii—Mn2—O1—C6 | −62.4 (3) | O1—C6—C7—C8 | −3.5 (5) |
O3w—Mn2—O1—C6 | 117.6 (3) | O2—C6—C7—C12 | −4.2 (5) |
O2wi—Mn1—N1—C5 | −146.1 (3) | O1—C6—C7—C12 | 177.7 (3) |
O2w—Mn1—N1—C5 | 33.9 (3) | C12—C7—C8—C9 | 0.4 (5) |
O1wi—Mn1—N1—C5 | −61.0 (3) | C6—C7—C8—C9 | −178.4 (3) |
O1w—Mn1—N1—C5 | 119.0 (3) | C7—C8—C9—C10 | −0.5 (5) |
O2wi—Mn1—N1—C1 | 46.1 (3) | C13—O3—C10—C11 | −172.9 (3) |
O2w—Mn1—N1—C1 | −133.9 (3) | C13—O3—C10—C9 | 7.2 (5) |
O1wi—Mn1—N1—C1 | 131.2 (3) | C8—C9—C10—O3 | 179.6 (3) |
O1w—Mn1—N1—C1 | −48.8 (3) | C8—C9—C10—C11 | −0.4 (5) |
C5—N1—C1—C2 | −1.8 (7) | O3—C10—C11—C12 | −178.6 (3) |
Mn1—N1—C1—C2 | 167.0 (4) | C9—C10—C11—C12 | 1.3 (6) |
N1—C1—C2—C3 | 0.7 (7) | C10—C11—C12—C7 | −1.5 (6) |
C1—C2—C3—C4 | 1.2 (6) | C8—C7—C12—C11 | 0.6 (5) |
C1—C2—C3—C3v | −179.9 (5) | C6—C7—C12—C11 | 179.4 (3) |
C2—C3—C4—C5 | −2.0 (6) | C10—O3—C13—C14 | 165.6 (3) |
C3v—C3—C4—C5 | 179.2 (4) | Mn2vi—O5—C14—O4 | 21.5 (5) |
C1—N1—C5—C4 | 1.0 (6) | Mn2vi—O5—C14—C13 | −155.6 (2) |
Mn1—N1—C5—C4 | −167.2 (4) | O3—C13—C14—O4 | 175.8 (3) |
C3—C4—C5—N1 | 0.9 (7) | O3—C13—C14—O5 | −6.8 (4) |
Mn2—O1—C6—O2 | 98.7 (4) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+2; (iii) x−1, y−1, z; (iv) −x+1, −y+2, −z+2; (v) −x, −y, −z+1; (vi) x+1, y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O2 | 0.85 (3) | 1.93 (4) | 2.711 (4) | 153 (5) |
O1w—H1w2···O2vii | 0.85 (3) | 1.82 (4) | 2.670 (4) | 172 (4) |
O2w—H2w1···O1vii | 0.85 (5) | 1.92 (4) | 2.767 (4) | 172 (5) |
O2w—H2w2···O4viii | 0.85 (5) | 1.79 (5) | 2.641 (4) | 177 (6) |
O3w—H3w1···O4iii | 0.85 (5) | 1.96 (4) | 2.743 (4) | 152 (5) |
O3w—H3w2···O4wix | 0.85 (5) | 1.96 (4) | 2.770 (4) | 159 (5) |
O4w—H4w1···O5x | 0.85 (5) | 2.17 (5) | 2.929 (4) | 149 (6) |
O4w—H4w2···O1w | 0.85 (5) | 2.17 (5) | 2.991 (4) | 163 (7) |
Symmetry codes: (iii) x−1, y−1, z; (vii) −x, −y+1, −z+1; (viii) x, y−1, z−1; (ix) x, y, z+1; (x) −x+1, −y+2, −z+1. |
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