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The asymmetric unit of the title compound, [Mn(H
2O)
6]Cl
2·2C
10H
8N
2O
2·2H
2O, consists of one half of the [Mn(H
2O)
6]
2+ cation, with the Mn atom on a centre of inversion, a chloride anion, a 4,4′-bipyridine
N,
N′-dioxide solvate and a solvent water molecule. 4,4′-Bipyridine
N,
N′-dioxide molecules link [Mn(H
2O)
6]
2+ cations through O—H
O hydrogen bonds into a two-dimensional sheet. These sheets are further connected by solvent water molecules and Cl
− anions into a three-dimensional network
via O—H
Cl and O—H
O hydrogen bonds.
Supporting information
CCDC reference: 643103
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.001 Å
- R factor = 0.041
- wR factor = 0.120
- Data-to-parameter ratio = 14.9
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mn1 - O3 .. 17.30 su
| Author Response: Outer atoms moving about the metal centre, room temperature
measurement.
|
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Mn1 - O4 .. 10.49 su
| Author Response: Outer atoms moving about the metal centre, room temperature
measurement.
|
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.83
PLAT230_ALERT_2_C Hirshfeld Test Diff for O1 - N1 .. 5.96 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for N2 - C9 .. 6.10 su
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn1
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.26
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1
C10 H8 N2 O2
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.830
Tmax scaled 0.828 Tmin scaled 0.812
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
6 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
0 ALERT type 5 Informative message, check
Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Hexaaquamanganese(II) dichloride 4,4'-bipyridine N,
N'-dioxide disolvate
dihydrate
top
Crystal data top
[Mn(H2O)6]Cl2·2C10H8N2O2·2H2O | Z = 1 |
Mr = 646.34 | F(000) = 335 |
Triclinic, P1 | Dx = 1.529 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.8062 (2) Å | Cell parameters from 25 reflections |
b = 10.2999 (5) Å | θ = 8.7–15.7° |
c = 10.5095 (6) Å | µ = 0.73 mm−1 |
α = 83.965 (5)° | T = 298 K |
β = 73.407 (4)° | Block, yellow |
γ = 88.769 (4)° | 0.35 × 0.28 × 0.26 mm |
V = 702.13 (6) Å3 | |
Data collection top
Enraf–Nonius CAD-4 MACH3 diffractometer | 2684 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.008 |
Graphite monochromator | θmax = 27.0°, θmin = 2.0° |
φ and ω scans | h = −8→8 |
Absorption correction: multi-scan (DENZO-SMN; Otwinowski & Minor, 1997) | k = −13→0 |
Tmin = 0.978, Tmax = 0.997 | l = −13→13 |
3249 measured reflections | 3 standard reflections every 120 min |
3075 independent reflections | intensity decay: 1.1% |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.041 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.120 | w = 1/[σ2(Fo2) + (0.0578P)2 + 0.5777P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.032 |
3075 reflections | Δρmax = 0.58 e Å−3 |
206 parameters | Δρmin = −0.35 e Å−3 |
11 restraints | Extinction correction: SHELXTL (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0441 (15) |
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 | |
Mn1 | 0.0000 | 0.5000 | 0.5000 | 0.03734 (5) | |
Cl1 | 0.20550 (5) | 0.10671 (3) | 0.56334 (3) | 0.05730 (8) | |
O1 | 0.18127 (14) | 0.30795 (6) | 0.13229 (7) | 0.0540 (2) | |
O2 | 0.36764 (12) | −0.52983 (6) | −0.22457 (7) | 0.0460 (2) | |
O3 | 0.08514 (13) | 0.38457 (7) | 0.66624 (7) | 0.0536 (2) | |
O4 | 0.30097 (13) | 0.59057 (8) | 0.43039 (10) | 0.0651 (3) | |
O5 | 0.09776 (16) | 0.33810 (7) | 0.38612 (7) | 0.0661 (3) | |
O6 | 0.65215 (16) | 0.14828 (9) | 0.59151 (10) | 0.0757 (3) | |
N1 | 0.20546 (12) | 0.19269 (7) | 0.08677 (7) | 0.0353 (2) | |
N2 | 0.33961 (12) | −0.41496 (7) | −0.17525 (7) | 0.03492 (19) | |
C1 | 0.16868 (16) | 0.08173 (9) | 0.17018 (9) | 0.0407 (3) | |
H1A | 0.1254 | 0.0861 | 0.2619 | 0.049* | |
C2 | 0.19445 (14) | −0.03803 (9) | 0.12107 (9) | 0.0371 (2) | |
H2A | 0.1687 | −0.1136 | 0.1803 | 0.044* | |
C3 | 0.25819 (12) | −0.04823 (8) | −0.01532 (8) | 0.0293 (2) | |
C4 | 0.29464 (14) | 0.06909 (9) | −0.09798 (8) | 0.0359 (2) | |
H4A | 0.3379 | 0.0672 | −0.1901 | 0.043* | |
C5 | 0.26803 (15) | 0.18694 (8) | −0.04634 (8) | 0.0367 (2) | |
H5A | 0.2933 | 0.2638 | −0.1036 | 0.044* | |
C6 | 0.28563 (12) | −0.17630 (8) | −0.07069 (8) | 0.0303 (2) | |
C7 | 0.25538 (15) | −0.29378 (9) | 0.01118 (9) | 0.0392 (3) | |
H7A | 0.2161 | −0.2926 | 0.1034 | 0.047* | |
C8 | 0.28266 (16) | −0.41170 (9) | −0.04213 (9) | 0.0407 (3) | |
H8A | 0.2616 | −0.4892 | 0.0141 | 0.049* | |
C9 | 0.36924 (16) | −0.30406 (9) | −0.25739 (9) | 0.0422 (3) | |
H9A | 0.4076 | −0.3077 | −0.3493 | 0.051* | |
C10 | 0.34354 (16) | −0.18518 (9) | −0.20717 (9) | 0.0409 (3) | |
H10A | 0.3653 | −0.1092 | −0.2657 | 0.049* | |
H9 | 0.2071 (12) | 0.4205 (13) | 0.6701 (14) | 0.100 (2)* | |
H10 | 0.151 (2) | 0.3091 (9) | 0.6337 (14) | 0.100 (2)* | |
H13 | 0.130 (2) | 0.3271 (15) | 0.2965 (8) | 0.100 (2)* | |
H14 | 0.1429 (19) | 0.2614 (9) | 0.4236 (13) | 0.100 (2)* | |
H16 | 0.7395 (17) | 0.0816 (7) | 0.5506 (10) | 0.100 (2)* | |
H15 | 0.5387 (9) | 0.1372 (15) | 0.5617 (11) | 0.100 (2)* | |
H12 | 0.347 (3) | 0.5818 (10) | 0.3362 (7) | 0.135 (7)* | |
H11 | 0.300 (3) | 0.6855 (7) | 0.4384 (11) | 0.131 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.04815 (10) | 0.02898 (8) | 0.03251 (8) | 0.00230 (8) | −0.00592 (7) | −0.00850 (7) |
Cl1 | 0.08489 (17) | 0.03639 (12) | 0.05079 (13) | 0.00955 (12) | −0.02019 (12) | −0.00477 (10) |
O1 | 0.0995 (5) | 0.0249 (3) | 0.0352 (3) | 0.0026 (3) | −0.0130 (3) | −0.0108 (2) |
O2 | 0.0668 (4) | 0.0253 (3) | 0.0440 (3) | 0.0027 (3) | −0.0098 (3) | −0.0118 (2) |
O3 | 0.0761 (4) | 0.0402 (4) | 0.0488 (3) | 0.0030 (3) | −0.0231 (3) | −0.0096 (3) |
O4 | 0.0568 (4) | 0.0453 (4) | 0.0810 (5) | −0.0049 (3) | 0.0044 (4) | −0.0185 (4) |
O5 | 0.1249 (6) | 0.0406 (3) | 0.0322 (3) | 0.0281 (4) | −0.0194 (4) | −0.0144 (3) |
O6 | 0.0941 (6) | 0.0451 (4) | 0.0753 (6) | 0.0011 (4) | −0.0013 (5) | −0.0145 (4) |
N1 | 0.0504 (4) | 0.0259 (3) | 0.0301 (3) | 0.0020 (3) | −0.0111 (3) | −0.0071 (3) |
N2 | 0.0442 (4) | 0.0260 (3) | 0.0342 (3) | 0.0023 (3) | −0.0087 (3) | −0.0088 (3) |
C1 | 0.0597 (5) | 0.0317 (4) | 0.0275 (4) | −0.0012 (4) | −0.0070 (4) | −0.0037 (3) |
C2 | 0.0518 (5) | 0.0262 (4) | 0.0304 (4) | −0.0006 (4) | −0.0080 (3) | −0.0010 (3) |
C3 | 0.0327 (3) | 0.0255 (3) | 0.0299 (3) | 0.0008 (3) | −0.0087 (3) | −0.0046 (3) |
C4 | 0.0512 (4) | 0.0287 (4) | 0.0264 (3) | 0.0000 (3) | −0.0085 (3) | −0.0038 (3) |
C5 | 0.0552 (5) | 0.0263 (4) | 0.0274 (4) | −0.0003 (4) | −0.0096 (3) | −0.0023 (3) |
C6 | 0.0343 (3) | 0.0251 (3) | 0.0312 (3) | 0.0004 (3) | −0.0081 (3) | −0.0048 (3) |
C7 | 0.0580 (5) | 0.0296 (4) | 0.0266 (4) | 0.0003 (4) | −0.0066 (4) | −0.0029 (3) |
C8 | 0.0593 (5) | 0.0258 (4) | 0.0332 (4) | −0.0002 (4) | −0.0074 (4) | −0.0015 (3) |
C9 | 0.0664 (5) | 0.0301 (4) | 0.0279 (4) | 0.0013 (4) | −0.0092 (4) | −0.0043 (3) |
C10 | 0.0632 (5) | 0.0266 (4) | 0.0302 (4) | 0.0023 (4) | −0.0099 (4) | −0.0011 (3) |
Geometric parameters (Å, º) top
Mn1—O5 | 2.1384 (8) | N2—C8 | 1.3447 (12) |
Mn1—O5i | 2.1384 (8) | C1—C2 | 1.3754 (13) |
Mn1—O4i | 2.1644 (8) | C1—H1A | 0.9300 |
Mn1—O4 | 2.1644 (8) | C2—C3 | 1.3886 (12) |
Mn1—O3 | 2.2167 (8) | C2—H2A | 0.9300 |
Mn1—O3i | 2.2167 (8) | C3—C4 | 1.3948 (11) |
O1—N1 | 1.3158 (10) | C3—C6 | 1.4840 (12) |
O2—N2 | 1.3295 (10) | C4—C5 | 1.3688 (13) |
O3—H9 | 0.929 (10) | C4—H4A | 0.9300 |
O3—H10 | 0.936 (10) | C5—H5A | 0.9300 |
O4—H12 | 0.962 (7) | C6—C10 | 1.3872 (12) |
O4—H11 | 0.990 (7) | C6—C7 | 1.3919 (12) |
O5—H13 | 0.923 (8) | C7—C8 | 1.3775 (13) |
O5—H14 | 0.931 (10) | C7—H7A | 0.9300 |
O6—H16 | 0.953 (8) | C8—H8A | 0.9300 |
O6—H15 | 0.926 (8) | C9—C10 | 1.3720 (13) |
N1—C1 | 1.3467 (11) | C9—H9A | 0.9300 |
N1—C5 | 1.3483 (11) | C10—H10A | 0.9300 |
N2—C9 | 1.3393 (11) | | |
| | | |
O5—Mn1—O5i | 180.00 (3) | N1—C1—C2 | 120.67 (8) |
O5—Mn1—O4i | 87.46 (4) | N1—C1—H1A | 119.7 |
O5i—Mn1—O4i | 92.54 (4) | C2—C1—H1A | 119.7 |
O5—Mn1—O4 | 92.54 (4) | C1—C2—C3 | 121.20 (8) |
O5i—Mn1—O4 | 87.46 (4) | C1—C2—H2A | 119.4 |
O4i—Mn1—O4 | 180.00 (4) | C3—C2—H2A | 119.4 |
O5—Mn1—O3 | 87.38 (3) | C2—C3—C4 | 116.19 (8) |
O5i—Mn1—O3 | 92.62 (3) | C2—C3—C6 | 122.18 (7) |
O4i—Mn1—O3 | 89.08 (3) | C4—C3—C6 | 121.62 (7) |
O4—Mn1—O3 | 90.92 (3) | C5—C4—C3 | 121.36 (8) |
O5—Mn1—O3i | 92.62 (3) | C5—C4—H4A | 119.3 |
O5i—Mn1—O3i | 87.38 (3) | C3—C4—H4A | 119.3 |
O4i—Mn1—O3i | 90.92 (3) | N1—C5—C4 | 120.64 (8) |
O4—Mn1—O3i | 89.08 (3) | N1—C5—H5A | 119.7 |
O3—Mn1—O3i | 180.00 (2) | C4—C5—H5A | 119.7 |
Mn1—O3—H9 | 106.3 (9) | C10—C6—C7 | 116.42 (8) |
Mn1—O3—H10 | 107.8 (9) | C10—C6—C3 | 121.64 (7) |
H9—O3—H10 | 92.0 (12) | C7—C6—C3 | 121.94 (8) |
Mn1—O4—H12 | 105.4 (11) | C8—C7—C6 | 121.08 (8) |
Mn1—O4—H11 | 113.6 (11) | C8—C7—H7A | 119.5 |
H12—O4—H11 | 105.9 (8) | C6—C7—H7A | 119.5 |
Mn1—O5—H13 | 134.3 (10) | N2—C8—C7 | 120.16 (8) |
Mn1—O5—H14 | 121.1 (8) | N2—C8—H8A | 119.9 |
H13—O5—H14 | 103.6 (13) | C7—C8—H8A | 119.9 |
H16—O6—H15 | 100.9 (12) | N2—C9—C10 | 120.57 (8) |
O1—N1—C1 | 121.35 (7) | N2—C9—H9A | 119.7 |
O1—N1—C5 | 118.71 (7) | C10—C9—H9A | 119.7 |
C1—N1—C5 | 119.93 (8) | C9—C10—C6 | 121.20 (8) |
O2—N2—C9 | 120.27 (7) | C9—C10—H10A | 119.4 |
O2—N2—C8 | 119.16 (7) | C6—C10—H10A | 119.4 |
C9—N2—C8 | 120.56 (8) | | |
Symmetry code: (i) −x, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H12···O2ii | 0.96 (1) | 2.05 (2) | 2.7559 (11) | 128 (2) |
O5—H13···O1 | 0.92 (1) | 1.69 (1) | 2.6146 (10) | 178 (2) |
O3—H9···O2iii | 0.93 (1) | 1.88 (1) | 2.7087 (12) | 148 (1) |
O4—H11···O6iv | 0.99 (1) | 1.73 (1) | 2.6934 (12) | 164 (1) |
O3—H10···Cl1 | 0.94 (1) | 2.27 (1) | 3.1741 (8) | 162 (1) |
O5—H14···Cl1 | 0.93 (1) | 2.17 (1) | 3.0754 (9) | 164 (1) |
O6—H15···Cl1 | 0.93 (1) | 2.29 (1) | 3.1795 (12) | 161 (1) |
O6—H16···Cl1v | 0.95 (1) | 2.35 (1) | 3.2209 (10) | 151 (1) |
Symmetry codes: (ii) −x+1, −y, −z; (iii) x, y+1, z+1; (iv) −x+1, −y+1, −z+1; (v) −x+1, −y, −z+1. |
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