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

The Co complex of the title compound, [Co₂(C₂O₄)Cl₂(C₅H₅N)₆]·C₅H₅N, is located on a crystallographic centre of inversion. The solvent pyridine mol­ecules are located on general positions. The Co centre is octa­hedrally coordinated by three pyridine ligands, one Cl atom and a chelating oxalate anion which bridges two Co centres.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.063
• wR factor = 0.190
• 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)  Co1    -   Cl1     ..      27.24 su
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 ....          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.62
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for        N41
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          8

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   4 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
   1 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion


checkCIF publication errors

Alert level A
PUBL022_ALERT_1_A There is a mismatched ~ on line 93
              [Co~2~(C~2~O~4~)~Cl~2~(C~5~H~5~N)~6~].C~5~H~5~N, is located on a
              If you require a ~ then it should be escaped
              with a \, i.e. \~
              Otherwise there must be a matching closing ~, e.g. C~2~H~4~

   1 ALERT level A = Data missing that is essential or data in wrong format
   0 ALERT level G = General alerts. Data that may be required is missing

---

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[chlorotripyridinecobalt(II)] pyridine disolvate

Crystal data

[Co2(C2O4)Cl2(C5H5N)6]·C5H5N	F(000) = 936
Mr = 909.58	Dx = 1.421 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 12780 reflections
a = 9.5335 (19) Å	θ = 2.2–25.3°
b = 10.518 (2) Å	µ = 0.96 mm^−1
c = 21.205 (4) Å	T = 173 K
β = 91.78 (3)°	Plate, colourless
V = 2125.3 (7) Å^3	0.28 × 0.22 × 0.12 mm
Z = 2

Data collection

Stoe IPDS-II two-circle diffractometer	3906 independent reflections
Radiation source: fine-focus sealed tube	2545 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.089
ω scans	θmax = 25.4°, θmin = 2.2°
Absorption correction: empirical (using intensity measurements) (MULABS; Spek, 2003; Blessing, 1995)	h = −11→11
Tmin = 0.775, Tmax = 0.894	k = −12→12
24340 measured reflections	l = −23→25

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.063	H-atom parameters constrained
wR(F^2) = 0.190	w = 1/[σ^2(Fo^2) + (0.1345P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.94	(Δ/σ)max < 0.001
3906 reflections	Δρmax = 1.61 e Å^−3
263 parameters	Δρmin = −0.62 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.014 (2)

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
Co1	0.64275 (6)	0.63803 (6)	0.91228 (3)	0.0593 (3)
Cl1	0.79203 (15)	0.82402 (14)	0.92068 (8)	0.0859 (5)
C1	0.4666 (4)	0.4574 (4)	0.9732 (2)	0.0562 (10)
O1	0.5081 (3)	0.4780 (3)	0.91827 (15)	0.0598 (7)
O2	0.3799 (3)	0.3764 (3)	0.98879 (16)	0.0611 (8)
N11	0.4508 (4)	0.7524 (4)	0.9128 (2)	0.0632 (10)
C12	0.4359 (6)	0.8421 (5)	0.9569 (3)	0.0735 (13)
H12	0.5133	0.8601	0.9848	0.088*
C13	0.3124 (6)	0.9100 (6)	0.9636 (3)	0.0848 (16)
H13	0.3058	0.9724	0.9957	0.102*
C14	0.2004 (6)	0.8862 (6)	0.9235 (4)	0.0872 (17)
H14	0.1154	0.9326	0.9267	0.105*
C15	0.2140 (6)	0.7933 (6)	0.8783 (3)	0.0829 (16)
H15	0.1379	0.7735	0.8501	0.100*
C16	0.3406 (5)	0.7289 (5)	0.8747 (3)	0.0702 (13)
H16	0.3488	0.6648	0.8435	0.084*
N21	0.8235 (4)	0.5090 (4)	0.91601 (19)	0.0610 (9)
C22	0.8332 (5)	0.4107 (5)	0.9551 (2)	0.0661 (12)
H22	0.7547	0.3914	0.9799	0.079*
C23	0.9511 (5)	0.3347 (5)	0.9619 (3)	0.0717 (13)
H23	0.9527	0.2650	0.9904	0.086*
C24	1.0661 (5)	0.3617 (5)	0.9266 (3)	0.0728 (13)
H24	1.1490	0.3118	0.9302	0.087*
C25	1.0567 (5)	0.4643 (5)	0.8855 (3)	0.0691 (13)
H25	1.1339	0.4861	0.8604	0.083*
C26	0.9349 (5)	0.5343 (5)	0.8815 (3)	0.0657 (12)
H26	0.9298	0.6037	0.8529	0.079*
N31	0.6328 (4)	0.6246 (4)	0.8107 (2)	0.0633 (10)
C32	0.6615 (5)	0.7243 (5)	0.7731 (3)	0.0682 (12)
H32	0.6881	0.8025	0.7923	0.082*
C33	0.6541 (6)	0.7182 (5)	0.7087 (3)	0.0759 (14)
H33	0.6759	0.7907	0.6842	0.091*
C34	0.6146 (6)	0.6056 (5)	0.6795 (3)	0.0759 (14)
H34	0.6081	0.5995	0.6348	0.091*
C35	0.5845 (6)	0.5017 (5)	0.7171 (3)	0.0751 (13)
H35	0.5580	0.4225	0.6988	0.090*
C36	0.5940 (5)	0.5158 (5)	0.7817 (3)	0.0702 (13)
H36	0.5719	0.4447	0.8072	0.084*
N41	0.1852 (6)	0.5750 (6)	0.7399 (3)	0.1028 (17)
C42	0.0728 (6)	0.5103 (6)	0.7167 (3)	0.0805 (15)
H42	0.0504	0.4312	0.7355	0.097*
C43	−0.0108 (6)	0.5530 (5)	0.6671 (3)	0.0770 (14)
H43	−0.0876	0.5037	0.6512	0.092*
C44	0.0201 (6)	0.6697 (6)	0.6409 (3)	0.0797 (15)
H44	−0.0359	0.7022	0.6068	0.096*
C45	0.1315 (6)	0.7378 (6)	0.6645 (3)	0.0785 (14)
H45	0.1535	0.8188	0.6476	0.094*
C46	0.2111 (7)	0.6868 (7)	0.7133 (3)	0.0925 (18)
H46	0.2895	0.7342	0.7291	0.111*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0544 (4)	0.0593 (4)	0.0645 (4)	−0.0024 (3)	0.0055 (3)	0.0029 (3)
Cl1	0.0758 (8)	0.0801 (9)	0.1025 (11)	0.0027 (6)	0.0142 (7)	0.0123 (7)
C1	0.047 (2)	0.059 (2)	0.062 (3)	0.0032 (18)	−0.0036 (19)	−0.005 (2)
O1	0.0603 (16)	0.0622 (17)	0.057 (2)	−0.0033 (13)	0.0041 (14)	−0.0016 (14)
O2	0.0540 (16)	0.0597 (17)	0.070 (2)	−0.0104 (14)	0.0020 (14)	0.0005 (14)
N11	0.055 (2)	0.060 (2)	0.075 (3)	−0.0016 (16)	0.0015 (18)	0.0016 (19)
C12	0.066 (3)	0.068 (3)	0.086 (4)	−0.005 (2)	0.006 (3)	−0.005 (3)
C13	0.074 (3)	0.069 (3)	0.113 (5)	0.003 (3)	0.020 (3)	−0.004 (3)
C14	0.065 (3)	0.075 (3)	0.123 (5)	0.010 (3)	0.016 (3)	0.010 (3)
C15	0.064 (3)	0.081 (4)	0.104 (5)	0.004 (3)	−0.001 (3)	0.001 (3)
C16	0.064 (3)	0.064 (3)	0.083 (4)	0.000 (2)	−0.006 (2)	0.004 (2)
N21	0.0548 (19)	0.064 (2)	0.064 (2)	−0.0006 (16)	0.0039 (17)	0.0003 (18)
C22	0.063 (3)	0.071 (3)	0.065 (3)	0.006 (2)	0.007 (2)	0.004 (2)
C23	0.064 (3)	0.077 (3)	0.074 (3)	0.008 (2)	0.003 (2)	0.007 (2)
C24	0.058 (3)	0.082 (3)	0.078 (3)	0.008 (2)	−0.001 (2)	−0.009 (3)
C25	0.054 (2)	0.082 (3)	0.071 (3)	−0.002 (2)	0.009 (2)	0.000 (3)
C26	0.058 (2)	0.068 (3)	0.072 (3)	−0.002 (2)	0.008 (2)	0.001 (2)
N31	0.063 (2)	0.059 (2)	0.068 (3)	0.0009 (17)	0.0068 (18)	0.0012 (18)
C32	0.072 (3)	0.061 (3)	0.072 (3)	0.002 (2)	0.003 (2)	0.003 (2)
C33	0.091 (4)	0.072 (3)	0.065 (3)	0.004 (3)	0.003 (3)	0.009 (2)
C34	0.075 (3)	0.087 (4)	0.065 (3)	0.005 (3)	−0.003 (2)	−0.004 (3)
C35	0.075 (3)	0.075 (3)	0.075 (4)	0.000 (3)	0.003 (3)	−0.007 (3)
C36	0.070 (3)	0.069 (3)	0.072 (3)	0.000 (2)	0.010 (2)	0.004 (2)
N41	0.105 (4)	0.106 (4)	0.096 (4)	−0.020 (3)	−0.021 (3)	0.030 (3)
C42	0.080 (3)	0.074 (3)	0.087 (4)	−0.006 (3)	−0.001 (3)	0.011 (3)
C43	0.072 (3)	0.079 (3)	0.080 (4)	−0.002 (3)	0.000 (3)	−0.006 (3)
C44	0.074 (3)	0.083 (4)	0.082 (4)	0.008 (3)	−0.002 (3)	0.009 (3)
C45	0.078 (3)	0.074 (3)	0.084 (4)	−0.001 (3)	0.011 (3)	0.009 (3)
C46	0.085 (4)	0.097 (4)	0.095 (5)	−0.021 (3)	−0.009 (3)	0.017 (4)

Geometric parameters (Å, º)

Co1—O2^i	2.121 (3)	C24—C25	1.388 (8)
Co1—O1	2.123 (3)	C24—H24	0.9500
Co1—N31	2.157 (4)	C25—C26	1.376 (7)
Co1—N11	2.191 (4)	C25—H25	0.9500
Co1—N21	2.193 (4)	C26—H26	0.9500
Co1—Cl1	2.4224 (17)	N31—C36	1.346 (7)
C1—O2	1.239 (5)	N31—C32	1.351 (6)
C1—O1	1.260 (6)	C32—C33	1.366 (8)
C1—C1^i	1.567 (9)	C32—H32	0.9500
O2—Co1^i	2.121 (3)	C33—C34	1.383 (8)
N11—C16	1.328 (6)	C33—H33	0.9500
N11—C12	1.338 (7)	C34—C35	1.389 (8)
C12—C13	1.389 (8)	C34—H34	0.9500
C12—H12	0.9500	C35—C36	1.378 (8)
C13—C14	1.367 (9)	C35—H35	0.9500
C13—H13	0.9500	C36—H36	0.9500
C14—C15	1.377 (9)	N41—C46	1.330 (8)
C14—H14	0.9500	N41—C42	1.350 (8)
C15—C16	1.388 (7)	C42—C43	1.375 (8)
C15—H15	0.9500	C42—H42	0.9500
C16—H16	0.9500	C43—C44	1.382 (8)
N21—C22	1.327 (6)	C43—H43	0.9500
N21—C26	1.335 (6)	C44—C45	1.364 (8)
C22—C23	1.383 (7)	C44—H44	0.9500
C22—H22	0.9500	C45—C46	1.373 (9)
C23—C24	1.376 (7)	C45—H45	0.9500
C23—H23	0.9500	C46—H46	0.9500
O2^i—Co1—O1	78.68 (12)	C24—C23—H23	120.5
O2^i—Co1—N31	168.52 (13)	C22—C23—H23	120.5
O1—Co1—N31	90.00 (14)	C23—C24—C25	117.7 (5)
O2^i—Co1—N11	85.61 (15)	C23—C24—H24	121.2
O1—Co1—N11	85.89 (13)	C25—C24—H24	121.2
N31—Co1—N11	91.75 (16)	C26—C25—C24	119.5 (5)
O2^i—Co1—N21	91.37 (14)	C26—C25—H25	120.2
O1—Co1—N21	89.04 (13)	C24—C25—H25	120.2
N31—Co1—N21	90.31 (15)	N21—C26—C25	122.9 (5)
N11—Co1—N21	174.52 (15)	N21—C26—H26	118.5
O2^i—Co1—Cl1	93.60 (9)	C25—C26—H26	118.5
O1—Co1—Cl1	172.21 (10)	C36—N31—C32	116.6 (5)
N31—Co1—Cl1	97.68 (12)	C36—N31—Co1	121.0 (3)
N11—Co1—Cl1	92.58 (11)	C32—N31—Co1	122.4 (3)
N21—Co1—Cl1	92.17 (11)	N31—C32—C33	123.3 (5)
O2—C1—O1	126.6 (4)	N31—C32—H32	118.3
O2—C1—C1^i	117.2 (5)	C33—C32—H32	118.3
O1—C1—C1^i	116.1 (5)	C32—C33—C34	119.5 (5)
C1—O1—Co1	113.6 (3)	C32—C33—H33	120.2
C1—O2—Co1^i	113.8 (3)	C34—C33—H33	120.2
C16—N11—C12	117.2 (4)	C33—C34—C35	118.3 (5)
C16—N11—Co1	122.6 (3)	C33—C34—H34	120.8
C12—N11—Co1	119.8 (3)	C35—C34—H34	120.8
N11—C12—C13	122.9 (5)	C36—C35—C34	118.6 (5)
N11—C12—H12	118.6	C36—C35—H35	120.7
C13—C12—H12	118.6	C34—C35—H35	120.7
C14—C13—C12	119.4 (6)	N31—C36—C35	123.7 (5)
C14—C13—H13	120.3	N31—C36—H36	118.2
C12—C13—H13	120.3	C35—C36—H36	118.2
C13—C14—C15	118.3 (5)	C46—N41—C42	116.5 (5)
C13—C14—H14	120.9	N41—C42—C43	123.3 (5)
C15—C14—H14	120.9	N41—C42—H42	118.3
C14—C15—C16	119.1 (6)	C43—C42—H42	118.3
C14—C15—H15	120.5	C42—C43—C44	118.1 (5)
C16—C15—H15	120.5	C42—C43—H43	120.9
N11—C16—C15	123.2 (5)	C44—C43—H43	120.9
N11—C16—H16	118.4	C45—C44—C43	119.5 (6)
C15—C16—H16	118.4	C45—C44—H44	120.2
C22—N21—C26	117.2 (4)	C43—C44—H44	120.2
C22—N21—Co1	123.0 (3)	C44—C45—C46	118.5 (5)
C26—N21—Co1	119.6 (3)	C44—C45—H45	120.8
N21—C22—C23	123.7 (5)	C46—C45—H45	120.8
N21—C22—H22	118.1	N41—C46—C45	124.0 (6)
C23—C22—H22	118.1	N41—C46—H46	118.0
C24—C23—C22	118.9 (5)	C45—C46—H46	118.0
O2—C1—O1—Co1	174.4 (3)	C26—N21—C22—C23	0.1 (8)
C1^i—C1—O1—Co1	−6.3 (6)	Co1—N21—C22—C23	−174.4 (4)
O2^i—Co1—O1—C1	6.9 (3)	N21—C22—C23—C24	0.4 (9)
N31—Co1—O1—C1	−171.2 (3)	C22—C23—C24—C25	−0.4 (8)
N11—Co1—O1—C1	−79.4 (3)	C23—C24—C25—C26	−0.1 (8)
N21—Co1—O1—C1	98.5 (3)	C22—N21—C26—C25	−0.7 (8)
O1—C1—O2—Co1^i	173.9 (3)	Co1—N21—C26—C25	174.1 (4)
C1^i—C1—O2—Co1^i	−5.4 (6)	C24—C25—C26—N21	0.6 (8)
O2^i—Co1—N11—C16	−128.8 (4)	O2^i—Co1—N31—C36	−29.5 (9)
O1—Co1—N11—C16	−49.9 (4)	O1—Co1—N31—C36	−20.1 (4)
N31—Co1—N11—C16	40.0 (4)	N11—Co1—N31—C36	−106.0 (4)
Cl1—Co1—N11—C16	137.7 (4)	N21—Co1—N31—C36	68.9 (4)
O2^i—Co1—N11—C12	44.4 (4)	Cl1—Co1—N31—C36	161.2 (4)
O1—Co1—N11—C12	123.3 (4)	O2^i—Co1—N31—C32	148.9 (6)
N31—Co1—N11—C12	−146.8 (4)	O1—Co1—N31—C32	158.3 (4)
Cl1—Co1—N11—C12	−49.0 (4)	N11—Co1—N31—C32	72.4 (4)
C16—N11—C12—C13	−0.4 (8)	N21—Co1—N31—C32	−112.7 (4)
Co1—N11—C12—C13	−174.0 (4)	Cl1—Co1—N31—C32	−20.4 (4)
N11—C12—C13—C14	−0.6 (9)	C36—N31—C32—C33	−0.7 (7)
C12—C13—C14—C15	1.2 (9)	Co1—N31—C32—C33	−179.1 (4)
C13—C14—C15—C16	−0.8 (9)	N31—C32—C33—C34	0.5 (8)
C12—N11—C16—C15	0.7 (8)	C32—C33—C34—C35	−0.4 (8)
Co1—N11—C16—C15	174.1 (4)	C33—C34—C35—C36	0.7 (8)
C14—C15—C16—N11	−0.1 (9)	C32—N31—C36—C35	1.0 (7)
O2^i—Co1—N21—C22	35.8 (4)	Co1—N31—C36—C35	179.4 (4)
O1—Co1—N21—C22	−42.8 (4)	C34—C35—C36—N31	−1.0 (8)
N31—Co1—N21—C22	−132.8 (4)	C46—N41—C42—C43	1.6 (11)
Cl1—Co1—N21—C22	129.5 (4)	N41—C42—C43—C44	−1.7 (10)
O2^i—Co1—N21—C26	−138.6 (4)	C42—C43—C44—C45	0.3 (9)
O1—Co1—N21—C26	142.8 (4)	C43—C44—C45—C46	1.0 (9)
N31—Co1—N21—C26	52.8 (4)	C42—N41—C46—C45	−0.2 (11)
Cl1—Co1—N21—C26	−44.9 (4)	C44—C45—C46—N41	−1.1 (11)

Symmetry code: (i) −x+1, −y+1, −z+2.