A compressed octa­hedral cobalt(II) complex in the crystal structure of di­aqua­[6,6′-sulfanediylbis(2,2′-bi­pyridine)]cobalt(II) dinitrate

The [Co(C₂₀H₁₄N₄S)(H₂O)₂]²⁺ cation in the title compound possesses pseudo-C_2v point-group symmetry.

Key indicators

• Single-crystal X-ray study
• T = 123 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.042
• wR factor = 0.090
• Data-to-parameter ratio = 15.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         S2 Check
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of         N6 Check
PLAT906_ALERT_3_C Large K value in the Analysis of Variance ......      5.073 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          3 Report

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          6 Note
PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          2 Report
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          4 Note
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          4 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         17 Note
PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          2 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          9 Note

   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
   7 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
   5 ALERT type 3 Indicator that the structure quality may be low
   4 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Diaqua[6,6'-sulfanediylbis(2,2'-bipyridine)]cobalt(II) dinitrate

Crystal data

[Co(C20H14N4S)(H2O)2](NO3)2	F(000) = 1148
Mr = 561.39	Dx = 1.683 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 13.412 (3) Å	Cell parameters from 5682 reflections
b = 11.421 (2) Å	θ = 3.1–27.5°
c = 15.441 (3) Å	µ = 0.93 mm^−1
β = 110.50 (3)°	T = 123 K
V = 2215.4 (9) Å^3	Block, yellow
Z = 4	0.15 × 0.14 × 0.11 mm

Data collection

Rigaku Saturn724 diffractometer	5045 independent reflections
Radiation source: Rotating Anode	3984 reflections with I > 2σ(I)
Detector resolution: 28.5714 pixels mm^-1	Rint = 0.044
dtprofit.ref scans	θmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan (CrystalClear; Rigaku, 2008)	h = −17→17
Tmin = 0.893, Tmax = 1.000	k = −14→10
17851 measured reflections	l = −20→19

Refinement

Refinement on F^2	4 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.042	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.090	w = 1/[σ^2(Fo^2) + (0.040P)^2 + 0.524P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.001
5045 reflections	Δρmax = 0.46 e Å^−3
337 parameters	Δρmin = −0.42 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
S2	0.34784 (7)	0.53580 (6)	0.48067 (4)	0.0421 (2)
Co1	0.24302 (2)	0.43855 (2)	0.24018 (2)	0.01606 (9)
O1	0.39231 (13)	0.40239 (14)	0.23348 (10)	0.0187 (3)
O2	0.09507 (14)	0.47032 (15)	0.24506 (13)	0.0285 (4)
O3	0.50179 (13)	0.23807 (13)	0.35394 (10)	0.0236 (4)
O4	0.54960 (14)	0.06402 (14)	0.40822 (11)	0.0300 (4)
O6	0.05056 (14)	0.33139 (14)	0.36815 (11)	0.0292 (4)
O5	0.47102 (14)	0.08860 (15)	0.26072 (10)	0.0297 (4)
O7	0.02144 (15)	0.14605 (15)	0.36918 (13)	0.0393 (5)
O8	−0.06083 (17)	0.2472 (2)	0.24938 (13)	0.0593 (7)
N5	0.50719 (15)	0.12943 (16)	0.34121 (13)	0.0198 (4)
N6	0.00328 (15)	0.24137 (17)	0.32853 (13)	0.0212 (4)
N2	0.19761 (15)	0.26188 (16)	0.19352 (12)	0.0186 (4)
N4	0.20317 (14)	0.55097 (15)	0.12099 (12)	0.0166 (4)
N3	0.29863 (14)	0.60458 (15)	0.29886 (12)	0.0172 (4)
N1	0.28384 (14)	0.34360 (15)	0.36610 (12)	0.0175 (4)
C7	0.18108 (19)	0.0673 (2)	0.24432 (16)	0.0238 (5)
H7A	0.1923	0.0149	0.2929	0.029*
C8	0.1315 (2)	0.0304 (2)	0.15461 (17)	0.0276 (6)
H8A	0.1085	−0.0466	0.1419	0.033*
C6	0.21437 (17)	0.18271 (19)	0.26220 (14)	0.0176 (5)
C4	0.30035 (18)	0.1515 (2)	0.43295 (15)	0.0229 (5)
H4A	0.2909	0.0711	0.4245	0.027*
C10	0.15035 (19)	0.2232 (2)	0.10636 (16)	0.0250 (5)
H10A	0.1398	0.2763	0.0583	0.030*
C9	0.1167 (2)	0.1098 (2)	0.08414 (16)	0.0280 (6)
H9A	0.0846	0.0871	0.0227	0.034*
C5	0.26838 (17)	0.22627 (19)	0.35760 (15)	0.0179 (5)
C2	0.36036 (19)	0.3163 (2)	0.53060 (16)	0.0242 (5)
H2A	0.3905	0.3495	0.5890	0.029*
C1	0.32874 (18)	0.3862 (2)	0.45197 (15)	0.0214 (5)
C3	0.34627 (19)	0.1974 (2)	0.52047 (16)	0.0262 (5)
H3A	0.3674	0.1486	0.5719	0.031*
C14	0.33856 (18)	0.8009 (2)	0.26565 (16)	0.0220 (5)
H14A	0.3370	0.8578	0.2221	0.026*
C16	0.23741 (17)	0.66245 (19)	0.13919 (14)	0.0175 (5)
C19	0.11790 (19)	0.6048 (2)	−0.03804 (15)	0.0236 (5)
H19A	0.0759	0.5828	−0.0977	0.028*
C17	0.21498 (19)	0.7466 (2)	0.07011 (15)	0.0232 (5)
H17A	0.2403	0.8226	0.0844	0.028*
C20	0.14367 (18)	0.5253 (2)	0.03312 (15)	0.0224 (5)
H20A	0.1184	0.4492	0.0197	0.027*
C11	0.34248 (18)	0.63032 (19)	0.38876 (15)	0.0202 (5)
C15	0.29568 (17)	0.69114 (18)	0.23791 (14)	0.0166 (5)
C18	0.15527 (19)	0.7174 (2)	−0.01954 (15)	0.0242 (5)
H18A	0.1405	0.7726	−0.0666	0.029*
C13	0.38377 (18)	0.8247 (2)	0.35920 (16)	0.0249 (5)
H13A	0.4132	0.8979	0.3793	0.030*
C12	0.38477 (19)	0.7396 (2)	0.42191 (16)	0.0240 (5)
H12B	0.4130	0.7544	0.4851	0.029*
H1WA	0.4237 (19)	0.3504 (18)	0.2663 (15)	0.029*
H1WB	0.4339 (18)	0.4572 (18)	0.2351 (17)	0.029*
H2WA	0.072 (2)	0.430 (2)	0.2791 (15)	0.029*
H2WB	0.0665 (19)	0.5317 (17)	0.2273 (17)	0.029*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S2	0.0871 (6)	0.0210 (3)	0.0148 (3)	0.0028 (4)	0.0135 (3)	−0.0002 (3)
Co1	0.02039 (16)	0.01296 (16)	0.01403 (17)	0.00085 (12)	0.00502 (12)	0.00167 (12)
O1	0.0214 (9)	0.0152 (8)	0.0188 (8)	0.0018 (7)	0.0061 (7)	0.0044 (6)
O2	0.0270 (10)	0.0227 (10)	0.0398 (11)	0.0072 (8)	0.0165 (8)	0.0158 (8)
O3	0.0325 (10)	0.0146 (8)	0.0223 (9)	0.0043 (7)	0.0077 (7)	0.0010 (7)
O4	0.0419 (11)	0.0178 (9)	0.0241 (9)	0.0056 (8)	0.0038 (8)	0.0073 (7)
O6	0.0407 (11)	0.0191 (9)	0.0325 (9)	−0.0100 (8)	0.0186 (8)	−0.0077 (7)
O5	0.0388 (11)	0.0276 (10)	0.0172 (9)	0.0020 (8)	0.0030 (8)	−0.0066 (7)
O7	0.0359 (11)	0.0206 (9)	0.0598 (12)	0.0024 (8)	0.0148 (9)	0.0163 (9)
O8	0.0515 (14)	0.0879 (18)	0.0237 (11)	−0.0330 (13)	−0.0057 (10)	0.0093 (11)
N5	0.0200 (10)	0.0177 (10)	0.0228 (10)	−0.0004 (8)	0.0087 (8)	−0.0011 (8)
N6	0.0193 (10)	0.0231 (11)	0.0231 (11)	0.0000 (8)	0.0097 (9)	0.0003 (9)
N2	0.0214 (10)	0.0158 (9)	0.0173 (10)	−0.0014 (8)	0.0052 (8)	0.0008 (8)
N4	0.0178 (9)	0.0159 (9)	0.0149 (9)	−0.0006 (8)	0.0041 (7)	0.0011 (7)
N3	0.0192 (9)	0.0161 (9)	0.0150 (9)	0.0023 (8)	0.0045 (8)	−0.0006 (8)
N1	0.0206 (10)	0.0162 (10)	0.0164 (9)	0.0025 (8)	0.0075 (8)	0.0027 (8)
C7	0.0293 (13)	0.0169 (12)	0.0281 (13)	−0.0005 (10)	0.0139 (11)	0.0028 (10)
C8	0.0337 (14)	0.0179 (12)	0.0329 (14)	−0.0062 (11)	0.0138 (11)	−0.0031 (10)
C6	0.0184 (11)	0.0155 (11)	0.0213 (12)	0.0029 (9)	0.0102 (9)	0.0037 (9)
C4	0.0254 (12)	0.0184 (12)	0.0254 (13)	0.0023 (10)	0.0095 (10)	0.0076 (10)
C10	0.0328 (14)	0.0204 (12)	0.0197 (12)	−0.0018 (11)	0.0064 (10)	0.0029 (10)
C9	0.0340 (14)	0.0250 (13)	0.0227 (13)	−0.0054 (11)	0.0071 (11)	−0.0035 (10)
C5	0.0188 (11)	0.0164 (11)	0.0219 (12)	0.0012 (9)	0.0113 (9)	0.0032 (9)
C2	0.0275 (13)	0.0272 (13)	0.0172 (12)	0.0040 (11)	0.0069 (10)	0.0031 (10)
C1	0.0252 (12)	0.0202 (12)	0.0198 (12)	0.0029 (10)	0.0091 (10)	0.0011 (10)
C3	0.0288 (13)	0.0283 (14)	0.0207 (12)	0.0032 (11)	0.0079 (10)	0.0112 (10)
C14	0.0214 (12)	0.0185 (12)	0.0251 (13)	−0.0028 (10)	0.0070 (10)	0.0014 (10)
C16	0.0165 (11)	0.0173 (12)	0.0182 (11)	0.0013 (9)	0.0055 (9)	0.0021 (9)
C19	0.0265 (13)	0.0253 (13)	0.0149 (11)	0.0013 (10)	0.0019 (10)	0.0008 (10)
C17	0.0315 (13)	0.0155 (11)	0.0222 (12)	−0.0021 (10)	0.0089 (10)	0.0022 (9)
C20	0.0271 (13)	0.0169 (12)	0.0187 (12)	−0.0019 (10)	0.0023 (10)	−0.0008 (9)
C11	0.0227 (12)	0.0185 (12)	0.0183 (12)	0.0050 (10)	0.0057 (9)	0.0006 (9)
C15	0.0176 (11)	0.0145 (11)	0.0174 (11)	0.0024 (9)	0.0059 (9)	0.0017 (9)
C18	0.0296 (13)	0.0239 (13)	0.0172 (12)	0.0022 (10)	0.0059 (10)	0.0091 (10)
C13	0.0235 (12)	0.0196 (12)	0.0284 (13)	−0.0027 (10)	0.0051 (10)	−0.0065 (10)
C12	0.0264 (13)	0.0244 (13)	0.0172 (12)	0.0011 (10)	0.0027 (10)	−0.0068 (10)

Geometric parameters (Å, º)

S2—C1	1.761 (2)	N1—C1	1.341 (3)
S2—C11	1.764 (2)	N1—C5	1.355 (3)
Co1—O2	2.0444 (18)	C7—C8	1.376 (3)
Co1—O1	2.0821 (17)	C7—C6	1.388 (3)
Co1—N3	2.1213 (18)	C8—C9	1.376 (3)
Co1—N1	2.1238 (17)	C6—C5	1.481 (3)
Co1—N4	2.1523 (18)	C4—C3	1.377 (3)
Co1—N2	2.1574 (18)	C4—C5	1.384 (3)
O3—N5	1.262 (2)	C10—C9	1.375 (3)
O4—N5	1.241 (2)	C2—C3	1.373 (3)
O6—N6	1.250 (2)	C2—C1	1.390 (3)
O5—N5	1.255 (2)	C14—C15	1.383 (3)
O7—N6	1.238 (2)	C14—C13	1.384 (3)
O8—N6	1.225 (2)	C16—C17	1.388 (3)
N2—C10	1.346 (3)	C16—C15	1.486 (3)
N2—C6	1.351 (3)	C19—C20	1.373 (3)
N4—C20	1.344 (3)	C19—C18	1.373 (3)
N4—C16	1.349 (3)	C17—C18	1.376 (3)
N3—C11	1.337 (3)	C11—C12	1.392 (3)
N3—C15	1.356 (3)	C13—C12	1.369 (3)
C1—S2—C11	115.45 (11)	C5—N1—Co1	115.76 (14)
O2—Co1—O1	178.59 (7)	C8—C7—C6	120.0 (2)
O2—Co1—N3	91.50 (7)	C7—C8—C9	118.6 (2)
O1—Co1—N3	89.90 (7)	N2—C6—C7	121.7 (2)
O2—Co1—N1	89.95 (7)	N2—C6—C5	116.40 (19)
O1—Co1—N1	90.02 (7)	C7—C6—C5	121.9 (2)
N3—Co1—N1	97.24 (7)	C3—C4—C5	119.4 (2)
O2—Co1—N4	88.40 (7)	N2—C10—C9	123.9 (2)
O1—Co1—N4	91.77 (7)	C10—C9—C8	118.7 (2)
N3—Co1—N4	77.10 (7)	N1—C5—C4	122.4 (2)
N1—Co1—N4	174.06 (7)	N1—C5—C6	115.68 (18)
O2—Co1—N2	90.81 (7)	C4—C5—C6	121.9 (2)
O1—Co1—N2	87.81 (7)	C3—C2—C1	118.8 (2)
N3—Co1—N2	174.08 (7)	N1—C1—C2	123.3 (2)
N1—Co1—N2	77.31 (7)	N1—C1—S2	125.20 (17)
N4—Co1—N2	108.41 (7)	C2—C1—S2	111.39 (17)
O4—N5—O5	120.48 (18)	C2—C3—C4	119.0 (2)
O4—N5—O3	119.77 (18)	C15—C14—C13	119.0 (2)
O5—N5—O3	119.74 (18)	N4—C16—C17	121.8 (2)
O8—N6—O7	119.9 (2)	N4—C16—C15	116.12 (18)
O8—N6—O6	120.1 (2)	C17—C16—C15	122.0 (2)
O7—N6—O6	119.96 (19)	C20—C19—C18	118.8 (2)
C10—N2—C6	117.12 (19)	C18—C17—C16	119.9 (2)
C10—N2—Co1	128.32 (15)	N4—C20—C19	123.9 (2)
C6—N2—Co1	114.45 (14)	N3—C11—C12	123.6 (2)
C20—N4—C16	117.03 (18)	N3—C11—S2	125.44 (17)
C20—N4—Co1	127.97 (15)	C12—C11—S2	110.88 (16)
C16—N4—Co1	114.86 (13)	N3—C15—C14	122.5 (2)
C11—N3—C15	117.11 (19)	N3—C15—C16	115.36 (19)
C11—N3—Co1	126.95 (15)	C14—C15—C16	122.0 (2)
C15—N3—Co1	115.77 (14)	C19—C18—C17	118.6 (2)
C1—N1—C5	117.09 (18)	C12—C13—C14	119.4 (2)
C1—N1—Co1	127.03 (15)	C13—C12—C11	118.4 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2WB···O7^i	0.80 (2)	2.02 (2)	2.766 (3)	155 (2)
O2—H2WA···O6	0.84 (2)	1.88 (2)	2.698 (2)	168 (3)
O1—H1WB···O5^ii	0.83 (2)	1.96 (2)	2.789 (2)	179 (3)
O1—H1WA···O3	0.80 (2)	1.89 (2)	2.688 (2)	174 (3)

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