Hexaaqua­nickel(II) 2-methyl-5-nitro­benzene­sulfonate tetra­hydrate

In the title complex, [Ni(H₂O)₆](C₇H₆NO₅S)₂·4H₂O, each Ni^II cation lies on an inversion center and is octa­hedrally coordinated by six water mol­ecules. The anions do not coordinate to the nickel, but act as counter-ions. The crystal structure is composed of alternating layers of [Ni(H₂O)₆]²⁺ cations and anions. The [Ni(H₂O)₆]²⁺ cations, water mol­ecules and anions are connected through a complex pattern of hydrogen-bonding inter­actions, resulting in a three-dimensional supra­molecular network.

Key indicators

• Single-crystal X-ray study
• T = 292 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.030
• wR factor = 0.086
• Data-to-parameter ratio = 17.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Ni1    -   O6      ..       5.01 su

   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
   1 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
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick,1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: SHELXTL.

Hexaaquanickel(II) 2-methyl-5-nitrobenzenesulfonate tetrahydrate

Crystal data

[Ni(H2O)6](C7H6NO5)2·4H2O	Z = 1
Mr = 671.25	F(000) = 350
Triclinic, P1	Dx = 1.648 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.2421 (4) Å	Cell parameters from 512 reflections
b = 7.6642 (4) Å	θ = 2.9–27.7°
c = 13.7999 (7) Å	µ = 0.96 mm^−1
α = 74.077 (1)°	T = 292 K
β = 76.324 (1)°	Plate, green
γ = 68.212 (1)°	0.55 × 0.25 × 0.09 mm
V = 676.14 (6) Å^3

Data collection

Bruker SMART APEXII CCD area-detector diffractometer	3086 independent reflections
Radiation source: fine-focus sealed tube	2653 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.012
φ and ω scans	θmax = 27.7°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −4→9
Tmin = 0.750, Tmax = 0.910	k = −9→9
3911 measured reflections	l = −18→17

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.030	H-atom parameters constrained
wR(F^2) = 0.086	w = 1/[σ^2(Fo^2) + (0.0507P)^2 + 0.2656P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max < 0.001
3086 reflections	Δρmax = 0.41 e Å^−3
180 parameters	Δρmin = −0.34 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0149 (8)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
S1	0.24316 (7)	0.22883 (6)	0.23666 (3)	0.03144 (14)
O1	0.4185 (2)	0.0744 (2)	0.27170 (11)	0.0445 (3)
O2	0.2546 (3)	0.4171 (2)	0.22791 (11)	0.0527 (4)
O3	0.0571 (2)	0.2064 (3)	0.29729 (12)	0.0563 (4)
O9	0.2750 (3)	0.6696 (2)	−0.12437 (13)	0.0572 (4)
O10	0.3431 (3)	0.4968 (3)	−0.23573 (11)	0.0559 (4)
N1	0.2995 (3)	0.5194 (2)	−0.14765 (12)	0.0389 (4)
C2	0.2670 (3)	0.3655 (2)	0.03332 (13)	0.0304 (3)
H2	0.2776	0.4723	0.0482	0.036*
C1	0.2421 (2)	0.2129 (2)	0.11072 (12)	0.0284 (3)
C6	0.2211 (3)	0.0523 (2)	0.08953 (14)	0.0329 (4)
C4	0.2608 (3)	0.1991 (3)	−0.09080 (14)	0.0383 (4)
H4	0.2694	0.1941	−0.1584	0.046*
C5	0.2329 (3)	0.0498 (3)	−0.01247 (15)	0.0392 (4)
H5	0.2217	−0.0559	−0.0283	0.047*
C3	0.2756 (3)	0.3562 (3)	−0.06617 (13)	0.0325 (4)
C7	0.1873 (4)	−0.1132 (3)	0.17118 (17)	0.0481 (5)
H7C	0.1898	−0.2121	0.1403	0.058*
H7D	0.0590	−0.0700	0.2124	0.058*
H7E	0.2916	−0.1631	0.2131	0.058*
Ni1	0.0000	0.5000	0.5000	0.02654 (13)
O4	0.2735 (2)	0.48723 (19)	0.41168 (9)	0.0362 (3)
H4A	0.3141	0.5717	0.4206	0.054*
H4B	0.2626	0.5083	0.3491	0.054*
O5	−0.0481 (2)	0.78303 (18)	0.49885 (10)	0.0393 (3)
H5A	−0.1320	0.8562	0.4590	0.059*
H5B	−0.0635	0.8210	0.5535	0.059*
O6	−0.1390 (2)	0.5914 (2)	0.37375 (10)	0.0403 (3)
H6A	−0.2655	0.6378	0.3908	0.060*
H6B	−0.1152	0.4978	0.3457	0.060*
O7	0.5481 (2)	0.2558 (2)	0.57709 (11)	0.0411 (3)
H7A	0.5869	0.1461	0.6158	0.062*
H7B	0.5598	0.2357	0.5179	0.062*
O8	0.6965 (2)	0.1021 (2)	0.38826 (11)	0.0457 (3)
H8A	0.6089	0.1143	0.3531	0.068*
H8B	0.7553	0.1687	0.3406	0.068*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
S1	0.0373 (3)	0.0356 (2)	0.0235 (2)	−0.01112 (19)	−0.00562 (16)	−0.00971 (16)
O1	0.0489 (8)	0.0459 (8)	0.0378 (7)	−0.0108 (6)	−0.0184 (6)	−0.0038 (6)
O2	0.0922 (12)	0.0395 (8)	0.0344 (7)	−0.0216 (8)	−0.0185 (7)	−0.0128 (6)
O3	0.0451 (8)	0.0981 (13)	0.0348 (8)	−0.0309 (9)	0.0055 (6)	−0.0276 (8)
O9	0.0811 (12)	0.0426 (8)	0.0474 (9)	−0.0258 (8)	−0.0048 (8)	−0.0049 (6)
O10	0.0757 (11)	0.0710 (11)	0.0260 (7)	−0.0325 (9)	−0.0107 (7)	−0.0034 (7)
N1	0.0411 (9)	0.0456 (9)	0.0302 (8)	−0.0156 (7)	−0.0085 (6)	−0.0036 (6)
C2	0.0326 (8)	0.0303 (8)	0.0306 (8)	−0.0089 (7)	−0.0060 (6)	−0.0109 (6)
C1	0.0295 (8)	0.0318 (8)	0.0249 (8)	−0.0068 (6)	−0.0048 (6)	−0.0113 (6)
C6	0.0328 (8)	0.0320 (8)	0.0359 (9)	−0.0099 (7)	−0.0053 (7)	−0.0108 (7)
C4	0.0429 (10)	0.0490 (11)	0.0287 (9)	−0.0152 (8)	−0.0053 (7)	−0.0168 (8)
C5	0.0451 (10)	0.0398 (10)	0.0416 (10)	−0.0159 (8)	−0.0063 (8)	−0.0201 (8)
C3	0.0326 (8)	0.0372 (9)	0.0272 (8)	−0.0102 (7)	−0.0055 (6)	−0.0068 (7)
C7	0.0656 (14)	0.0392 (10)	0.0459 (11)	−0.0250 (10)	−0.0092 (10)	−0.0069 (8)
Ni1	0.02737 (18)	0.02968 (19)	0.02246 (18)	−0.00607 (12)	−0.00515 (11)	−0.00863 (11)
O4	0.0362 (7)	0.0460 (8)	0.0294 (7)	−0.0153 (6)	−0.0007 (5)	−0.0138 (6)
O5	0.0507 (8)	0.0327 (7)	0.0333 (7)	−0.0081 (6)	−0.0097 (6)	−0.0102 (5)
O6	0.0377 (7)	0.0492 (8)	0.0324 (7)	−0.0034 (6)	−0.0119 (6)	−0.0158 (6)
O7	0.0421 (7)	0.0431 (7)	0.0380 (7)	−0.0130 (6)	−0.0112 (6)	−0.0054 (6)
O8	0.0465 (8)	0.0455 (8)	0.0442 (8)	−0.0172 (6)	−0.0149 (6)	0.0019 (6)

Geometric parameters (Å, º)

S1—O2	1.4460 (15)	C7—H7C	0.9600
S1—O3	1.4512 (16)	C7—H7D	0.9600
S1—O1	1.4521 (15)	C7—H7E	0.9600
S1—C1	1.7775 (16)	Ni1—O4	2.049 (1)
O9—N1	1.218 (2)	Ni1—O5	2.062 (1)
O10—N1	1.225 (2)	Ni1—O6	2.044 (1)
N1—C3	1.469 (2)	O4—H4A	0.8500
C2—C3	1.380 (2)	O4—H4B	0.8500
C2—C1	1.386 (2)	O5—H5A	0.8500
C2—H2	0.9300	O5—H5B	0.8500
C1—C6	1.408 (2)	O6—H6A	0.8500
C6—C5	1.395 (3)	O6—H6B	0.8500
C6—C7	1.501 (3)	O7—H7A	0.8500
C4—C5	1.381 (3)	O7—H7B	0.8500
C4—C3	1.383 (3)	O8—H8A	0.8500
C4—H4	0.9300	O8—H8B	0.8500
C5—H5	0.9300
O2—S1—O3	112.30 (11)	C2—C3—C4	121.96 (17)
O2—S1—O1	112.79 (10)	C2—C3—N1	118.53 (16)
O3—S1—O1	112.01 (10)	C4—C3—N1	119.50 (16)
O2—S1—C1	105.64 (8)	C6—C7—H7C	109.5
O3—S1—C1	107.02 (8)	C6—C7—H7D	109.5
O1—S1—C1	106.52 (8)	H7C—C7—H7D	109.5
O9—N1—O10	123.52 (17)	C6—C7—H7E	109.5
O9—N1—C3	118.56 (16)	H7C—C7—H7E	109.5
O10—N1—C3	117.92 (17)	H7D—C7—H7E	109.5
C3—C2—C1	118.85 (15)	O6^i—Ni1—O6	180.000 (1)
C3—C2—H2	120.6	O6^i—Ni1—O4	88.62 (5)
C1—C2—H2	120.6	O6—Ni1—O4	91.38 (5)
C2—C1—C6	121.19 (15)	O4^i—Ni1—O4	180.00 (7)
C2—C1—S1	116.69 (12)	O6^i—Ni1—O5	91.42 (5)
C6—C1—S1	122.12 (13)	O6—Ni1—O5	88.58 (5)
C5—C6—C1	117.45 (16)	O4^i—Ni1—O5	91.26 (5)
C5—C6—C7	119.60 (17)	O4—Ni1—O5	88.74 (6)
C1—C6—C7	122.95 (17)	O5—Ni1—O5^i	180.0
C5—C4—C3	118.29 (17)	H4A—O4—H4B	109.0
C5—C4—H4	120.9	H5A—O5—H5B	114.1
C3—C4—H4	120.9	H6A—O6—H6B	108.4
C4—C5—C6	122.22 (17)	H7A—O7—H7B	106.4
C4—C5—H5	118.9	H8A—O8—H8B	93.4
C6—C5—H5	118.9

Symmetry code: (i) −x, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O4—H4A···O7^ii	0.85	1.94	2.779 (2)	169
O4—H4B···O2	0.85	2.00	2.777 (2)	151
O5—H5A···O8^iii	0.85	1.97	2.768 (2)	156
O5—H5B···O3^i	0.85	2.02	2.821 (2)	156
O6—H6A···O7^i	0.85	1.89	2.742 (2)	178
O6—H6B···O3	0.85	2.31	3.118 (3)	158
O7—H7A···O1^iv	0.85	1.96	2.777 (2)	160
O7—H7B···O8	0.85	2.15	2.957 (2)	157
O8—H8A···O1	0.85	2.12	2.953 (2)	167
O8—H8B···O3^v	0.85	2.23	2.914 (2)	137

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