The crystal structure of the title compound, [Mn(NO
3)(C
10H
8N
2)(H
2O)
3]NO
3, contains a monomeric [Mn(NO
3)(bpy)(H
2O)
3]
+ cation (bpy is 2,2'-bipyridine) and a nitrate anion. The Mn
II ion is coordinated by one chelating bpy [Mn-N 2.241 (3) and 2.259 (3) Å], three water molecules [Mn-O 2.120 (3)-2.188 (3) Å] and a nitrate ligand [Mn-O 2.228 (2) Å] in a distorted octahedral geometry. There are O
H-O hydrogen-bonding interactions between the ligated water molecules and the ligated and unligated nitrate anions, resulting in double columns of stacked cations and anions.
Supporting information
CCDC reference: 184483
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL (Siemens, 1994); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL (Bruker, 1997).
Triaqua(2,2'-bipyridine-
κ2N,
N')(nitrato-
κO)manganese(II) nitrate
top
Crystal data top
[Mn(C10H8N2)(NO3)(H2O)3]NO3 | F(000) = 796 |
Mr = 389.19 | Dx = 1.661 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.5797 (5) Å | Cell parameters from 2683 reflections |
b = 9.5007 (4) Å | θ = 1.9–25.1° |
c = 14.8683 (6) Å | µ = 0.90 mm−1 |
β = 107.899 (1)° | T = 293 K |
V = 1556.57 (11) Å3 | Block, yellow |
Z = 4 | 0.42 × 0.34 × 0.24 mm |
Data collection top
Siemens SMART CCD area-detector diffractometer | 2708 independent reflections |
Radiation source: fine-focus sealed tube | 2032 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.021 |
ω scan | θmax = 25.1°, θmin = 1.9° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −8→13 |
Tmin = 0.615, Tmax = 0.805 | k = −6→11 |
5036 measured reflections | l = −17→17 |
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.135 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.93 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
2708 reflections | (Δ/σ)max < 0.001 |
241 parameters | Δρmax = 0.33 e Å−3 |
5 restraints | Δρmin = −0.32 e Å−3 |
Special details top
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 | |
Mn | 0.80984 (4) | 0.23694 (5) | 0.10385 (3) | 0.0429 (2) | |
N1 | 0.6118 (2) | 0.2602 (2) | 0.0256 (2) | 0.0457 (6) | |
N2 | 0.7091 (3) | 0.0821 (3) | 0.16762 (18) | 0.0480 (6) | |
N3 | 0.7852 (2) | 0.4354 (3) | 0.2657 (2) | 0.0522 (7) | |
N4 | 1.0614 (3) | 0.2572 (3) | 0.4320 (2) | 0.0561 (8) | |
C1 | 0.5695 (3) | 0.3469 (4) | −0.0475 (3) | 0.0596 (9) | |
H1A | 0.6249 | 0.3970 | −0.0688 | 0.072* | |
C2 | 0.4480 (3) | 0.3659 (4) | −0.0930 (3) | 0.0665 (10) | |
H2A | 0.4219 | 0.4273 | −0.1439 | 0.080* | |
C3 | 0.3672 (4) | 0.2931 (4) | −0.0619 (3) | 0.0710 (11) | |
H3A | 0.2844 | 0.3049 | −0.0910 | 0.085* | |
C4 | 0.4083 (3) | 0.2012 (4) | 0.0131 (3) | 0.0631 (9) | |
H4A | 0.3536 | 0.1500 | 0.0347 | 0.076* | |
C5 | 0.5327 (3) | 0.1862 (3) | 0.0559 (2) | 0.0455 (7) | |
C6 | 0.5863 (3) | 0.0874 (3) | 0.1355 (2) | 0.0474 (7) | |
C7 | 0.5164 (4) | 0.0042 (4) | 0.1746 (3) | 0.0648 (10) | |
H7A | 0.4322 | 0.0089 | 0.1522 | 0.078* | |
C8 | 0.5726 (4) | −0.0851 (4) | 0.2467 (3) | 0.0769 (12) | |
H8A | 0.5263 | −0.1416 | 0.2735 | 0.092* | |
C9 | 0.6967 (5) | −0.0922 (4) | 0.2800 (3) | 0.0744 (12) | |
H9A | 0.7359 | −0.1528 | 0.3290 | 0.089* | |
C10 | 0.7615 (4) | −0.0062 (4) | 0.2382 (2) | 0.0620 (10) | |
H10A | 0.8458 | −0.0099 | 0.2602 | 0.074* | |
O1 | 0.8308 (3) | 0.0874 (3) | 0.0011 (2) | 0.0808 (9) | |
H1B | 0.862 (4) | 0.010 (3) | 0.020 (3) | 0.074 (14)* | |
H1C | 0.819 (5) | 0.092 (6) | −0.0575 (15) | 0.12 (2)* | |
O2 | 0.9859 (3) | 0.1927 (4) | 0.1960 (2) | 0.0757 (8) | |
H2B | 1.003 (6) | 0.210 (6) | 0.258 (5) | 0.14 (2)* | |
H2C | 1.045 (3) | 0.144 (5) | 0.190 (4) | 0.12 (2)* | |
O3 | 0.8581 (3) | 0.4001 (3) | 0.0179 (2) | 0.0617 (7) | |
H3B | 0.890 (4) | 0.474 (3) | 0.046 (3) | 0.097 (16)* | |
H3C | 0.899 (5) | 0.365 (7) | −0.014 (4) | 0.16 (3)* | |
O4 | 0.8093 (2) | 0.4291 (2) | 0.18970 (17) | 0.0637 (7) | |
O5 | 0.7428 (4) | 0.3354 (3) | 0.2940 (2) | 0.1069 (12) | |
O6 | 0.8012 (3) | 0.5451 (3) | 0.3116 (2) | 0.0857 (9) | |
O7 | 1.1102 (4) | 0.2705 (4) | 0.5173 (3) | 0.1172 (14) | |
O8 | 1.0666 (4) | 0.3509 (4) | 0.3786 (2) | 0.1095 (12) | |
O9 | 1.0110 (3) | 0.1466 (3) | 0.4010 (2) | 0.0830 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn | 0.0379 (3) | 0.0473 (3) | 0.0421 (3) | −0.00061 (19) | 0.0104 (2) | −0.00210 (19) |
N1 | 0.0402 (14) | 0.0476 (14) | 0.0474 (15) | −0.0016 (11) | 0.0106 (12) | 0.0009 (11) |
N2 | 0.0585 (18) | 0.0443 (14) | 0.0419 (14) | −0.0019 (12) | 0.0165 (13) | −0.0045 (11) |
N3 | 0.0464 (16) | 0.0539 (17) | 0.0547 (17) | 0.0004 (13) | 0.0133 (13) | −0.0127 (14) |
N4 | 0.0430 (16) | 0.066 (2) | 0.060 (2) | 0.0004 (13) | 0.0169 (14) | −0.0034 (16) |
C1 | 0.048 (2) | 0.062 (2) | 0.065 (2) | 0.0017 (17) | 0.0108 (17) | 0.0124 (18) |
C2 | 0.051 (2) | 0.076 (2) | 0.066 (2) | 0.0092 (19) | 0.0075 (18) | 0.0068 (19) |
C3 | 0.042 (2) | 0.083 (3) | 0.079 (3) | 0.008 (2) | 0.0072 (19) | 0.003 (2) |
C4 | 0.046 (2) | 0.072 (2) | 0.074 (3) | −0.0072 (18) | 0.0209 (18) | −0.011 (2) |
C5 | 0.0447 (18) | 0.0436 (16) | 0.0493 (18) | −0.0040 (14) | 0.0160 (15) | −0.0141 (14) |
C6 | 0.054 (2) | 0.0436 (16) | 0.0494 (18) | −0.0066 (14) | 0.0229 (15) | −0.0113 (13) |
C7 | 0.073 (3) | 0.059 (2) | 0.073 (2) | −0.0084 (19) | 0.039 (2) | −0.0025 (19) |
C8 | 0.098 (4) | 0.067 (2) | 0.082 (3) | −0.009 (2) | 0.051 (3) | 0.007 (2) |
C9 | 0.116 (4) | 0.058 (2) | 0.051 (2) | 0.003 (2) | 0.027 (2) | 0.0087 (17) |
C10 | 0.077 (3) | 0.0529 (19) | 0.050 (2) | 0.0050 (18) | 0.0115 (19) | 0.0008 (16) |
O1 | 0.109 (3) | 0.0703 (19) | 0.0646 (19) | 0.0142 (17) | 0.0287 (18) | −0.0180 (16) |
O2 | 0.0518 (16) | 0.103 (2) | 0.0607 (18) | 0.0250 (16) | 0.0004 (13) | −0.0150 (16) |
O3 | 0.0674 (17) | 0.0561 (15) | 0.0717 (17) | −0.0122 (13) | 0.0361 (14) | −0.0068 (13) |
O4 | 0.0801 (18) | 0.0662 (15) | 0.0500 (14) | 0.0054 (12) | 0.0277 (13) | −0.0108 (11) |
O5 | 0.170 (4) | 0.0701 (19) | 0.111 (3) | −0.038 (2) | 0.087 (3) | −0.0273 (18) |
O6 | 0.110 (2) | 0.0755 (18) | 0.085 (2) | −0.0271 (16) | 0.0494 (18) | −0.0439 (16) |
O7 | 0.119 (3) | 0.165 (4) | 0.065 (2) | −0.035 (2) | 0.024 (2) | −0.021 (2) |
O8 | 0.117 (3) | 0.094 (2) | 0.102 (2) | −0.032 (2) | 0.011 (2) | 0.030 (2) |
O9 | 0.097 (2) | 0.0676 (17) | 0.0755 (19) | −0.0011 (16) | 0.0140 (16) | −0.0071 (15) |
Geometric parameters (Å, º) top
Mn—O1 | 2.153 (3) | C3—C4 | 1.381 (6) |
Mn—O2 | 2.120 (3) | C3—H3A | 0.9300 |
Mn—O3 | 2.188 (3) | C4—C5 | 1.391 (5) |
Mn—O4 | 2.228 (2) | C4—H4A | 0.9300 |
Mn—N1 | 2.241 (3) | C5—C6 | 1.489 (5) |
Mn—N2 | 2.259 (3) | C6—C7 | 1.381 (5) |
N1—C1 | 1.332 (4) | C7—C8 | 1.365 (6) |
N1—C5 | 1.337 (4) | C7—H7A | 0.9300 |
N2—C10 | 1.334 (4) | C8—C9 | 1.370 (6) |
N2—C6 | 1.354 (4) | C8—H8A | 0.9300 |
N3—O5 | 1.202 (4) | C9—C10 | 1.380 (5) |
N3—O6 | 1.228 (4) | C9—H9A | 0.9300 |
N3—O4 | 1.246 (3) | C10—H10A | 0.9300 |
N4—O8 | 1.206 (4) | O1—H1B | 0.827 (19) |
N4—O9 | 1.222 (4) | O1—H1C | 0.84 (2) |
N4—O7 | 1.227 (4) | O2—H2B | 0.90 (7) |
C1—C2 | 1.372 (5) | O2—H2C | 0.85 (2) |
C1—H1A | 0.9300 | O3—H3B | 0.84 (4) |
C2—C3 | 1.354 (5) | O3—H3C | 0.84 (6) |
C2—H2A | 0.9300 | | |
| | | |
O2—Mn—O1 | 91.82 (13) | C2—C3—H3A | 120.1 |
O2—Mn—O3 | 98.65 (13) | C4—C3—H3A | 120.1 |
O1—Mn—O3 | 87.04 (13) | C3—C4—C5 | 119.0 (4) |
O2—Mn—O4 | 87.93 (11) | C3—C4—H4A | 120.5 |
O1—Mn—O4 | 165.33 (12) | C5—C4—H4A | 120.5 |
O3—Mn—O4 | 78.50 (10) | N1—C5—C4 | 120.8 (3) |
O2—Mn—N1 | 169.30 (12) | N1—C5—C6 | 115.9 (3) |
O1—Mn—N1 | 90.99 (12) | C4—C5—C6 | 123.2 (3) |
O3—Mn—N1 | 91.81 (10) | N2—C6—C7 | 121.2 (3) |
O4—Mn—N1 | 91.95 (10) | N2—C6—C5 | 116.1 (3) |
O2—Mn—N2 | 96.76 (12) | C7—C6—C5 | 122.7 (3) |
O1—Mn—N2 | 93.05 (12) | C8—C7—C6 | 119.1 (4) |
O3—Mn—N2 | 164.58 (11) | C8—C7—H7A | 120.4 |
O4—Mn—N2 | 101.55 (9) | C6—C7—H7A | 120.4 |
N1—Mn—N2 | 72.77 (10) | C7—C8—C9 | 120.5 (4) |
C1—N1—C5 | 118.8 (3) | C7—C8—H8A | 119.7 |
C1—N1—Mn | 123.1 (2) | C9—C8—H8A | 119.7 |
C5—N1—Mn | 118.1 (2) | C8—C9—C10 | 117.6 (4) |
C10—N2—C6 | 118.4 (3) | C8—C9—H9A | 121.2 |
C10—N2—Mn | 124.8 (2) | C10—C9—H9A | 121.2 |
C6—N2—Mn | 116.7 (2) | N2—C10—C9 | 123.2 (4) |
O5—N3—O6 | 119.0 (3) | N2—C10—H10A | 118.4 |
O5—N3—O4 | 120.5 (3) | C9—C10—H10A | 118.4 |
O6—N3—O4 | 120.4 (3) | Mn—O1—H1B | 118 (3) |
O8—N4—O9 | 120.1 (3) | Mn—O1—H1C | 133 (4) |
O8—N4—O7 | 120.3 (4) | H1B—O1—H1C | 109 (5) |
O9—N4—O7 | 119.5 (3) | Mn—O2—H2B | 119 (4) |
N1—C1—C2 | 123.2 (3) | Mn—O2—H2C | 133 (4) |
N1—C1—H1A | 118.4 | H2B—O2—H2C | 106 (5) |
C2—C1—H1A | 118.4 | Mn—O3—H3B | 117 (3) |
C3—C2—C1 | 118.4 (4) | Mn—O3—H3C | 110 (5) |
C3—C2—H2A | 120.8 | H3B—O3—H3C | 112 (6) |
C1—C2—H2A | 120.8 | N3—O4—Mn | 126.9 (2) |
C2—C3—C4 | 119.7 (4) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1B···O8i | 0.83 (2) | 2.12 (2) | 2.890 (5) | 156 (4) |
O2—H2C···O6i | 0.85 (2) | 2.02 (2) | 2.868 (4) | 173 (5) |
O3—H3C···O9ii | 0.84 (6) | 2.07 (3) | 2.870 (4) | 159 (7) |
O3—H3B···O9iii | 0.84 (4) | 2.02 (2) | 2.848 (4) | 169 (5) |
Symmetry codes: (i) −x+2, y−1/2, −z+1/2; (ii) x, −y+1/2, z−1/2; (iii) −x+2, y+1/2, −z+1/2. |