Literature DB >> 21582369

Poly[octa-μ-aqua-tetra-aqua-bis(μ(4)-5-sulfonatobenzene-1,3-dicarboxyl-ato)nickel(II)tetra-sodium].

Bing-Yu Zhang¹, Jing-Jing Nie, Duan-Jun Xu.

Abstract

In the crystal structure of the title compound, [Na(4)Ni(C(8)H(3)O(7)S)(2)(H(2)O)(12)](n), the Ni(II) cation occupies an inversion centre and is coordinated by the carboxyl groups of the sulfoisophthalate trianions and water mol-ecules in a distorted octa-hedral geometry. Two independent Na(I) atoms are connected by the carboxyl and sulfonate groups of the sulfoisophthalate ligands anions and water mol-ecules in a distorted octa-hedral geometry. The sulfoisophthalate ligands and coordinated water mol-ecules 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.

Entities: Chemical Disease Gene Species

Year: 2009 PMID： 21582369 PMCID： PMC2969070 DOI： 10.1107/S1600536809009489

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

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 = 853.19 Monoclinic, 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[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 0.071 S = 1.08 3107 reflections 223 parameters H-atom parameters constrained Δρmax = 0.42 e Å−3 Δρmin = −0.40 e Å−3 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 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809009489/ng2561sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809009489/ng2561Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[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

Rigaku R-AXIS RAPID IP diffractometer	3107 independent reflections
Radiation source: fine-focus sealed tube	2866 reflections with I > 2σ(I)
graphite	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 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

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.

	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)

	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)

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)

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

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) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) .

2 in total

1. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

2. Poly[octa-μ-aqua-tetra-aqua-bis(μ-5-sul-fon-atobenzene-1,3-dicarboxyl-ato)cobalt(II)tetra-sodium].

Authors: Bing-Yu Zhang; Jing-Jing Nie; Duan-Jun Xu
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-03-11

2 in total