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The structure of the title compound, [Ni(ths)(bbip)(dmf)]·­H2O [ths is thio­sulfate, S2O3; bbip is 2,6-bis(1H-benz­imidazol-2-yl)­pyridine, C21H13N5; and dmf is di­methyl­form­amide, C3H7NO], is monomeric, with the nickel ion octahe­drally surrounded by an N,N',N''-tridentate bbip mol­ecule, an S,O-bidentate ths mol­ecule and an O-monodentate dmf mol­ecule. The H atoms of the hydration water mol­ecule and the amino groups of bbip are involved in hydrogen bonding and determine a spatial organization of broad layers parallel to (001), which are connected by weak interactions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103008667/ob1117sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270103008667/ob1117Isup2.hkl
Contains datablock I

CCDC reference: 219544

Comment top

The coordination properties of the thiosulfate group have been extensively studied by our group in connection with their relevance in the discussion of dπ-pπ bonding in sulfur oxoanions. The anion has proven to be a quite versatile ligand, since it contains atoms classified as both soft and hard bases (Pearson, 1973). This situation produces a variety of coordination modes, especially when the metal ion is intermediate between classes a and b in the aforementioned classification. One factor that seems to influence the manner in which the ligand coordinates is the geometry of the organic ligands present in the complex. In this context, we have found the reaction between Ni2+ and S2O32−, in the presence of polynitrogenated bases, to be a very prolific one, with a variety of compounds of varied characteristics being generated (Freire et al., 1999; Freire, Baggio, Mombru et al., 2000; Freire, Baggio, Mariezcurrena et al., 2000; Freire, Baggio, Suescun et al., 2000), including products that are the result of redox processes (Freire, Baggio & Baggio, 2001). In this paper, we report an X-ray structural study of the title compound, (I).

The structure of (I) is monomeric, with the nickel ion surrounded by three different ligands, viz. a tridentate bisbenzimidazolylpyridine molecule (bbip), a bidentate thiosulfate molecule (ths) and a monodentate dimethylformamide molecule (dmf). The result is a highly distorted octahedral environment for the cation, with adjacent coordination sites subtending angles as low as 76.78 (10)°, (expected 90°) and opposite centers 153.71 (11)° apart (expected 180°).

The bbip ligand does not depart from the geometry it usually presents when complexed to a cation: the unprotonated imidazolyl N atoms are cis to the pyridyl N atom, thus defining the tridentate bite. Because of the restraints imposed by this chelate character, the three coordinated N atoms in the ligand are constrained not to be equidistant from the cation, the central Ni—N2 bond being shorter [2.054 (3) Å versus 2.107 (3) Å and 2.124 (3) Å for the other two bonds]. In addition, the stress arising from coordination tends to distort the molecule into a concave shape, the lateral wings being bent with respect to the central ring by 6.1 (1)° and 6.8 (1)°, respectively.

The ths anion binds through the common (S,O) chelate mode; a search in the November 2002 release of the Cambridge Structural Database (CSD; Allen, 2002) showed 11 such coordinations of the anion out of the 49 entries in which it appears bound to a metal. In the present structure, the S1 atom occupies the remaining equatorial site, in the plane defined by bbip and opposite to the central (and shortest) Ni—N2 bond. This behaviour appears to be common in these type of compounds, as it has also been observed in Ni(tpy)(ths)(H2O) (Freire, Baggio, Goeta et al., 2001), which is the only other reported ths complex with a tridentate base.

The structure of the ths anion displays a variety of S—O bond lengths, which are inversely related to the degree of compromise in coordination of the corresponding O atoms. Thus atom O1, which bonds directly to nickel and is also involved in a medium-strength hydrogen bond, forms the longest (i.e. weakest) bond [S2—O1 = 1.494 (2) Å]. The intermediate bond length involves atom O2, which only takes part in hydrogen bonding [S2—O2 = 1.473 (2) Å. Finally, O3 (which is not involved in any other interaction) provides the shortest (i.e. strongest) bond [S2—O3 = 1.441 (2) Å]. This effect is accompanied by a reduction of the corresponding S—S—O angle, which is directly related to the S—O bond enlargement (Table 1). This behavior has been observed previously in a variety of sulfur oxoanions (Freire, Baggio, Mombru et al., 2000; Freire, Baggio, Mariezcurrena et al., 2000; Harvey et al., 2001, 2002).

A monodentate dmf molecule completes the coordination around the Ni atom. The ligand geometry is unexceptional, and although a wide range of C—N and CO bond length values are reported in the literature, those in (I) [1.312 (4) Å and 1.236 (4) Å] are close to the mean values obtained from ca 950 cases found in the CSD, viz. 1.32 (5) Å and 1.23 (6) Å, respectively.

The water molecule and imidazolyl H atoms participate in strong hydrogen-bonding interactions (Table 2). The water molecule, acting as a donor, links two centrosymmetrically related molecules, thus forming a closed loop centered at (1/2,1/2,1/2). These groups, in turn, interact with their homologous groups in neighboring cells through the remaining hydrogen bonds, mediated by the imidazolyl H atoms. The result is the build up of broad two-dimensional structures along c, parallel to (001) and one unit cell wide. Sheets interact with each other in this direction through weaker C—H···O contacts and van der Waal's forces. The packing is such as to drive the aromatic groups away from each other, thus preventing any kind of ππ interaction between them.

Experimental top

The title compound, (I), was obtained by slow diffusion of two unperturbed solutions. The lower solution was an aqueous solution of nickel nitrate and sodium thiosulfate; the upper solution was a dmf solution of bbip, the main three components being in a 1:3:1 molar ratio. Crystal growth took place at the interface of the two solutions, giving rise to green prisms of (I) suitable for X-ray diffraction.

Refinement top

H atoms attached to C atoms were added at their expected positions and refined as riding. Methyl H atoms were also allowed to rotate. H atoms attached to the water molecule and to the protonated N atoms in bbip were found in the final? difference Fourier map and refined with restrained N—H, O—H [0.90 (3) Å] and H···H (.66× O—H) distances.

Computing details top

Data collection: SMART-NT (Bruker, 2001); cell refinement: SMART-NT (Bruker, 2001); data reduction: SAINT-NT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL/PC (Sheldrick, 1994); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I), showing the atom-numbering scheme and displacement ellipsoids at the 40% probablity level.
[Figure 2] Fig. 2. A schematic packing view of (I) along b. Hydrogen bonds are represented by heavy broken lines. H atoms bonded to C atoms have been omitted for clarity.
(I) top
Crystal data top
[Ni(S2O3)(C21H13N5)(CH7NO)]·H2OZ = 2
Mr = 573.29F(000) = 592
Triclinic, P1Dx = 1.615 Mg m3
a = 9.3815 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.4096 (8) ÅCell parameters from 78 reflections
c = 15.1968 (13) Åθ = 4.1–23.3°
α = 72.124 (2)°µ = 1.05 mm1
β = 83.169 (2)°T = 293 K
γ = 67.423 (2)°Prisms, green
V = 1178.91 (17) Å30.35 × 0.25 × 0.16 mm
Data collection top
CCD area detector
diffractometer
4505 independent reflections
Radiation source: fine-focus sealed tube3230 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
ϕ and ω scansθmax = 26.0°, θmin = 1.4°
Absorption correction: part of the refinement model (ΔF)
(SADABS in SAINT-NT; Bruker, 2000)
h = 511
Tmin = 0.73, Tmax = 0.81k = 1111
5399 measured reflectionsl = 1818
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: mixed
wR(F2) = 0.109H atoms treated by a mixture of independent and constrained refinement
S = 0.87 w = 1/[σ2(Fo2) + (0.061P)2]
where P = (Fo2 + 2Fc2)/3
4505 reflections(Δ/σ)max = 0.004
335 parametersΔρmax = 0.41 e Å3
3 restraintsΔρmin = 0.40 e Å3
Crystal data top
[Ni(S2O3)(C21H13N5)(CH7NO)]·H2Oγ = 67.423 (2)°
Mr = 573.29V = 1178.91 (17) Å3
Triclinic, P1Z = 2
a = 9.3815 (8) ÅMo Kα radiation
b = 9.4096 (8) ŵ = 1.05 mm1
c = 15.1968 (13) ÅT = 293 K
α = 72.124 (2)°0.35 × 0.25 × 0.16 mm
β = 83.169 (2)°
Data collection top
CCD area detector
diffractometer
4505 independent reflections
Absorption correction: part of the refinement model (ΔF)
(SADABS in SAINT-NT; Bruker, 2000)
3230 reflections with I > 2σ(I)
Tmin = 0.73, Tmax = 0.81Rint = 0.038
5399 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0393 restraints
wR(F2) = 0.109H atoms treated by a mixture of independent and constrained refinement
S = 0.87Δρmax = 0.41 e Å3
4505 reflectionsΔρmin = 0.40 e Å3
335 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni0.81382 (5)0.41298 (5)0.75171 (3)0.03156 (14)
S10.67156 (10)0.24134 (10)0.82124 (6)0.0395 (2)
S20.59107 (10)0.32539 (10)0.69089 (6)0.0373 (2)
O10.6588 (3)0.4507 (3)0.64681 (15)0.0410 (6)
O20.6527 (3)0.1985 (3)0.64375 (16)0.0477 (6)
O30.4248 (3)0.3918 (3)0.68928 (19)0.0591 (8)
N10.6766 (3)0.6399 (3)0.77208 (18)0.0342 (6)
N20.9151 (3)0.5638 (3)0.66603 (18)0.0332 (6)
N31.0022 (3)0.2564 (3)0.69552 (18)0.0352 (6)
N40.6359 (3)0.9005 (3)0.73352 (19)0.0401 (7)
H4A0.6468 (7)0.9948 (4)0.7073 (6)0.048*
N51.2094 (3)0.2289 (3)0.60459 (19)0.0405 (7)
H5A1.2831 (16)0.2513 (6)0.5667 (14)0.049*
C10.5572 (4)0.7105 (4)0.8261 (2)0.0335 (7)
C20.4685 (4)0.6459 (4)0.8934 (2)0.0387 (8)
H2A0.48470.53720.90960.046*
C30.3564 (4)0.7472 (5)0.9351 (3)0.0470 (9)
H3A0.29580.70630.98090.056*
C40.3303 (4)0.9105 (5)0.9107 (3)0.0530 (10)
H4B0.25200.97580.94030.064*
C50.4161 (4)0.9778 (4)0.8446 (3)0.0506 (10)
H5B0.39851.08680.82880.061*
C60.5304 (4)0.8754 (4)0.8024 (2)0.0375 (8)
C70.7187 (4)0.7573 (4)0.7187 (2)0.0357 (8)
C80.8480 (4)0.7220 (4)0.6545 (2)0.0346 (8)
C90.9030 (4)0.8290 (4)0.5898 (2)0.0436 (9)
H9A0.85540.93910.58140.052*
C101.0308 (4)0.7673 (4)0.5384 (2)0.0455 (9)
H10A1.06960.83680.49440.055*
C111.1016 (4)0.6040 (4)0.5513 (2)0.0430 (9)
H11A1.18930.56220.51790.052*
C121.0382 (4)0.5045 (4)0.6154 (2)0.0349 (8)
C131.0862 (4)0.3301 (4)0.6383 (2)0.0362 (8)
C141.2051 (4)0.0773 (4)0.6427 (2)0.0397 (8)
C151.3027 (4)0.0703 (4)0.6320 (3)0.0487 (10)
H15A1.38830.08090.59320.058*
C161.2653 (5)0.1998 (5)0.6821 (3)0.0540 (11)
H16A1.32780.30130.67730.065*
C171.1363 (5)0.1839 (4)0.7402 (3)0.0522 (10)
H17A1.11640.27540.77340.063*
C181.0381 (4)0.0373 (4)0.7495 (2)0.0445 (9)
H18A0.95130.02690.78730.053*
C191.0752 (4)0.0950 (4)0.6994 (2)0.0360 (8)
O1A0.9368 (3)0.3551 (3)0.87102 (16)0.0434 (6)
C1A1.0673 (4)0.3577 (4)0.8722 (2)0.0395 (8)
H1AA1.11150.39240.81560.047*
N1A1.1485 (3)0.3154 (4)0.9468 (2)0.0425 (7)
C2A1.2994 (5)0.3266 (6)0.9427 (3)0.0730 (14)
H2AA1.32590.36650.87940.110*
H2AB1.37490.22220.96940.110*
H2AC1.29700.39850.97650.110*
C3A1.0894 (5)0.2565 (6)1.0370 (3)0.0690 (13)
H3AA0.98940.25511.03070.103*
H3AB1.08110.32551.07410.103*
H3AC1.15840.14961.06630.103*
O1W0.4479 (3)0.2713 (3)0.49596 (17)0.0468 (6)
H1WA0.512 (3)0.262 (4)0.5367 (18)0.056*
H1WB0.434 (4)0.360 (3)0.4499 (16)0.056*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0352 (3)0.0271 (2)0.0347 (2)0.01412 (18)0.00095 (18)0.00880 (18)
S10.0454 (5)0.0378 (5)0.0384 (5)0.0217 (4)0.0030 (4)0.0079 (4)
S20.0403 (5)0.0274 (4)0.0468 (5)0.0136 (4)0.0055 (4)0.0107 (4)
O10.0553 (15)0.0304 (12)0.0398 (13)0.0221 (11)0.0101 (11)0.0015 (10)
O20.0646 (17)0.0331 (13)0.0501 (15)0.0183 (12)0.0050 (12)0.0162 (12)
O30.0355 (15)0.0576 (17)0.085 (2)0.0118 (13)0.0126 (13)0.0232 (15)
N10.0371 (16)0.0263 (14)0.0400 (16)0.0127 (12)0.0006 (12)0.0095 (12)
N20.0378 (16)0.0294 (14)0.0348 (15)0.0161 (12)0.0020 (12)0.0085 (12)
N30.0376 (16)0.0291 (14)0.0375 (16)0.0130 (12)0.0029 (12)0.0079 (12)
N40.0501 (18)0.0241 (14)0.0468 (18)0.0134 (13)0.0001 (14)0.0117 (13)
N50.0390 (17)0.0444 (18)0.0418 (17)0.0169 (14)0.0098 (13)0.0189 (14)
C10.0341 (18)0.0312 (17)0.0365 (18)0.0114 (14)0.0034 (14)0.0111 (15)
C20.040 (2)0.040 (2)0.0387 (19)0.0177 (16)0.0018 (16)0.0099 (16)
C30.041 (2)0.055 (2)0.047 (2)0.0201 (18)0.0066 (17)0.0166 (19)
C40.046 (2)0.053 (2)0.059 (3)0.0090 (19)0.0053 (19)0.027 (2)
C50.054 (2)0.035 (2)0.059 (3)0.0086 (18)0.001 (2)0.0179 (19)
C60.039 (2)0.0340 (19)0.041 (2)0.0123 (15)0.0027 (16)0.0138 (16)
C70.042 (2)0.0318 (18)0.0371 (19)0.0159 (15)0.0031 (15)0.0114 (15)
C80.044 (2)0.0322 (18)0.0341 (18)0.0192 (15)0.0017 (15)0.0104 (15)
C90.058 (2)0.0347 (19)0.042 (2)0.0257 (17)0.0005 (18)0.0060 (16)
C100.056 (2)0.046 (2)0.041 (2)0.0334 (19)0.0045 (18)0.0062 (17)
C110.044 (2)0.052 (2)0.041 (2)0.0268 (18)0.0071 (16)0.0154 (18)
C120.039 (2)0.0352 (18)0.0348 (18)0.0179 (15)0.0019 (15)0.0114 (15)
C130.037 (2)0.0394 (19)0.0357 (19)0.0160 (16)0.0046 (15)0.0151 (16)
C140.041 (2)0.040 (2)0.040 (2)0.0115 (16)0.0029 (16)0.0158 (16)
C150.041 (2)0.047 (2)0.058 (2)0.0033 (18)0.0061 (18)0.028 (2)
C160.059 (3)0.038 (2)0.063 (3)0.0019 (19)0.018 (2)0.024 (2)
C170.066 (3)0.033 (2)0.056 (2)0.0141 (19)0.012 (2)0.0107 (18)
C180.052 (2)0.0345 (19)0.045 (2)0.0143 (17)0.0031 (17)0.0094 (17)
C190.038 (2)0.0307 (18)0.0371 (19)0.0076 (15)0.0025 (15)0.0127 (15)
O1A0.0386 (14)0.0494 (15)0.0442 (14)0.0167 (12)0.0060 (11)0.0131 (12)
C1A0.047 (2)0.0357 (19)0.038 (2)0.0172 (17)0.0012 (16)0.0116 (16)
N1A0.0374 (17)0.0534 (19)0.0412 (17)0.0190 (14)0.0032 (13)0.0156 (15)
C2A0.050 (3)0.108 (4)0.077 (3)0.040 (3)0.006 (2)0.031 (3)
C3A0.066 (3)0.098 (4)0.041 (2)0.033 (3)0.003 (2)0.013 (2)
O1W0.0504 (17)0.0458 (15)0.0419 (15)0.0194 (13)0.0026 (12)0.0080 (12)
Geometric parameters (Å, º) top
Ni—N22.054 (3)C7—C81.464 (4)
Ni—O1A2.080 (2)C8—C91.384 (4)
Ni—N32.107 (3)C9—C101.380 (5)
Ni—N12.124 (3)C9—H9A0.9300
Ni—O12.142 (2)C10—C111.380 (5)
Ni—S12.4037 (10)C10—H10A0.9300
S1—S22.0137 (12)C11—C121.382 (4)
S2—O31.441 (2)C11—H11A0.9300
S2—O21.473 (2)C12—C131.462 (4)
S2—O11.494 (2)C14—C151.386 (5)
N1—C71.320 (4)C14—C191.391 (5)
N1—C11.384 (4)C15—C161.372 (5)
N2—C81.338 (4)C15—H15A0.9300
N2—C121.339 (4)C16—C171.398 (5)
N3—C131.321 (4)C16—H16A0.9300
N3—C191.391 (4)C17—C181.373 (5)
N4—C71.345 (4)C17—H17A0.9300
N4—C61.383 (4)C18—C191.392 (5)
N4—H4A0.894 (6)C18—H18A0.9300
N5—C131.349 (4)O1A—C1A1.236 (4)
N5—C141.379 (4)C1A—N1A1.312 (4)
N5—H5A0.893 (18)C1A—H1AA0.9300
C1—C21.383 (4)N1A—C3A1.443 (5)
C1—C61.407 (4)N1A—C2A1.451 (4)
C2—C31.363 (5)C2A—H2AA0.9600
C2—H2A0.9300C2A—H2AB0.9600
C3—C41.394 (5)C2A—H2AC0.9600
C3—H3A0.9300C3A—H3AA0.9600
C4—C51.366 (5)C3A—H3AB0.9600
C4—H4B0.9300C3A—H3AC0.9600
C5—C61.383 (5)O1W—H1WA0.88 (3)
C5—H5B0.9300O1W—H1WB0.89 (3)
N2—Ni—O1A97.71 (10)N4—C7—C8127.1 (3)
N2—Ni—N377.01 (10)N2—C8—C9121.2 (3)
O1A—Ni—N391.86 (10)N2—C8—C7110.8 (3)
N2—Ni—N176.78 (10)C9—C8—C7128.1 (3)
O1A—Ni—N189.61 (10)C10—C9—C8117.9 (3)
N3—Ni—N1153.71 (11)C10—C9—H9A121.0
N2—Ni—O193.34 (9)C8—C9—H9A121.0
O1A—Ni—O1168.70 (9)C11—C10—C9121.0 (3)
N3—Ni—O192.91 (9)C11—C10—H10A119.5
N1—Ni—O190.65 (9)C9—C10—H10A119.5
N2—Ni—S1167.51 (8)C10—C11—C12117.9 (3)
O1A—Ni—S194.58 (7)C10—C11—H11A121.0
N3—Ni—S1100.47 (8)C12—C11—H11A121.0
N1—Ni—S1105.58 (8)N2—C12—C11121.2 (3)
O1—Ni—S174.48 (7)N2—C12—C13110.3 (3)
S2—S1—Ni79.99 (4)C11—C12—C13128.5 (3)
O3—S2—O2111.37 (15)N3—C13—N5112.9 (3)
O3—S2—O1112.01 (15)N3—C13—C12120.0 (3)
O2—S2—O1108.68 (14)N5—C13—C12127.1 (3)
O3—S2—S1111.21 (12)N5—C14—C15131.1 (3)
O2—S2—S1110.54 (10)N5—C14—C19106.4 (3)
O1—S2—S1102.70 (10)C15—C14—C19122.5 (3)
S2—O1—Ni101.97 (11)C16—C15—C14115.9 (4)
C7—N1—C1105.5 (3)C16—C15—H15A122.0
C7—N1—Ni112.9 (2)C14—C15—H15A122.0
C1—N1—Ni141.5 (2)C15—C16—C17122.1 (4)
C8—N2—C12120.7 (3)C15—C16—H16A118.9
C8—N2—Ni119.4 (2)C17—C16—H16A118.9
C12—N2—Ni119.5 (2)C18—C17—C16121.9 (4)
C13—N3—C19105.4 (3)C18—C17—H17A119.0
C13—N3—Ni113.0 (2)C16—C17—H17A119.0
C19—N3—Ni141.5 (2)C17—C18—C19116.5 (4)
C7—N4—C6106.8 (3)C17—C18—H18A121.7
C7—N4—H4A128.6 (4)C19—C18—H18A121.7
C6—N4—H4A124.5 (4)N3—C19—C14108.6 (3)
C13—N5—C14106.7 (3)N3—C19—C18130.4 (3)
C13—N5—H5A128.4 (4)C14—C19—C18121.0 (3)
C14—N5—H5A124.9 (4)C1A—O1A—Ni124.7 (2)
C2—C1—N1131.0 (3)O1A—C1A—N1A125.3 (3)
C2—C1—C6120.3 (3)O1A—C1A—H1AA117.4
N1—C1—C6108.7 (3)N1A—C1A—H1AA117.4
C3—C2—C1117.6 (3)C1A—N1A—C3A120.6 (3)
C3—C2—H2A121.2C1A—N1A—C2A122.0 (3)
C1—C2—H2A121.2C3A—N1A—C2A117.4 (3)
C2—C3—C4121.6 (4)N1A—C2A—H2AA109.5
C2—C3—H3A119.2N1A—C2A—H2AB109.5
C4—C3—H3A119.2H2AA—C2A—H2AB109.5
C5—C4—C3122.1 (4)N1A—C2A—H2AC109.5
C5—C4—H4B119.0H2AA—C2A—H2AC109.5
C3—C4—H4B119.0H2AB—C2A—H2AC109.5
C4—C5—C6116.5 (4)N1A—C3A—H3AA109.5
C4—C5—H5B121.7N1A—C3A—H3AB109.5
C6—C5—H5B121.7H3AA—C3A—H3AB109.5
C5—C6—N4132.4 (3)N1A—C3A—H3AC109.5
C5—C6—C1121.9 (3)H3AA—C3A—H3AC109.5
N4—C6—C1105.7 (3)H3AB—C3A—H3AC109.5
N1—C7—N4113.2 (3)H1WA—O1W—H1WB110 (2)
N1—C7—C8119.7 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O20.88 (3)2.01 (3)2.877 (3)168 (3)
O1W—H1WB···O1i0.89 (3)1.90 (3)2.752 (3)162 (3)
N4—H4A···O2ii0.89 (1)1.88 (1)2.773 (4)174 (1)
N5—H5A···O1Wiii0.89 (2)1.81 (2)2.700 (4)173 (1)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z; (iii) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Ni(S2O3)(C21H13N5)(CH7NO)]·H2O
Mr573.29
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.3815 (8), 9.4096 (8), 15.1968 (13)
α, β, γ (°)72.124 (2), 83.169 (2), 67.423 (2)
V3)1178.91 (17)
Z2
Radiation typeMo Kα
µ (mm1)1.05
Crystal size (mm)0.35 × 0.25 × 0.16
Data collection
DiffractometerCCD area detector
diffractometer
Absorption correctionPart of the refinement model (ΔF)
(SADABS in SAINT-NT; Bruker, 2000)
Tmin, Tmax0.73, 0.81
No. of measured, independent and
observed [I > 2σ(I)] reflections
5399, 4505, 3230
Rint0.038
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.039, 0.109, 0.87
No. of reflections4505
No. of parameters335
No. of restraints3
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.41, 0.40

Computer programs: SMART-NT (Bruker, 2001), SAINT-NT (Bruker, 2000), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP in SHELXTL/PC (Sheldrick, 1994).

Selected geometric parameters (Å, º) top
Ni—N22.054 (3)Ni—S12.4037 (10)
Ni—O1A2.080 (2)S1—S22.0137 (12)
Ni—N32.107 (3)S2—O31.441 (2)
Ni—N12.124 (3)S2—O21.473 (2)
Ni—O12.142 (2)S2—O11.494 (2)
N2—Ni—O1A97.71 (10)O1A—Ni—S194.58 (7)
N2—Ni—N377.01 (10)N3—Ni—S1100.47 (8)
O1A—Ni—N391.86 (10)N1—Ni—S1105.58 (8)
N2—Ni—N176.78 (10)O1—Ni—S174.48 (7)
O1A—Ni—N189.61 (10)O3—S2—O2111.37 (15)
N3—Ni—N1153.71 (11)O3—S2—O1112.01 (15)
N2—Ni—O193.34 (9)O2—S2—O1108.68 (14)
O1A—Ni—O1168.70 (9)O3—S2—S1111.21 (12)
N3—Ni—O192.91 (9)O2—S2—S1110.54 (10)
N1—Ni—O190.65 (9)O1—S2—S1102.70 (10)
N2—Ni—S1167.51 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O20.88 (3)2.01 (3)2.877 (3)168 (3)
O1W—H1WB···O1i0.89 (3)1.90 (3)2.752 (3)162 (3)
N4—H4A···O2ii0.894 (6)1.882 (7)2.773 (4)174.0 (10)
N5—H5A···O1Wiii0.893 (18)1.813 (17)2.700 (4)172.9 (11)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z; (iii) x+1, y, z.
 

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