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In the title compound, [Ni(H2O)6](C6H4NO3)2, the NiII atom lies on a special position of 2/m site symmetry in an octa­hedron made up of water mol­ecules. The anions show orientational disorder over mirror planes and are linked together by a pair of N—H...O hydrogen bonds into a dianion. The complex cations and dianions are connected through O—H...O hydrogen bonds to form a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805014923/ob6517sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805014923/ob6517Isup2.hkl
Contains datablock I

CCDC reference: 274605

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](i-O) = 0.003 Å
  • Disorder in main residue
  • R factor = 0.041
  • wR factor = 0.111
  • Data-to-parameter ratio = 8.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Ni1 PLAT301_ALERT_3_B Main Residue Disorder ......................... 29.00 Perc.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.519 0.794 Tmin' and Tmax expected: 0.664 0.785 RR' = 0.773 Please check that your absorption correction is appropriate. REFLT03_ALERT_3_C Reflection count < 95% complete From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _diffrn_reflns_theta_full 27.50 From the CIF: _reflns_number_total 974 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 1030 Completeness (_total/calc) 94.56% PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.95 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.76 PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.62 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.06 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat O1W -H1W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat O2W -H2W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat O2W -H2W2 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat O1W -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat O2W -H3# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat O2W -H3# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat O2W -H4# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(4), Rep 0.840(10) ...... 4.00 su-Rat O2W -H4# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.83(3), Rep 1.830(10) ...... 3.00 su-Rat H1# -O1 1.555 1.555 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 19 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 11 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 7 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: atomic coordinates taken from the isostructural Zn analog (Zhang et al., 2005); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Hexaaquanickel(II) bis(6-hydroxypyridine-3-carboxylate) top
Crystal data top
[Ni(H2O)6](C6H4NO3)2F(000) = 460
Mr = 443.01Dx = 1.729 Mg m3
Monoclinic, C2/mMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1513 reflections
a = 11.556 (1) Åθ = 2.7–27.4°
b = 9.767 (1) ŵ = 1.21 mm1
c = 7.5422 (8) ÅT = 295 K
β = 91.320 (2)°Block, light green
V = 851.1 (2) Å30.33 × 0.28 × 0.20 mm
Z = 2
Data collection top
Bruker APEX area-detector
diffractometer
974 independent reflections
Radiation source: fine-focus sealed tube939 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.036
φ and ω scansθmax = 27.5°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1414
Tmin = 0.519, Tmax = 0.794k = 1212
2640 measured reflectionsl = 79
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.111H atoms treated by a mixture of independent and constrained refinement
S = 1.12 w = 1/[σ2(Fo2) + (0.0467P)2 + 1.687P]
where P = (Fo2 + 2Fc2)/3
974 reflections(Δ/σ)max = 0.001
113 parametersΔρmax = 0.44 e Å3
14 restraintsΔρmin = 0.30 e Å3
Special details top

Refinement. A dimensionless value, 2µ*r (r = equivalent radius of crystal) of 0.39, was used in the absorption correction step.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.50000.50000.50000.0247 (2)
O10.8316 (2)0.6132 (2)0.6587 (4)0.047 (1)
O21.3234 (3)0.5755 (5)0.9708 (6)0.038 (1)0.50
O1w0.6252 (2)0.6436 (3)0.5003 (4)0.059 (1)
O2w0.4911 (3)0.50000.2271 (5)0.069 (1)
N11.1464 (4)0.6540 (6)0.8856 (7)0.037 (1)0.50
C11.0379 (5)0.6374 (7)0.8162 (7)0.033 (2)0.50
C21.0004 (4)0.510 (1)0.7601 (6)0.032 (1)0.50
C31.0769 (5)0.4022 (7)0.7772 (9)0.033 (2)0.50
C41.1872 (5)0.4178 (7)0.8480 (9)0.036 (2)0.50
C51.2241 (5)0.5484 (6)0.9041 (8)0.029 (1)0.50
C60.8782 (3)0.50000.6855 (5)0.030 (1)
H2o1.32460.65781.00730.046*0.50
H1w10.688 (2)0.623 (3)0.551 (5)0.05 (1)*
H1w20.626 (2)0.7228 (18)0.457 (4)0.04 (1)*
H2w10.429 (2)0.50000.167 (6)0.07 (2)*
H2w20.549 (3)0.50000.161 (6)0.06 (2)*
H10.98850.71230.80640.040*0.50
H31.05310.31570.73950.040*0.50
H41.23650.34290.85860.043*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0177 (3)0.0296 (4)0.0264 (4)0.0000.0046 (2)0.000
O10.043 (1)0.035 (1)0.062 (2)0.0030 (9)0.023 (1)0.008 (1)
O20.022 (2)0.051 (2)0.040 (3)0.002 (2)0.010 (2)0.005 (2)
O1w0.031 (1)0.044 (1)0.099 (2)0.012 (1)0.028 (1)0.031 (1)
O2w0.033 (2)0.150 (4)0.025 (2)0.0000.006 (1)0.000
N10.028 (2)0.037 (3)0.044 (3)0.001 (2)0.017 (2)0.000 (2)
C10.027 (4)0.037 (4)0.036 (4)0.001 (3)0.013 (3)0.000 (3)
C20.025 (2)0.045 (4)0.025 (2)0.012 (6)0.006 (2)0.008 (5)
C30.028 (4)0.035 (4)0.037 (4)0.003 (3)0.002 (3)0.006 (3)
C40.030 (4)0.031 (4)0.047 (5)0.000 (3)0.005 (3)0.006 (3)
C50.025 (3)0.031 (3)0.032 (4)0.004 (2)0.002 (2)0.001 (2)
C60.029 (2)0.034 (2)0.027 (2)0.0000.008 (2)0.000
Geometric parameters (Å, º) top
Ni1—O1w2.015 (2)C3—C41.379 (7)
Ni1—O1wi2.015 (2)C4—C51.408 (7)
Ni1—O1wii2.015 (2)C6—O1iii1.244 (3)
Ni1—O1wiii2.015 (2)C6—C2iii1.512 (6)
Ni1—O2w2.059 (4)O2—H2O0.85
Ni1—O2wii2.059 (4)O1w—H1w10.84 (1)
O1—C61.244 (3)O1w—H1w20.84 (1)
O2—C51.270 (7)O2w—H2w10.84 (1)
N1—C11.357 (7)O2w—H2w20.84 (1)
N1—C51.372 (6)C1—H10.93
C1—C21.379 (9)C3—H30.93
C2—C31.380 (8)C4—H40.93
C2—C61.512 (6)
O1wii—Ni1—O1w180C3—C4—C5119.2 (6)
O1wii—Ni1—O1wiii91.8 (2)O2—C5—N1117.8 (5)
O1w—Ni1—O1wiii88.2 (2)O2—C5—C4124.9 (5)
O1wii—Ni1—O1wi88.2 (2)N1—C5—C4117.2 (6)
O1w—Ni1—O1wi91.8 (2)O1iii—C6—O1125.4 (4)
O1wiii—Ni1—O1wi180O1iii—C6—C2iii113.5 (5)
O1wii—Ni1—O2wii91.2 (1)O1—C6—C2iii121.1 (5)
O1w—Ni1—O2wii88.8 (1)O1iii—C6—C2121.1 (5)
O1wiii—Ni1—O2wii88.8 (1)O1—C6—C2113.5 (5)
O1wi—Ni1—O2wii91.2 (1)Ni1—O1w—H1w1117 (2)
O1wii—Ni1—O2w88.8 (1)Ni1—O1w—H1w2131 (2)
O1w—Ni1—O2w91.2 (1)H1w1—O1w—H1w2112 (2)
O1wiii—Ni1—O2w91.2 (1)Ni1—O2w—H2w1124 (4)
O1wi—Ni1—O2w88.8 (1)Ni1—O2w—H2w2125 (4)
O2wii—Ni1—O2w180H2w1—O2w—H2w2111 (2)
C1—N1—C5123.1 (6)N1—C1—H1119.8
N1—C1—C2120.5 (6)C2—C1—H1119.8
C3—C2—C1117.6 (5)C4—C3—H3118.8
C3—C2—C6125.1 (8)C2—C3—H3118.8
C1—C2—C6117.2 (7)C3—C4—H4120.4
C4—C3—C2122.4 (6)C5—C4—H4120.4
C5—N1—C1—C20.0 (3)C3—C4—C5—O2179.9 (6)
N1—C1—C2—C30.1 (3)C3—C4—C5—N10.4 (7)
N1—C1—C2—C6179.6 (4)C3—C2—C6—O1iii11.3 (7)
C1—C2—C3—C40.3 (6)C1—C2—C6—O1iii168.4 (4)
C6—C2—C3—C4179.4 (5)C3—C2—C6—O1169.9 (4)
C2—C3—C4—C50.5 (8)C1—C2—C6—O110.4 (5)
C1—N1—C5—O2180.0 (5)C3—C2—C6—C2iii10.7 (4)
C1—N1—C5—C40.2 (6)C1—C2—C6—C2iii169.0 (3)
Symmetry codes: (i) x+1, y, z+1; (ii) x+1, y+1, z+1; (iii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O10.84 (1)1.83 (1)2.659 (3)169 (3)
O1w—H1w2···O1iv0.84 (1)1.90 (1)2.713 (3)164 (3)
O2w—H2w1···O2v0.84 (1)2.03 (2)2.804 (5)152 (3)
O2w—H2w1···O2v0.84 (1)2.03 (2)2.804 (5)152 (3)
O2w—H2w2···O2vi0.84 (1)1.94 (1)2.741 (6)158 (1)
O2w—H2w2···O2vii0.84 (1)1.94 (1)2.741 (6)158 (1)
O2—H2o···N1viii0.852.032.874 (7)170
Symmetry codes: (iv) x+3/2, y+3/2, z+1; (v) x1, y, z1; (vi) x+2, y+1, z+1; (vii) x+2, y, z+1; (viii) x+5/2, y+3/2, z+2.
 

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