Synthesis, crystal structure and Hirshfeld surface analysis of tetra­aqua­bis­(isonicotinamide-κN¹)cobalt(II) succinate

In the title Co^II complex, both the cation and succinate anion are located about individual inversion centres. In the crystal, the ions are linked via O—H...O and N—H...O hydrogen bonds, forming a three-dimensional framework.

Key indicators

• Single-crystal X-ray study
• T = 296 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.034
• wR factor = 0.087
• Data-to-parameter ratio = 12.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      4.230 Check
PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min).          6 Note
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         15 Report
PLAT918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) .          1 Check

Alert level G
PLAT063_ALERT_4_G Crystal Size Likely too Large for Beam Size ....       0.68 mm
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Co1      --O4        .        5.2 s.u.
PLAT794_ALERT_5_G Tentative Bond Valency for Co1       (II)      .       1.85 Info
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          2 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   5 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   4 ALERT level G = General information/check it is not something unexpected

   0 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
   4 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

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Computing details

Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA (Stoe & Cie, 2002); data reduction: X-RED32 (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2017 (Sheldrick, 2015); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2008); software used to prepare material for publication: SHELXL2017 (Sheldrick, 2015) and PLATON (Spek, 2009).

Tetraaquabis(isonicotinamide-κN¹)cobalt(II) butanedioate

Crystal data

[Co(C6H6N2O)2(H2O)4](C4H4O4)	F(000) = 510
Mr = 491.32	Dx = 1.582 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 9.6757 (8) Å	Cell parameters from 8789 reflections
b = 10.0381 (8) Å	θ = 3.1–30.2°
c = 11.4947 (10) Å	µ = 0.89 mm^−1
β = 112.489 (6)°	T = 296 K
V = 1031.53 (15) Å^3	Prism, red
Z = 2	0.68 × 0.49 × 0.37 mm

Data collection

Stoe IPDS 2 diffractometer	2125 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus	1709 reflections with I > 2σ(I)
Detector resolution: 6.67 pixels mm^-1	Rint = 0.033
rotation method scans	θmax = 26.5°, θmin = 4.0°
Absorption correction: integration (X-RED32; Stoe & Cie, 2002)	h = −12→12
Tmin = 0.664, Tmax = 0.770	k = −12→12
5748 measured reflections	l = −14→10

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)] = 0.034	Hydrogen site location: mixed
wR(F^2) = 0.087	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0544P)^2 + 0.0723P] where P = (Fo^2 + 2Fc^2)/3
2125 reflections	(Δ/σ)max < 0.001
166 parameters	Δρmax = 0.28 e Å^−3
0 restraints	Δρmin = −0.38 e Å^−3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Co1	0.500000	0.500000	1.000000	0.02416 (13)
O3	0.40225 (19)	0.64528 (17)	0.85930 (16)	0.0323 (3)
O4	0.39411 (19)	0.34772 (15)	0.87503 (16)	0.0314 (3)
O2	0.44508 (19)	0.36520 (15)	0.66478 (15)	0.0372 (4)
O5	1.08679 (19)	0.30825 (16)	0.80841 (18)	0.0450 (4)
O1	0.2865 (2)	0.53407 (16)	0.62211 (16)	0.0413 (4)
N2	0.68645 (19)	0.47784 (15)	0.94294 (17)	0.0284 (4)
N1	1.0405 (3)	0.5081 (3)	0.7144 (3)	0.0523 (6)
C1	1.0166 (2)	0.4142 (2)	0.7847 (2)	0.0340 (5)
C2	0.9000 (2)	0.4398 (2)	0.8388 (2)	0.0291 (4)
C5	0.7381 (2)	0.5790 (2)	0.8958 (2)	0.0336 (5)
H5	0.700517	0.663743	0.898389	0.040*
C7	0.3809 (2)	0.4648 (2)	0.6004 (2)	0.0296 (4)
C3	0.8494 (3)	0.3354 (2)	0.8895 (2)	0.0348 (5)
H3	0.886482	0.249919	0.889455	0.042*
C6	0.8434 (2)	0.5649 (2)	0.8438 (2)	0.0343 (5)
H6	0.876190	0.638596	0.812443	0.041*
C4	0.7441 (3)	0.3579 (2)	0.9399 (2)	0.0353 (5)
H4	0.711309	0.286121	0.973646	0.042*
C8	0.4207 (3)	0.5013 (3)	0.4888 (3)	0.0535 (7)
H8A	0.368960	0.440472	0.420345	0.064*
H8B	0.382876	0.590118	0.461003	0.064*
H1A	0.982 (4)	0.584 (4)	0.697 (4)	0.083 (12)*
H1B	1.107 (4)	0.495 (3)	0.683 (4)	0.076 (11)*
H4A	0.403 (3)	0.355 (3)	0.812 (3)	0.035 (7)*
H3A	0.449 (3)	0.711 (3)	0.857 (3)	0.049 (8)*
H3B	0.373 (4)	0.612 (3)	0.792 (3)	0.055 (9)*
H4B	0.304 (4)	0.330 (3)	0.858 (3)	0.065 (10)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0267 (2)	0.02335 (19)	0.0296 (2)	−0.00065 (15)	0.01885 (15)	0.00042 (15)
O3	0.0388 (9)	0.0293 (8)	0.0331 (9)	−0.0031 (7)	0.0184 (7)	0.0019 (7)
O4	0.0343 (9)	0.0338 (8)	0.0335 (9)	−0.0035 (6)	0.0211 (7)	−0.0022 (6)
O2	0.0519 (10)	0.0311 (7)	0.0413 (9)	0.0079 (7)	0.0319 (8)	0.0046 (6)
O5	0.0432 (9)	0.0380 (9)	0.0700 (12)	−0.0002 (7)	0.0399 (9)	−0.0086 (8)
O1	0.0469 (9)	0.0431 (9)	0.0443 (10)	0.0117 (7)	0.0291 (8)	0.0043 (7)
N2	0.0296 (8)	0.0264 (9)	0.0373 (9)	−0.0010 (6)	0.0217 (7)	−0.0014 (7)
N1	0.0506 (12)	0.0602 (14)	0.0686 (15)	0.0086 (12)	0.0479 (12)	0.0121 (12)
C1	0.0285 (11)	0.0403 (12)	0.0406 (12)	−0.0040 (9)	0.0214 (10)	−0.0073 (9)
C2	0.0257 (10)	0.0333 (10)	0.0336 (11)	−0.0011 (8)	0.0174 (9)	−0.0032 (8)
C5	0.0368 (12)	0.0252 (10)	0.0475 (13)	0.0038 (8)	0.0260 (10)	0.0045 (9)
C7	0.0323 (10)	0.0304 (10)	0.0309 (11)	−0.0036 (8)	0.0175 (9)	−0.0010 (8)
C3	0.0368 (12)	0.0258 (10)	0.0515 (13)	−0.0003 (8)	0.0276 (10)	−0.0027 (9)
C6	0.0349 (11)	0.0320 (11)	0.0450 (13)	0.0004 (9)	0.0253 (10)	0.0076 (9)
C4	0.0400 (12)	0.0262 (10)	0.0516 (14)	−0.0018 (9)	0.0307 (11)	0.0014 (9)
C8	0.0439 (14)	0.0825 (19)	0.0455 (14)	0.0135 (14)	0.0298 (12)	0.0250 (14)

Geometric parameters (Å, º)

Co1—O4^i	2.0794 (16)	N1—H1A	0.92 (4)
Co1—O3	2.1134 (15)	N1—H1B	0.87 (4)
Co1—O4	2.0795 (16)	C1—C2	1.504 (3)
Co1—N2^i	2.1540 (16)	C2—C3	1.377 (3)
Co1—O3^i	2.1134 (15)	C2—C6	1.381 (3)
Co1—N2	2.1540 (16)	C5—C6	1.372 (3)
O3—H3A	0.81 (3)	C5—H5	0.9300
O3—H3B	0.79 (4)	C7—C8	1.519 (3)
O4—H4A	0.77 (3)	C3—C4	1.370 (3)
O4—H4B	0.83 (4)	C3—H3	0.9300
O2—C7	1.257 (3)	C6—H6	0.9300
O5—C1	1.235 (3)	C4—H4	0.9300
O1—C7	1.247 (3)	C8—C8^ii	1.456 (5)
N2—C4	1.333 (3)	C8—H8A	0.9700
N2—C5	1.334 (3)	C8—H8B	0.9700
N1—C1	1.317 (3)
O3—Co1—O3^i	180	O5—C1—N1	122.8 (2)
O4^i—Co1—O4	180	O5—C1—C2	119.4 (2)
N2^i—Co1—N2	180	N1—C1—C2	117.8 (2)
O4^i—Co1—O3	88.82 (7)	C3—C2—C6	117.62 (18)
O4—Co1—O3	91.18 (7)	C3—C2—C1	119.32 (18)
O4^i—Co1—O3^i	91.18 (7)	C6—C2—C1	123.03 (19)
O4—Co1—O3^i	88.82 (7)	N2—C5—C6	123.66 (19)
O4^i—Co1—N2^i	87.85 (6)	N2—C5—H5	118.2
O4—Co1—N2^i	92.15 (7)	C6—C5—H5	118.2
O3—Co1—N2^i	88.85 (6)	O1—C7—O2	124.09 (19)
O3^i—Co1—N2^i	91.15 (6)	O1—C7—C8	118.4 (2)
O4^i—Co1—N2	92.15 (7)	O2—C7—C8	117.47 (19)
O4—Co1—N2	87.85 (6)	C4—C3—C2	119.73 (19)
O3—Co1—N2	91.15 (6)	C4—C3—H3	120.1
O3^i—Co1—N2	88.85 (6)	C2—C3—H3	120.1
Co1—O3—H3A	120 (2)	C5—C6—C2	118.99 (19)
Co1—O3—H3B	110 (2)	C5—C6—H6	120.5
H3A—O3—H3B	108 (3)	C2—C6—H6	120.5
Co1—O4—H4A	112 (2)	N2—C4—C3	123.14 (19)
Co1—O4—H4B	121 (2)	N2—C4—H4	118.4
H4A—O4—H4B	106 (3)	C3—C4—H4	118.4
C4—N2—C5	116.83 (17)	C8^ii—C8—C7	115.9 (3)
C4—N2—Co1	120.60 (13)	C8^ii—C8—H8A	108.3
C5—N2—Co1	122.14 (13)	C7—C8—H8A	108.3
C1—N1—H1A	119 (3)	C8^ii—C8—H8B	108.3
C1—N1—H1B	119 (2)	C7—C8—H8B	108.3
H1A—N1—H1B	122 (3)	H8A—C8—H8B	107.4
O5—C1—C2—C3	−14.5 (3)	N2—C5—C6—C2	0.2 (4)
N1—C1—C2—C3	166.3 (2)	C3—C2—C6—C5	−1.4 (3)
O5—C1—C2—C6	163.5 (2)	C1—C2—C6—C5	−179.5 (2)
N1—C1—C2—C6	−15.7 (3)	C5—N2—C4—C3	−1.2 (4)
C4—N2—C5—C6	1.1 (4)	Co1—N2—C4—C3	171.39 (19)
Co1—N2—C5—C6	−171.37 (19)	C2—C3—C4—N2	0.0 (4)
C6—C2—C3—C4	1.4 (4)	O1—C7—C8—C8^ii	136.1 (3)
C1—C2—C3—C4	179.5 (2)	O2—C7—C8—C8^ii	−44.5 (5)

Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) −x+1, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3B···O1	0.79 (4)	1.97 (4)	2.756 (3)	176 (3)
O4—H4A···O2	0.77 (3)	1.88 (3)	2.651 (2)	174 (3)
O3—H3A···O2^iii	0.81 (3)	1.92 (3)	2.729 (2)	175 (3)
O4—H4B···O5^iv	0.83 (4)	1.97 (4)	2.801 (2)	174 (3)
N1—H1A···O5^v	0.92 (4)	2.34 (4)	3.227 (3)	160 (3)
N1—H1B···O1^vi	0.87 (4)	2.14 (4)	2.966 (3)	160 (3)
C5—H5···O2^iii	0.93	2.41	3.307 (3)	161
C6—H6···O5^v	0.93	2.31	3.223 (3)	167

Symmetry codes: (iii) −x+1, y+1/2, −z+3/2; (iv) x−1, y, z; (v) −x+2, y+1/2, −z+3/2; (vi) x+1, y, z.