Crystal structure of aqua­tris­(isonicotinamide-κN)bis­(thio­cyanato-κN)cobalt(II) 2.5-hydrate

In the crystal structure of the title compound, the Co^II cations are coordinated by two terminal N-bonded thio­cyanate anions, three isonicotinamide ligands and one water mol­ecule into discrete octa­hedral complexes that are connected by classical and non-classical hydrogen bonding into a three-dimensional network.

Key indicators

• Single-crystal X-ray study
• T = 200 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.040
• wR factor = 0.094
• Data-to-parameter ratio = 18.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT480_ALERT_4_C Long H...A H-Bond Reported H11    ..  S2      ..       2.96 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H21    ..  N2      ..       2.65 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H32    ..  S2      ..       3.00 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2O2   ..  N31     ..       2.66 Ang.
PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           5 Note
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600         14 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          4 Note

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         13 Report
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...       0.50 Check
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       5.52 Why ?
PLAT230_ALERT_2_G Hirshfeld Test Diff for    S1     --  C1      ..        7.9 s.u.
PLAT230_ALERT_2_G Hirshfeld Test Diff for    S2     --  C2      ..        7.6 s.u.
PLAT230_ALERT_2_G Hirshfeld Test Diff for    N2     --  C2      ..        5.2 s.u.
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          7 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         40 Note
PLAT933_ALERT_2_G Number of OMIT records in Embedded RES .........          3 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density           4 Note

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

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   6 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

---

Computing details

Data collection: X-AREA (Stoe, 2008); cell refinement: X-AREA (Stoe, 2008); data reduction: X-AREA (Stoe, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Aquatris(isonicotinamide-κN)bis(thiocyanato-κN)cobalt(II) 2.5-hydrate

Crystal data

[Co(NCS)2(C6H6N2O)3(H2O)]·2.5H2O	F(000) = 2496
Mr = 604.53	Dx = 1.539 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 19.2539 (16) Å	Cell parameters from 6260 reflections
b = 13.1442 (8) Å	θ = 4.3–56°
c = 20.7913 (16) Å	µ = 0.87 mm^−1
β = 97.327 (10)°	T = 200 K
V = 5218.8 (7) Å^3	Block, red-brown
Z = 8	0.11 × 0.08 × 0.06 mm

Data collection

Stoe IPDS-2 diffractometer	5098 reflections with I > 2σ(I)
ω–scans	Rint = 0.060
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe, 2008)	θmax = 28.0°, θmin = 2.6°
Tmin = 0.775, Tmax = 0.920	h = −25→25
29661 measured reflections	k = −17→17
6260 independent reflections	l = −27→27

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.040	H-atom parameters constrained
wR(F^2) = 0.094	w = 1/[σ^2(Fo^2) + (0.0525P)^2 + 5.523P] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max = 0.001
6260 reflections	Δρmax = 0.33 e Å^−3
339 parameters	Δρmin = −0.55 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	0.18635 (2)	0.67227 (2)	0.31272 (2)	0.01581 (7)
N1	0.14313 (9)	0.70880 (14)	0.39620 (8)	0.0246 (3)
C1	0.10950 (9)	0.72960 (14)	0.43682 (9)	0.0186 (3)
S1	0.06154 (3)	0.75764 (4)	0.49356 (3)	0.02889 (12)
N2	0.22147 (9)	0.62103 (13)	0.22769 (8)	0.0233 (3)
C2	0.25664 (10)	0.61371 (14)	0.18638 (9)	0.0201 (4)
S2	0.30765 (3)	0.60830 (4)	0.12936 (3)	0.02793 (12)
N11	0.12709 (8)	0.79048 (12)	0.25649 (8)	0.0209 (3)
C11	0.12791 (11)	0.88801 (16)	0.27443 (10)	0.0262 (4)
H11	0.1524	0.9059	0.3155	0.031*
C12	0.09489 (11)	0.96437 (16)	0.23626 (10)	0.0269 (4)
H12	0.0975	1.0329	0.2509	0.032*
C13	0.05785 (10)	0.94012 (15)	0.17636 (9)	0.0206 (4)
C14	0.05573 (11)	0.83848 (16)	0.15789 (10)	0.0264 (4)
H14	0.0305	0.8182	0.1177	0.032*
C15	0.09093 (11)	0.76706 (15)	0.19885 (10)	0.0263 (4)
H15	0.0894	0.6979	0.1855	0.032*
C16	0.02360 (11)	1.02471 (16)	0.13489 (10)	0.0250 (4)
N12	−0.01376 (10)	0.99985 (14)	0.07899 (9)	0.0324 (4)
H12A	−0.0341	1.0476	0.0536	0.039*
H12B	−0.0182	0.9356	0.0673	0.039*
O11	0.03115 (10)	1.11340 (12)	0.15299 (8)	0.0415 (4)
N21	0.27358 (8)	0.77939 (12)	0.33884 (8)	0.0187 (3)
C21	0.32723 (10)	0.78644 (16)	0.30338 (10)	0.0246 (4)
H21	0.3289	0.7402	0.2685	0.030*
C22	0.38017 (10)	0.85805 (16)	0.31536 (10)	0.0235 (4)
H22	0.4164	0.8613	0.2884	0.028*
C23	0.37979 (9)	0.92477 (14)	0.36683 (9)	0.0174 (3)
C24	0.32564 (10)	0.91704 (15)	0.40465 (9)	0.0207 (4)
H24	0.3239	0.9609	0.4407	0.025*
C25	0.27411 (10)	0.84428 (15)	0.38891 (9)	0.0212 (4)
H25	0.2371	0.8400	0.4150	0.025*
C26	0.43638 (9)	1.00411 (14)	0.37791 (9)	0.0187 (4)
N22	0.45023 (9)	1.04280 (14)	0.43691 (8)	0.0252 (4)
H22A	0.4825	1.0902	0.4449	0.030*
H22B	0.4272	1.0212	0.4682	0.030*
O21	0.46730 (7)	1.03177 (11)	0.33192 (7)	0.0231 (3)
N31	0.24699 (8)	0.55232 (12)	0.36533 (7)	0.0182 (3)
C31	0.24100 (10)	0.45608 (15)	0.34455 (9)	0.0222 (4)
H31	0.2135	0.4428	0.3042	0.027*
C32	0.27278 (10)	0.37491 (15)	0.37887 (10)	0.0235 (4)
H32	0.2667	0.3076	0.3625	0.028*
C33	0.31380 (9)	0.39326 (14)	0.43780 (9)	0.0183 (3)
C34	0.32139 (10)	0.49318 (15)	0.45905 (10)	0.0238 (4)
H34	0.3497	0.5088	0.4986	0.029*
C35	0.28715 (11)	0.56976 (15)	0.42182 (10)	0.0245 (4)
H35	0.2924	0.6378	0.4370	0.029*
C36	0.35105 (10)	0.31096 (15)	0.47912 (9)	0.0203 (4)
N32	0.32523 (10)	0.21708 (13)	0.47146 (9)	0.0283 (4)
H32A	0.3452	0.1668	0.4949	0.034*
H32B	0.2882	0.2054	0.4430	0.034*
O31	0.40296 (7)	0.33185 (11)	0.51840 (7)	0.0257 (3)
O1	0.09982 (7)	0.56631 (11)	0.29295 (7)	0.0226 (3)
H1O1	0.0844	0.5474	0.2552	0.034*
H2O1	0.0639	0.5683	0.3120	0.034*
O2	0.38171 (8)	1.02681 (13)	0.55143 (7)	0.0324 (3)
H1O2	0.4007	1.0670	0.5798	0.049*
H2O2	0.3617	0.9813	0.5707	0.049*
O3	0.43909 (14)	0.17955 (15)	0.62254 (12)	0.0672 (7)
H1O3	0.4391	0.2301	0.5978	0.101*
H2O3	0.4411	0.2036	0.6602	0.101*
O4	0.5000	0.73797 (19)	0.2500	0.0451 (6)
H1O4	0.5181	0.7008	0.2238	0.068*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.01664 (12)	0.01500 (12)	0.01570 (12)	−0.00072 (9)	0.00174 (9)	0.00114 (9)
N1	0.0253 (8)	0.0258 (9)	0.0237 (8)	−0.0016 (7)	0.0075 (7)	−0.0018 (7)
C1	0.0190 (8)	0.0162 (8)	0.0196 (8)	−0.0020 (7)	−0.0014 (7)	0.0010 (7)
S1	0.0318 (3)	0.0333 (3)	0.0232 (2)	0.0063 (2)	0.0099 (2)	−0.0006 (2)
N2	0.0264 (8)	0.0240 (9)	0.0200 (8)	−0.0008 (7)	0.0048 (6)	−0.0017 (6)
C2	0.0245 (9)	0.0144 (8)	0.0202 (9)	0.0006 (7)	−0.0012 (7)	0.0016 (7)
S2	0.0301 (3)	0.0310 (3)	0.0243 (2)	0.0070 (2)	0.0096 (2)	0.0061 (2)
N11	0.0225 (8)	0.0187 (8)	0.0205 (8)	0.0005 (6)	−0.0010 (6)	0.0020 (6)
C11	0.0303 (10)	0.0226 (10)	0.0230 (9)	0.0048 (8)	−0.0067 (8)	−0.0034 (8)
C12	0.0331 (10)	0.0188 (9)	0.0267 (10)	0.0045 (8)	−0.0044 (8)	−0.0048 (8)
C13	0.0208 (9)	0.0199 (9)	0.0205 (9)	0.0029 (7)	0.0009 (7)	0.0016 (7)
C14	0.0316 (10)	0.0222 (10)	0.0222 (9)	0.0012 (8)	−0.0084 (8)	0.0000 (8)
C15	0.0342 (10)	0.0158 (9)	0.0259 (10)	−0.0007 (8)	−0.0083 (8)	0.0000 (8)
C16	0.0282 (10)	0.0209 (10)	0.0256 (10)	0.0060 (8)	0.0020 (8)	0.0015 (8)
N12	0.0417 (10)	0.0221 (9)	0.0294 (9)	0.0076 (8)	−0.0105 (8)	0.0027 (7)
O11	0.0673 (12)	0.0199 (8)	0.0337 (9)	0.0107 (8)	−0.0072 (8)	−0.0019 (7)
N21	0.0172 (7)	0.0158 (7)	0.0227 (8)	−0.0023 (6)	0.0012 (6)	0.0014 (6)
C21	0.0255 (9)	0.0214 (10)	0.0279 (10)	−0.0026 (8)	0.0071 (8)	−0.0058 (8)
C22	0.0221 (9)	0.0225 (10)	0.0273 (10)	−0.0032 (7)	0.0083 (7)	−0.0022 (8)
C23	0.0160 (8)	0.0147 (8)	0.0209 (9)	−0.0002 (6)	0.0000 (6)	0.0041 (7)
C24	0.0204 (8)	0.0212 (9)	0.0205 (9)	−0.0032 (7)	0.0027 (7)	−0.0025 (7)
C25	0.0189 (8)	0.0222 (10)	0.0228 (9)	−0.0041 (7)	0.0041 (7)	−0.0011 (7)
C26	0.0163 (8)	0.0171 (9)	0.0223 (9)	0.0011 (7)	0.0010 (7)	0.0027 (7)
N22	0.0237 (8)	0.0284 (9)	0.0235 (8)	−0.0098 (7)	0.0031 (6)	−0.0026 (7)
O21	0.0214 (6)	0.0260 (7)	0.0220 (7)	−0.0043 (5)	0.0026 (5)	0.0057 (6)
N31	0.0199 (7)	0.0159 (7)	0.0185 (7)	0.0005 (6)	0.0007 (6)	0.0015 (6)
C31	0.0256 (9)	0.0195 (9)	0.0197 (9)	0.0016 (7)	−0.0043 (7)	−0.0037 (7)
C32	0.0292 (10)	0.0159 (9)	0.0239 (9)	−0.0003 (7)	−0.0024 (8)	−0.0017 (7)
C33	0.0178 (8)	0.0163 (9)	0.0206 (9)	0.0008 (6)	0.0016 (7)	0.0008 (7)
C34	0.0270 (9)	0.0190 (9)	0.0231 (9)	0.0007 (7)	−0.0058 (7)	−0.0013 (7)
C35	0.0297 (10)	0.0160 (9)	0.0252 (10)	−0.0007 (7)	−0.0068 (8)	−0.0011 (7)
C36	0.0212 (8)	0.0189 (9)	0.0209 (9)	0.0032 (7)	0.0026 (7)	−0.0009 (7)
N32	0.0318 (9)	0.0162 (8)	0.0337 (10)	0.0011 (7)	−0.0085 (7)	0.0036 (7)
O31	0.0254 (7)	0.0227 (7)	0.0267 (7)	0.0016 (6)	−0.0057 (6)	−0.0004 (6)
O1	0.0187 (6)	0.0271 (7)	0.0220 (7)	−0.0063 (5)	0.0023 (5)	−0.0021 (6)
O2	0.0374 (8)	0.0337 (9)	0.0272 (8)	−0.0031 (7)	0.0085 (6)	0.0033 (7)
O3	0.1016 (18)	0.0296 (10)	0.0598 (14)	−0.0097 (11)	−0.0299 (13)	0.0075 (9)
O4	0.0690 (18)	0.0284 (13)	0.0415 (14)	0.000	0.0211 (13)	0.000

Geometric parameters (Å, º)

Co1—N1	2.0746 (17)	C23—C24	1.387 (3)
Co1—N2	2.0834 (17)	C23—C26	1.505 (2)
Co1—O1	2.1703 (13)	C24—C25	1.387 (3)
Co1—N31	2.1725 (16)	C24—H24	0.9500
Co1—N11	2.1778 (16)	C25—H25	0.9500
Co1—N21	2.2059 (15)	C26—O21	1.244 (2)
N1—C1	1.161 (3)	C26—N22	1.323 (3)
C1—S1	1.6304 (19)	N22—H22A	0.8800
N2—C2	1.164 (3)	N22—H22B	0.8800
C2—S2	1.635 (2)	N31—C31	1.337 (2)
N11—C11	1.335 (3)	N31—C35	1.341 (2)
N11—C15	1.343 (3)	C31—C32	1.382 (3)
C11—C12	1.383 (3)	C31—H31	0.9500
C11—H11	0.9500	C32—C33	1.392 (3)
C12—C13	1.391 (3)	C32—H32	0.9500
C12—H12	0.9500	C33—C34	1.387 (3)
C13—C14	1.389 (3)	C33—C36	1.505 (3)
C13—C16	1.506 (3)	C34—C35	1.384 (3)
C14—C15	1.385 (3)	C34—H34	0.9500
C14—H14	0.9500	C35—H35	0.9500
C15—H15	0.9500	C36—O31	1.238 (2)
C16—O11	1.228 (3)	C36—N32	1.332 (3)
C16—N12	1.327 (3)	N32—H32A	0.8800
N12—H12A	0.8800	N32—H32B	0.8800
N12—H12B	0.8800	O1—H1O1	0.8401
N21—C25	1.345 (2)	O1—H2O1	0.8398
N21—C21	1.347 (2)	O2—H1O2	0.8401
C21—C22	1.386 (3)	O2—H2O2	0.8400
C21—H21	0.9500	O3—H1O3	0.8400
C22—C23	1.384 (3)	O3—H2O3	0.8400
C22—H22	0.9500	O4—H1O4	0.8400
N1—Co1—N2	173.17 (7)	C22—C21—H21	118.5
N1—Co1—O1	85.81 (6)	C23—C22—C21	119.53 (18)
N2—Co1—O1	87.49 (6)	C23—C22—H22	120.2
N1—Co1—N31	89.65 (6)	C21—C22—H22	120.2
N2—Co1—N31	88.90 (6)	C22—C23—C24	118.04 (17)
O1—Co1—N31	88.85 (6)	C22—C23—C26	118.85 (16)
N1—Co1—N11	92.60 (7)	C24—C23—C26	123.08 (17)
N2—Co1—N11	88.83 (7)	C25—C24—C23	118.91 (18)
O1—Co1—N11	91.10 (6)	C25—C24—H24	120.5
N31—Co1—N11	177.74 (6)	C23—C24—H24	120.5
N1—Co1—N21	91.16 (6)	N21—C25—C24	123.68 (17)
N2—Co1—N21	95.51 (6)	N21—C25—H25	118.2
O1—Co1—N21	176.67 (6)	C24—C25—H25	118.2
N31—Co1—N21	89.76 (6)	O21—C26—N22	122.75 (17)
N11—Co1—N21	90.41 (6)	O21—C26—C23	119.55 (17)
C1—N1—Co1	169.72 (16)	N22—C26—C23	117.69 (16)
N1—C1—S1	179.25 (19)	C26—N22—H22A	120.0
C2—N2—Co1	159.31 (16)	C26—N22—H22B	120.0
N2—C2—S2	177.44 (19)	H22A—N22—H22B	120.0
C11—N11—C15	117.13 (17)	C31—N31—C35	117.46 (16)
C11—N11—Co1	123.26 (13)	C31—N31—Co1	120.35 (12)
C15—N11—Co1	119.48 (13)	C35—N31—Co1	121.99 (13)
N11—C11—C12	123.26 (18)	N31—C31—C32	123.31 (17)
N11—C11—H11	118.4	N31—C31—H31	118.3
C12—C11—H11	118.4	C32—C31—H31	118.3
C11—C12—C13	119.55 (19)	C31—C32—C33	119.01 (18)
C11—C12—H12	120.2	C31—C32—H32	120.5
C13—C12—H12	120.2	C33—C32—H32	120.5
C14—C13—C12	117.48 (18)	C34—C33—C32	117.99 (17)
C14—C13—C16	123.79 (18)	C34—C33—C36	118.40 (17)
C12—C13—C16	118.71 (18)	C32—C33—C36	123.60 (17)
C15—C14—C13	119.15 (18)	C35—C34—C33	119.14 (18)
C15—C14—H14	120.4	C35—C34—H34	120.4
C13—C14—H14	120.4	C33—C34—H34	120.4
N11—C15—C14	123.41 (19)	N31—C35—C34	123.07 (18)
N11—C15—H15	118.3	N31—C35—H35	118.5
C14—C15—H15	118.3	C34—C35—H35	118.5
O11—C16—N12	122.13 (19)	O31—C36—N32	122.80 (18)
O11—C16—C13	119.94 (19)	O31—C36—C33	120.18 (17)
N12—C16—C13	117.93 (18)	N32—C36—C33	117.02 (17)
C16—N12—H12A	120.0	C36—N32—H32A	120.0
C16—N12—H12B	120.0	C36—N32—H32B	120.0
H12A—N12—H12B	120.0	H32A—N32—H32B	120.0
C25—N21—C21	116.72 (16)	Co1—O1—H1O1	122.5
C25—N21—Co1	121.72 (12)	Co1—O1—H2O1	123.2
C21—N21—Co1	121.48 (13)	H1O1—O1—H2O1	103.7
N21—C21—C22	123.09 (18)	H1O2—O2—H2O2	107.4
N21—C21—H21	118.5	H1O3—O3—H2O3	105.6

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C11—H11···S2^i	0.95	2.96	3.646 (2)	130
C14—H14···S1^ii	0.95	2.84	3.785 (2)	172
C15—H15···O21^iii	0.95	2.45	3.324 (3)	153
N12—H12A···O31^iv	0.88	2.07	2.922 (2)	163
N12—H12B···S1^ii	0.88	2.74	3.592 (2)	164
C21—H21···N2	0.95	2.65	3.245 (3)	122
C22—H22···O4	0.95	2.49	3.234 (2)	136
C24—H24···O2	0.95	2.58	3.423 (3)	149
C25—H25···N1	0.95	2.49	3.107 (2)	122
N22—H22A···S1^v	0.88	2.79	3.6484 (18)	165
N22—H22B···O2	0.88	2.04	2.873 (2)	158
C32—H32···S2^iii	0.95	3.00	3.826 (2)	146
N32—H32A···O2^vi	0.88	2.25	3.121 (2)	172
N32—H32B···S2^iii	0.88	2.57	3.4083 (19)	160
O1—H1O1···O21^iii	0.84	1.96	2.7858 (19)	166
O1—H2O1···O21^vii	0.84	2.01	2.8106 (19)	158
O2—H1O2···O3^viii	0.84	1.83	2.650 (3)	164
O2—H2O2···N1^ix	0.84	2.60	3.337 (2)	148
O2—H2O2···N31^ix	0.84	2.66	3.363 (2)	143
O3—H1O3···O31	0.84	2.17	2.966 (3)	158
O3—H2O3···O4^x	0.84	2.20	2.963 (2)	152
O4—H1O4···O11^xi	0.84	1.91	2.723 (2)	163

Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x, y, −z+1/2; (iii) −x+1/2, y−1/2, −z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) x+1/2, y+1/2, z; (vi) x, y−1, z; (vii) x−1/2, y−1/2, z; (viii) x, y+1, z; (ix) −x+1/2, −y+3/2, −z+1; (x) −x+1, −y+1, −z+1; (xi) x+1/2, y−1/2, z.