μ-Oxalato-bis­[chloro­tripyridine­manganese(II)] pyridine disolvate

The Mn complex of the title compound, [Mn₂(C₂O₄)Cl₂(C₅H₅N)₆]·2C₅H₅N, is located on a crystallographic centre of inversion. The pyridine solvent mol­ecules are located on general positions. Each Mn centre is octa­hedrally coordinated by three pyridine ligands, one Cl atom and a chelating oxalate dianion which bridges the two Mn centres.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.002 Å
• R factor = 0.027
• wR factor = 0.079
• Data-to-parameter ratio = 18.7

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT369_ALERT_2_B Long   C(sp2)-C(sp2) Bond  C1     -   C1_a   ...       1.57 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Mn1    -   Cl1     ..       8.41 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Mn1    -   O1      ..       6.45 su

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

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 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: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

µ-Oxalato-bis[chlorotripyridinemanganese(II)] pyridine disolvate

Crystal data

[Mn2(C2O4)Cl2(C5H5N)6]·2C5H5N	Z = 1
Mr = 901.60	F(000) = 464
Triclinic, P1	Dx = 1.414 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.7867 (8) Å	Cell parameters from 15958 reflections
b = 10.1883 (9) Å	θ = 2.6–27.2°
c = 10.9221 (9) Å	µ = 0.77 mm^−1
α = 79.096 (7)°	T = 173 K
β = 82.110 (7)°	Plate, colourless
γ = 89.374 (7)°	0.42 × 0.14 × 0.12 mm
V = 1059.13 (15) Å^3

Data collection

Stoe IPDS-II two-circle diffractometer	4899 independent reflections
Radiation source: fine-focus sealed tube	4456 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
ω scans	θmax = 27.7°, θmin = 2.6°
Absorption correction: multi-scan (MULABS; Blessing, 1995; Spek, 2003)	h = −12→12
Tmin = 0.737, Tmax = 0.913	k = −13→13
15958 measured reflections	l = −14→13

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)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.079	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0473P)^2 + 0.1483P] where P = (Fo^2 + 2Fc^2)/3
4899 reflections	(Δ/σ)max < 0.001
262 parameters	Δρmax = 0.31 e Å^−3
0 restraints	Δρmin = −0.45 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
Mn1	0.364821 (18)	0.179941 (16)	0.323015 (16)	0.02776 (7)
Cl1	0.24336 (4)	0.16727 (4)	0.14458 (3)	0.04645 (10)
C1	0.52707 (11)	0.06041 (10)	0.52552 (10)	0.0245 (2)
O1	0.48980 (9)	0.17474 (8)	0.47746 (8)	0.02919 (17)
O2	0.60313 (8)	0.03402 (8)	0.60989 (8)	0.02940 (17)
N11	0.57929 (11)	0.17541 (10)	0.20202 (10)	0.0331 (2)
C12	0.60470 (16)	0.08572 (13)	0.12670 (13)	0.0410 (3)
H12	0.5299	0.0337	0.1138	0.049*
C13	0.73584 (19)	0.06550 (16)	0.06664 (16)	0.0525 (4)
H13	0.7502	0.0005	0.0145	0.063*
C14	0.84452 (17)	0.14139 (18)	0.08412 (16)	0.0536 (4)
H14	0.9351	0.1296	0.0441	0.064*
C15	0.81974 (16)	0.23508 (16)	0.16091 (15)	0.0464 (3)
H15	0.8928	0.2890	0.1743	0.056*
C16	0.68655 (14)	0.24863 (13)	0.21767 (13)	0.0374 (3)
H16	0.6700	0.3130	0.2704	0.045*
N21	0.16833 (11)	0.17624 (10)	0.46699 (11)	0.0353 (2)
C22	0.17132 (15)	0.15621 (14)	0.59143 (14)	0.0418 (3)
H22	0.2583	0.1556	0.6210	0.050*
C23	0.05323 (17)	0.13638 (16)	0.67886 (17)	0.0506 (4)
H23	0.0596	0.1214	0.7664	0.061*
C24	−0.07457 (16)	0.13864 (14)	0.63689 (19)	0.0526 (4)
H24	−0.1571	0.1246	0.6950	0.063*
C25	−0.07902 (15)	0.16164 (15)	0.50939 (19)	0.0508 (4)
H25	−0.1649	0.1657	0.4776	0.061*
C26	0.04310 (14)	0.17872 (13)	0.42839 (16)	0.0426 (3)
H26	0.0388	0.1930	0.3405	0.051*
N31	0.38207 (10)	0.40698 (10)	0.28494 (9)	0.0286 (2)
C32	0.38456 (12)	0.47469 (12)	0.37883 (12)	0.0329 (2)
H32	0.3819	0.4256	0.4623	0.039*
C33	0.39086 (13)	0.61344 (13)	0.35921 (14)	0.0393 (3)
H33	0.3919	0.6580	0.4280	0.047*
C34	0.39562 (14)	0.68532 (13)	0.23833 (15)	0.0415 (3)
H34	0.4000	0.7802	0.2225	0.050*
C35	0.39384 (14)	0.61687 (13)	0.14031 (14)	0.0398 (3)
H35	0.3973	0.6640	0.0561	0.048*
C36	0.38691 (13)	0.47825 (12)	0.16752 (12)	0.0332 (2)
H36	0.3855	0.4316	0.1001	0.040*
N41	0.76913 (13)	0.54819 (14)	0.31933 (13)	0.0468 (3)
C42	0.88782 (16)	0.50591 (15)	0.35806 (14)	0.0433 (3)
H42	0.8867	0.4677	0.4446	0.052*
C43	1.01255 (15)	0.51405 (15)	0.28050 (15)	0.0450 (3)
H43	1.0944	0.4817	0.3129	0.054*
C44	1.01556 (15)	0.57024 (18)	0.15492 (15)	0.0495 (4)
H44	1.0996	0.5773	0.0989	0.059*
C45	0.89427 (16)	0.61600 (18)	0.11217 (15)	0.0504 (4)
H45	0.8930	0.6555	0.0263	0.060*
C46	0.77482 (15)	0.60311 (17)	0.19694 (16)	0.0487 (3)
H46	0.6917	0.6350	0.1669	0.058*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.03240 (11)	0.02339 (10)	0.02918 (10)	0.00175 (7)	−0.01048 (7)	−0.00486 (7)
Cl1	0.0581 (2)	0.04415 (18)	0.04476 (19)	0.00357 (15)	−0.02752 (16)	−0.01319 (14)
C1	0.0244 (5)	0.0236 (5)	0.0260 (5)	−0.0012 (4)	−0.0030 (4)	−0.0059 (4)
O1	0.0367 (4)	0.0218 (4)	0.0312 (4)	0.0013 (3)	−0.0109 (3)	−0.0059 (3)
O2	0.0334 (4)	0.0244 (4)	0.0328 (4)	−0.0001 (3)	−0.0125 (3)	−0.0059 (3)
N11	0.0397 (5)	0.0301 (5)	0.0301 (5)	−0.0004 (4)	−0.0054 (4)	−0.0069 (4)
C12	0.0533 (8)	0.0334 (6)	0.0379 (7)	−0.0009 (5)	−0.0053 (6)	−0.0111 (5)
C13	0.0674 (10)	0.0443 (8)	0.0461 (8)	0.0084 (7)	0.0031 (7)	−0.0180 (6)
C14	0.0487 (8)	0.0551 (9)	0.0513 (9)	0.0085 (7)	0.0078 (7)	−0.0068 (7)
C15	0.0414 (7)	0.0521 (8)	0.0443 (8)	−0.0054 (6)	−0.0038 (6)	−0.0068 (6)
C16	0.0416 (7)	0.0373 (6)	0.0345 (6)	−0.0034 (5)	−0.0058 (5)	−0.0088 (5)
N21	0.0339 (5)	0.0266 (5)	0.0450 (6)	0.0011 (4)	−0.0057 (5)	−0.0053 (4)
C22	0.0398 (7)	0.0403 (7)	0.0447 (7)	0.0028 (5)	−0.0031 (6)	−0.0089 (6)
C23	0.0530 (8)	0.0427 (8)	0.0509 (9)	0.0029 (6)	0.0067 (7)	−0.0061 (6)
C24	0.0402 (7)	0.0328 (7)	0.0778 (11)	0.0002 (5)	0.0123 (7)	−0.0072 (7)
C25	0.0328 (6)	0.0351 (7)	0.0826 (12)	0.0020 (5)	−0.0054 (7)	−0.0084 (7)
C26	0.0362 (6)	0.0319 (6)	0.0596 (9)	0.0029 (5)	−0.0115 (6)	−0.0054 (6)
N31	0.0307 (5)	0.0256 (4)	0.0300 (5)	0.0027 (4)	−0.0055 (4)	−0.0059 (4)
C32	0.0347 (6)	0.0327 (6)	0.0336 (6)	0.0035 (5)	−0.0085 (5)	−0.0096 (5)
C33	0.0360 (6)	0.0340 (6)	0.0531 (8)	0.0030 (5)	−0.0091 (6)	−0.0195 (6)
C34	0.0350 (6)	0.0250 (5)	0.0628 (9)	0.0007 (5)	−0.0038 (6)	−0.0060 (6)
C35	0.0399 (6)	0.0318 (6)	0.0419 (7)	0.0027 (5)	−0.0007 (5)	0.0039 (5)
C36	0.0367 (6)	0.0314 (6)	0.0307 (6)	0.0035 (5)	−0.0034 (5)	−0.0049 (5)
N41	0.0376 (6)	0.0541 (7)	0.0486 (7)	−0.0024 (5)	−0.0002 (5)	−0.0136 (6)
C42	0.0504 (8)	0.0422 (7)	0.0368 (7)	−0.0009 (6)	−0.0060 (6)	−0.0061 (5)
C43	0.0383 (7)	0.0483 (8)	0.0489 (8)	0.0061 (6)	−0.0125 (6)	−0.0064 (6)
C44	0.0359 (7)	0.0655 (10)	0.0440 (8)	0.0006 (6)	−0.0014 (6)	−0.0053 (7)
C45	0.0475 (8)	0.0614 (9)	0.0398 (7)	0.0002 (7)	−0.0108 (6)	0.0004 (7)
C46	0.0350 (7)	0.0589 (9)	0.0546 (9)	0.0043 (6)	−0.0138 (6)	−0.0118 (7)

Geometric parameters (Å, º)

Mn1—O2^i	2.1980 (8)	C24—C25	1.374 (3)
Mn1—O1	2.2081 (8)	C24—H24	0.9500
Mn1—N31	2.2754 (10)	C25—C26	1.377 (2)
Mn1—N21	2.3068 (11)	C25—H25	0.9500
Mn1—N11	2.3267 (11)	C26—H26	0.9500
Mn1—Cl1	2.4418 (4)	N31—C32	1.3428 (15)
C1—O2	1.2512 (14)	N31—C36	1.3438 (16)
C1—O1	1.2559 (13)	C32—C33	1.3898 (18)
C1—C1^i	1.569 (2)	C32—H32	0.9500
O2—Mn1^i	2.1980 (8)	C33—C34	1.378 (2)
N11—C12	1.3404 (16)	C33—H33	0.9500
N11—C16	1.3424 (17)	C34—C35	1.386 (2)
C12—C13	1.391 (2)	C34—H34	0.9500
C12—H12	0.9500	C35—C36	1.3875 (18)
C13—C14	1.377 (3)	C35—H35	0.9500
C13—H13	0.9500	C36—H36	0.9500
C14—C15	1.384 (2)	N41—C42	1.330 (2)
C14—H14	0.9500	N41—C46	1.342 (2)
C15—C16	1.382 (2)	C42—C43	1.381 (2)
C15—H15	0.9500	C42—H42	0.9500
C16—H16	0.9500	C43—C44	1.379 (2)
N21—C22	1.3400 (19)	C43—H43	0.9500
N21—C26	1.3482 (17)	C44—C45	1.379 (2)
C22—C23	1.385 (2)	C44—H44	0.9500
C22—H22	0.9500	C45—C46	1.379 (2)
C23—C24	1.389 (2)	C45—H45	0.9500
C23—H23	0.9500	C46—H46	0.9500
O2^i—Mn1—O1	75.70 (3)	C22—C23—H23	120.4
O2^i—Mn1—N31	163.65 (3)	C24—C23—H23	120.4
O1—Mn1—N31	88.58 (3)	C25—C24—C23	118.49 (14)
O2^i—Mn1—N21	91.16 (4)	C25—C24—H24	120.8
O1—Mn1—N21	88.94 (4)	C23—C24—H24	120.8
N31—Mn1—N21	93.03 (4)	C24—C25—C26	118.92 (15)
O2^i—Mn1—N11	85.14 (4)	C24—C25—H25	120.5
O1—Mn1—N11	83.28 (4)	C26—C25—H25	120.5
N31—Mn1—N11	88.65 (4)	N21—C26—C25	123.60 (16)
N21—Mn1—N11	172.00 (4)	N21—C26—H26	118.2
O2^i—Mn1—Cl1	99.76 (2)	C25—C26—H26	118.2
O1—Mn1—Cl1	173.76 (2)	C32—N31—C36	117.62 (10)
N31—Mn1—Cl1	95.56 (3)	C32—N31—Mn1	121.40 (8)
N21—Mn1—Cl1	95.47 (3)	C36—N31—Mn1	120.96 (8)
N11—Mn1—Cl1	92.14 (3)	N31—C32—C33	122.84 (12)
O2—C1—O1	126.19 (10)	N31—C32—H32	118.6
O2—C1—C1^i	117.15 (11)	C33—C32—H32	118.6
O1—C1—C1^i	116.66 (12)	C34—C33—C32	118.94 (12)
C1—O1—Mn1	115.03 (7)	C34—C33—H33	120.5
C1—O2—Mn1^i	115.26 (7)	C32—C33—H33	120.5
C12—N11—C16	117.40 (12)	C33—C34—C35	118.91 (12)
C12—N11—Mn1	120.52 (9)	C33—C34—H34	120.5
C16—N11—Mn1	121.46 (9)	C35—C34—H34	120.5
N11—C12—C13	122.87 (14)	C34—C35—C36	118.75 (12)
N11—C12—H12	118.6	C34—C35—H35	120.6
C13—C12—H12	118.6	C36—C35—H35	120.6
C14—C13—C12	118.84 (14)	N31—C36—C35	122.94 (12)
C14—C13—H13	120.6	N31—C36—H36	118.5
C12—C13—H13	120.6	C35—C36—H36	118.5
C13—C14—C15	118.96 (14)	C42—N41—C46	116.32 (13)
C13—C14—H14	120.5	N41—C42—C43	124.15 (14)
C15—C14—H14	120.5	N41—C42—H42	117.9
C16—C15—C14	118.65 (14)	C43—C42—H42	117.9
C16—C15—H15	120.7	C44—C43—C42	118.43 (13)
C14—C15—H15	120.7	C44—C43—H43	120.8
N11—C16—C15	123.28 (13)	C42—C43—H43	120.8
N11—C16—H16	118.4	C45—C44—C43	118.76 (14)
C15—C16—H16	118.4	C45—C44—H44	120.6
C22—N21—C26	116.95 (13)	C43—C44—H44	120.6
C22—N21—Mn1	122.70 (9)	C46—C45—C44	118.50 (14)
C26—N21—Mn1	119.90 (10)	C46—C45—H45	120.8
N21—C22—C23	122.88 (14)	C44—C45—H45	120.8
N21—C22—H22	118.6	N41—C46—C45	123.85 (14)
C23—C22—H22	118.6	N41—C46—H46	118.1
C22—C23—C24	119.13 (16)	C45—C46—H46	118.1
O2—C1—O1—Mn1	176.61 (9)	C26—N21—C22—C23	1.1 (2)
C1^i—C1—O1—Mn1	−3.33 (15)	Mn1—N21—C22—C23	−171.25 (11)
O2^i—Mn1—O1—C1	3.79 (8)	N21—C22—C23—C24	−0.8 (2)
N31—Mn1—O1—C1	−171.69 (8)	C22—C23—C24—C25	−0.5 (2)
N21—Mn1—O1—C1	95.26 (8)	C23—C24—C25—C26	1.3 (2)
N11—Mn1—O1—C1	−82.88 (8)	C22—N21—C26—C25	−0.2 (2)
O1—C1—O2—Mn1^i	176.64 (9)	Mn1—N21—C26—C25	172.39 (11)
C1^i—C1—O2—Mn1^i	−3.43 (15)	C24—C25—C26—N21	−1.1 (2)
O2^i—Mn1—N11—C12	52.68 (10)	O2^i—Mn1—N31—C32	−50.36 (17)
O1—Mn1—N11—C12	128.82 (10)	O1—Mn1—N31—C32	−34.62 (9)
N31—Mn1—N11—C12	−142.46 (10)	N21—Mn1—N31—C32	54.24 (9)
Cl1—Mn1—N11—C12	−46.94 (10)	N11—Mn1—N31—C32	−117.93 (9)
O2^i—Mn1—N11—C16	−118.04 (10)	Cl1—Mn1—N31—C32	150.04 (9)
O1—Mn1—N11—C16	−41.90 (10)	O2^i—Mn1—N31—C36	131.19 (12)
N31—Mn1—N11—C16	46.83 (10)	O1—Mn1—N31—C36	146.93 (9)
Cl1—Mn1—N11—C16	142.35 (10)	N21—Mn1—N31—C36	−124.21 (9)
C16—N11—C12—C13	0.7 (2)	N11—Mn1—N31—C36	63.62 (9)
Mn1—N11—C12—C13	−170.40 (12)	Cl1—Mn1—N31—C36	−28.40 (9)
N11—C12—C13—C14	−0.6 (2)	C36—N31—C32—C33	0.47 (18)
C12—C13—C14—C15	0.1 (3)	Mn1—N31—C32—C33	−178.02 (9)
C13—C14—C15—C16	0.2 (2)	N31—C32—C33—C34	−0.40 (19)
C12—N11—C16—C15	−0.4 (2)	C32—C33—C34—C35	0.06 (19)
Mn1—N11—C16—C15	170.63 (11)	C33—C34—C35—C36	0.19 (19)
C14—C15—C16—N11	−0.1 (2)	C32—N31—C36—C35	−0.21 (18)
O2^i—Mn1—N21—C22	67.37 (10)	Mn1—N31—C36—C35	178.29 (10)
O1—Mn1—N21—C22	−8.30 (10)	C34—C35—C36—N31	−0.1 (2)
N31—Mn1—N21—C22	−96.83 (10)	C46—N41—C42—C43	−0.8 (2)
Cl1—Mn1—N21—C22	167.29 (10)	N41—C42—C43—C44	0.5 (2)
O2^i—Mn1—N21—C26	−104.74 (10)	C42—C43—C44—C45	0.1 (3)
O1—Mn1—N21—C26	179.59 (10)	C43—C44—C45—C46	−0.2 (3)
N31—Mn1—N21—C26	91.07 (10)	C42—N41—C46—C45	0.6 (2)
Cl1—Mn1—N21—C26	−4.82 (9)	C44—C45—C46—N41	−0.1 (3)

Symmetry code: (i) −x+1, −y, −z+1.