Poly[octa-μ-aqua-tetra­aqua­bis(μ4-5-sulfonatobenzene-1,3-dicarboxyl­ato)nickel(II)tetra­sodium]

Zhang, B.-Y.; Nie, J.-J.; Xu, D.-J.

doi:10.1107/S1600536809009489

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 4| April 2009| Pages m429-m430

doi:10.1107/S1600536809009489

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Poly[octa-μ-aqua-tetraaquabis(μ₄-5-sulfonatobenzene-1,3-dicarboxylato)nickel(II)tetrasodium]

Bing-Yu Zhang,^a Jing-Jing Nie ^a and Duan-Jun Xu ^a ^*

^aDepartment of Chemistry, Zhejiang University, People's Republic of China
^*Correspondence e-mail: xudj@mail.hz.zj.cn

(Received 12 March 2009; accepted 14 March 2009; online 25 March 2009)

In the crystal structure of the title compound, [Na₄Ni(C₈H₃O₇S)₂(H₂O)₁₂]_n, the Ni^II cation occupies an inversion centre and is coordinated by the carboxyl groups of the sulfoisophthalate trianions and water molecules in a distorted octahedral geometry. Two independent Na^I atoms are connected by the carboxyl and sulfonate groups of the sulfoisophthalate ligands anions and water molecules in a distorted octahedral geometry. The sulfoisophthalate ligands and coordinated water molecules bridge the Ni^II and Na^I cations, forming a three-dimensional polymeric structure. Weak π–π stacking is present between parallel benzene rings [centroid–centroid distance = 3.9349 (10) Å]. Extensive O—H⋯O and C—H⋯O hydrogen bonding helps to stabilize the crystal structure.

Related literature

For general background, see: Su & Xu (2004 ); Pan et al. (2006 ). For the isotypic structure of the Co analogue, see: Zhang et al. (2009 ).

Experimental

Crystal data

[Na₄Ni(C₈H₃O₇S)₂(H₂O)₁₂]
M_r = 853.19
Monoclinic, P 2₁ /n
a = 7.8770 (9) Å
b = 17.229 (2) Å
c = 11.7474 (13) Å
β = 93.292 (4)°
V = 1591.7 (3) Å³
Z = 2
Mo Kα radiation
μ = 0.90 mm⁻¹
T = 295 K
0.30 × 0.22 × 0.20 mm

Data collection

Rigaku R-AXIS RAPID IP diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.770, T_max = 0.835
17574 measured reflections
3107 independent reflections
2866 reflections with I > 2σ(I)
R_int = 0.023

Refinement

R[F² > 2σ(F²)] = 0.025
wR(F²) = 0.071
S = 1.08
3107 reflections
223 parameters
H-atom parameters constrained
Δρ_max = 0.42 e Å⁻³
Δρ_min = −0.40 e Å⁻³

Table 1
Selected bond lengths (Å)

Ni—O1	2.0252 (11)
Ni—O8	2.0731 (14)
Ni—O9	2.0727 (11)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O8—H8A⋯O13ⁱ	0.84	2.03	2.861 (2)	173
O8—H8B⋯O4ⁱⁱ	0.85	1.99	2.8130 (19)	162
O9—H9A⋯O7ⁱⁱⁱ	0.85	2.16	2.9854 (17)	163
O9—H9B⋯O2	0.84	1.82	2.6168 (17)	159
O10—H10A⋯O7ⁱⁱ	0.83	2.04	2.8553 (19)	167
O10—H10B⋯O3^iv	0.85	1.83	2.6615 (19)	165
O11—H11A⋯O7ⁱⁱⁱ	0.89	1.90	2.7659 (18)	167
O11—H11B⋯O3^iv	0.87	1.92	2.783 (2)	175
O12—H12A⋯O1^v	0.84	2.11	2.9470 (18)	173
O12—H12B⋯O4^vi	0.89	2.04	2.8994 (19)	163
O13—H13A⋯O4ⁱⁱ	0.84	1.94	2.733 (2)	157
O13—H13B⋯O6^vii	0.88	2.21	2.9486 (19)	141
C7—H7⋯O11^viii	0.93	2.50	3.371 (2)	157
Symmetry codes: (i) -x+2, -y+1, -z+1; (ii) -x+1, -y+1, -z; (iii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iv) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (v) -x+1, -y+1, -z+1; (vi) x+1, y, z+1; (vii) $[-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (viii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ .

Data collection: PROCESS-AUTO (Rigaku, 1998 ); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809009489/ng2561sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809009489/ng2561Isup2.hkl

checkCIF report

Comment top

As a part of investigation on π-π stacking between aromatic rings (Su & Xu, 2004; Pan et al., 2006), the title Ni^II compound has recently been prepared in our laboratory, and its crystal structure is reported here.

A part of the three dimensional polymeric structure of the title compound is shown in Fig. 1. The Ni^II compound is isomorphous with the Co^II compound (Zhang et al., 2009). The Ni atom occupies a special position in an inversion centre and assumes a distorted NiO₆ octahedral geometry, The Ni—O bond distances (Table 1) are about 0.03 Å shorter than corresponding Co—O bond distances found in the isomorphous Co^II compound. Both crystallograohically indenpendent Na^I atoms are in distorted octahedral coordination geometry. The sulfoisophthalate trianions and water molecules bridge the metal atoms to form the polymeric structure.

The extensive O—H···O hydrogen bonding network presents in the crystal structue (Table 2), weak C—H···O hydrogen bonding also helps to stabilize the crystal structure. The distance between parallel the C2-benzne plane and C2^v-benzene plane is 3.551 (9) Å [symmetry code: (v) 1 - x, 1 - y, -z], and the centroids distance between the benzene rings is 3.9349 (10) Å. These findings suggest a weak π-π stacking involving sulfoisophthlate ligand.

Related literature top

For general background, see: Su & Xu (2004); Pan et al. (2006). For a related structure, see: Zhang et al. (2009).

Experimental top

A water-ethanol solution (25 ml, 3:2) containing monosodium 5-sulfoisophthalate (0.270 g, 1 mmol), Na₂CO₃ (0.212 g, 2 mmol) and NiCl₂.6H₂O (0.600 g, 2.5 mmol) was refluxed for 8 h and filtered after cooling to room temperature. The single crystals of the title compound were obtained from the filtrate after 3 weeks.

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

Fig. 1. A part of the polymeric structure of the title compound with 50% probability displacement (arbitrary spheres for H atoms) [symmetry codes: (i) -x + 3/2,+y - 1/2,-z + 1/2; (ii) -x + 1/2,+y - 1/2,-z + 1/2; (iii) -x + 1,-y + 1,-z + 1; (iv) x - 1/2,-y + 1/2,+z - 1/2; (v) -x + 1,-y + 1,-z].

Poly[octa-µ-aqua-tetraaquabis(µ₄-5-sulfonatobenzene-1,3- dicarboxylato)nickel(II)tetrasodium] top

Crystal data top

[Na₄Ni(C₈H₃O₇S)₂(H₂O)₁₂]	F(000) = 876
M_r = 853.19	D_x = 1.780 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 2356 reflections
a = 7.8770 (9) Å	θ = 2.5–25.0°
b = 17.229 (2) Å	µ = 0.90 mm⁻¹
c = 11.7474 (13) Å	T = 295 K
β = 93.292 (4)°	Prism, green
V = 1591.7 (3) Å³	0.30 × 0.22 × 0.20 mm
Z = 2

Data collection top

Rigaku R-AXIS RAPID IP diffractometer	3107 independent reflections
Radiation source: fine-focus sealed tube	2866 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.023
Detector resolution: 10.0 pixels mm^-1	θ_max = 26.0°, θ_min = 2.1°
ω scans	h = −9→9
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −21→21
T_min = 0.770, T_max = 0.835	l = −14→14
17574 measured reflections

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)] = 0.025	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.071	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.0384P)² + 0.7337P] where P = (F_o² + 2F_c²)/3
3107 reflections	(Δ/σ)_max = 0.001
223 parameters	Δρ_max = 0.42 e Å⁻³
0 restraints	Δρ_min = −0.40 e Å⁻³

Crystal data top

[Na₄Ni(C₈H₃O₇S)₂(H₂O)₁₂]	V = 1591.7 (3) Å³
M_r = 853.19	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 7.8770 (9) Å	µ = 0.90 mm⁻¹
b = 17.229 (2) Å	T = 295 K
c = 11.7474 (13) Å	0.30 × 0.22 × 0.20 mm
β = 93.292 (4)°

Data collection top

Rigaku R-AXIS RAPID IP diffractometer	3107 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	2866 reflections with I > 2σ(I)
T_min = 0.770, T_max = 0.835	R_int = 0.023
17574 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	0 restraints
wR(F²) = 0.071	H-atom parameters constrained
S = 1.08	Δρ_max = 0.42 e Å⁻³
3107 reflections	Δρ_min = −0.40 e Å⁻³
223 parameters

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.

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 (Å²) top

	x	y	z	U_iso*/U_eq
Ni	0.5000	0.5000	0.5000	0.01887 (10)
Na1	0.82068 (9)	0.33240 (4)	0.45637 (6)	0.02989 (18)
Na2	0.40578 (9)	0.26823 (4)	0.20100 (6)	0.02845 (17)
S	0.28801 (5)	0.73027 (2)	0.01772 (3)	0.01908 (11)
O1	0.42320 (16)	0.52266 (7)	0.33588 (10)	0.0244 (3)
O2	0.42591 (19)	0.40594 (7)	0.25407 (10)	0.0335 (3)
O3	0.1627 (2)	0.37896 (8)	−0.12900 (12)	0.0456 (4)
O4	0.11757 (18)	0.47912 (8)	−0.24403 (11)	0.0332 (3)
O5	0.45777 (16)	0.74769 (7)	−0.01724 (11)	0.0279 (3)
O6	0.25488 (18)	0.76128 (7)	0.12908 (10)	0.0291 (3)
O7	0.15727 (16)	0.75328 (7)	−0.06942 (11)	0.0267 (3)
O8	0.75086 (17)	0.51710 (9)	0.46157 (11)	0.0362 (3)
H8A	0.8191	0.5403	0.5074	0.054*
H8B	0.7789	0.5274	0.3941	0.054*
O9	0.53288 (16)	0.38303 (6)	0.46643 (10)	0.0238 (3)
H9A	0.4645	0.3534	0.4997	0.036*
H9B	0.5021	0.3785	0.3975	0.036*
O10	0.70115 (18)	0.26289 (7)	0.28653 (11)	0.0336 (3)
H10A	0.7540	0.2629	0.2277	0.050*
H10B	0.6997	0.2152	0.3041	0.050*
O11	0.68483 (16)	0.21970 (8)	0.55884 (12)	0.0327 (3)
H11A	0.5764	0.2266	0.5724	0.049*
H11B	0.6788	0.1866	0.5033	0.049*
O12	0.87077 (17)	0.37265 (7)	0.65035 (11)	0.0312 (3)
H12A	0.7926	0.4047	0.6585	0.047*
H12B	0.9552	0.3964	0.6897	0.047*
O13	1.03972 (18)	0.40442 (8)	0.36780 (12)	0.0354 (3)
H13A	1.0040	0.4338	0.3148	0.053*
H13B	1.1122	0.3726	0.3378	0.053*
C1	0.4055 (2)	0.47741 (9)	0.25112 (14)	0.0205 (3)
C2	0.3474 (2)	0.51522 (9)	0.13980 (14)	0.0211 (3)
C3	0.3448 (2)	0.59532 (9)	0.12908 (13)	0.0210 (3)
H3	0.3862	0.6266	0.1889	0.025*
C4	0.2800 (2)	0.62800 (9)	0.02841 (14)	0.0187 (3)
C5	0.2204 (2)	0.58282 (9)	−0.06300 (14)	0.0218 (3)
H5	0.1774	0.6060	−0.1301	0.026*
C6	0.2258 (2)	0.50242 (9)	−0.05294 (14)	0.0224 (4)
C7	0.2909 (2)	0.46959 (10)	0.04849 (14)	0.0244 (4)
H7	0.2966	0.4159	0.0551	0.029*
C8	0.1644 (2)	0.44968 (10)	−0.15014 (14)	0.0240 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni	0.02441 (18)	0.01777 (16)	0.01396 (16)	0.00201 (11)	−0.00293 (12)	−0.00019 (10)
Na1	0.0270 (4)	0.0368 (4)	0.0256 (4)	0.0015 (3)	−0.0011 (3)	0.0022 (3)
Na2	0.0305 (4)	0.0314 (4)	0.0234 (4)	−0.0003 (3)	0.0012 (3)	−0.0038 (3)
S	0.0229 (2)	0.01610 (19)	0.0184 (2)	−0.00051 (15)	0.00256 (15)	0.00059 (14)
O1	0.0382 (7)	0.0198 (6)	0.0145 (6)	0.0029 (5)	−0.0053 (5)	−0.0005 (5)
O2	0.0610 (9)	0.0186 (6)	0.0196 (6)	0.0057 (6)	−0.0087 (6)	0.0003 (5)
O3	0.0870 (12)	0.0189 (7)	0.0285 (7)	−0.0022 (7)	−0.0168 (7)	−0.0035 (5)
O4	0.0503 (8)	0.0298 (7)	0.0181 (6)	0.0013 (6)	−0.0090 (6)	−0.0012 (5)
O5	0.0249 (7)	0.0297 (7)	0.0294 (7)	−0.0062 (5)	0.0045 (5)	−0.0013 (5)
O6	0.0448 (8)	0.0212 (6)	0.0221 (7)	−0.0007 (5)	0.0094 (6)	−0.0036 (5)
O7	0.0272 (7)	0.0243 (6)	0.0284 (7)	0.0031 (5)	−0.0006 (5)	0.0058 (5)
O8	0.0294 (7)	0.0570 (9)	0.0223 (7)	−0.0067 (6)	0.0020 (5)	−0.0017 (6)
O9	0.0336 (7)	0.0187 (6)	0.0185 (6)	0.0011 (5)	−0.0041 (5)	−0.0004 (5)
O10	0.0472 (8)	0.0290 (7)	0.0246 (7)	0.0009 (6)	0.0034 (6)	0.0035 (5)
O11	0.0276 (7)	0.0317 (7)	0.0381 (8)	0.0043 (5)	−0.0047 (6)	−0.0062 (6)
O12	0.0337 (7)	0.0291 (7)	0.0304 (7)	0.0028 (5)	−0.0013 (6)	−0.0073 (5)
O13	0.0381 (8)	0.0312 (7)	0.0370 (8)	0.0066 (6)	0.0037 (6)	0.0064 (6)
C1	0.0265 (9)	0.0194 (8)	0.0153 (8)	0.0006 (6)	−0.0020 (6)	0.0009 (6)
C2	0.0269 (9)	0.0205 (8)	0.0155 (8)	0.0012 (7)	−0.0012 (6)	0.0005 (6)
C3	0.0268 (9)	0.0203 (8)	0.0157 (8)	−0.0007 (6)	0.0002 (6)	−0.0017 (6)
C4	0.0213 (8)	0.0166 (7)	0.0185 (8)	−0.0010 (6)	0.0024 (6)	0.0004 (6)
C5	0.0276 (9)	0.0218 (8)	0.0156 (8)	0.0006 (7)	−0.0023 (6)	0.0023 (6)
C6	0.0290 (9)	0.0219 (8)	0.0161 (8)	−0.0005 (7)	−0.0021 (7)	−0.0012 (6)
C7	0.0360 (10)	0.0170 (8)	0.0198 (8)	−0.0003 (7)	−0.0024 (7)	−0.0005 (6)
C8	0.0312 (9)	0.0221 (8)	0.0182 (8)	−0.0002 (7)	−0.0027 (7)	−0.0026 (6)

Geometric parameters (Å, º) top

Ni—O1ⁱ	2.0252 (11)	O5—Na1^vii	2.3545 (14)
Ni—O1	2.0252 (11)	O5—Na2^vi	2.4814 (14)
Ni—O8ⁱ	2.0731 (14)	O6—Na2^viii	2.4271 (14)
Ni—O8	2.0731 (14)	O8—H8A	0.8407
Ni—O9	2.0727 (11)	O8—H8B	0.8534
Ni—O9ⁱ	2.0727 (11)	O9—H9A	0.8532
Na1—O5ⁱⁱ	2.3545 (14)	O9—H9B	0.8358
Na1—O12	2.3930 (14)	O10—H10A	0.8273
Na1—O13	2.4095 (16)	O10—H10B	0.8481
Na1—O9	2.4382 (14)	O11—Na2ⁱⁱⁱ	2.3511 (15)
Na1—O10	2.4669 (15)	O11—H11A	0.8860
Na1—O11	2.5519 (16)	O11—H11B	0.8656
Na1—Na2ⁱⁱⁱ	3.3901 (10)	O12—Na2ⁱⁱⁱ	2.5105 (15)
Na2—O11^iv	2.3511 (15)	O12—H12A	0.8368
Na2—O6^v	2.4271 (14)	O12—H12B	0.8876
Na2—O2	2.4561 (14)	O13—H13A	0.8386
Na2—O5^vi	2.4814 (14)	O13—H13B	0.8789
Na2—O10	2.4825 (16)	C1—C2	1.508 (2)
Na2—O12^iv	2.5105 (15)	C2—C7	1.383 (2)
Na2—Na1^iv	3.3901 (10)	C2—C3	1.386 (2)
S—O6	1.4505 (12)	C3—C4	1.381 (2)
S—O5	1.4525 (13)	C3—H3	0.9300
S—O7	1.4645 (13)	C4—C5	1.386 (2)
S—C4	1.7680 (16)	C5—C6	1.391 (2)
O1—C1	1.266 (2)	C5—H5	0.9300
O2—C1	1.242 (2)	C6—C7	1.390 (2)
O3—C8	1.244 (2)	C6—C8	1.517 (2)
O4—C8	1.250 (2)	C7—H7	0.9300

O1ⁱ—Ni—O1	180.0	O7—S—C4	107.03 (7)
O1ⁱ—Ni—O9	87.70 (5)	C1—O1—Ni	130.04 (11)
O1—Ni—O9	92.30 (5)	C1—O2—Na2	160.79 (11)
O1ⁱ—Ni—O9ⁱ	92.30 (5)	S—O5—Na1^vii	136.10 (8)
O1—Ni—O9ⁱ	87.70 (5)	S—O5—Na2^vi	132.45 (8)
O9—Ni—O9ⁱ	180.000 (1)	Na1^vii—O5—Na2^vi	88.98 (5)
O1ⁱ—Ni—O8ⁱ	90.09 (5)	S—O6—Na2^viii	152.77 (8)
O1—Ni—O8ⁱ	89.91 (5)	Ni—O8—H8A	120.7
O9—Ni—O8ⁱ	91.97 (5)	Ni—O8—H8B	122.2
O9ⁱ—Ni—O8ⁱ	88.03 (5)	H8A—O8—H8B	107.8
O1ⁱ—Ni—O8	89.91 (5)	Ni—O9—Na1	118.93 (6)
O1—Ni—O8	90.09 (5)	Ni—O9—H9A	114.0
O9—Ni—O8	88.03 (5)	Na1—O9—H9A	114.9
O9ⁱ—Ni—O8	91.97 (5)	Ni—O9—H9B	104.1
O8ⁱ—Ni—O8	180.0	Na1—O9—H9B	98.0
O5ⁱⁱ—Na1—O12	79.14 (5)	H9A—O9—H9B	103.4
O5ⁱⁱ—Na1—O13	85.05 (5)	Na1—O10—Na2	127.93 (6)
O12—Na1—O13	100.31 (5)	Na1—O10—H10A	119.3
O5ⁱⁱ—Na1—O9	151.89 (5)	Na2—O10—H10A	99.6
O12—Na1—O9	87.31 (5)	Na1—O10—H10B	106.5
O13—Na1—O9	121.84 (5)	Na2—O10—H10B	96.3
O5ⁱⁱ—Na1—O10	100.75 (5)	H10A—O10—H10B	102.5
O12—Na1—O10	160.96 (6)	Na2ⁱⁱⁱ—O11—Na1	87.39 (5)
O13—Na1—O10	98.64 (5)	Na2ⁱⁱⁱ—O11—H11A	122.8
O9—Na1—O10	84.27 (5)	Na1—O11—H11A	114.7
O5ⁱⁱ—Na1—O11	73.06 (5)	Na2ⁱⁱⁱ—O11—H11B	126.9
O12—Na1—O11	79.75 (5)	Na1—O11—H11B	98.8
O13—Na1—O11	157.76 (5)	H11A—O11—H11B	102.2
O9—Na1—O11	80.39 (5)	Na1—O12—Na2ⁱⁱⁱ	87.44 (5)
O10—Na1—O11	82.02 (5)	Na1—O12—H12A	102.6
O5ⁱⁱ—Na1—Na2ⁱⁱⁱ	47.04 (4)	Na2ⁱⁱⁱ—O12—H12A	133.0
O12—Na1—Na2ⁱⁱⁱ	47.71 (4)	Na1—O12—H12B	135.0
O13—Na1—Na2ⁱⁱⁱ	121.18 (4)	Na2ⁱⁱⁱ—O12—H12B	104.7
O9—Na1—Na2ⁱⁱⁱ	106.32 (4)	H12A—O12—H12B	99.8
O10—Na1—Na2ⁱⁱⁱ	119.01 (4)	Na1—O13—H13A	114.4
O11—Na1—Na2ⁱⁱⁱ	43.85 (3)	Na1—O13—H13B	110.5
O11^iv—Na2—O6^v	100.89 (5)	H13A—O13—H13B	106.1
O11^iv—Na2—O2	97.43 (5)	O2—C1—O1	125.48 (15)
O6^v—Na2—O2	82.41 (5)	O2—C1—C2	118.99 (14)
O11^iv—Na2—O5^vi	74.44 (5)	O1—C1—C2	115.47 (14)
O6^v—Na2—O5^vi	169.25 (5)	C7—C2—C3	119.56 (15)
O2—Na2—O5^vi	107.62 (5)	C7—C2—C1	119.68 (15)
O11^iv—Na2—O10	158.30 (6)	C3—C2—C1	120.73 (14)
O6^v—Na2—O10	100.73 (5)	C4—C3—C2	119.12 (15)
O2—Na2—O10	83.55 (5)	C4—C3—H3	120.4
O5^vi—Na2—O10	84.57 (5)	C2—C3—H3	120.4
O11^iv—Na2—O12^iv	81.40 (5)	C3—C4—C5	121.77 (15)
O6^v—Na2—O12^iv	95.27 (5)	C3—C4—S	117.02 (12)
O2—Na2—O12^iv	177.18 (6)	C5—C4—S	121.10 (12)
O5^vi—Na2—O12^iv	74.58 (5)	C4—C5—C6	119.09 (15)
O10—Na2—O12^iv	98.50 (5)	C4—C5—H5	120.5
O11^iv—Na2—Na1^iv	48.76 (4)	C6—C5—H5	120.5
O6^v—Na2—Na1^iv	125.80 (4)	C7—C6—C5	119.09 (15)
O2—Na2—Na1^iv	135.72 (4)	C7—C6—C8	119.18 (14)
O5^vi—Na2—Na1^iv	43.98 (3)	C5—C6—C8	121.73 (15)
O10—Na2—Na1^iv	117.34 (4)	C2—C7—C6	121.34 (15)
O12^iv—Na2—Na1^iv	44.84 (3)	C2—C7—H7	119.3
O6—S—O5	113.27 (8)	C6—C7—H7	119.3
O6—S—O7	112.03 (8)	O3—C8—O4	124.58 (16)
O5—S—O7	111.61 (8)	O3—C8—C6	116.32 (15)
O6—S—C4	107.10 (7)	O4—C8—C6	119.10 (15)
O5—S—C4	105.26 (8)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8A···O13^ix	0.84	2.03	2.861 (2)	173
O8—H8B···O4^vi	0.85	1.99	2.8130 (19)	162
O9—H9A···O7^v	0.85	2.16	2.9854 (17)	163
O9—H9B···O2	0.84	1.82	2.6168 (17)	159
O10—H10A···O7^vi	0.83	2.04	2.8553 (19)	167
O10—H10B···O3ⁱⁱⁱ	0.85	1.83	2.6615 (19)	165
O11—H11A···O7^v	0.89	1.90	2.7659 (18)	167
O11—H11B···O3ⁱⁱⁱ	0.87	1.92	2.783 (2)	175
O12—H12A···O1ⁱ	0.84	2.11	2.9470 (18)	173
O12—H12B···O4^x	0.89	2.04	2.8994 (19)	163
O13—H13A···O4^vi	0.84	1.94	2.733 (2)	157
O13—H13B···O6ⁱⁱ	0.88	2.21	2.9486 (19)	141
C7—H7···O11^iv	0.93	2.50	3.371 (2)	157

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

Experimental details

Crystal data
Chemical formula	[Na₄Ni(C₈H₃O₇S)₂(H₂O)₁₂]
M_r	853.19
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	295
a, b, c (Å)	7.8770 (9), 17.229 (2), 11.7474 (13)
β (°)	93.292 (4)
V (Å³)	1591.7 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.90
Crystal size (mm)	0.30 × 0.22 × 0.20

Data collection
Diffractometer	Rigaku R-AXIS RAPID IP diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.770, 0.835
No. of measured, independent and observed [I > 2σ(I)] reflections	17574, 3107, 2866
R_int	0.023
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.071, 1.08
No. of reflections	3107
No. of parameters	223
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.42, −0.40

Computer programs: PROCESS-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).

Selected bond lengths (Å) top

Ni—O1	2.0252 (11)	Ni—O9	2.0727 (11)
Ni—O8	2.0731 (14)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O8—H8A···O13ⁱ	0.84	2.03	2.861 (2)	173
O8—H8B···O4ⁱⁱ	0.85	1.99	2.8130 (19)	162
O9—H9A···O7ⁱⁱⁱ	0.85	2.16	2.9854 (17)	163
O9—H9B···O2	0.84	1.82	2.6168 (17)	159
O10—H10A···O7ⁱⁱ	0.83	2.04	2.8553 (19)	167
O10—H10B···O3^iv	0.85	1.83	2.6615 (19)	165
O11—H11A···O7ⁱⁱⁱ	0.89	1.90	2.7659 (18)	167
O11—H11B···O3^iv	0.87	1.92	2.783 (2)	175
O12—H12A···O1^v	0.84	2.11	2.9470 (18)	173
O12—H12B···O4^vi	0.89	2.04	2.8994 (19)	163
O13—H13A···O4ⁱⁱ	0.84	1.94	2.733 (2)	157
O13—H13B···O6^vii	0.88	2.21	2.9486 (19)	141
C7—H7···O11^viii	0.93	2.50	3.371 (2)	157

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

Acknowledgements

The work was supported by the ZIJIN project of Zhejiang University, China.

References

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