Di­aqua­diiso­thio­cyanato­bis­(pyridine N-oxide)­cobalt(II)

In the title mononuclear complex, [Co(NCS)₂(C₅H₅NO)₂(H₂O)₂], cobalt(II) has a distorted octahedral coordination formed by two N atoms from two thio­cyanate anions and four O atoms from two water mol­ecules and two pyridine N-oxide mol­ecules. The complexes are connected to each other by O—H...O and O—H...S hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.007 Å
• R factor = 0.043
• wR factor = 0.124
• Data-to-parameter ratio = 13.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Co1    -   N2      ..       5.06 su
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C11
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          7
PLAT354_ALERT_3_C Short   O-H Bond (0.82A)   O2     -   H13    ...       0.71 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          5
            O2  -CO1 -O4  -N3    167.00  3.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #          9
            O1  -CO1 -O3  -N4   -115.00  0.60   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         11
            N2  -CO1 -N1  -C12   -19.70  1.60   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         20
            N1  -CO1 -N2  -C11    -4.80  1.90   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         25
            CO1 -N2  -C11 -S1    150.00  9.00   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         26
            CO1 -N1  -C12 -S2     88.00 12.00   1.555   1.555   1.555   1.555

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
   7 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

Diaquadiisothiocyanatobis(pyridine N-oxide)cobalt(II)

Crystal data

[Co(NCS)2(C5H5NO)2(H2O)2]	Z = 2
Mr = 401.32	F(000) = 410
Triclinic, P1	Dx = 1.598 Mg m^−3
a = 5.4773 (15) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.326 (3) Å	Cell parameters from 1753 reflections
c = 13.726 (4) Å	θ = 2.4–26.3°
α = 86.366 (4)°	µ = 1.30 mm^−1
β = 78.985 (4)°	T = 298 K
γ = 88.921 (4)°	Prism, pink
V = 834.1 (4) Å^3	0.20 × 0.09 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer	2892 independent reflections
Radiation source: fine-focus sealed tube	2582 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.022
φ and ω scans	θmax = 25.0°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −6→6
Tmin = 0.781, Tmax = 0.903	k = −11→13
4291 measured reflections	l = −16→16

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)] = 0.043	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.124	H-atom parameters constrained
S = 1.14	w = 1/[σ^2(Fo^2) + (0.046P)^2 + 1.1096P] where P = (Fo^2 + 2Fc^2)/3
2892 reflections	(Δ/σ)max = 0.001
212 parameters	Δρmax = 0.35 e Å^−3
0 restraints	Δρmin = −0.31 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
Co1	0.44658 (9)	0.28224 (4)	0.60217 (3)	0.02712 (18)
S2	0.0731 (2)	0.21153 (13)	0.32869 (9)	0.0523 (3)
S1	0.4233 (3)	0.25529 (14)	0.95619 (9)	0.0619 (4)
O2	0.7303 (5)	0.4132 (2)	0.5564 (2)	0.0348 (6)
H14	0.8951	0.4039	0.5760	0.071 (17)*
H13	0.7685	0.4367	0.5067	0.047 (16)*
O4	0.1655 (5)	0.1555 (3)	0.6421 (2)	0.0391 (7)
O3	0.1903 (5)	0.4272 (2)	0.62044 (19)	0.0322 (6)
O1	0.7376 (5)	0.1553 (2)	0.5647 (2)	0.0369 (7)
H11	0.8119	0.1548	0.5025	0.08 (2)*
H12	0.8767	0.1601	0.5884	0.033 (11)*
N1	0.3561 (7)	0.2783 (3)	0.4642 (2)	0.0394 (8)
N3	0.1589 (6)	0.0778 (3)	0.7206 (2)	0.0301 (7)
N4	0.1620 (6)	0.4809 (3)	0.7071 (2)	0.0291 (7)
N2	0.4863 (6)	0.2777 (3)	0.7496 (3)	0.0338 (8)
C11	0.4555 (7)	0.2690 (3)	0.8359 (3)	0.0309 (9)
C12	0.2408 (7)	0.2491 (3)	0.4075 (3)	0.0317 (9)
C7	−0.0436 (8)	0.4612 (4)	0.7753 (3)	0.0409 (10)
H7	−0.1653	0.4108	0.7633	0.049*
C5	−0.0399 (8)	0.0761 (4)	0.7936 (3)	0.0410 (10)
H5	−0.1690	0.1299	0.7905	0.049*
C8	0.3418 (8)	0.5504 (4)	0.7235 (3)	0.0362 (9)
H8	0.4842	0.5625	0.6750	0.043*
C9	0.3171 (9)	0.6043 (4)	0.8120 (3)	0.0448 (11)
H9	0.4435	0.6518	0.8240	0.054*
C1	0.3473 (8)	0.0019 (4)	0.7242 (3)	0.0390 (10)
H1	0.4839	0.0028	0.6722	0.047*
C3	0.1345 (10)	−0.0812 (4)	0.8791 (3)	0.0483 (12)
H3	0.1264	−0.1359	0.9331	0.058*
C6	−0.0745 (9)	0.5159 (5)	0.8635 (3)	0.0505 (12)
H6	−0.2196	0.5038	0.9106	0.061*
C2	0.3393 (9)	−0.0765 (4)	0.8040 (4)	0.0472 (11)
H2	0.4733	−0.1273	0.8075	0.057*
C4	−0.0556 (9)	−0.0045 (4)	0.8734 (3)	0.0452 (11)
H4	−0.1966	−0.0066	0.9234	0.054*
C10	0.1043 (10)	0.5871 (4)	0.8824 (3)	0.0491 (12)
H10	0.0834	0.6239	0.9422	0.059*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0227 (3)	0.0334 (3)	0.0253 (3)	−0.0027 (2)	−0.0056 (2)	0.0020 (2)
S2	0.0449 (7)	0.0751 (9)	0.0429 (6)	−0.0020 (6)	−0.0192 (5)	−0.0148 (6)
S1	0.0697 (9)	0.0853 (10)	0.0277 (6)	0.0041 (7)	−0.0031 (6)	0.0006 (6)
O2	0.0278 (15)	0.0427 (17)	0.0327 (16)	−0.0097 (12)	−0.0058 (12)	0.0091 (13)
O4	0.0300 (15)	0.0459 (17)	0.0426 (16)	−0.0115 (13)	−0.0145 (13)	0.0166 (13)
O3	0.0283 (14)	0.0387 (15)	0.0303 (14)	0.0022 (11)	−0.0076 (11)	−0.0032 (11)
O1	0.0215 (14)	0.0484 (17)	0.0393 (17)	0.0016 (12)	−0.0034 (12)	−0.0006 (13)
N1	0.039 (2)	0.051 (2)	0.0283 (18)	−0.0117 (17)	−0.0077 (16)	0.0029 (15)
N3	0.0276 (17)	0.0297 (17)	0.0335 (17)	−0.0059 (13)	−0.0092 (14)	0.0050 (13)
N4	0.0259 (17)	0.0294 (17)	0.0313 (17)	0.0008 (13)	−0.0056 (13)	0.0035 (13)
N2	0.0315 (18)	0.0343 (18)	0.036 (2)	−0.0018 (14)	−0.0093 (15)	0.0022 (14)
C11	0.026 (2)	0.032 (2)	0.034 (2)	0.0012 (16)	−0.0063 (16)	0.0028 (16)
C12	0.030 (2)	0.036 (2)	0.027 (2)	−0.0013 (17)	0.0000 (17)	0.0018 (16)
C7	0.026 (2)	0.055 (3)	0.040 (2)	−0.0048 (19)	−0.0032 (18)	0.003 (2)
C5	0.034 (2)	0.043 (2)	0.044 (2)	0.0026 (19)	−0.0051 (19)	−0.0011 (19)
C8	0.030 (2)	0.035 (2)	0.041 (2)	−0.0023 (17)	−0.0023 (17)	0.0026 (17)
C9	0.051 (3)	0.035 (2)	0.051 (3)	−0.002 (2)	−0.015 (2)	−0.006 (2)
C1	0.027 (2)	0.036 (2)	0.051 (3)	−0.0026 (17)	−0.0023 (18)	0.0017 (19)
C3	0.063 (3)	0.042 (3)	0.041 (2)	−0.008 (2)	−0.016 (2)	0.011 (2)
C6	0.039 (3)	0.067 (3)	0.038 (2)	0.003 (2)	0.008 (2)	0.005 (2)
C2	0.043 (3)	0.035 (2)	0.063 (3)	0.0018 (19)	−0.014 (2)	0.007 (2)
C4	0.047 (3)	0.050 (3)	0.036 (2)	−0.003 (2)	−0.001 (2)	0.002 (2)
C10	0.062 (3)	0.048 (3)	0.038 (2)	0.011 (2)	−0.012 (2)	−0.008 (2)

Geometric parameters (Å, º)

Co1—N1	2.051 (3)	N2—C11	1.162 (5)
Co1—N2	2.074 (3)	C7—C6	1.375 (6)
Co1—O4	2.096 (3)	C7—H7	0.9300
Co1—O3	2.136 (3)	C5—C4	1.371 (6)
Co1—O1	2.137 (3)	C5—H5	0.9300
Co1—O2	2.146 (3)	C8—C9	1.377 (6)
S2—C12	1.627 (4)	C8—H8	0.9300
S1—C11	1.624 (4)	C9—C10	1.373 (7)
O2—H14	0.9924	C9—H9	0.9300
O2—H13	0.7105	C1—C2	1.360 (6)
O4—N3	1.342 (4)	C1—H1	0.9300
O3—N4	1.352 (4)	C3—C4	1.354 (7)
O1—H11	0.8727	C3—C2	1.371 (7)
O1—H12	0.8882	C3—H3	0.9300
N1—C12	1.158 (5)	C6—C10	1.353 (7)
N3—C5	1.331 (5)	C6—H6	0.9300
N3—C1	1.337 (5)	C2—H2	0.9300
N4—C7	1.332 (5)	C4—H4	0.9300
N4—C8	1.332 (5)	C10—H10	0.9300
N1—Co1—N2	171.72 (13)	N1—C12—S2	178.2 (4)
N1—Co1—O4	83.60 (12)	N4—C7—C6	119.5 (4)
N2—Co1—O4	88.86 (12)	N4—C7—H7	120.3
N1—Co1—O3	84.51 (13)	C6—C7—H7	120.3
N2—Co1—O3	92.54 (12)	N3—C5—C4	120.4 (4)
O4—Co1—O3	93.28 (11)	N3—C5—H5	119.8
N1—Co1—O1	91.21 (13)	C4—C5—H5	119.8
N2—Co1—O1	92.80 (12)	N4—C8—C9	120.2 (4)
O4—Co1—O1	94.57 (12)	N4—C8—H8	119.9
O3—Co1—O1	170.59 (10)	C9—C8—H8	119.9
N1—Co1—O2	94.44 (12)	C10—C9—C8	119.4 (4)
N2—Co1—O2	93.08 (12)	C10—C9—H9	120.3
O4—Co1—O2	178.00 (10)	C8—C9—H9	120.3
O3—Co1—O2	86.15 (11)	N3—C1—C2	120.0 (4)
O1—Co1—O2	85.83 (11)	N3—C1—H1	120.0
Co1—O2—H14	121.1	C2—C1—H1	120.0
Co1—O2—H13	124.3	C4—C3—C2	118.7 (4)
H14—O2—H13	99.5	C4—C3—H3	120.6
N3—O4—Co1	121.9 (2)	C2—C3—H3	120.6
N4—O3—Co1	116.8 (2)	C10—C6—C7	120.6 (4)
Co1—O1—H11	117.5	C10—C6—H6	119.7
Co1—O1—H12	119.7	C7—C6—H6	119.7
H11—O1—H12	95.2	C1—C2—C3	120.3 (4)
C12—N1—Co1	154.8 (3)	C1—C2—H2	119.9
C5—N3—C1	120.6 (3)	C3—C2—H2	119.9
C5—N3—O4	119.0 (3)	C3—C4—C5	119.9 (4)
C1—N3—O4	120.3 (3)	C3—C4—H4	120.1
C7—N4—C8	121.4 (4)	C5—C4—H4	120.1
C7—N4—O3	119.1 (3)	C6—C10—C9	119.0 (4)
C8—N4—O3	119.5 (3)	C6—C10—H10	120.5
C11—N2—Co1	165.5 (3)	C9—C10—H10	120.5
N2—C11—S1	177.9 (4)
N1—Co1—O4—N3	156.1 (3)	O3—Co1—N2—C11	64.1 (13)
N2—Co1—O4—N3	−27.3 (3)	O1—Co1—N2—C11	−123.6 (13)
O3—Co1—O4—N3	−119.8 (3)	O2—Co1—N2—C11	150.4 (13)
O1—Co1—O4—N3	65.4 (3)	Co1—N2—C11—S1	150 (9)
O2—Co1—O4—N3	167 (3)	Co1—N1—C12—S2	88 (12)
N1—Co1—O3—N4	−178.2 (2)	C8—N4—C7—C6	1.7 (6)
N2—Co1—O3—N4	9.6 (2)	O3—N4—C7—C6	−179.7 (4)
O4—Co1—O3—N4	98.6 (2)	C1—N3—C5—C4	−0.6 (6)
O1—Co1—O3—N4	−115.0 (6)	O4—N3—C5—C4	178.1 (4)
O2—Co1—O3—N4	−83.4 (2)	C7—N4—C8—C9	−0.4 (6)
N2—Co1—N1—C12	−19.7 (16)	O3—N4—C8—C9	−179.0 (4)
O4—Co1—N1—C12	4.8 (8)	N4—C8—C9—C10	−1.0 (7)
O3—Co1—N1—C12	−89.1 (8)	C5—N3—C1—C2	−1.3 (6)
O1—Co1—N1—C12	99.3 (8)	O4—N3—C1—C2	−180.0 (4)
O2—Co1—N1—C12	−174.8 (8)	N4—C7—C6—C10	−1.6 (7)
Co1—O4—N3—C5	121.1 (3)	N3—C1—C2—C3	2.4 (7)
Co1—O4—N3—C1	−60.2 (4)	C4—C3—C2—C1	−1.5 (7)
Co1—O3—N4—C7	−105.3 (3)	C2—C3—C4—C5	−0.4 (7)
Co1—O3—N4—C8	73.3 (4)	N3—C5—C4—C3	1.5 (7)
N1—Co1—N2—C11	−4.8 (19)	C7—C6—C10—C9	0.2 (7)
O4—Co1—N2—C11	−29.1 (13)	C8—C9—C10—C6	1.1 (7)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11···S2^i	0.87	2.59	3.433 (3)	164
O1—H12···O4^i	0.89	1.87	2.753 (4)	175
O2—H14···O3^i	0.99	1.86	2.833 (4)	165
O2—H13···O3^ii	0.71	2.23	2.901 (4)	157

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