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The title compound, (C2H7N4O)2[MnCl4(H2O)2], contains a molecular network of C2H7N4O+ cations and [Mn(H2O)2Cl4]2− trans-octahedral anions (Mn site symmetry 2/m). An extensive network of N—H...Cl, N—H...(Cl,Cl), N—H...O, O—H...O and O—H...Cl links results in a structure with a three-dimensional hydrogen-bonding network. The compound is isostructural with its copper- and cobalt-containing congeners.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301523X/cf6272sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680301523X/cf6272Isup2.hkl
Contains datablock I

CCDC reference: 221628

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Mn-O) = 0.001 Å
  • R factor = 0.031
  • wR factor = 0.078
  • Data-to-parameter ratio = 30.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: isostructural with Co complex; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and ATOMS (Shape Software, 1999); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
(C2H7N4O)2[Mn(H2O)2Cl4]F(000) = 446
Mr = 439.00Dx = 1.773 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 6.4106 (3) ÅCell parameters from 2931 reflections
b = 11.4036 (6) Åθ = 2.5–32.3°
c = 11.5775 (6) ŵ = 1.48 mm1
β = 103.640 (1)°T = 293 K
V = 822.49 (7) Å3Block, colourless
Z = 20.33 × 0.23 × 0.19 mm
Data collection top
Bruker SMART1000 CCD
diffractometer
2947 independent reflections
Radiation source: fine-focus sealed tube2122 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
ω scansθmax = 32.5°, θmin = 2.5°
Absorption correction: multi-scan
(SADABS; Bruker, 1999)
h = 99
Tmin = 0.644, Tmax = 0.768k = 1117
8334 measured reflectionsl = 1716
Refinement top
Refinement on F2Primary atom site location: from isostructural phase
Least-squares matrix: fullHydrogen site location: difmap (O-H) and geom (N-H)
R[F2 > 2σ(F2)] = 0.031H-atom parameters constrained
wR(F2) = 0.078 w = 1/[σ2(Fo2) + (0.0411P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.95(Δ/σ)max < 0.001
2947 reflectionsΔρmax = 0.40 e Å3
97 parametersΔρmin = 0.23 e Å3
0 restraints
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
xyzUiso*/Ueq
Mn10.00000.50000.00000.02798 (8)
Cl10.00427 (7)0.49621 (3)0.21671 (3)0.03772 (10)
Cl20.31918 (6)0.64019 (3)0.04754 (3)0.03472 (10)
O10.24682 (17)0.36239 (9)0.03072 (9)0.0312 (2)
H10.21700.29770.00930.037*
H20.35900.38090.00450.037*
O20.70236 (19)0.35420 (10)0.44553 (10)0.0438 (3)
N10.4764 (2)0.29980 (12)0.27397 (11)0.0419 (3)
H30.49650.22620.28870.050*
H40.39060.32230.20900.050*
N20.5298 (2)0.49315 (10)0.31684 (11)0.0334 (3)
H50.43040.50440.25350.040*
N30.5662 (2)0.69142 (12)0.32318 (12)0.0437 (3)
H60.62070.75520.35700.052*
H70.47330.69420.25620.052*
N40.7653 (2)0.58247 (13)0.47515 (11)0.0398 (3)
H80.82180.64520.51050.048*
H90.80160.51500.50680.048*
C10.5773 (2)0.37802 (13)0.35087 (13)0.0326 (3)
C20.6251 (2)0.58967 (13)0.37387 (13)0.0309 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.02756 (16)0.02426 (15)0.03128 (15)0.00143 (11)0.00524 (11)0.00018 (12)
Cl10.0396 (2)0.0422 (2)0.03286 (17)0.00100 (16)0.01143 (15)0.00047 (16)
Cl20.03229 (18)0.03009 (18)0.04105 (18)0.00478 (14)0.00721 (13)0.00079 (15)
O10.0314 (5)0.0233 (5)0.0402 (5)0.0002 (4)0.0112 (4)0.0022 (4)
O20.0500 (7)0.0292 (6)0.0433 (6)0.0001 (5)0.0068 (5)0.0078 (5)
N10.0525 (8)0.0259 (7)0.0408 (7)0.0029 (6)0.0020 (6)0.0020 (6)
N20.0338 (7)0.0263 (6)0.0355 (6)0.0021 (5)0.0009 (5)0.0031 (5)
N30.0603 (9)0.0256 (7)0.0397 (7)0.0024 (6)0.0006 (6)0.0003 (6)
N40.0423 (7)0.0303 (7)0.0408 (6)0.0008 (6)0.0022 (5)0.0020 (6)
C10.0326 (8)0.0272 (8)0.0374 (7)0.0004 (5)0.0068 (6)0.0041 (6)
C20.0312 (7)0.0286 (7)0.0336 (7)0.0003 (6)0.0088 (5)0.0011 (6)
Geometric parameters (Å, º) top
Mn1—O12.1971 (10)N1—H40.860
Mn1—O1i2.1971 (10)N2—C21.3529 (19)
Mn1—Cl1i2.5031 (4)N2—C11.3839 (18)
Mn1—Cl12.5031 (4)N2—H50.860
Mn1—Cl2i2.5523 (4)N3—C21.3147 (19)
Mn1—Cl22.5523 (4)N3—H60.860
O1—H10.787N3—H70.860
O1—H20.870N4—C21.3011 (18)
O2—C11.2260 (17)N4—H80.860
N1—C11.317 (2)N4—H90.860
N1—H30.860
O1—Mn1—O1i180.0C1—N1—H3120.0
O1—Mn1—Cl1i90.68 (3)C1—N1—H4120.0
O1i—Mn1—Cl1i89.32 (3)H3—N1—H4120.0
O1—Mn1—Cl189.32 (3)C2—N2—C1126.10 (13)
O1i—Mn1—Cl190.68 (3)C2—N2—H5117.0
Cl1i—Mn1—Cl1180.0C1—N2—H5117.0
O1—Mn1—Cl2i95.60 (3)C2—N3—H6120.0
O1i—Mn1—Cl2i84.40 (3)C2—N3—H7120.0
Cl1i—Mn1—Cl2i88.622 (12)H6—N3—H7120.0
Cl1—Mn1—Cl2i91.378 (12)C2—N4—H8120.0
O1—Mn1—Cl284.40 (3)C2—N4—H9120.0
O1i—Mn1—Cl295.60 (3)H8—N4—H9120.0
Cl1i—Mn1—Cl291.378 (12)O2—C1—N1124.57 (14)
Cl1—Mn1—Cl288.622 (12)O2—C1—N2121.22 (14)
Cl2i—Mn1—Cl2180.0N1—C1—N2114.21 (13)
Mn1—O1—H1120.4N4—C2—N3121.50 (15)
Mn1—O1—H2113.2N4—C2—N2121.67 (14)
H1—O1—H2106.1N3—C2—N2116.82 (14)
Symmetry code: (i) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O2ii0.791.882.6499 (15)167
O1—H2···Cl2iii0.872.293.1227 (11)159
N1—H3···Cl1iv0.862.623.4649 (14)166
N1—H4···O10.862.102.9415 (17)165
N2—H5···Cl10.862.673.2944 (14)131
N2—H5···Cl20.862.793.5170 (13)143
N3—H6···Cl2v0.862.573.3282 (15)148
N3—H6···Cl1vi0.862.933.5213 (14)127
N3—H7···Cl20.862.463.2635 (14)155
N4—H8···Cl2v0.862.493.2692 (15)152
N4—H9···O20.862.012.6441 (18)129
Symmetry codes: (ii) x1/2, y+1/2, z1/2; (iii) x+1, y+1, z; (iv) x+1/2, y1/2, z+1/2; (v) x+1/2, y+3/2, z+1/2; (vi) x+1/2, y+1/2, z+1/2.
 

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