trans-Diaquabis­(2-carboxyl­ato-4-nitro­pyridine 1-oxide-κ²O¹,O²)manganese(II) dihydrate

In the centrosymmetric title complex, [Mn(C₆H₃N₂O₅)₂(H₂O)₂]·2H₂O, each Mn^II ion has a six-coordinate octa­hedral environment within an O₆ donor set. The presence of O—H...O hydrogen-bonding inter­actions links adjacent mol­ecules into a two-dimensional array.

Key indicators

• Single-crystal X-ray study
• T = 297 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.053
• wR factor = 0.132
• Data-to-parameter ratio = 13.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT369_ALERT_2_C Long   C(sp2)-C(sp2) Bond  C1     -   C6     ...       1.53 Ang.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   2 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
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: XSCANS (Siemens, 1999); cell refinement: XSCANS; data reduction: SHELXTL (Sheldrick, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Diaqua-trans-bis(2-carboxylato-4-nitropyridine-1-oxido-κ²O,O') manganese(II) dihydrate

Crystal data

[Mn(C6H3N2O5)2(OH2)2]·2H2O	Z = 1
Mr = 493.21	F(000) = 251
Triclinic, P1	Dx = 1.822 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.566 (6) Å	Cell parameters from 4336 reflections
b = 7.766 (9) Å	θ = 3.0–27.5°
c = 8.582 (8) Å	µ = 0.82 mm^−1
α = 65.57 (4)°	T = 297 K
β = 78.95 (4)°	Prism, red
γ = 89.14 (4)°	0.15 × 0.15 × 0.10 mm
V = 449.4 (8) Å^3

Data collection

Bruker P4 diffractometer	1656 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.052
Graphite monochromator	θmax = 27.5°, θmin = 3.0°
ω scans	h = −9→9
Absorption correction: ψ scan (SADABS; Sheldrick, 1996)	k = −10→10
Tmin = 0.884, Tmax = 0.921	l = −10→11
4441 measured reflections	139 standard reflections every 0 min
2061 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.053	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.132	H atoms treated by a mixture of independent and constrained refinement
S = 0.97	w = 1/[σ^2(Fo^2) + (0.0861P)^2 + 0.01P] where P = (Fo^2 + 2Fc^2)/3
2061 reflections	(Δ/σ)max < 0.001
158 parameters	Δρmax = 0.98 e Å^−3
0 restraints	Δρmin = −0.56 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Mn	0.5000	0.5000	0.0000	0.0298 (2)
O1	0.5076 (2)	0.3152 (3)	−0.1264 (2)	0.0374 (4)
O2	0.2175 (2)	0.4529 (2)	0.0217 (3)	0.0368 (4)
O3	0.3965 (2)	0.0909 (3)	−0.1848 (2)	0.0381 (4)
O4	−0.0535 (3)	−0.3785 (3)	0.2770 (3)	0.0595 (6)
O5	−0.1879 (3)	−0.3229 (3)	0.4945 (3)	0.0578 (6)
O6	0.5000 (3)	0.2431 (3)	0.2393 (3)	0.0424 (5)
H6A	0.539 (5)	0.257 (5)	0.322 (5)	0.049 (9)*
H6B	0.550 (6)	0.156 (7)	0.226 (6)	0.067 (12)*
O7	0.6485 (3)	0.2749 (4)	0.4985 (3)	0.0506 (5)
H7A	0.580 (6)	0.228 (7)	0.596 (6)	0.073 (13)*
H7B	0.684 (7)	0.393 (10)	0.476 (8)	0.107 (19)*
N1	0.1516 (2)	0.2759 (3)	0.0989 (3)	0.0290 (4)
N2	−0.0855 (3)	−0.2765 (3)	0.3538 (3)	0.0369 (5)
C1	0.2259 (3)	0.1407 (3)	0.0483 (3)	0.0279 (5)
C2	0.1473 (3)	−0.0421 (3)	0.1329 (3)	0.0300 (5)
H2A	0.1940	−0.1360	0.0995	0.036*
C3	−0.0003 (3)	−0.0841 (3)	0.2667 (3)	0.0302 (5)
C4	−0.0742 (3)	0.0534 (4)	0.3166 (3)	0.0329 (5)
H4A	−0.1742	0.0238	0.4076	0.039*
C5	0.0032 (3)	0.2334 (4)	0.2290 (3)	0.0335 (5)
H5A	−0.0463	0.3288	0.2586	0.040*
C6	0.3906 (3)	0.1892 (3)	−0.1007 (3)	0.0294 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn	0.0326 (3)	0.0197 (3)	0.0363 (3)	−0.00106 (17)	−0.00615 (18)	−0.0112 (2)
O1	0.0376 (9)	0.0325 (10)	0.0418 (10)	−0.0048 (7)	0.0006 (7)	−0.0189 (8)
O2	0.0361 (9)	0.0186 (8)	0.0514 (11)	0.0014 (6)	−0.0064 (7)	−0.0113 (8)
O3	0.0449 (10)	0.0346 (10)	0.0373 (10)	−0.0011 (7)	−0.0015 (7)	−0.0203 (8)
O4	0.0761 (15)	0.0278 (11)	0.0701 (16)	−0.0053 (9)	0.0023 (11)	−0.0231 (11)
O5	0.0651 (14)	0.0399 (13)	0.0472 (12)	−0.0118 (9)	0.0074 (9)	−0.0051 (10)
O6	0.0559 (11)	0.0290 (11)	0.0411 (11)	0.0051 (8)	−0.0134 (8)	−0.0121 (9)
O7	0.0602 (13)	0.0464 (14)	0.0385 (11)	−0.0057 (9)	0.0030 (9)	−0.0163 (10)
N1	0.0300 (9)	0.0207 (10)	0.0357 (11)	0.0028 (6)	−0.0067 (7)	−0.0111 (8)
N2	0.0415 (11)	0.0222 (11)	0.0397 (12)	−0.0007 (8)	−0.0080 (8)	−0.0058 (9)
C1	0.0310 (11)	0.0232 (12)	0.0312 (11)	0.0042 (8)	−0.0079 (8)	−0.0123 (9)
C2	0.0335 (11)	0.0220 (11)	0.0351 (12)	0.0031 (8)	−0.0071 (8)	−0.0124 (10)
C3	0.0334 (12)	0.0219 (12)	0.0324 (12)	0.0013 (8)	−0.0091 (8)	−0.0074 (10)
C4	0.0333 (12)	0.0310 (13)	0.0335 (12)	0.0025 (8)	−0.0032 (8)	−0.0142 (11)
C5	0.0354 (12)	0.0279 (13)	0.0405 (13)	0.0057 (8)	−0.0052 (9)	−0.0185 (11)
C6	0.0332 (11)	0.0230 (12)	0.0300 (11)	0.0038 (8)	−0.0066 (8)	−0.0089 (9)

Geometric parameters (Å, º)

Mn—O1	2.121 (3)	O7—H7A	0.83 (5)
Mn—O1^i	2.121 (3)	O7—H7B	0.89 (7)
Mn—O2^i	2.133 (2)	N1—C5	1.357 (3)
Mn—O2	2.133 (2)	N1—C1	1.369 (3)
Mn—O6^i	2.193 (3)	N2—C3	1.458 (3)
Mn—O6	2.193 (3)	C1—C2	1.380 (4)
O1—C6	1.250 (3)	C1—C6	1.528 (3)
O2—N1	1.311 (3)	C2—C3	1.372 (3)
O3—C6	1.244 (3)	C2—H2A	0.9300
O4—N2	1.219 (3)	C3—C4	1.380 (4)
O5—N2	1.216 (3)	C4—C5	1.360 (4)
O6—H6A	0.87 (4)	C4—H4A	0.9300
O6—H6B	0.81 (5)	C5—H5A	0.9300
O1—Mn—O2	80.51 (8)	C5—N1—C1	121.4 (2)
O1—Mn—O6	85.91 (13)	O5—N2—O4	124.2 (2)
O1—Mn—O2^i	99.49 (8)	O5—N2—C3	118.4 (2)
O1—Mn—O6^i	94.09 (13)	O4—N2—C3	117.3 (2)
O2—Mn—O6	91.59 (9)	N1—C1—C2	118.7 (2)
O2—Mn—O6^i	88.41 (9)	N1—C1—C6	121.4 (2)
O2^i—Mn—O6	88.41 (9)	C2—C1—C6	119.9 (2)
O2^i—Mn—O6^i	91.59 (9)	C3—C2—C1	119.4 (2)
O1^i—Mn—O6^i	85.91 (13)	C3—C2—H2A	120.3
O1^i—Mn—O6	94.09 (13)	C1—C2—H2A	120.3
O1^i—Mn—O2	99.49 (8)	C2—C3—C4	121.4 (2)
O1^i—Mn—O2^i	80.51 (8)	C2—C3—N2	119.4 (2)
O1—Mn—O1^i	180	C4—C3—N2	119.1 (2)
O2^i—Mn—O2	180	C5—C4—C3	118.2 (2)
O6^i—Mn—O6	180	C5—C4—H4A	120.9
C6—O1—Mn	127.87 (16)	C3—C4—H4A	120.9
N1—O2—Mn	116.41 (13)	N1—C5—C4	120.9 (2)
Mn—O6—H6A	117 (3)	N1—C5—H5A	119.5
Mn—O6—H6B	116 (3)	C4—C5—H5A	119.5
H6A—O6—H6B	107 (4)	O3—C6—O1	125.6 (2)
H7A—O7—H7B	109 (5)	O3—C6—C1	114.4 (2)
O2—N1—C5	116.9 (2)	O1—C6—C1	120.0 (2)
O2—N1—C1	121.7 (2)

Symmetry code: (i) −x+1, −y+1, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6A···O7	0.87 (4)	1.91 (4)	2.774 (4)	174 (3)
O6—H6B···O3^ii	0.81 (5)	2.11 (5)	2.892 (4)	163 (4)
O7—H7A···O3^iii	0.83 (5)	2.00 (5)	2.819 (4)	171 (4)

Symmetry codes: (ii) −x+1, −y, −z; (iii) x, y, z+1.