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The title complex, [Ni(C2H1N9)(C10H8N2)2]·6H2O, was prepared under hydro­thermal reaction conditions. The asymmetric unit contains the nickel complex and six solvent water mol­ecules. The NiII ion is coordinated in a distorted octa­hedral geometry defined by four N atoms from two 2,2′-bipyridine ligands and two N atoms from the 5,5′-imino­bis(tetra­zolate) (BTA2−) anions. In the crystal structure, an extensive range of O—H...N and O—H...O hydrogen bonds links the complex and the water mol­ecules into a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807058370/sj2411sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807058370/sj2411Isup2.hkl
Contains datablock I

CCDC reference: 672693

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.028
  • wR factor = 0.075
  • Data-to-parameter ratio = 13.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 30 Ang. PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 16 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - N10 .. 5.02 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - N11 .. 5.07 su PLAT245_ALERT_2_C U(iso) H27 Smaller than U(eq) O5 by ... 0.01 AngSq
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Ni1 (2) 2.12
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 1 ALERT type 5 Informative message, check

Comment top

Metal complexes of N,N-bis-(1(2)H-tetrazol-5-yl)-amine have not been extensively examined even though the deprotonated ligand contains nine potentially electron-donating nitrogen atoms (Friedrich et al., 2005). The asymmetric unit of the title compound (I) comprises a Ni(II) cation, two 2,2'-bipyridine and one HBTA2- ligands and six solvent water molecules. Each NiII atom is coordinated to six N atoms from two 2,2'-bipyridine and one HBTA2- ligands to form a distorted mononuclear octahedral complex. (Table 1 and Fig. 1). In the crystal structure, an extensive range of O—H···N and O—H···O hydrogen bonds link the complex and water molecules into a three dimensional network, Table 2, Fig. 2.

Related literature top

Other complexes of the N,N-bis[1(2H)-tetrazol-5-yl]amine ligand are rare; for a related copper(II) complex, see: Friedrich et al. (2005).

Experimental top

A mixture of Ni(Cl)2·6H2O (0.024 g, 0.1 mmol), bistetrazolylimine (0.031 g, 0.02 mmol) and water (20 ml) was heated in a 25 ml Teflon-lined autoclave at 433 K for 3 d, followed by slow cooling to room temperature. The resulting mixture was filtered, washed with 95% methanol and red crystals were collected and dried in air. Elemental analysis, calcd (%) for C22H29N13Ni1O6: C 41.90, H 4.60, N 28.89; found(%): C 41.66, H 4.93, N 28.71.

Refinement top

All hydrogen atoms were located in difference Fourier maps and freely refined with isotropic displacement parameters.

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2005); software used to prepare material for publication: SHELXTL (Bruker, 2005).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), with atom labels and 30% probability displacement ellipsoids for non-H atoms.
[Figure 2] Fig. 2. The packing of the complex, showing a three-dimensional network connected by O—H···N and O—H···O hydrogen bonds (dashed lines). H atoms not involved in hydrogen bonding have been omitted.
Bis(2,2'-bipyridine)[5,5'-iminobis(tetrazolato)]nickel(II) hexahydrate top
Crystal data top
[Ni(C2HN9)(C10H8N2)2]·6H2OF(000) = 1312.0
Mr = 630.27Dx = 1.480 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5453 reflections
a = 13.3435 (3) Åθ = 1.0–27.5°
b = 13.3741 (3) ŵ = 0.75 mm1
c = 15.9408 (3) ÅT = 296 K
β = 96.166 (1)°Block, red
V = 2828.29 (10) Å30.25 × 0.25 × 0.13 mm
Z = 4
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
6503 independent reflections
Radiation source: fine-focus sealed tube5453 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ϕ and ω scansθmax = 27.5°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1716
Tmin = 0.830, Tmax = 0.907k = 1617
6514 measured reflectionsl = 2020
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028All H-atom parameters refined
wR(F2) = 0.075 w = 1/[σ2(Fo2) + (0.0359P)2 + 0.8759P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.033
6503 reflectionsΔρmax = 0.32 e Å3
496 parametersΔρmin = 0.30 e Å3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0018
Crystal data top
[Ni(C2HN9)(C10H8N2)2]·6H2OV = 2828.29 (10) Å3
Mr = 630.27Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.3435 (3) ŵ = 0.75 mm1
b = 13.3741 (3) ÅT = 296 K
c = 15.9408 (3) Å0.25 × 0.25 × 0.13 mm
β = 96.166 (1)°
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
6503 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
5453 reflections with I > 2σ(I)
Tmin = 0.830, Tmax = 0.907Rint = 0.024
6514 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.075All H-atom parameters refined
S = 1.03Δρmax = 0.32 e Å3
6503 reflectionsΔρmin = 0.30 e Å3
496 parameters
Special details top

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 (Å2) top
xyzUiso*/Ueq
Ni10.721520 (13)0.120775 (13)0.874767 (11)0.02942 (7)
C10.59648 (11)0.30488 (11)0.90861 (9)0.0327 (3)
N40.50270 (10)0.33969 (10)0.90652 (9)0.0394 (3)
N10.60038 (9)0.21948 (9)0.86584 (8)0.0331 (3)
N50.67785 (10)0.35362 (11)0.94830 (10)0.0422 (3)
N60.80563 (9)0.24861 (9)0.90063 (8)0.0331 (3)
N30.44671 (10)0.27279 (11)0.85844 (9)0.0422 (3)
N70.90583 (10)0.26122 (11)0.89697 (9)0.0426 (3)
N20.50342 (9)0.20166 (10)0.83404 (8)0.0390 (3)
N80.93118 (11)0.34970 (12)0.92545 (11)0.0530 (4)
N90.85003 (11)0.39895 (11)0.94812 (10)0.0487 (4)
C20.77503 (11)0.33450 (11)0.93208 (9)0.0337 (3)
N100.74488 (10)0.12590 (9)0.74820 (8)0.0385 (3)
N110.84590 (9)0.02420 (9)0.87217 (8)0.0349 (3)
C80.87850 (11)0.01380 (12)0.79555 (10)0.0376 (3)
C70.82656 (12)0.07651 (12)0.72765 (10)0.0385 (3)
N120.70809 (9)0.09258 (9)1.00247 (7)0.0332 (3)
C110.96054 (14)0.10370 (14)0.92476 (14)0.0516 (4)
C30.69266 (16)0.18066 (15)0.68884 (11)0.0541 (5)
C120.88732 (13)0.03314 (13)0.93510 (11)0.0429 (4)
C90.95315 (13)0.05460 (15)0.78158 (13)0.0519 (5)
C60.85729 (16)0.08335 (16)0.64746 (12)0.0543 (5)
C100.99352 (14)0.11430 (15)0.84671 (14)0.0572 (5)
C40.71786 (19)0.18806 (17)0.60757 (12)0.0652 (6)
C50.8023 (2)0.13933 (17)0.58733 (12)0.0657 (6)
N130.62922 (10)0.00624 (9)0.86724 (8)0.0361 (3)
C140.74236 (14)0.11884 (14)1.15098 (11)0.0474 (4)
C180.61425 (11)0.04722 (11)0.94200 (10)0.0370 (3)
C130.74823 (13)0.14660 (13)1.06856 (10)0.0399 (3)
C170.65970 (11)0.00724 (11)1.01771 (10)0.0354 (3)
C220.58868 (14)0.05149 (14)0.79670 (12)0.0487 (4)
C160.65403 (15)0.02582 (15)1.09968 (12)0.0514 (4)
C150.69570 (16)0.03107 (16)1.16643 (12)0.0551 (5)
C190.55832 (15)0.13399 (13)0.94686 (13)0.0504 (4)
C200.51727 (16)0.17936 (15)0.87395 (14)0.0582 (5)
C210.53251 (16)0.13798 (15)0.79769 (14)0.0587 (5)
O10.88828 (12)0.53330 (12)0.08779 (10)0.0591 (4)
O20.62370 (14)0.49551 (13)0.06176 (10)0.0710 (5)
O30.86502 (14)0.35155 (15)0.18119 (12)0.0705 (4)
O60.09069 (16)0.14894 (15)0.86339 (14)0.0818 (5)
O40.64923 (18)0.37076 (15)0.19747 (13)0.0818 (5)
O50.22910 (15)0.30002 (18)0.87163 (17)0.0998 (8)
H10.6674 (14)0.4000 (15)0.9771 (12)0.046 (5)*
H190.941 (2)0.562 (2)0.0823 (17)0.089 (9)*
H180.876 (2)0.503 (2)0.0403 (18)0.099 (10)*
H200.578 (2)0.534 (2)0.0649 (17)0.089 (9)*
H210.625 (2)0.461 (2)0.1060 (18)0.091 (9)*
H230.906 (2)0.349 (2)0.2174 (19)0.091 (11)*
H220.880 (2)0.404 (2)0.1587 (18)0.095 (10)*
H250.630 (2)0.371 (2)0.245 (2)0.094 (11)*
H240.710 (2)0.359 (2)0.1999 (19)0.101 (12)*
H260.283 (2)0.297 (2)0.8633 (17)0.091 (10)*
H280.133 (2)0.193 (2)0.8757 (16)0.082 (9)*
H20.6373 (16)0.2133 (16)0.7053 (12)0.061 (6)*
H30.6782 (16)0.2259 (17)0.5682 (14)0.067 (6)*
H40.8253 (18)0.1469 (17)0.5331 (15)0.077 (7)*
H50.9156 (16)0.0511 (16)0.6364 (13)0.066 (6)*
H60.9746 (14)0.0575 (15)0.7262 (13)0.056 (5)*
H71.0420 (16)0.1609 (16)0.8382 (12)0.062 (6)*
H80.9863 (16)0.1419 (16)0.9707 (13)0.059 (6)*
H90.8632 (13)0.0252 (13)0.9892 (11)0.041 (5)*
H100.7829 (13)0.2045 (14)1.0568 (11)0.044 (5)*
H110.7717 (15)0.1569 (15)1.1940 (12)0.053 (5)*
H130.6198 (16)0.0869 (17)1.1047 (13)0.060 (6)*
H120.6918 (16)0.0081 (16)1.2213 (14)0.069 (6)*
H170.5993 (14)0.0226 (14)0.7453 (12)0.045 (5)*
H140.5487 (15)0.1618 (16)0.9997 (13)0.064 (6)*
H160.5067 (17)0.1663 (17)0.7484 (14)0.070 (6)*
H150.4802 (16)0.2377 (17)0.8765 (12)0.063 (6)*
H290.035 (3)0.178 (3)0.867 (2)0.140 (14)*
H270.211 (2)0.354 (2)0.8758 (18)0.085 (10)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.02916 (11)0.02725 (10)0.03302 (10)0.00047 (7)0.00869 (7)0.00243 (7)
C10.0313 (7)0.0298 (7)0.0387 (7)0.0022 (6)0.0115 (6)0.0013 (6)
N40.0325 (7)0.0364 (7)0.0510 (7)0.0043 (6)0.0117 (6)0.0013 (6)
N10.0278 (6)0.0312 (6)0.0409 (6)0.0003 (5)0.0068 (5)0.0021 (5)
N50.0341 (7)0.0356 (7)0.0580 (8)0.0006 (6)0.0104 (6)0.0175 (6)
N60.0273 (6)0.0320 (6)0.0414 (6)0.0015 (5)0.0105 (5)0.0013 (5)
N30.0302 (7)0.0423 (8)0.0548 (8)0.0015 (6)0.0082 (6)0.0030 (6)
N70.0288 (7)0.0444 (8)0.0563 (8)0.0037 (6)0.0116 (6)0.0054 (6)
N20.0300 (7)0.0394 (7)0.0479 (7)0.0021 (5)0.0052 (5)0.0005 (6)
N80.0349 (8)0.0490 (9)0.0764 (11)0.0098 (6)0.0116 (7)0.0122 (8)
N90.0372 (8)0.0396 (8)0.0695 (10)0.0077 (6)0.0076 (7)0.0122 (7)
C20.0318 (7)0.0307 (7)0.0391 (7)0.0024 (6)0.0062 (6)0.0025 (6)
N100.0425 (7)0.0379 (7)0.0365 (6)0.0035 (6)0.0104 (5)0.0026 (5)
N110.0317 (6)0.0312 (6)0.0421 (7)0.0007 (5)0.0056 (5)0.0058 (5)
C80.0315 (8)0.0366 (8)0.0455 (8)0.0032 (6)0.0078 (6)0.0137 (6)
C70.0403 (8)0.0355 (8)0.0413 (8)0.0045 (7)0.0123 (6)0.0109 (6)
N120.0324 (6)0.0323 (6)0.0358 (6)0.0006 (5)0.0079 (5)0.0006 (5)
C110.0412 (10)0.0439 (10)0.0665 (12)0.0080 (8)0.0095 (9)0.0068 (9)
C30.0660 (13)0.0539 (11)0.0440 (9)0.0177 (10)0.0129 (9)0.0037 (8)
C120.0371 (9)0.0402 (9)0.0507 (9)0.0039 (7)0.0017 (7)0.0030 (7)
C90.0394 (9)0.0593 (11)0.0577 (11)0.0069 (8)0.0084 (8)0.0232 (9)
C60.0604 (12)0.0584 (11)0.0481 (10)0.0001 (10)0.0239 (9)0.0107 (9)
C100.0385 (10)0.0538 (11)0.0772 (13)0.0144 (8)0.0044 (9)0.0243 (10)
C40.0919 (17)0.0631 (13)0.0416 (10)0.0147 (12)0.0109 (10)0.0073 (9)
C50.0970 (18)0.0636 (13)0.0410 (10)0.0010 (12)0.0279 (11)0.0031 (9)
N130.0343 (7)0.0322 (6)0.0421 (7)0.0016 (5)0.0060 (5)0.0054 (5)
C140.0502 (10)0.0561 (11)0.0358 (8)0.0015 (8)0.0040 (7)0.0024 (8)
C180.0318 (8)0.0304 (8)0.0497 (9)0.0006 (6)0.0086 (6)0.0002 (6)
C130.0438 (9)0.0386 (8)0.0378 (8)0.0037 (7)0.0058 (7)0.0018 (6)
C170.0319 (7)0.0324 (8)0.0430 (8)0.0005 (6)0.0089 (6)0.0029 (6)
C220.0500 (10)0.0481 (10)0.0485 (10)0.0061 (8)0.0068 (8)0.0110 (8)
C160.0569 (11)0.0462 (10)0.0521 (10)0.0092 (9)0.0103 (8)0.0127 (8)
C150.0621 (12)0.0648 (12)0.0390 (9)0.0037 (10)0.0081 (8)0.0115 (8)
C190.0504 (11)0.0377 (9)0.0639 (11)0.0091 (8)0.0094 (9)0.0029 (8)
C200.0549 (11)0.0380 (10)0.0821 (14)0.0139 (9)0.0092 (10)0.0080 (9)
C210.0547 (12)0.0534 (11)0.0675 (13)0.0126 (9)0.0043 (10)0.0251 (10)
O10.0485 (8)0.0625 (9)0.0674 (9)0.0159 (7)0.0111 (7)0.0119 (7)
O20.0947 (13)0.0624 (10)0.0601 (9)0.0376 (9)0.0285 (8)0.0006 (7)
O30.0740 (11)0.0698 (11)0.0654 (10)0.0050 (9)0.0035 (9)0.0078 (8)
O60.0624 (11)0.0695 (11)0.1171 (15)0.0019 (10)0.0259 (11)0.0158 (10)
O40.0784 (14)0.0903 (13)0.0747 (12)0.0025 (10)0.0016 (10)0.0195 (10)
O50.0458 (10)0.0870 (15)0.169 (2)0.0099 (10)0.0244 (12)0.0504 (14)
Geometric parameters (Å, º) top
Ni1—N62.0624 (12)C6—H50.92 (2)
Ni1—N102.0754 (13)C10—H70.92 (2)
Ni1—N12.0800 (12)C4—C51.369 (3)
Ni1—N132.0941 (13)C4—H30.93 (2)
Ni1—N122.0968 (12)C5—H40.95 (2)
Ni1—N112.1070 (12)N13—C221.339 (2)
C1—N41.3322 (19)N13—C181.346 (2)
C1—N11.3340 (18)C14—C151.363 (3)
C1—N51.363 (2)C14—C131.376 (2)
N4—N31.3502 (19)C14—H110.91 (2)
N1—N21.3589 (17)C18—C191.386 (2)
N5—C21.3732 (19)C18—C171.483 (2)
N5—H10.794 (19)C13—H100.931 (19)
N6—C21.3348 (19)C17—C161.389 (2)
N6—N71.3551 (17)C22—C211.379 (3)
N3—N21.3007 (19)C22—H170.930 (18)
N7—N81.299 (2)C16—C151.376 (3)
N8—N91.349 (2)C16—H130.94 (2)
N9—C21.325 (2)C15—H120.93 (2)
N10—C31.333 (2)C19—C201.372 (3)
N10—C71.345 (2)C19—H140.94 (2)
N11—C121.334 (2)C20—C211.371 (3)
N11—C81.3470 (19)C20—H150.93 (2)
C8—C91.388 (2)C21—H160.91 (2)
C8—C71.481 (2)O1—H190.81 (3)
C7—C61.387 (2)O1—H180.86 (3)
N12—C131.341 (2)O2—H200.80 (3)
N12—C171.3462 (19)O2—H210.84 (3)
C11—C101.371 (3)O3—H230.75 (3)
C11—C121.381 (2)O3—H220.82 (3)
C11—H80.93 (2)O6—H280.82 (3)
C3—C41.377 (3)O6—H290.85 (4)
C3—H20.92 (2)O4—H250.83 (3)
C12—H90.959 (17)O4—H240.82 (3)
C9—C101.373 (3)O5—H260.75 (3)
C9—H60.96 (2)O5—H270.76 (3)
C6—C51.367 (3)
N6—Ni1—N1091.81 (5)N11—C12—C11122.98 (17)
N6—Ni1—N183.67 (5)N11—C12—H9117.4 (10)
N10—Ni1—N196.27 (5)C11—C12—H9119.6 (10)
N6—Ni1—N13171.13 (5)C10—C9—C8119.48 (17)
N10—Ni1—N1396.89 (5)C10—C9—H6122.8 (12)
N1—Ni1—N1393.61 (5)C8—C9—H6117.7 (12)
N6—Ni1—N1293.24 (5)C5—C6—C7119.54 (19)
N10—Ni1—N12170.80 (5)C5—C6—H5121.5 (13)
N1—Ni1—N1291.93 (5)C7—C6—H5118.9 (13)
N13—Ni1—N1278.39 (5)C11—C10—C9119.21 (17)
N6—Ni1—N1195.69 (5)C11—C10—H7120.3 (13)
N10—Ni1—N1178.48 (5)C9—C10—H7120.5 (13)
N1—Ni1—N11174.71 (5)C5—C4—C3118.5 (2)
N13—Ni1—N1187.78 (5)C5—C4—H3121.7 (13)
N12—Ni1—N1193.35 (5)C3—C4—H3119.8 (14)
N4—C1—N1111.99 (13)C6—C5—C4119.27 (18)
N4—C1—N5122.95 (13)C6—C5—H4119.5 (14)
N1—C1—N5125.04 (13)C4—C5—H4121.2 (14)
C1—N4—N3104.10 (12)C22—N13—C18118.33 (14)
C1—N1—N2104.66 (12)C22—N13—Ni1126.65 (12)
C1—N1—Ni1125.53 (10)C18—N13—Ni1114.95 (10)
N2—N1—Ni1128.02 (9)C15—C14—C13118.61 (17)
C1—N5—C2123.02 (13)C15—C14—H11121.0 (13)
C1—N5—H1117.5 (14)C13—C14—H11120.4 (13)
C2—N5—H1118.9 (14)N13—C18—C19121.49 (16)
C2—N6—N7104.61 (12)N13—C18—C17115.73 (13)
C2—N6—Ni1127.34 (10)C19—C18—C17122.78 (15)
N7—N6—Ni1127.80 (10)N12—C13—C14123.10 (16)
N2—N3—N4110.50 (12)N12—C13—H10117.1 (11)
N8—N7—N6108.62 (13)C14—C13—H10119.8 (11)
N3—N2—N1108.74 (12)N12—C17—C16121.02 (15)
N7—N8—N9110.61 (13)N12—C17—C18115.58 (13)
C2—N9—N8104.00 (13)C16—C17—C18123.40 (15)
N9—C2—N6112.16 (13)N13—C22—C21122.71 (18)
N9—C2—N5123.47 (14)N13—C22—H17117.7 (11)
N6—C2—N5124.35 (13)C21—C22—H17119.6 (11)
C3—N10—C7118.20 (14)C15—C16—C17119.54 (17)
C3—N10—Ni1125.93 (11)C15—C16—H13124.9 (13)
C7—N10—Ni1115.52 (11)C17—C16—H13115.6 (13)
C12—N11—C8118.31 (14)C14—C15—C16119.40 (17)
C12—N11—Ni1126.95 (11)C14—C15—H12121.7 (14)
C8—N11—Ni1114.38 (10)C16—C15—H12118.9 (14)
N11—C8—C9121.38 (16)C20—C19—C18119.42 (18)
N11—C8—C7115.65 (13)C20—C19—H14120.2 (13)
C9—C8—C7122.92 (15)C18—C19—H14120.4 (13)
N10—C7—C6121.32 (17)C21—C20—C19119.28 (18)
N10—C7—C8115.33 (13)C21—C20—H15120.6 (13)
C6—C7—C8123.34 (16)C19—C20—H15120.1 (13)
C13—N12—C17118.28 (13)C20—C21—C22118.77 (19)
C13—N12—Ni1126.68 (11)C20—C21—H16121.4 (14)
C17—N12—Ni1114.86 (10)C22—C21—H16119.8 (15)
C10—C11—C12118.62 (19)H19—O1—H18102 (2)
C10—C11—H8122.1 (13)H20—O2—H21104 (3)
C12—C11—H8119.3 (13)H23—O3—H22101 (3)
N10—C3—C4123.09 (19)H28—O6—H29104 (3)
N10—C3—H2115.6 (13)H25—O4—H24111 (3)
C4—C3—H2121.3 (13)H26—O5—H27113 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N5—H1···O2i0.794 (19)1.99 (2)2.770 (2)167.7 (19)
O1—H19···N8ii0.81 (3)2.09 (3)2.899 (2)174 (3)
O1—H18···N9iii0.86 (3)2.02 (3)2.864 (2)165 (3)
O2—H20···N4iv0.80 (3)2.08 (3)2.853 (2)161 (3)
O2—H21···O40.84 (3)1.90 (3)2.724 (3)168 (3)
O3—H23···N2v0.75 (3)2.26 (3)2.981 (2)163 (3)
O3—H22···O10.82 (3)2.08 (3)2.885 (3)168 (3)
O4—H25···O6v0.83 (3)2.03 (3)2.849 (3)171 (3)
O4—H24···O30.82 (3)2.12 (3)2.930 (3)167 (3)
Symmetry codes: (i) x, y, z+1; (ii) x+2, y+1, z+1; (iii) x, y, z1; (iv) x+1, y+1, z+1; (v) x+1/2, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Ni(C2HN9)(C10H8N2)2]·6H2O
Mr630.27
Crystal system, space groupMonoclinic, P21/n
Temperature (K)296
a, b, c (Å)13.3435 (3), 13.3741 (3), 15.9408 (3)
β (°) 96.166 (1)
V3)2828.29 (10)
Z4
Radiation typeMo Kα
µ (mm1)0.75
Crystal size (mm)0.25 × 0.25 × 0.13
Data collection
DiffractometerBruker SMART APEX CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.830, 0.907
No. of measured, independent and
observed [I > 2σ(I)] reflections
6514, 6503, 5453
Rint0.024
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.075, 1.03
No. of reflections6503
No. of parameters496
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.32, 0.30

Computer programs: SMART (Bruker, 2003), SAINT-Plus (Bruker, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2005).

Selected geometric parameters (Å, º) top
Ni1—N62.0624 (12)Ni1—N132.0941 (13)
Ni1—N102.0754 (13)Ni1—N122.0968 (12)
Ni1—N12.0800 (12)Ni1—N112.1070 (12)
N6—Ni1—N183.67 (5)N10—Ni1—N12170.80 (5)
N10—Ni1—N196.27 (5)N13—Ni1—N1278.39 (5)
N6—Ni1—N13171.13 (5)N1—Ni1—N11174.71 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N5—H1···O2i0.794 (19)1.99 (2)2.770 (2)167.7 (19)
O1—H19···N8ii0.81 (3)2.09 (3)2.899 (2)174 (3)
O1—H18···N9iii0.86 (3)2.02 (3)2.864 (2)165 (3)
O2—H20···N4iv0.80 (3)2.08 (3)2.853 (2)161 (3)
O2—H21···O40.84 (3)1.90 (3)2.724 (3)168 (3)
O3—H23···N2v0.75 (3)2.26 (3)2.981 (2)163 (3)
O3—H22···O10.82 (3)2.08 (3)2.885 (3)168 (3)
O4—H25···O6v0.83 (3)2.03 (3)2.849 (3)171 (3)
O4—H24···O30.82 (3)2.12 (3)2.930 (3)167 (3)
Symmetry codes: (i) x, y, z+1; (ii) x+2, y+1, z+1; (iii) x, y, z1; (iv) x+1, y+1, z+1; (v) x+1/2, y+1/2, z1/2.
 

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