Diaqua­sulfato(2,4,6-tri-2-pyridyl-1,3,5-triazine)nickel(II) dihydrate

Díaz de Vivar, M.E.; Baggio, S.; Baggio, R.

doi:10.1107/S1600536806011640

Buy article online - an online subscription or single-article purchase is required to access this article.

Diaquasulfato(2,4,6-tri-2-pyridyl-1,3,5-triazine)nickel(II) dihydrate

M. E. Díaz de Vivar, S. Baggio and R. Baggio

The title compound, [Ni(SO₄)(C₁₈H₁₂N₆)(H₂O)₂]·2H₂O, is isostructural with the zinc and cobalt analogues already reported in the literature. The compound is monomeric, with an octahedral Ni centre coordinated by a tridentate 2,4,6-tri-2-pyridyl-1,3,5-triazine ligand, two water molecules and a monodentate sulfate ligand. The presence of two additional water molecules of crystallization leads to a total of eight hydrogen-bond donors, from which a very complex hydrogen-bonding scheme is built up.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806011640/bt2030sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806011640/bt2030Isup2.hkl Contains datablock I

CCDC reference: 608370

checkCIF report

Key indicators

Single-crystal X-ray study
T = 295 K
Mean (C-C) = 0.005 Å
R factor = 0.053
wR factor = 0.119
Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          8

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

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: MSC/AFC Diffractometer Control Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-NT (Bruker, 2000); software used to prepare material for publication: SHELXTL-NT (Bruker, 2000) and PLATON (Spek, 2005).

Diaquasulfato(2,4,6-tri-2-pyridyl-1,3,5-triazine)nickel(II) dihydrate top

Crystal data top

[Ni(SO₄)(C₁₈H₁₂N₆)(H₂O)₂]·2H₂O	Z = 2
M_r = 539.17	F(000) = 556
Triclinic, P1	D_x = 1.720 Mg m⁻³
Hall symbol: -P_1	Mo Kα radiation, λ = 0.71073 Å
a = 7.6338 (15) Å	Cell parameters from 25 reflections
b = 11.681 (2) Å	θ = 7.5–17.5°
c = 12.420 (2) Å	µ = 1.10 mm⁻¹
α = 85.513 (3)°	T = 295 K
β = 75.529 (3)°	Prisms, green
γ = 76.129 (3)°	0.28 × 0.14 × 0.10 mm
V = 1040.9 (3) Å³

Data collection top

Rigaku AFC-6 diffractometer	3405 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.063
Graphite monochromator	θ_max = 28.0°, θ_min = 1.7°
ω/2θ scans	h = −9→9
Absorption correction: ψ scan (North et al., 1968)	k = −15→15
T_min = 0.75, T_max = 0.90	l = −2→16
4980 measured reflections	3 standard reflections every 150 reflections
4438 independent reflections	intensity decay: <2%

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.053	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.119	H atoms treated by a mixture of independent and constrained refinement
S = 0.97	w = 1/[σ²(F_o²) + (0.0697P)²] where P = (F_o² + 2F_c²)/3
4438 reflections	(Δ/σ)_max < 0.001
331 parameters	Δρ_max = 0.53 e Å⁻³
24 restraints	Δρ_min = −0.39 e Å⁻³

Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.43706 (6)	0.26097 (4)	0.22524 (4)	0.02134 (14)
S	0.81989 (12)	0.19084 (8)	0.31447 (7)	0.0248 (2)
O1	0.6689 (3)	0.1646 (2)	0.2732 (2)	0.0323 (6)
O2	0.8604 (3)	0.3021 (2)	0.2641 (2)	0.0365 (6)
O3	0.7627 (5)	0.2011 (3)	0.4348 (2)	0.0521 (8)
O4	0.9853 (3)	0.0941 (2)	0.2826 (2)	0.0391 (7)
N1	0.5919 (4)	0.2458 (2)	0.0528 (2)	0.0250 (6)
N2	0.5264 (4)	0.4086 (2)	0.1934 (2)	0.0235 (6)
N3	0.3250 (4)	0.3505 (3)	0.3782 (2)	0.0279 (7)
N4	0.7044 (4)	0.5247 (2)	0.0737 (2)	0.0252 (6)
N5	0.5516 (4)	0.5842 (2)	0.2596 (2)	0.0270 (7)
N6	0.8079 (4)	0.7343 (3)	0.0353 (3)	0.0314 (7)
C1	0.6176 (5)	0.1596 (3)	−0.0180 (3)	0.0311 (9)
H1	0.5655	0.0953	0.0076	0.037*
C2	0.7171 (5)	0.1610 (4)	−0.1265 (3)	0.0364 (9)
H2	0.7328	0.0988	−0.1729	0.044*
C3	0.7921 (5)	0.2550 (4)	−0.1645 (3)	0.0373 (9)
H3	0.8578	0.2580	−0.2382	0.045*
C4	0.7717 (5)	0.3462 (3)	−0.0947 (3)	0.0283 (8)
H4	0.8230	0.4109	−0.1196	0.034*
C5	0.6727 (5)	0.3373 (3)	0.0128 (3)	0.0241 (7)
C6	0.6345 (4)	0.4289 (3)	0.0972 (3)	0.0219 (7)
C7	0.6572 (5)	0.5993 (3)	0.1581 (3)	0.0278 (8)
C8	0.4874 (5)	0.4869 (3)	0.2727 (3)	0.0225 (7)
C9	0.3673 (5)	0.4568 (3)	0.3776 (3)	0.0252 (7)
C10	0.2990 (5)	0.5290 (3)	0.4687 (3)	0.0309 (8)
H10	0.3270	0.6026	0.4658	0.037*
C11	0.1892 (5)	0.4912 (4)	0.5638 (3)	0.0355 (9)
H11	0.1429	0.5382	0.6263	0.043*
C12	0.1497 (5)	0.3830 (4)	0.5642 (3)	0.0394 (10)
H12	0.0753	0.3557	0.6274	0.047*
C13	0.2199 (5)	0.3148 (4)	0.4714 (3)	0.0348 (9)
H13	0.1933	0.2409	0.4735	0.042*
C14	0.7219 (5)	0.7110 (3)	0.1390 (3)	0.0272 (8)
C15	0.6859 (5)	0.7884 (3)	0.2269 (3)	0.0349 (9)
H15	0.6230	0.7702	0.2981	0.042*
C16	0.7458 (6)	0.8915 (3)	0.2050 (4)	0.0404 (10)
H16	0.7273	0.9440	0.2615	0.049*
C17	0.8323 (6)	0.9152 (4)	0.0995 (4)	0.0420 (10)
H17	0.8725	0.9851	0.0829	0.050*
C18	0.8612 (6)	0.8366 (3)	0.0168 (4)	0.0383 (10)
H18	0.9203	0.8552	−0.0551	0.046*
O1W	0.3417 (4)	0.1102 (2)	0.2522 (2)	0.0348 (6)
H1WA	0.382 (3)	0.0739 (15)	0.3035 (17)	0.042*
H1WB	0.2285 (5)	0.1291 (11)	0.274 (2)	0.042*
O2W	0.1963 (3)	0.3468 (2)	0.1740 (2)	0.0335 (6)
H2WB	0.205 (2)	0.335 (2)	0.1086 (7)	0.040*
H2WA	0.1054 (13)	0.324 (2)	0.2104 (17)	0.040*
O3W	0.9979 (5)	0.1233 (3)	0.5900 (3)	0.0673 (10)
H3WA	0.915 (3)	0.168 (3)	0.566 (3)	0.081*
H3WB	0.946 (4)	0.080 (3)	0.636 (3)	0.081*
O4W	0.3827 (7)	−0.0232 (4)	0.4402 (3)	0.0869 (14)
H4WB	0.301 (5)	0.017 (3)	0.488 (4)	0.104*
H4WA	0.364 (7)	−0.0898 (17)	0.451 (4)	0.104*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.0206 (2)	0.0215 (2)	0.0252 (3)	−0.00938 (17)	−0.00710 (17)	−0.00073 (17)
S	0.0237 (5)	0.0252 (4)	0.0297 (5)	−0.0096 (3)	−0.0107 (4)	0.0021 (4)
O1	0.0269 (13)	0.0266 (13)	0.0504 (17)	−0.0101 (11)	−0.0193 (12)	0.0019 (12)
O2	0.0271 (14)	0.0260 (14)	0.0635 (19)	−0.0140 (11)	−0.0181 (13)	0.0061 (12)
O3	0.071 (2)	0.059 (2)	0.0340 (17)	−0.0265 (17)	−0.0150 (15)	−0.0027 (14)
O4	0.0260 (14)	0.0312 (14)	0.0627 (19)	−0.0087 (11)	−0.0140 (13)	0.0017 (13)
N1	0.0253 (16)	0.0223 (15)	0.0287 (16)	−0.0029 (12)	−0.0099 (12)	−0.0059 (12)
N2	0.0200 (15)	0.0251 (15)	0.0274 (16)	−0.0074 (12)	−0.0071 (12)	0.0001 (12)
N3	0.0244 (16)	0.0337 (17)	0.0272 (17)	−0.0111 (13)	−0.0062 (12)	0.0035 (13)
N4	0.0264 (16)	0.0206 (15)	0.0313 (17)	−0.0098 (12)	−0.0081 (12)	0.0011 (12)
N5	0.0381 (18)	0.0158 (14)	0.0320 (17)	−0.0095 (13)	−0.0144 (14)	0.0010 (12)
N6	0.0356 (18)	0.0307 (17)	0.0366 (18)	−0.0190 (14)	−0.0157 (14)	0.0063 (14)
C1	0.031 (2)	0.0243 (19)	0.046 (2)	−0.0090 (15)	−0.0209 (17)	−0.0040 (17)
C2	0.041 (2)	0.042 (2)	0.031 (2)	−0.0054 (19)	−0.0180 (18)	−0.0105 (17)
C3	0.034 (2)	0.051 (3)	0.022 (2)	−0.0068 (19)	−0.0017 (16)	−0.0029 (17)
C4	0.0245 (18)	0.0293 (19)	0.031 (2)	−0.0035 (15)	−0.0089 (15)	0.0008 (15)
C5	0.0237 (18)	0.0236 (18)	0.0254 (19)	−0.0047 (14)	−0.0076 (14)	−0.0002 (14)
C6	0.0231 (17)	0.0218 (16)	0.0267 (19)	−0.0100 (14)	−0.0139 (14)	0.0057 (14)
C7	0.033 (2)	0.0188 (17)	0.034 (2)	−0.0090 (15)	−0.0117 (16)	0.0049 (15)
C8	0.0253 (18)	0.0196 (17)	0.0273 (19)	−0.0074 (14)	−0.0140 (14)	0.0036 (14)
C9	0.0193 (17)	0.0298 (19)	0.0295 (19)	−0.0077 (14)	−0.0088 (14)	−0.0026 (15)
C10	0.032 (2)	0.036 (2)	0.027 (2)	−0.0089 (16)	−0.0091 (16)	−0.0023 (16)
C11	0.033 (2)	0.044 (2)	0.028 (2)	−0.0005 (18)	−0.0094 (16)	−0.0113 (17)
C12	0.035 (2)	0.063 (3)	0.021 (2)	−0.015 (2)	−0.0051 (16)	0.0049 (18)
C13	0.036 (2)	0.039 (2)	0.033 (2)	−0.0184 (18)	−0.0088 (17)	0.0074 (17)
C14	0.0280 (19)	0.0182 (17)	0.043 (2)	−0.0116 (14)	−0.0176 (16)	0.0050 (15)
C15	0.040 (2)	0.028 (2)	0.043 (2)	−0.0091 (17)	−0.0202 (18)	−0.0013 (17)
C16	0.044 (2)	0.027 (2)	0.061 (3)	−0.0145 (18)	−0.026 (2)	−0.0050 (19)
C17	0.045 (2)	0.033 (2)	0.058 (3)	−0.0172 (19)	−0.027 (2)	0.015 (2)
C18	0.042 (2)	0.036 (2)	0.043 (2)	−0.0185 (18)	−0.0177 (19)	0.0159 (19)
O1W	0.0310 (14)	0.0275 (14)	0.0521 (18)	−0.0125 (12)	−0.0171 (13)	0.0045 (12)
O2W	0.0238 (13)	0.0392 (15)	0.0384 (15)	−0.0093 (12)	−0.0098 (11)	0.0071 (12)
O3W	0.083 (3)	0.071 (3)	0.065 (2)	−0.042 (2)	−0.035 (2)	0.0259 (19)
O4W	0.132 (4)	0.093 (3)	0.071 (3)	−0.072 (3)	−0.058 (3)	0.044 (2)

Geometric parameters (Å, º) top

Ni—N2	1.979 (3)	C4—H4	0.9300
Ni—O1W	2.036 (2)	C5—C6	1.484 (5)
Ni—O1	2.055 (2)	C7—C14	1.485 (4)
Ni—O2W	2.095 (2)	C8—C9	1.466 (5)
Ni—N3	2.123 (3)	C9—C10	1.381 (5)
Ni—N1	2.170 (3)	C10—C11	1.376 (5)
S—O3	1.455 (3)	C10—H10	0.9300
S—O2	1.465 (2)	C11—C12	1.367 (6)
S—O4	1.471 (3)	C11—H11	0.9300
S—O1	1.475 (2)	C12—C13	1.372 (6)
N1—C1	1.335 (4)	C12—H12	0.9300
N1—C5	1.360 (4)	C13—H13	0.9300
N2—C6	1.312 (4)	C14—C15	1.403 (5)
N2—C8	1.326 (4)	C15—C16	1.374 (5)
N3—C13	1.333 (4)	C15—H15	0.9300
N3—C9	1.355 (4)	C16—C17	1.352 (6)
N4—C6	1.334 (4)	C16—H16	0.9300
N4—C7	1.339 (4)	C17—C18	1.372 (6)
N5—C8	1.325 (4)	C17—H17	0.9300
N5—C7	1.340 (4)	C18—H18	0.9300
N6—C14	1.331 (5)	O1W—H1WA	0.82 (3)
N6—C18	1.338 (5)	O1W—H1WB	0.82 (2)
C1—C2	1.372 (5)	O2W—H2WA	0.82 (2)
C1—H1	0.9300	O2W—H2WB	0.82 (2)
C2—C3	1.357 (5)	O3W—H3WA	0.82 (3)
C2—H2	0.9300	O3W—H3WB	0.83 (3)
C3—C4	1.382 (5)	O4W—H4WA	0.82 (2)
C3—H3	0.9300	O4W—H4WB	0.83 (5)
C4—C5	1.370 (5)

N2—Ni—O1W	177.71 (11)	N1—C5—C4	123.7 (3)
N2—Ni—O1	95.37 (10)	N1—C5—C6	112.5 (3)
O1W—Ni—O1	86.27 (10)	C4—C5—C6	123.8 (3)
N2—Ni—O2W	88.80 (10)	N2—C6—N4	124.0 (3)
O1W—Ni—O2W	89.52 (10)	N2—C6—C5	114.9 (3)
O1—Ni—O2W	175.54 (10)	N4—C6—C5	121.1 (3)
N2—Ni—N3	77.37 (11)	N4—C7—N5	125.9 (3)
O1W—Ni—N3	104.15 (11)	N4—C7—C14	118.3 (3)
O1—Ni—N3	93.81 (11)	N5—C7—C14	115.8 (3)
O2W—Ni—N3	88.65 (11)	N5—C8—N2	123.5 (3)
N2—Ni—N1	75.95 (11)	N5—C8—C9	122.2 (3)
O1W—Ni—N1	102.49 (11)	N2—C8—C9	114.4 (3)
O1—Ni—N1	89.62 (10)	N3—C9—C10	121.7 (3)
O2W—Ni—N1	89.84 (10)	N3—C9—C8	114.0 (3)
N3—Ni—N1	153.31 (11)	C10—C9—C8	124.3 (3)
O3—S—O2	109.53 (17)	C11—C10—C9	119.4 (4)
O3—S—O4	110.37 (18)	C11—C10—H10	120.3
O2—S—O4	109.90 (15)	C9—C10—H10	120.3
O3—S—O1	109.48 (17)	C12—C11—C10	118.5 (4)
O2—S—O1	109.29 (14)	C12—C11—H11	120.8
O4—S—O1	108.24 (15)	C10—C11—H11	120.8
S—O1—Ni	136.17 (15)	C11—C12—C13	119.9 (4)
C1—N1—C5	116.6 (3)	C11—C12—H12	120.0
C1—N1—Ni	128.8 (3)	C13—C12—H12	120.0
C5—N1—Ni	114.7 (2)	N3—C13—C12	122.4 (4)
C6—N2—C8	117.9 (3)	N3—C13—H13	118.8
C6—N2—Ni	121.9 (2)	C12—C13—H13	118.8
C8—N2—Ni	120.0 (2)	N6—C14—C15	123.0 (3)
C13—N3—C9	118.1 (3)	N6—C14—C7	116.7 (3)
C13—N3—Ni	127.9 (3)	C15—C14—C7	120.3 (3)
C9—N3—Ni	114.1 (2)	C16—C15—C14	118.3 (4)
C6—N4—C7	114.1 (3)	C16—C15—H15	120.9
C8—N5—C7	114.6 (3)	C14—C15—H15	120.9
C14—N6—C18	117.0 (3)	C17—C16—C15	118.6 (4)
N1—C1—C2	123.3 (4)	C17—C16—H16	120.7
N1—C1—H1	118.4	C15—C16—H16	120.7
C2—C1—H1	118.4	C16—C17—C18	120.3 (4)
C3—C2—C1	118.6 (4)	C16—C17—H17	119.8
C3—C2—H2	120.7	C18—C17—H17	119.8
C1—C2—H2	120.7	N6—C18—C17	122.8 (4)
C2—C3—C4	120.6 (4)	N6—C18—H18	118.6
C2—C3—H3	119.7	C17—C18—H18	118.6
C4—C3—H3	119.7	H1WA—O1W—H1WB	106 (3)
C5—C4—C3	117.2 (3)	H2WB—O2W—H2WA	107 (2)
C5—C4—H4	121.4	H3WA—O3W—H3WB	105 (3)
C3—C4—H4	121.4	H4WB—O4W—H4WA	105 (4)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O4W	0.82 (3)	1.97 (2)	2.746 (4)	158 (2)
O1W—H1WB···O4ⁱ	0.82 (2)	1.97 (1)	2.702 (3)	148 (2)
O2W—H2WA···O2ⁱ	0.82 (2)	1.89 (2)	2.686 (3)	162 (2)
O2W—H2WB···N6ⁱⁱ	0.82 (2)	2.05 (2)	2.846 (4)	164 (3)
O3W—H3WA···O3	0.82 (3)	2.19 (3)	2.905 (5)	146 (4)
O3W—H3WB···O4ⁱⁱⁱ	0.82 (3)	2.21 (3)	2.878 (4)	139 (3)
O4W—H4WA···O3^iv	0.82 (2)	2.07 (4)	2.774 (4)	145 (3)
O4W—H4WB···O3Wⁱ	0.83 (5)	2.43 (5)	3.220 (7)	161 (5)
C11—H11···O2^v	0.93	2.39	3.241 (5)	153
C13—H13···O3Wⁱ	0.93	2.41	3.178 (5)	140

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

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.

E-mail address*
Repeat e-mail address* (for error checking)

Format*	PDF (US $40)
	HTML (US $40)
	PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number (non-UK EC countries only)
Country*

Terms and conditions of use
Contact us

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page