Tetra­aqua­bis(3,5-dihydroxy­benzoato-κO)nickel(II) trihydrate

The covalently bonded monodentate carboxyl­ate groups in the title compound, [Ni(C₇H₅O₄)₂(H₂O)₄]·3H₂O, are trans to each other; the octa­hedrally coordinated Ni atom lies on a pseudo-center of inversion that relates the carboxyl­ate groups to each other as well as two coordinated water mol­ecules to the other two. Extensive hydrogen bonding leads to the formation of a three-dimensional network.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.037
• wR factor = 0.121
• Data-to-parameter ratio = 13.7

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT094_ALERT_2_B Ratio of Maximum / Minimum Residual Density ....       5.12
PLAT417_ALERT_2_B Short Inter D-H..H-D       H2W2   ..  H2W2    ..       2.08 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.44
PLAT417_ALERT_2_C Short Inter D-H..H-D       H4W2   ..  H4W2    ..       2.14 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........         14
PLAT731_ALERT_1_C Bond    Calc     0.85(2), Rep    0.845(9) ......       2.22 su-Rat
              O8   -H8O     1.555   1.555

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 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

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Computing details

Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Tetraaquabis(3,5-dihydroxybenzoato-κO)nickel(II) trihydrate

Crystal data

[Ni(C7H5O4)2(H2O)4]·3H2O	F(000) = 1024
Mr = 491.04	Dx = 1.662 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 18064 reflections
a = 9.250 (2) Å	θ = 3.0–27.5°
b = 19.736 (4) Å	µ = 1.07 mm^−1
c = 10.797 (2) Å	T = 295 K
β = 95.24 (2)°	Prism, green
V = 1962.9 (7) Å^3	0.38 × 0.27 × 0.21 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID IP diffractometer	4443 independent reflections
Radiation source: fine-focus sealed tube	3727 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.016
ω scans	θmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −11→12
Tmin = 0.618, Tmax = 0.807	k = −25→24
18979 measured reflections	l = −13→14

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.037	Hydrogen site location: difference Fourier map
wR(F^2) = 0.121	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0875P)^2 + 0.1403P] where P = (Fo^2 + 2Fc^2)/3
4443 reflections	(Δ/σ)max = 0.001
325 parameters	Δρmax = 1.74 e Å^−3
24 restraints	Δρmin = −0.34 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.49104 (2)	0.499669 (8)	0.74871 (2)	0.0212 (1)
O1	0.4426 (2)	0.4135 (1)	0.8411 (1)	0.0306 (3)
O2	0.5456 (2)	0.3354 (1)	0.7288 (1)	0.0320 (3)
O3	0.4192 (2)	0.1131 (1)	0.9225 (1)	0.0415 (4)
O4	0.1549 (2)	0.2791 (1)	1.1266 (1)	0.0344 (3)
O5	0.5381 (1)	0.5873 (1)	0.6603 (1)	0.0265 (3)
O6	0.4315 (2)	0.6621 (1)	0.7764 (1)	0.0326 (3)
O7	0.6020 (2)	0.8890 (1)	0.6349 (2)	0.0451 (4)
O8	0.8090 (2)	0.7277 (1)	0.3745 (1)	0.0350 (3)
O1w	0.2818 (2)	0.5051 (1)	0.6709 (2)	0.0450 (4)
O2w	0.4280 (2)	0.5519 (1)	0.9043 (1)	0.0306 (3)
O3w	0.7016 (2)	0.4977 (1)	0.8269 (2)	0.0352 (4)
O4w	0.5570 (2)	0.4459 (1)	0.5980 (1)	0.0332 (3)
O5w	0.5809 (2)	0.0928 (1)	0.7247 (2)	0.0545 (4)
O6w	0.3889 (2)	0.0138 (1)	0.5907 (2)	0.0731 (6)
O7w	0.4202 (2)	0.9015 (1)	0.8294 (2)	0.0452 (4)
C1	0.4696 (2)	0.3524 (1)	0.8136 (2)	0.0223 (3)
C2	0.4052 (2)	0.2980 (1)	0.8891 (1)	0.0222 (3)
C3	0.4433 (2)	0.2309 (1)	0.8694 (2)	0.0268 (4)
C4	0.3834 (2)	0.1803 (1)	0.9367 (2)	0.0270 (4)
C5	0.2876 (2)	0.1951 (1)	1.0242 (2)	0.0271 (4)
C6	0.2497 (2)	0.2622 (1)	1.0428 (2)	0.0248 (3)
C7	0.3079 (2)	0.3140 (1)	0.9757 (2)	0.0243 (3)
C8	0.5110 (2)	0.6474 (1)	0.6925 (2)	0.0212 (3)
C9	0.5799 (2)	0.7040 (1)	0.6252 (1)	0.0211 (3)
C10	0.5567 (2)	0.7703 (1)	0.6617 (2)	0.0260 (3)
C11	0.6202 (2)	0.8226 (1)	0.6013 (2)	0.0279 (4)
C12	0.7045 (2)	0.8100 (1)	0.5039 (2)	0.0290 (4)
C13	0.7271 (2)	0.7435 (1)	0.4693 (2)	0.0252 (3)
C14	0.6662 (2)	0.6901 (1)	0.5301 (2)	0.0241 (3)
H3o	0.464 (3)	0.106 (1)	0.858 (2)	0.050*
H4o	0.121 (2)	0.243 (1)	1.156 (2)	0.041*
H7o	0.546 (2)	0.891 (1)	0.692 (2)	0.054*
H8o	0.840 (2)	0.765 (1)	0.347 (2)	0.042*
H1w1	0.241 (2)	0.539 (1)	0.638 (2)	0.054*
H1w2	0.230 (2)	0.471 (1)	0.666 (2)	0.054*
H2w1	0.432 (2)	0.590 (1)	0.871 (2)	0.037*
H2w2	0.483 (2)	0.550 (1)	0.972 (1)	0.037*
H3w1	0.748 (2)	0.461 (1)	0.840 (2)	0.042*
H3w2	0.758 (2)	0.531 (1)	0.815 (2)	0.042*
H4w1	0.552 (3)	0.407 (1)	0.631 (2)	0.040*
H4w2	0.510 (2)	0.448 (1)	0.527 (1)	0.040*
H5w1	0.518 (2)	0.073 (1)	0.677 (2)	0.065*
H5w2	0.605 (3)	0.130 (1)	0.695 (2)	0.065*
H6w1	0.303 (2)	0.024 (2)	0.610 (2)	0.088*
H6w2	0.388 (3)	0.015 (2)	0.510 (1)	0.088*
H7w1	0.463 (3)	0.903 (1)	0.903 (1)	0.054*
H7w2	0.380 (3)	0.863 (1)	0.833 (2)	0.054*
H3	0.5084	0.2203	0.8116	0.032*
H5	0.2491	0.1606	1.0699	0.033*
H7	0.2821	0.3588	0.9886	0.029*
H10	0.4991	0.7794	0.7260	0.031*
H12	0.7451	0.8456	0.4625	0.035*
H14	0.6833	0.6456	0.5073	0.029*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0284 (2)	0.0148 (2)	0.0220 (2)	0.0008 (1)	0.0110 (1)	0.0028 (1)
O1	0.0472 (8)	0.0156 (5)	0.0322 (6)	0.0003 (5)	0.0213 (6)	0.0037 (5)
O2	0.0467 (8)	0.0218 (6)	0.0309 (6)	0.0036 (5)	0.0218 (6)	0.0039 (5)
O3	0.0559 (9)	0.0168 (6)	0.0565 (9)	0.0022 (5)	0.0304 (7)	0.0029 (6)
O4	0.0427 (7)	0.0241 (6)	0.0404 (7)	−0.0005 (5)	0.0251 (6)	0.0033 (5)
O5	0.0415 (7)	0.0137 (5)	0.0266 (6)	−0.0013 (5)	0.0164 (5)	0.0018 (4)
O6	0.0487 (8)	0.0197 (6)	0.0335 (7)	0.0036 (5)	0.0249 (6)	0.0034 (5)
O7	0.0569 (9)	0.0156 (6)	0.068 (1)	−0.0044 (6)	0.0363 (8)	−0.0046 (6)
O8	0.0477 (8)	0.0240 (6)	0.0376 (7)	−0.0049 (5)	0.0275 (6)	0.0001 (5)
O1w	0.0339 (8)	0.0306 (8)	0.069 (1)	−0.0055 (5)	−0.0057 (8)	0.0132 (7)
O2w	0.0460 (8)	0.0223 (6)	0.0256 (6)	0.0041 (5)	0.0143 (6)	0.0028 (5)
O3w	0.0309 (8)	0.0285 (8)	0.0462 (9)	0.0019 (5)	0.0033 (7)	0.0058 (5)
O4w	0.0540 (9)	0.0213 (6)	0.0263 (6)	0.0003 (5)	0.0151 (6)	0.0001 (5)
O5w	0.058 (1)	0.0324 (8)	0.077 (1)	0.0042 (7)	0.0248 (9)	−0.0019 (8)
O6w	0.058 (1)	0.102 (2)	0.060 (1)	0.016 (1)	0.010 (1)	−0.001 (1)
O7w	0.0522 (9)	0.0308 (7)	0.0541 (9)	0.0081 (6)	0.0133 (7)	0.0007 (7)
C1	0.0272 (8)	0.0173 (7)	0.0231 (7)	−0.0005 (6)	0.0067 (6)	0.0024 (6)
C2	0.0269 (8)	0.0191 (7)	0.0213 (7)	−0.0024 (6)	0.0066 (6)	0.0026 (6)
C3	0.0338 (9)	0.0184 (7)	0.0301 (8)	−0.0001 (6)	0.0128 (7)	0.0013 (6)
C4	0.0312 (9)	0.0167 (7)	0.0342 (8)	−0.0009 (6)	0.0093 (7)	0.0019 (6)
C5	0.0308 (9)	0.0198 (7)	0.0322 (8)	−0.0021 (6)	0.0104 (7)	0.0068 (6)
C6	0.0257 (8)	0.0252 (8)	0.0248 (8)	−0.0010 (6)	0.0087 (6)	0.0015 (6)
C7	0.0306 (8)	0.0173 (7)	0.0263 (8)	0.0001 (6)	0.0091 (7)	0.0013 (6)
C8	0.0254 (8)	0.0180 (7)	0.0211 (7)	−0.0001 (6)	0.0069 (6)	0.0011 (6)
C9	0.0243 (7)	0.0160 (7)	0.0235 (7)	−0.0024 (6)	0.0051 (6)	0.0025 (6)
C10	0.0303 (8)	0.0195 (7)	0.0300 (8)	−0.0007 (6)	0.0130 (7)	−0.0008 (6)
C11	0.0313 (9)	0.0150 (7)	0.0388 (9)	−0.0022 (6)	0.0111 (7)	−0.0006 (6)
C12	0.0311 (9)	0.0204 (8)	0.0375 (9)	−0.0033 (6)	0.0141 (7)	0.0044 (7)
C13	0.0275 (8)	0.0221 (8)	0.0272 (7)	−0.0022 (6)	0.0091 (7)	0.0021 (6)
C14	0.0298 (8)	0.0174 (7)	0.0262 (8)	−0.0012 (6)	0.0085 (7)	0.0000 (6)

Geometric parameters (Å, º)

Ni1—O1	2.042 (1)	C11—C12	1.387 (2)
Ni1—O5	2.042 (1)	C12—C13	1.387 (2)
Ni1—O1w	2.041 (2)	C13—C14	1.387 (2)
Ni1—O2w	2.098 (1)	O3—H3o	0.85 (1)
Ni1—O3w	2.051 (2)	O4—H4o	0.85 (1)
Ni1—O4w	2.080 (1)	O7—H7o	0.84 (1)
O1—C1	1.272 (2)	O1w—H1w1	0.83 (1)
O2—C1	1.250 (2)	O1w—H1w2	0.83 (1)
O3—C4	1.379 (2)	O2w—H2w1	0.84 (1)
O4—C6	1.358 (2)	O2w—H2w2	0.85 (1)
O5—C8	1.2671 (19)	O3w—H3w1	0.84 (1)
O6—C8	1.253 (2)	O3w—H3w2	0.85 (1)
O7—C11	1.374 (2)	O4w—H4w1	0.85 (1)
O8—C13	1.364 (2)	O4w—H4w2	0.84 (1)
O8—H8o	0.845 (9)	O5w—H5w1	0.84 (1)
C1—C2	1.504 (2)	O5w—H5w2	0.85 (1)
C2—C3	1.391 (2)	O6w—H6w1	0.86 (1)
C2—C7	1.393 (2)	O6w—H6w2	0.87 (1)
C3—C4	1.381 (2)	O7w—H7w1	0.86 (1)
C4—C5	1.384 (2)	O7w—H7w2	0.85 (1)
C5—C6	1.389 (2)	C3—H3	0.93
C6—C7	1.389 (2)	C5—H5	0.93
C8—C9	1.504 (2)	C7—H7	0.93
C9—C14	1.385 (2)	C10—H10	0.93
C9—C10	1.390 (2)	C12—H12	0.93
C10—C11	1.381 (2)	C14—H14	0.93
O1—Ni1—O5	178.47 (4)	O7—C11—C10	121.3 (2)
O1—Ni1—O1w	90.16 (6)	O7—C11—C12	117.5 (1)
O1—Ni1—O2w	85.90 (5)	C10—C11—C12	121.2 (2)
O1—Ni1—O3w	91.48 (6)	C13—C12—C11	118.9 (2)
O1—Ni1—O4w	92.91 (5)	O8—C13—C12	121.7 (2)
O5—Ni1—O1w	89.85 (6)	O8—C13—C14	117.3 (2)
O5—Ni1—O2w	92.57 (5)	C12—C13—C14	120.9 (2)
O5—Ni1—O3w	88.48 (6)	C9—C14—C13	119.2 (2)
O5—Ni1—O4w	88.62 (5)	C4—O3—H3o	113 (2)
O1w—Ni1—O2w	88.92 (8)	C6—O4—H4o	110 (2)
O1w—Ni1—O3w	178.04 (4)	C11—O7—H7o	109 (2)
O1w—Ni1—O4w	92.29 (8)	C13—O8—H8o	108 (2)
O2w—Ni1—O3w	90.13 (7)	Ni1—O1w—H1w1	126 (2)
O2w—Ni1—O4w	178.31 (4)	Ni1—O1w—H1w2	120 (2)
O3w—Ni1—O4w	88.70 (7)	H1w1—O1w—H1w2	114 (2)
C1—O1—Ni1	128.3 (1)	Ni1—O2w—H2w1	94 (2)
C8—O5—Ni1	127.5 (1)	Ni1—O2w—H2w2	119 (2)
O2—C1—O1	124.1 (2)	H2w1—O2w—H2w2	112 (1)
O2—C1—C2	118.9 (2)	Ni1—O3w—H3w1	123 (1)
O1—C1—C2	117.1 (1)	Ni1—O3w—H3w2	120 (1)
C3—C2—C7	120.5 (1)	H3w1—O3w—H3w2	112 (2)
C3—C2—C1	118.6 (1)	Ni1—O4w—H4w1	96 (2)
C7—C2—C1	121.0 (2)	Ni1—O4w—H4w2	122 (2)
C4—C3—C2	119.2 (2)	H4w1—O4w—H4w2	112 (1)
O3—C4—C3	121.7 (2)	H5w1—O5w—H5w2	112 (2)
O3—C4—C5	117.0 (1)	H6w1—O6w—H6w2	108 (2)
C3—C4—C5	121.3 (2)	H7w1—O7w—H7w2	100 (2)
C4—C5—C6	119.0 (2)	C4—C3—H3	120.4
O4—C6—C5	121.2 (2)	C2—C3—H3	120.4
O4—C6—C7	118.0 (2)	C4—C5—H5	120.5
C5—C6—C7	120.8 (2)	C6—C5—H5	120.5
C6—C7—C2	119.2 (2)	C6—C7—H7	120.4
O6—C8—O5	124.0 (2)	C2—C7—H7	120.4
O6—C8—C9	118.7 (1)	C11—C10—H10	120.4
O5—C8—C9	117.3 (1)	C9—C10—H10	120.4
C14—C9—C10	120.7 (1)	C13—C12—H12	120.6
C14—C9—C8	120.7 (1)	C11—C12—H12	120.6
C10—C9—C8	118.6 (1)	C9—C14—H14	120.4
C11—C10—C9	119.1 (2)	C13—C14—H14	120.4
O1w—Ni1—O1—C1	101.1 (2)	O4—C6—C7—C2	−179.9 (2)
O3w—Ni1—O1—C1	−80.0 (2)	C5—C6—C7—C2	0.0 (3)
O4w—Ni1—O1—C1	8.8 (2)	C3—C2—C7—C6	0.3 (3)
O2w—Ni1—O1—C1	−170.0 (2)	C1—C2—C7—C6	179.4 (2)
O1w—Ni1—O5—C8	80.0 (2)	Ni1—O5—C8—O6	−10.5 (3)
O3w—Ni1—O5—C8	−99.0 (2)	Ni1—O5—C8—C9	169.3 (1)
O4w—Ni1—O5—C8	172.2 (2)	O6—C8—C9—C14	−178.7 (2)
O2w—Ni1—O5—C8	−9.0 (2)	O5—C8—C9—C14	1.5 (2)
Ni1—O1—C1—O2	7.5 (3)	O6—C8—C9—C10	2.2 (2)
Ni1—O1—C1—C2	−172.6 (2)	O5—C8—C9—C10	−177.6 (2)
O2—C1—C2—C3	5.8 (2)	C14—C9—C10—C11	0.5 (3)
O1—C1—C2—C3	−174.1 (2)	C8—C9—C10—C11	179.5 (2)
O2—C1—C2—C7	−173.4 (2)	C9—C10—C11—O7	−179.3 (2)
O1—C1—C2—C7	6.7 (2)	C9—C10—C11—C12	1.0 (3)
C7—C2—C3—C4	0.1 (3)	O7—C11—C12—C13	178.9 (2)
C1—C2—C3—C4	−179.1 (2)	C10—C11—C12—C13	−1.4 (3)
C2—C3—C4—O3	−178.9 (2)	C11—C12—C13—O8	−179.9 (2)
C2—C3—C4—C5	−0.8 (3)	C11—C12—C13—C14	0.3 (3)
O3—C4—C5—C6	179.2 (2)	C10—C9—C14—C13	−1.5 (3)
C3—C4—C5—C6	1.0 (3)	C8—C9—C14—C13	179.5 (2)
C4—C5—C6—O4	179.3 (2)	O8—C13—C14—C9	−178.7 (2)
C4—C5—C6—C7	−0.7 (3)	C12—C13—C14—C9	1.1 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O3—H3o···O5w	0.85 (1)	1.90 (1)	2.746 (2)	175 (3)
O4—H4o···O2^i	0.85 (1)	1.90 (1)	2.749 (2)	178 (2)
O7—H7o···O7w	0.84 (1)	1.98 (1)	2.818 (2)	175 (2)
O8—H8o···O6^ii	0.85 (1)	1.87 (1)	2.711 (2)	171 (2)
O1w—H1w1···O3^iii	0.83 (1)	2.14 (1)	2.944 (2)	162 (2)
O1w—H1w2···O7w^iv	0.83 (1)	1.95 (1)	2.771 (2)	169 (2)
O2w—H2w1···O6	0.84 (1)	1.75 (1)	2.578 (2)	170 (2)
O2w—H2w2···O1^v	0.85 (1)	2.19 (1)	2.976 (2)	152 (2)
O3w—H3w1···O7^vi	0.84 (1)	1.99 (1)	2.818 (2)	167 (2)
O3w—H3w2···O5w^vii	0.85 (1)	2.01 (1)	2.843 (2)	168 (2)
O4w—H4w1···O2	0.85 (1)	1.77 (1)	2.606 (2)	168 (2)
O4w—H4w2···O5^viii	0.84 (1)	2.15 (1)	2.921 (2)	153 (2)
O5w—H5w1···O6w	0.84 (1)	1.86 (1)	2.685 (3)	169 (2)
O5w—H5w2···O4^ix	0.85 (1)	2.00 (1)	2.848 (2)	178 (3)
O6w—H6w1···O2w^iv	0.86 (1)	2.20 (1)	3.031 (3)	162 (2)
O6w—H6w2···O7^viii	0.87 (1)	2.47 (2)	3.108 (3)	131 (3)
O7w—H7w1···O3^v	0.86 (1)	2.12 (1)	2.956 (2)	168 (2)
O7w—H7w2···O8^x	0.85 (1)	1.98 (1)	2.808 (2)	168 (2)

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