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The title compound, [MnNi(CN)4(C5H5N)2], has a layered structure of a two-dimensional network complex Mn(py)2Ni(CN)4, in which linkages of cyanide between the equatorial coordination sites of octahedral MnII ions (site symmetry 2/m) and those of square planar NiII ions (site symmetry 2/m) form a square mesh network. Pyridine ligands (located on mirror planes) coordinate to the axial sites of the MnII ions from both sides of the network.
Supporting information
CCDC reference: 613750
Key indicators
- Single-crystal X-ray study
- T = 153 K
- Mean (C-C) = 0.019 Å
- R factor = 0.078
- wR factor = 0.239
- Data-to-parameter ratio = 24.1
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT341_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ... 19
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.586 0.789
Tmin(prime) and Tmax expected: 0.653 0.789
RR(prime) = 0.898
Please check that your absorption correction is appropriate.
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.88
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.74 Ratio
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 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
4 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) and PLATON (Spek, 2003).
poly[dipyridinemanganese(II)-µ-cyano-nickelate(II)-tri-µ-cyano]
top
Crystal data top
[MnNi(CN)4(C5H5N)2] | F(000) = 378 |
Mr = 375.93 | Dx = 1.563 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -C 2y | Cell parameters from 7694 reflections |
a = 15.684 (8) Å | θ = 3.1–32.6° |
b = 7.459 (3) Å | µ = 1.97 mm−1 |
c = 7.067 (4) Å | T = 153 K |
β = 104.93 (2)° | Block, pale yellow |
V = 798.8 (7) Å3 | 0.21 × 0.20 × 0.12 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID imaging-plate diffractometer | 1518 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 1246 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
Detector resolution: 10.0 pixels mm-1 | θmax = 32.6°, θmin = 3.0° |
ω scans | h = −23→23 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −10→10 |
Tmin = 0.586, Tmax = 0.789 | l = −10→10 |
8928 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)] = 0.078 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.239 | H-atom parameters constrained |
S = 1.22 | w = 1/[σ2(Fo2) + (0.0283P)2 + 28.8858P] where P = (Fo2 + 2Fc2)/3 |
1518 reflections | (Δ/σ)max = 0.001 |
63 parameters | Δρmax = 1.02 e Å−3 |
0 restraints | Δρmin = −0.84 e Å−3 |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All su's are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles. The arrangement of the pyridines is ruled by the MnNi(CN)4 two-dimensional
network structure, so that the packing of the pyridines is considerably loose.
For example, the thickness of two aromatic rings which are layered by π-π
stacking is considered to be 6.8 Å (3.4 Å + 3.4 Å). However, the
corresponding length in the title compound is 7.459 (3) Å, which is the
length of the b axis. This loose packing brings the large displacement
factors of the atoms of the pyridines and the poor bond length accuracy. |
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 | |
Mn1 | 0.0000 | 0.0000 | 0.0000 | 0.0149 (4) | |
Ni1 | 0.0000 | 0.5000 | 0.5000 | 0.0141 (3) | |
N1 | 0.0323 (4) | 0.2105 (7) | 0.2294 (8) | 0.0238 (10) | |
C1 | 0.0229 (4) | 0.3228 (8) | 0.3326 (8) | 0.0185 (10) | |
N11 | 0.1411 (5) | 0.0000 | −0.0275 (13) | 0.0239 (15) | |
C11 | 0.2060 (8) | 0.0000 | 0.1344 (16) | 0.042 (3) | |
C12 | 0.2948 (8) | 0.0000 | 0.132 (2) | 0.051 (3) | |
C13 | 0.3182 (8) | 0.0000 | −0.037 (2) | 0.046 (3) | |
C14 | 0.2516 (9) | 0.0000 | −0.207 (2) | 0.051 (4) | |
C15 | 0.1642 (8) | 0.0000 | −0.1967 (17) | 0.042 (3) | |
H11 | 0.1918 | 0.0000 | 0.2573 | 0.051* | |
H12 | 0.3393 | 0.0000 | 0.2517 | 0.061* | |
H13 | 0.3785 | 0.0000 | −0.0399 | 0.055* | |
H14 | 0.2651 | 0.0000 | −0.3304 | 0.061* | |
H15 | 0.1188 | 0.0000 | −0.3155 | 0.050* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0208 (8) | 0.0105 (7) | 0.0158 (7) | 0.000 | 0.0089 (6) | 0.000 |
Ni1 | 0.0215 (7) | 0.0101 (6) | 0.0121 (6) | 0.000 | 0.0070 (5) | 0.000 |
N1 | 0.031 (3) | 0.017 (2) | 0.026 (2) | −0.001 (2) | 0.013 (2) | −0.0044 (19) |
C1 | 0.022 (2) | 0.013 (2) | 0.022 (2) | −0.0016 (19) | 0.0078 (19) | −0.0017 (19) |
N11 | 0.026 (4) | 0.012 (3) | 0.037 (4) | 0.000 | 0.013 (3) | 0.000 |
C11 | 0.030 (5) | 0.075 (9) | 0.024 (4) | 0.000 | 0.011 (4) | 0.000 |
C12 | 0.022 (5) | 0.076 (10) | 0.053 (7) | 0.000 | 0.005 (5) | 0.000 |
C13 | 0.025 (5) | 0.041 (6) | 0.080 (9) | 0.000 | 0.029 (6) | 0.000 |
C14 | 0.039 (6) | 0.076 (10) | 0.050 (7) | 0.000 | 0.036 (6) | 0.000 |
C15 | 0.042 (6) | 0.066 (8) | 0.027 (5) | 0.000 | 0.026 (5) | 0.000 |
Geometric parameters (Å, º) top
Ni1—C1 | 1.869 (6) | C13—C14 | 1.374 (19) |
Mn1—N1 | 2.220 (5) | C14—C15 | 1.39 (2) |
Mn1—N11 | 2.271 (8) | C11—H11 | 0.9500 |
N1—C1 | 1.145 (8) | C12—H12 | 0.9500 |
N11—C11 | 1.321 (14) | C13—H13 | 0.9500 |
N11—C15 | 1.336 (15) | C14—H14 | 0.9500 |
C11—C12 | 1.397 (18) | C15—H15 | 0.9500 |
C12—C13 | 1.337 (19) | | |
| | | |
Ni1—C1—N1 | 176.2 (6) | C11—C12—C13 | 121.0 (12) |
C1—Ni1—C1i | 90.0 (3) | C12—C13—C14 | 117.3 (13) |
C1—Ni1—C1ii | 90.0 (3) | C13—C14—C15 | 119.4 (12) |
C1—Ni1—C1iii | 180.00 | N11—C15—C14 | 123.0 (11) |
N1—Mn1—N1iv | 90.0 (2) | N11—C11—H11 | 119.00 |
N1—Mn1—N1v | 90.0 (2) | C12—C11—H11 | 119.00 |
N1—Mn1—N1vi | 180.00 | C11—C12—H12 | 120.00 |
N1—Mn1—N11 | 91.1 (2) | C13—C12—H12 | 119.00 |
N1—Mn1—N11iv | 88.9 (2) | C12—C13—H13 | 122.00 |
N11—Mn1—N11iv | 180.00 | C14—C13—H13 | 121.00 |
Mn1—N1—C1 | 160.1 (6) | C13—C14—H14 | 120.00 |
Mn1—N11—C11 | 118.5 (7) | C15—C14—H14 | 120.00 |
Mn1—N11—C15 | 124.9 (8) | N11—C15—H15 | 118.00 |
C11—N11—C15 | 116.7 (10) | C14—C15—H15 | 119.00 |
N11—C11—C12 | 122.5 (11) | | |
| | | |
N1—Mn1—N11—C11 | 45.03 (14) | Mn1—N11—C11—C12 | 180.00 (2) |
N1—Mn1—N11—C15 | −134.97 (14) | Mn1—N11—C15—C14 | −180.00 (2) |
Symmetry codes: (i) −x, y, −z+1; (ii) x, −y+1, z; (iii) −x, −y+1, −z+1; (iv) −x, y, −z; (v) x, −y, z; (vi) −x, −y, −z. |
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