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In the title compound, {[Ni(C16H17FN3O3)2]·2H2O}n, the NiII atom (site symmetry \overline{1}) exists in a distorted trans-NiN2O4 octa­hedral geometry defined by two monodentate N-bonded and two bidentate O,O-bonded 1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-yl)-1,4-dihydro­quinoline-3-carboxyl­ate (norf) mono­anions. The extended two-dimensional structure is a square grid. N—H...O hydrogen bonds are present in the crystal structure. The water O atom is disordered over two positions; the site occupancy factors are ca. 0.77 and 0.23.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807060813/hb2657sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807060813/hb2657Isup2.hkl
Contains datablock I

CCDC reference: 672754

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.003 Å
  • H-atom completeness 90%
  • Disorder in solvent or counterion
  • R factor = 0.035
  • wR factor = 0.108
  • Data-to-parameter ratio = 13.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT430_ALERT_2_B Short Inter D...A Contact O1W .. O2 .. 2.80 Ang. PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O2W .. 2.79 Ang.
Alert level C CHEMW01_ALERT_1_C The difference between the given and expected weight for compound is greater 1 mass unit. Check that all hydrogen atoms have been taken into account. PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.60 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - O1 .. 5.39 su PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.03 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O1W PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O2W PLAT411_ALERT_2_C Short Inter H...H Contact H5 .. H14B .. 2.11 Ang.
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C32 H38 F2 N6 Ni1 O8 Atom count from the _atom_site data: C32 H34 F2 N6 Ni1 O8 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum C32 H38 F2 N6 Ni O8 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 64.00 64.00 0.00 H 76.00 68.00 8.00 F 4.00 4.00 0.00 N 12.00 12.00 0.00 Ni 2.00 2.00 0.00 O 16.00 16.00 0.00 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

Norfloxacin (Hnorf, 1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl) -3-quinoline carboxylic acid) is member of the class of quinolones that is used to treat infections (Mizuki et al., 1996). Cadmium(II) and zinc(II) derivatives of norf have been reported (Chen et al., 2001; Wang et al., 2004). The title nickel(II) derivative, (I), a two-dimensional coordination polymer in which the anion acts in a bridging mode, is reported here (Fig. 1).

The Ni(II) atom in (I) is coordinated by four oxygen atoms and two N atoms from four norfloxacin ligands (two monodentate-N and two O,O-bidentate) to form a square grid propagating in (100) (Fig. 2). The disordered, uncoordinated, water molecules occupy the cavities.

Related literature top

For the cadmium and zinc complexes of the norf anion, see: Chen et al. (2001); Wang et al.(2004). For background on the medicinal uses of Norfloxacin, see: Mizuki et al. (1996).

Experimental top

A mixture of Ni(NO3)2.6H2O (0.07 g, 0.25 mmol), Hnorf (0.16 g, 0.5 mmol), and water (12 ml) was stirred for 20 min in air. The mixture was then transferred to a 23 ml Teflon-lined hydrothermal bomb. The bomb was kept at 433 K for 72 h under autogenous pressure. After cooling, green prisms of (I) were obtained from the reaction mixture.

Refinement top

The carbon-bound H atoms were positioned geometrically (C—H = 0.93–0.97 Å) and were included in the refinement in the riding model approximation, with U(H) = 1.2Ueq(C). The H on Nitrogen atoms were located in a difference Fourier map, and were refined with a distance restraint of N—H = 0.86 (1) /%A and with Uiso(H) = 1.2Ueq(N).

The water molecules is disordered over two sites in a 0.771 (7):0.229 (7) ratio. The water H atoms could not be located in the present study.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); 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, 1998); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), extended to show the Ni coordination, showing 50% displacement ellipsoids for the non-hydrogen atoms. Symmetry codes: (i) x, y, z; (ii) -x, y + 1/2, -z + 1/2; (iii) -x, -y, -z; (iv) x, -y - 1/2, z - 1/2.
[Figure 2] Fig. 2. A view of part of a two-dimensional polymeric sheet in (I) showing the square-grid connectivity (H atoms and water molecule O atoms omitted for clarity).
Poly[[bis[µ-1-ethyl-6-fluoro-4-oxo-7-(piperazin-1-yl)-1,4-dihydroquinoline- 3-carboxylato]nickel(II)] dihydrate] top
Crystal data top
[Ni(C16H17FN3O3)2]·2H2OF(000) = 756
Mr = 727.36Dx = 1.474 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 8072 reflections
a = 5.8389 (2) Åθ = 1.8–25.5°
b = 21.5704 (8) ŵ = 0.66 mm1
c = 13.2408 (4) ÅT = 295 K
β = 100.763 (1)°Prism, green
V = 1638.31 (10) Å30.32 × 0.26 × 0.18 mm
Z = 2
Data collection top
Bruker SMART CCD
diffractometer
3037 independent reflections
Radiation source: fine-focus sealed tube2766 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
ω scansθmax = 25.5°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 67
Tmin = 0.816, Tmax = 0.890k = 2620
8473 measured reflectionsl = 1613
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)] = 0.035Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H atoms treated by a mixture of independent and constrained refinement
S = 0.97 w = 1/[σ2(Fo2) + (0.0692P)2 + 1.1691P]
where P = (Fo2 + 2Fc2)/3
3037 reflections(Δ/σ)max < 0.001
232 parametersΔρmax = 0.66 e Å3
1 restraintΔρmin = 0.36 e Å3
Crystal data top
[Ni(C16H17FN3O3)2]·2H2OV = 1638.31 (10) Å3
Mr = 727.36Z = 2
Monoclinic, P21/cMo Kα radiation
a = 5.8389 (2) ŵ = 0.66 mm1
b = 21.5704 (8) ÅT = 295 K
c = 13.2408 (4) Å0.32 × 0.26 × 0.18 mm
β = 100.763 (1)°
Data collection top
Bruker SMART CCD
diffractometer
3037 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
2766 reflections with I > 2σ(I)
Tmin = 0.816, Tmax = 0.890Rint = 0.023
8473 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0351 restraint
wR(F2) = 0.108H atoms treated by a mixture of independent and constrained refinement
S = 0.97Δρmax = 0.66 e Å3
3037 reflectionsΔρmin = 0.36 e Å3
232 parameters
Special details top

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.

#==============================================================================

# 8. REFINEMENT DATA

_refine_special_details

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
O1W0.212 (3)0.5083 (3)0.9619 (4)0.269 (7)0.771 (7)
O2W0.530 (7)0.4676 (10)0.9199 (13)0.269 (7)0.229 (7)
Ni10.00000.50000.50000.02183 (14)
F10.6987 (2)0.25278 (6)0.66313 (11)0.0456 (4)
O10.2244 (3)0.50862 (6)0.60039 (12)0.0278 (3)
O20.3489 (4)0.50317 (7)0.74766 (15)0.0507 (5)
O30.1702 (2)0.43116 (6)0.59199 (10)0.0270 (3)
N10.0082 (3)0.34446 (8)0.84271 (12)0.0288 (4)
N20.5781 (3)0.18573 (8)0.82650 (13)0.0282 (4)
N30.7581 (3)0.06548 (7)0.90923 (13)0.0260 (4)
H3N0.633 (3)0.0444 (11)0.893 (2)0.046 (7)*
C10.2232 (4)0.48474 (9)0.68784 (16)0.0276 (4)
C20.0695 (3)0.42936 (8)0.72119 (14)0.0259 (4)
C30.1112 (3)0.40744 (8)0.67023 (14)0.0236 (4)
C40.2286 (3)0.35113 (8)0.71319 (14)0.0244 (4)
C50.4086 (3)0.32589 (9)0.66939 (15)0.0279 (4)
H50.45510.34620.61460.034*
C60.5158 (3)0.27262 (9)0.70514 (16)0.0281 (4)
C70.4534 (3)0.23790 (9)0.78697 (15)0.0260 (4)
C80.2748 (3)0.26310 (9)0.83045 (15)0.0285 (4)
H80.22580.24190.88380.034*
C90.1661 (3)0.31940 (9)0.79669 (15)0.0257 (4)
C100.1149 (3)0.39704 (9)0.80463 (15)0.0285 (4)
H100.22940.41290.83770.034*
C110.0729 (4)0.31627 (11)0.93573 (17)0.0370 (5)
H11A0.08750.27180.92600.044*
H11B0.22390.33210.94380.044*
C120.1007 (6)0.32911 (15)1.0321 (2)0.0613 (8)
H12A0.25220.31531.02360.092*
H12B0.05570.30741.08860.092*
H12C0.10540.37281.04590.092*
C130.5224 (5)0.16096 (11)0.92160 (18)0.0445 (6)
H13A0.37550.13870.90650.053*
H13B0.50530.19480.96780.053*
C140.7127 (5)0.11770 (11)0.97288 (17)0.0428 (6)
H14A0.85550.14130.99250.051*
H14B0.67020.10171.03530.051*
C150.6156 (4)0.13449 (10)0.75747 (16)0.0351 (5)
H15A0.66240.15120.69640.042*
H15B0.47100.11190.73620.042*
C160.8036 (4)0.09047 (10)0.81179 (16)0.0353 (5)
H16A0.81850.05620.76610.042*
H16B0.95150.11230.82500.042*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O1W0.64 (2)0.116 (4)0.061 (3)0.061 (7)0.082 (6)0.012 (3)
O2W0.64 (2)0.116 (4)0.061 (3)0.061 (7)0.082 (6)0.012 (3)
Ni10.0265 (2)0.0140 (2)0.0229 (2)0.00066 (11)0.00080 (14)0.00301 (11)
F10.0492 (8)0.0390 (7)0.0566 (8)0.0183 (6)0.0304 (7)0.0168 (6)
O10.0312 (8)0.0212 (7)0.0292 (8)0.0046 (5)0.0007 (6)0.0038 (5)
O20.0658 (13)0.0475 (11)0.0436 (11)0.0328 (8)0.0230 (9)0.0142 (7)
O30.0312 (7)0.0203 (7)0.0287 (7)0.0025 (5)0.0036 (5)0.0078 (5)
N10.0328 (9)0.0266 (9)0.0280 (8)0.0069 (7)0.0085 (7)0.0076 (7)
N20.0378 (9)0.0207 (8)0.0262 (8)0.0095 (7)0.0062 (7)0.0048 (6)
N30.0290 (9)0.0182 (8)0.0291 (8)0.0020 (6)0.0009 (7)0.0012 (6)
C10.0309 (10)0.0218 (9)0.0288 (10)0.0043 (8)0.0022 (8)0.0000 (8)
C20.0293 (9)0.0198 (9)0.0264 (9)0.0036 (7)0.0005 (7)0.0014 (7)
C30.0266 (9)0.0190 (9)0.0226 (9)0.0014 (7)0.0016 (7)0.0001 (7)
C40.0274 (9)0.0200 (9)0.0246 (9)0.0020 (7)0.0015 (7)0.0029 (7)
C50.0331 (10)0.0245 (10)0.0269 (10)0.0014 (8)0.0075 (8)0.0063 (8)
C60.0293 (10)0.0253 (10)0.0308 (10)0.0056 (8)0.0086 (8)0.0034 (8)
C70.0303 (10)0.0207 (9)0.0254 (10)0.0017 (7)0.0011 (8)0.0028 (7)
C80.0342 (10)0.0247 (10)0.0272 (10)0.0048 (8)0.0074 (8)0.0082 (8)
C90.0288 (10)0.0226 (9)0.0249 (9)0.0028 (7)0.0030 (7)0.0035 (7)
C100.0313 (10)0.0252 (10)0.0288 (10)0.0064 (8)0.0048 (8)0.0013 (8)
C110.0414 (12)0.0368 (12)0.0365 (12)0.0077 (9)0.0171 (9)0.0132 (9)
C120.076 (2)0.071 (2)0.0359 (13)0.0055 (16)0.0105 (13)0.0087 (13)
C130.0620 (15)0.0395 (13)0.0373 (12)0.0287 (11)0.0227 (11)0.0183 (10)
C140.0663 (15)0.0355 (12)0.0274 (11)0.0278 (11)0.0113 (10)0.0083 (9)
C150.0493 (13)0.0261 (10)0.0279 (10)0.0076 (9)0.0026 (9)0.0011 (8)
C160.0465 (12)0.0287 (11)0.0312 (11)0.0124 (9)0.0089 (9)0.0022 (9)
Geometric parameters (Å, º) top
Ni1—O1i2.0415 (15)C4—C91.405 (3)
Ni1—O12.0415 (15)C5—C61.351 (3)
Ni1—O32.0552 (13)C5—H50.9300
Ni1—O3i2.0552 (13)C6—C71.419 (3)
Ni1—N3ii2.1908 (16)C7—C81.392 (3)
Ni1—N3iii2.1908 (16)C8—C91.404 (3)
F1—C61.362 (2)C8—H80.9300
O1—C11.266 (3)C10—H100.9300
O2—C11.241 (3)C11—C121.500 (4)
O3—C31.260 (2)C11—H11A0.9700
N1—C101.346 (2)C11—H11B0.9700
N1—C91.389 (2)C12—H12A0.9600
N1—C111.484 (2)C12—H12B0.9600
N2—C71.389 (2)C12—H12C0.9600
N2—C131.460 (3)C13—C141.512 (3)
N2—C151.476 (3)C13—H13A0.9700
N3—C141.461 (3)C13—H13B0.9700
N3—C161.468 (3)C14—H14A0.9700
N3—Ni1iv2.1908 (16)C14—H14B0.9700
N3—H3N0.852 (10)C15—C161.526 (3)
C1—C21.510 (3)C15—H15A0.9700
C2—C101.373 (3)C15—H15B0.9700
C2—C31.435 (3)C16—H16A0.9700
C3—C41.457 (3)C16—H16B0.9700
C4—C51.401 (3)
O1i—Ni1—O1180.0N2—C7—C6121.60 (18)
O1i—Ni1—O391.26 (5)C8—C7—C6115.36 (18)
O1—Ni1—O388.74 (5)C7—C8—C9122.36 (18)
O1i—Ni1—O3i88.74 (5)C7—C8—H8118.8
O1—Ni1—O3i91.26 (5)C9—C8—H8118.8
O3—Ni1—O3i180.0N1—C9—C8121.44 (17)
O1i—Ni1—N3ii90.60 (6)N1—C9—C4118.35 (17)
O1—Ni1—N3ii89.40 (6)C8—C9—C4120.20 (18)
O3—Ni1—N3ii92.88 (6)N1—C10—C2125.71 (18)
O3i—Ni1—N3ii87.12 (6)N1—C10—H10117.1
O1i—Ni1—N3iii89.40 (6)C2—C10—H10117.1
O1—Ni1—N3iii90.60 (6)N1—C11—C12113.2 (2)
O3—Ni1—N3iii87.12 (6)N1—C11—H11A108.9
O3i—Ni1—N3iii92.88 (6)C12—C11—H11A108.9
N3ii—Ni1—N3iii180.0N1—C11—H11B108.9
C1—O1—Ni1131.60 (13)C12—C11—H11B108.9
C3—O3—Ni1127.19 (12)H11A—C11—H11B107.8
C10—N1—C9119.29 (16)C11—C12—H12A109.5
C10—N1—C11118.96 (16)C11—C12—H12B109.5
C9—N1—C11121.70 (16)H12A—C12—H12B109.5
C7—N2—C13115.85 (16)C11—C12—H12C109.5
C7—N2—C15120.08 (16)H12A—C12—H12C109.5
C13—N2—C15110.05 (17)H12B—C12—H12C109.5
C14—N3—C16107.83 (16)N2—C13—C14110.48 (18)
C14—N3—Ni1iv110.40 (12)N2—C13—H13A109.6
C16—N3—Ni1iv121.00 (13)C14—C13—H13A109.6
C14—N3—H3N108.2 (18)N2—C13—H13B109.6
C16—N3—H3N105.5 (18)C14—C13—H13B109.6
Ni1iv—N3—H3N103.1 (18)H13A—C13—H13B108.1
O2—C1—O1123.41 (18)N3—C14—C13114.48 (19)
O2—C1—C2117.17 (18)N3—C14—H14A108.6
O1—C1—C2119.38 (18)C13—C14—H14A108.6
C10—C2—C3118.71 (17)N3—C14—H14B108.6
C10—C2—C1116.33 (17)C13—C14—H14B108.6
C3—C2—C1124.92 (17)H14A—C14—H14B107.6
O3—C3—C2126.23 (17)N2—C15—C16110.53 (16)
O3—C3—C4118.58 (17)N2—C15—H15A109.5
C2—C3—C4115.15 (16)C16—C15—H15A109.5
C5—C4—C9117.48 (17)N2—C15—H15B109.5
C5—C4—C3119.79 (17)C16—C15—H15B109.5
C9—C4—C3122.71 (17)H15A—C15—H15B108.1
C6—C5—C4121.30 (18)N3—C16—C15114.23 (17)
C6—C5—H5119.4N3—C16—H16A108.7
C4—C5—H5119.4C15—C16—H16A108.7
C5—C6—F1118.13 (17)N3—C16—H16B108.7
C5—C6—C7123.23 (19)C15—C16—H16B108.7
F1—C6—C7118.58 (17)H16A—C16—H16B107.6
N2—C7—C8122.76 (18)
O3—Ni1—O1—C17.83 (18)F1—C6—C7—N21.9 (3)
N3ii—Ni1—O1—C1100.72 (18)C5—C6—C7—C81.2 (3)
N3iii—Ni1—O1—C179.28 (18)F1—C6—C7—C8176.00 (17)
O1i—Ni1—O3—C3174.28 (15)N2—C7—C8—C9173.20 (18)
O1—Ni1—O3—C35.72 (15)C6—C7—C8—C90.8 (3)
N3ii—Ni1—O3—C383.62 (15)C10—N1—C9—C8176.91 (19)
N3iii—Ni1—O3—C396.38 (15)C11—N1—C9—C85.8 (3)
Ni1—O1—C1—O2166.39 (17)C10—N1—C9—C41.7 (3)
Ni1—O1—C1—C216.1 (3)C11—N1—C9—C4175.62 (18)
O2—C1—C2—C1012.3 (3)C7—C8—C9—N1178.50 (19)
O1—C1—C2—C10165.38 (19)C7—C8—C9—C42.9 (3)
O2—C1—C2—C3170.1 (2)C5—C4—C9—N1178.51 (17)
O1—C1—C2—C312.2 (3)C3—C4—C9—N12.9 (3)
Ni1—O3—C3—C29.7 (3)C5—C4—C9—C82.9 (3)
Ni1—O3—C3—C4168.14 (12)C3—C4—C9—C8175.70 (18)
C10—C2—C3—O3178.57 (18)C9—N1—C10—C20.8 (3)
C1—C2—C3—O31.0 (3)C11—N1—C10—C2178.1 (2)
C10—C2—C3—C40.7 (3)C3—C2—C10—N12.0 (3)
C1—C2—C3—C4176.88 (17)C1—C2—C10—N1175.80 (19)
O3—C3—C4—C52.2 (3)C10—N1—C11—C12101.8 (2)
C2—C3—C4—C5179.76 (17)C9—N1—C11—C1275.5 (3)
O3—C3—C4—C9176.37 (17)C7—N2—C13—C14163.1 (2)
C2—C3—C4—C91.7 (3)C15—N2—C13—C1456.5 (3)
C9—C4—C5—C60.9 (3)C16—N3—C14—C1353.9 (3)
C3—C4—C5—C6177.74 (19)Ni1iv—N3—C14—C13171.88 (17)
C4—C5—C6—F1176.03 (18)N2—C13—C14—N357.8 (3)
C4—C5—C6—C71.2 (3)C7—N2—C15—C16166.05 (18)
C13—N2—C7—C84.2 (3)C13—N2—C15—C1655.5 (2)
C15—N2—C7—C8131.9 (2)C14—N3—C16—C1552.7 (2)
C13—N2—C7—C6169.5 (2)Ni1iv—N3—C16—C15178.92 (14)
C15—N2—C7—C654.4 (3)N2—C15—C16—N355.4 (2)
C5—C6—C7—N2175.37 (18)
Symmetry codes: (i) x, y+1, z+1; (ii) x1, y+1/2, z1/2; (iii) x+1, y+1/2, z+3/2; (iv) x+1, y1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H3N···O2v0.85 (1)2.43 (2)3.159 (2)145 (2)
Symmetry code: (v) x, y1/2, z+3/2.

Experimental details

Crystal data
Chemical formula[Ni(C16H17FN3O3)2]·2H2O
Mr727.36
Crystal system, space groupMonoclinic, P21/c
Temperature (K)295
a, b, c (Å)5.8389 (2), 21.5704 (8), 13.2408 (4)
β (°) 100.763 (1)
V3)1638.31 (10)
Z2
Radiation typeMo Kα
µ (mm1)0.66
Crystal size (mm)0.32 × 0.26 × 0.18
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.816, 0.890
No. of measured, independent and
observed [I > 2σ(I)] reflections
8473, 3037, 2766
Rint0.023
(sin θ/λ)max1)0.606
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.035, 0.108, 0.97
No. of reflections3037
No. of parameters232
No. of restraints1
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.66, 0.36

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998), SHELXTL.

Selected bond lengths (Å) top
Ni1—O12.0415 (15)Ni1—N3i2.1908 (16)
Ni1—O32.0552 (13)
Symmetry code: (i) x+1, y+1/2, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3—H3N···O2ii0.852 (10)2.425 (17)3.159 (2)145 (2)
Symmetry code: (ii) x, y1/2, z+3/2.
 

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