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The crystal structure of the title compound, [Ni(C6H6N4S2)2(H2O)2][Ni(C7H3NO4)2]·5H2O, consists of NiII complex cations, NiII complex anions and five uncoordinated water mol­ecules. In both the complex cation and anion, the NiII ions assume a distorted octa­hedral coordination. There is extensive hydrogen bonding between water mol­ecules, complex cations and complex anions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806031473/om2038sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806031473/om2038Isup2.hkl
Contains datablock I

CCDC reference: 621454

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.008 Å
  • H-atom completeness 94%
  • Disorder in solvent or counterion
  • R factor = 0.054
  • wR factor = 0.143
  • Data-to-parameter ratio = 13.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for S22 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 17.00 Perc. PLAT322_ALERT_2_C Check Hybridisation of S11 in Main Residue . ? PLAT322_ALERT_2_C Check Hybridisation of S12 in Main Residue . ? PLAT322_ALERT_2_C Check Hybridisation of S21 in Main Residue . ? PLAT322_ALERT_2_C Check Hybridisation of S22 in Main Residue . ? PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C35 - C36 ... 1.53 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8
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:C26 H32 N10 Ni2 O15 S4 Atom count from the _atom_site data: C26 H30 N10 Ni2 O15 S4 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 4 From the CIF: _chemical_formula_sum C26 H32 N10 Ni2 O15 S4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 104.00 104.00 0.00 H 128.00 120.00 8.00 N 40.00 40.00 0.00 Ni 8.00 8.00 0.00 O 60.00 60.00 0.00 S 16.00 16.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 7 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 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Diaqua(2,2'-diamino-4,4'-bi-1,3-thiazole-κ2N3,N3')nickel(II) (pyridine-2,6-dicarboxylato-κ3O,N,O')nickel(II) pentahydrate top
Crystal data top
[Ni(C6H6N4S2)2(H2O)2][Ni(C7H3NO4)2]·5H2OF(000) = 1992
Mr = 970.28Dx = 1.671 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4080 reflections
a = 11.7980 (11) Åθ = 2.8–25.0°
b = 18.5558 (17) ŵ = 1.27 mm1
c = 17.6429 (17) ÅT = 295 K
β = 92.964 (2)°Prism, green
V = 3857.2 (6) Å30.23 × 0.20 × 0.18 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID
diffractometer
6988 independent reflections
Radiation source: fine-focus sealed tube4180 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.070
Detector resolution: 10.00 pixels mm-1θmax = 25.2°, θmin = 2.0°
ω scansh = 1414
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 2218
Tmin = 0.740, Tmax = 0.800l = 2115
20280 measured reflections
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)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.143H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0575P)2 + 0.3071P]
where P = (Fo2 + 2Fc2)/3
6988 reflections(Δ/σ)max = 0.003
517 parametersΔρmax = 0.77 e Å3
0 restraintsΔρmin = 0.49 e Å3
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*/UeqOcc. (<1)
Ni10.34817 (5)0.42495 (3)0.79496 (4)0.03453 (19)
Ni20.48018 (6)0.19513 (3)0.49892 (4)0.0381 (2)
S110.58889 (13)0.23372 (8)0.86220 (10)0.0581 (5)
S120.55030 (14)0.44771 (9)0.57778 (10)0.0597 (5)
S210.57826 (14)0.58022 (9)0.94336 (10)0.0634 (5)
S220.11147 (15)0.62391 (10)0.74905 (11)0.0746 (6)
N110.4552 (3)0.3362 (2)0.8159 (2)0.0372 (10)
N120.4044 (4)0.2810 (2)0.9294 (3)0.0562 (13)
H12A0.34650.30860.93330.067*
H12B0.41980.24860.96320.067*
N130.4484 (3)0.4318 (2)0.7015 (2)0.0389 (11)
N140.3805 (4)0.5291 (3)0.6278 (3)0.0743 (17)
H14A0.33120.54040.66000.089*
H14B0.38540.55400.58700.089*
N210.4467 (3)0.5009 (2)0.8584 (2)0.0389 (11)
N220.6152 (4)0.4436 (2)0.9046 (3)0.0562 (14)
H22A0.59830.40420.88100.067*
H22B0.67750.44680.93200.067*
N230.2500 (3)0.5199 (2)0.7763 (2)0.0420 (11)
N240.0967 (4)0.4892 (3)0.6939 (3)0.0749 (17)
H24A0.12050.44560.68940.090*
H24B0.03490.50260.66990.090*
N310.5328 (3)0.1172 (2)0.5662 (2)0.0339 (10)
N410.4223 (3)0.2744 (2)0.4344 (2)0.0339 (10)
O10.2336 (3)0.36151 (19)0.7281 (2)0.0495 (10)
H1A0.18880.32380.73670.074*
H1B0.27480.34970.69020.074*
O20.2543 (3)0.39981 (17)0.88964 (18)0.0386 (9)
H2B0.23770.44340.90720.058*
H2A0.18530.37460.88110.058*
O310.3501 (3)0.11826 (18)0.4803 (2)0.0413 (9)
O320.2940 (3)0.01071 (18)0.5197 (2)0.0424 (9)
O330.6407 (3)0.23512 (19)0.5420 (2)0.0503 (10)
O340.7724 (3)0.2124 (2)0.6351 (2)0.0579 (11)
O410.5590 (3)0.17606 (18)0.3912 (2)0.0441 (9)
O420.5660 (3)0.2218 (2)0.2746 (2)0.0618 (12)
O430.3844 (3)0.2531 (2)0.5757 (2)0.0476 (10)
O440.2605 (3)0.3440 (2)0.5782 (2)0.0578 (11)
C110.5386 (4)0.3284 (3)0.7636 (3)0.0416 (13)
C120.6170 (5)0.2765 (3)0.7791 (4)0.0595 (17)
H120.67730.26570.74910.071*
C130.4706 (5)0.2885 (3)0.8708 (3)0.0434 (14)
C140.5314 (4)0.3786 (3)0.6995 (3)0.0410 (13)
C150.5940 (5)0.3789 (3)0.6378 (3)0.0519 (15)
H150.65220.34660.62900.062*
C160.4502 (5)0.4723 (3)0.6412 (3)0.0470 (14)
C210.3974 (5)0.5689 (3)0.8616 (3)0.0420 (14)
C220.4559 (5)0.6168 (3)0.9036 (4)0.0646 (19)
H220.43330.66420.91060.078*
C230.5444 (4)0.5001 (3)0.8989 (3)0.0416 (14)
C240.2917 (5)0.5793 (3)0.8172 (3)0.0446 (14)
C250.2281 (5)0.6386 (3)0.8098 (4)0.0639 (18)
H250.24470.68210.83420.077*
C260.1549 (5)0.5353 (3)0.7374 (3)0.0543 (16)
C310.6305 (4)0.1250 (3)0.6083 (3)0.0351 (12)
C320.6692 (4)0.0715 (3)0.6572 (3)0.0445 (14)
H320.73610.07710.68680.053*
C330.6059 (5)0.0094 (3)0.6610 (3)0.0465 (14)
H330.63160.02790.69260.056*
C340.5048 (4)0.0015 (3)0.6187 (3)0.0424 (14)
H340.46180.04030.62160.051*
C350.4694 (4)0.0583 (3)0.5715 (3)0.0330 (12)
C360.3616 (4)0.0618 (3)0.5199 (3)0.0343 (12)
C370.6866 (5)0.1969 (3)0.5948 (3)0.0438 (14)
C410.4514 (4)0.2798 (3)0.3624 (3)0.0393 (13)
C420.4100 (5)0.3352 (3)0.3163 (3)0.0507 (15)
H420.42930.33890.26600.061*
C430.3386 (5)0.3850 (3)0.3479 (4)0.0532 (16)
H430.30940.42280.31840.064*
C440.3106 (5)0.3792 (3)0.4218 (3)0.0449 (14)
H440.26360.41310.44310.054*
C450.3533 (4)0.3221 (3)0.4643 (3)0.0371 (13)
C470.5331 (5)0.2213 (3)0.3402 (3)0.0443 (14)
C460.3308 (5)0.3053 (3)0.5461 (3)0.0426 (14)
O1W0.9091 (4)0.3262 (2)0.6586 (3)0.0841 (15)
H1WA0.84610.29410.65080.126*
H1WB0.95960.30590.69370.126*
O2W0.7073 (5)0.3532 (3)0.4625 (3)0.121 (2)
H2WA0.71400.32250.50450.181*
H2WB0.77120.38310.46400.181*
O3W0.0201 (6)0.3301 (4)0.5273 (3)0.156 (3)
H3WA0.00320.30390.56210.233*
H3WB0.07480.35410.55140.233*
O4W0.8631 (5)0.4785 (3)0.6365 (4)0.145 (3)
H4A0.83410.47740.58560.218*
H4B0.82370.43940.65420.218*
O5WA0.135 (3)0.4788 (13)0.5138 (13)0.266 (9)0.50
O5WB0.098 (3)0.5529 (13)0.5214 (13)0.266 (9)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0287 (4)0.0387 (4)0.0361 (4)0.0013 (3)0.0010 (3)0.0021 (3)
Ni20.0389 (4)0.0353 (4)0.0400 (4)0.0009 (3)0.0014 (3)0.0044 (3)
S110.0525 (10)0.0550 (10)0.0661 (12)0.0191 (7)0.0052 (8)0.0038 (9)
S120.0670 (11)0.0590 (10)0.0553 (10)0.0030 (8)0.0253 (9)0.0015 (8)
S210.0567 (10)0.0613 (10)0.0713 (12)0.0170 (8)0.0036 (9)0.0202 (9)
S220.0603 (11)0.0759 (12)0.0878 (14)0.0296 (9)0.0073 (10)0.0251 (11)
N110.037 (3)0.036 (2)0.038 (3)0.0018 (19)0.001 (2)0.003 (2)
N120.059 (3)0.055 (3)0.055 (3)0.006 (2)0.009 (3)0.016 (3)
N130.035 (2)0.044 (3)0.038 (3)0.001 (2)0.004 (2)0.004 (2)
N140.076 (4)0.078 (4)0.073 (4)0.028 (3)0.033 (3)0.032 (3)
N210.034 (3)0.044 (3)0.039 (3)0.004 (2)0.003 (2)0.003 (2)
N220.042 (3)0.053 (3)0.072 (4)0.000 (2)0.022 (3)0.013 (3)
N230.035 (3)0.050 (3)0.041 (3)0.007 (2)0.002 (2)0.005 (2)
N240.055 (3)0.100 (4)0.067 (4)0.018 (3)0.027 (3)0.004 (3)
N310.032 (2)0.037 (2)0.033 (3)0.0001 (19)0.003 (2)0.001 (2)
N410.031 (2)0.037 (2)0.034 (3)0.0001 (18)0.004 (2)0.003 (2)
O10.044 (2)0.065 (3)0.040 (2)0.0184 (18)0.0130 (18)0.011 (2)
O20.0328 (19)0.043 (2)0.040 (2)0.0005 (15)0.0041 (16)0.0098 (17)
O310.038 (2)0.043 (2)0.042 (2)0.0023 (16)0.0047 (17)0.0068 (19)
O320.037 (2)0.045 (2)0.044 (2)0.0109 (17)0.0055 (18)0.0054 (18)
O330.050 (2)0.043 (2)0.057 (3)0.0090 (18)0.001 (2)0.005 (2)
O340.042 (2)0.058 (3)0.072 (3)0.0099 (19)0.011 (2)0.014 (2)
O410.045 (2)0.041 (2)0.046 (2)0.0111 (17)0.0074 (19)0.0009 (19)
O420.068 (3)0.080 (3)0.039 (3)0.028 (2)0.016 (2)0.006 (2)
O430.057 (2)0.046 (2)0.040 (2)0.0014 (19)0.0075 (19)0.0070 (19)
O440.057 (3)0.075 (3)0.042 (2)0.017 (2)0.008 (2)0.011 (2)
C110.034 (3)0.047 (3)0.045 (4)0.000 (2)0.004 (3)0.005 (3)
C120.047 (4)0.064 (4)0.067 (5)0.015 (3)0.006 (3)0.005 (4)
C130.044 (3)0.041 (3)0.044 (4)0.001 (3)0.008 (3)0.002 (3)
C140.032 (3)0.042 (3)0.049 (4)0.002 (2)0.004 (3)0.006 (3)
C150.053 (4)0.053 (4)0.051 (4)0.008 (3)0.017 (3)0.001 (3)
C160.044 (3)0.052 (4)0.046 (4)0.001 (3)0.006 (3)0.000 (3)
C210.042 (3)0.037 (3)0.048 (4)0.000 (3)0.009 (3)0.004 (3)
C220.070 (4)0.037 (3)0.087 (5)0.001 (3)0.005 (4)0.010 (4)
C230.037 (3)0.046 (3)0.042 (3)0.011 (3)0.002 (3)0.004 (3)
C240.048 (3)0.036 (3)0.051 (4)0.004 (3)0.014 (3)0.005 (3)
C250.063 (4)0.051 (4)0.078 (5)0.015 (3)0.009 (4)0.005 (4)
C260.042 (4)0.074 (4)0.046 (4)0.018 (3)0.002 (3)0.008 (3)
C310.032 (3)0.036 (3)0.037 (3)0.002 (2)0.002 (2)0.006 (3)
C320.036 (3)0.060 (4)0.036 (3)0.008 (3)0.008 (3)0.000 (3)
C330.044 (3)0.051 (4)0.043 (4)0.000 (3)0.004 (3)0.008 (3)
C340.044 (3)0.038 (3)0.045 (4)0.007 (2)0.001 (3)0.006 (3)
C350.030 (3)0.033 (3)0.035 (3)0.001 (2)0.000 (2)0.001 (2)
C360.030 (3)0.039 (3)0.034 (3)0.003 (2)0.008 (2)0.000 (3)
C370.038 (3)0.044 (3)0.049 (4)0.000 (3)0.005 (3)0.013 (3)
C410.043 (3)0.041 (3)0.034 (3)0.001 (2)0.003 (3)0.007 (3)
C420.055 (4)0.052 (4)0.045 (4)0.005 (3)0.001 (3)0.013 (3)
C430.060 (4)0.046 (4)0.052 (4)0.013 (3)0.011 (3)0.004 (3)
C440.046 (3)0.040 (3)0.048 (4)0.009 (3)0.008 (3)0.007 (3)
C450.038 (3)0.034 (3)0.040 (3)0.004 (2)0.002 (3)0.006 (3)
C470.046 (3)0.048 (4)0.039 (4)0.006 (3)0.003 (3)0.003 (3)
C460.042 (3)0.045 (3)0.041 (3)0.007 (3)0.003 (3)0.005 (3)
O1W0.082 (3)0.077 (3)0.091 (4)0.030 (3)0.014 (3)0.010 (3)
O2W0.109 (4)0.097 (4)0.160 (6)0.013 (3)0.038 (4)0.074 (4)
O3W0.168 (6)0.203 (7)0.098 (5)0.081 (5)0.037 (4)0.061 (5)
O4W0.091 (4)0.127 (5)0.214 (8)0.018 (4)0.039 (5)0.010 (5)
O5WA0.36 (2)0.28 (2)0.146 (10)0.02 (2)0.053 (13)0.031 (19)
O5WB0.36 (2)0.28 (2)0.146 (10)0.02 (2)0.053 (13)0.031 (19)
Geometric parameters (Å, º) top
Ni1—O12.107 (3)O2—H2A0.9445
Ni1—O22.104 (3)O31—C361.262 (5)
Ni1—N112.097 (4)O32—C361.240 (5)
Ni1—N132.083 (4)O33—C371.269 (6)
Ni1—N212.110 (4)O34—C371.241 (6)
Ni1—N232.125 (4)O41—C471.257 (6)
Ni2—O312.109 (3)O42—C471.241 (6)
Ni2—O332.137 (4)O43—C461.257 (6)
Ni2—O412.187 (4)O44—C461.254 (6)
Ni2—O432.104 (4)C11—C121.353 (7)
Ni2—N311.952 (4)C11—C141.464 (7)
Ni2—N411.961 (4)C12—H120.9300
S11—C121.714 (7)C14—C151.347 (7)
S11—C131.740 (5)C15—H150.9300
S12—C151.722 (6)C21—C221.328 (7)
S12—C161.730 (6)C21—C241.451 (7)
S21—C221.711 (6)C22—H220.9300
S21—C231.718 (5)C24—C251.334 (7)
S22—C251.722 (7)C25—H250.9300
S22—C261.738 (6)C31—C321.378 (7)
N11—C131.317 (6)C31—C371.513 (7)
N11—C111.391 (6)C32—C331.376 (7)
N12—C131.334 (7)C32—H320.9300
N12—H12A0.8600C33—C341.381 (7)
N12—H12B0.8600C33—H330.9300
N13—C161.303 (6)C34—C351.393 (6)
N13—C141.392 (6)C34—H340.9300
N14—C161.350 (7)C35—C361.526 (7)
N14—H14A0.8600C41—C421.384 (7)
N14—H14B0.8600C41—C471.516 (7)
N21—C231.325 (6)C42—C431.386 (8)
N21—C211.392 (6)C42—H420.9300
N22—C231.340 (6)C43—C441.367 (8)
N22—H22A0.8600C43—H430.9300
N22—H22B0.8600C44—C451.378 (7)
N23—C261.316 (6)C44—H440.9300
N23—C241.392 (6)C45—C461.513 (7)
N24—C261.319 (7)O1W—H1WA0.9567
N24—H24A0.8600O1W—H1WB0.9183
N24—H24B0.8600O2W—H2WA0.9357
N31—C351.330 (6)O2W—H2WB0.9364
N31—C311.347 (6)O3W—H3WA0.8158
N41—C451.330 (6)O3W—H3WB0.8767
N41—C411.337 (6)O4W—H4A0.9446
O1—H1A0.8946O4W—H4B0.9252
O1—H1B0.8733O5WA—O5WB1.45 (3)
O2—H2B0.8912
N13—Ni1—N1180.01 (17)C11—C12—H12125.0
N13—Ni1—O2170.49 (14)S11—C12—H12125.0
N11—Ni1—O291.29 (15)N11—C13—N12125.2 (5)
N13—Ni1—O187.99 (15)N11—C13—S11114.1 (4)
N11—Ni1—O191.30 (15)N12—C13—S11120.7 (4)
O2—Ni1—O188.40 (13)C15—C14—N13115.7 (5)
N13—Ni1—N2193.39 (16)C15—C14—C11127.9 (5)
N11—Ni1—N2196.93 (16)N13—C14—C11116.4 (5)
O2—Ni1—N2191.43 (15)C14—C15—S12109.9 (4)
O1—Ni1—N21171.77 (15)C14—C15—H15125.0
N13—Ni1—N2398.83 (16)S12—C15—H15125.0
N11—Ni1—N23175.75 (16)N13—C16—N14124.0 (5)
O2—Ni1—N2390.12 (15)N13—C16—S12114.6 (4)
O1—Ni1—N2392.75 (16)N14—C16—S12121.5 (5)
N21—Ni1—N2379.02 (17)C22—C21—N21115.1 (5)
N31—Ni2—N41177.53 (17)C22—C21—C24128.4 (5)
N31—Ni2—O4398.73 (16)N21—C21—C24116.6 (5)
N41—Ni2—O4378.93 (16)C21—C22—S21111.5 (4)
N31—Ni2—O3178.41 (15)C21—C22—H22124.2
N41—Ni2—O31100.83 (14)S21—C22—H22124.2
O43—Ni2—O3192.01 (14)N21—C23—N22124.8 (5)
N31—Ni2—O3378.06 (15)N21—C23—S21114.4 (4)
N41—Ni2—O33102.84 (15)N22—C23—S21120.8 (4)
O43—Ni2—O3395.11 (14)C25—C24—N23114.8 (5)
O31—Ni2—O33156.18 (14)C25—C24—C21128.7 (6)
N31—Ni2—O41105.81 (15)N23—C24—C21116.5 (4)
N41—Ni2—O4176.57 (15)C24—C25—S22110.9 (5)
O43—Ni2—O41155.32 (14)C24—C25—H25124.5
O31—Ni2—O4195.40 (14)S22—C25—H25124.5
O33—Ni2—O4187.51 (14)N23—C26—N24124.6 (6)
C12—S11—C1389.8 (3)N23—C26—S22113.1 (5)
C15—S12—C1689.4 (3)N24—C26—S22122.4 (4)
C22—S21—C2389.1 (3)N31—C31—C32120.9 (5)
C25—S22—C2689.6 (3)N31—C31—C37112.2 (4)
C13—N11—C11110.1 (4)C32—C31—C37126.9 (5)
C13—N11—Ni1135.7 (4)C33—C32—C31118.1 (5)
C11—N11—Ni1113.9 (3)C33—C32—H32121.0
C13—N12—H12A120.0C31—C32—H32121.0
C13—N12—H12B120.0C32—C33—C34121.2 (5)
H12A—N12—H12B120.0C32—C33—H33119.4
C16—N13—C14110.4 (5)C34—C33—H33119.4
C16—N13—Ni1135.7 (4)C33—C34—C35117.9 (5)
C14—N13—Ni1113.9 (3)C33—C34—H34121.1
C16—N14—H14A120.0C35—C34—H34121.1
C16—N14—H14B120.0N31—C35—C34120.7 (4)
H14A—N14—H14B120.0N31—C35—C36112.1 (4)
C23—N21—C21109.9 (4)C34—C35—C36127.2 (4)
C23—N21—Ni1136.0 (4)O32—C36—O31125.6 (5)
C21—N21—Ni1114.0 (3)O32—C36—C35119.0 (5)
C23—N22—H22A120.0O31—C36—C35115.4 (4)
C23—N22—H22B120.0O34—C37—O33126.5 (5)
H22A—N22—H22B120.0O34—C37—C31117.7 (5)
C26—N23—C24111.6 (5)O33—C37—C31115.8 (5)
C26—N23—Ni1134.7 (4)N41—C41—C42120.9 (5)
C24—N23—Ni1113.6 (3)N41—C41—C47112.9 (5)
C26—N24—H24A120.0C42—C41—C47126.2 (5)
C26—N24—H24B120.0C41—C42—C43117.5 (5)
H24A—N24—H24B120.0C41—C42—H42121.2
C35—N31—C31121.2 (4)C43—C42—H42121.2
C35—N31—Ni2119.3 (3)C44—C43—C42120.9 (5)
C31—N31—Ni2119.4 (3)C44—C43—H43119.5
C45—N41—C41121.3 (4)C42—C43—H43119.5
C45—N41—Ni2118.1 (4)C43—C44—C45118.6 (5)
C41—N41—Ni2120.6 (3)C43—C44—H44120.7
Ni1—O1—H1A135.2C45—C44—H44120.7
Ni1—O1—H1B101.7N41—C45—C44120.7 (5)
H1A—O1—H1B106.9N41—C45—C46112.5 (5)
Ni1—O2—H2B102.1C44—C45—C46126.8 (5)
Ni1—O2—H2A117.9O42—C47—O41126.7 (5)
H2B—O2—H2A107.6O42—C47—C41117.9 (5)
C36—O31—Ni2114.7 (3)O41—C47—C41115.3 (5)
C37—O33—Ni2113.8 (3)O44—C46—O43125.8 (5)
C47—O41—Ni2114.6 (3)O44—C46—C45117.8 (5)
C46—O43—Ni2113.7 (3)O43—C46—C45116.5 (5)
C12—C11—N11116.0 (5)H1WA—O1W—H1WB108.3
C12—C11—C14128.4 (5)H2WA—O2W—H2WB107.7
N11—C11—C14115.6 (4)H3WA—O3W—H3WB98.1
C11—C12—S11110.0 (5)H4A—O4W—H4B98.0
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1A···O42i0.891.832.672 (5)155
O1—H1B···O440.871.982.700 (5)139
O2—H2A···O41i0.941.782.702 (5)165
O2—H2B···O32ii0.891.852.686 (5)156
O1W—H1WA···O340.961.762.676 (6)159
O1W—H1WB···O42iii0.921.922.831 (6)171
O2W—H2WA···O330.931.972.739 (7)138
O2W—H2WB···O5WBiv0.941.952.89 (3)174
O3W—H3WA···O1Wv0.822.122.720 (8)130
O3W—H3WB···O5WA0.882.523.09 (3)123
O3W—H3WB···O440.882.232.942 (8)139
O4W—H4A···O5WAiv0.941.982.77 (2)139
O4W—H4A···O5WBiv0.942.162.91 (2)135
O4W—H4B···O1W0.922.332.900 (7)120
N12—H12A···O20.862.132.891 (5)147
N12—H12B···O3Wiii0.862.162.975 (8)158
N14—H14A···N230.862.343.111 (6)149
N14—H14B···O2Wiv0.862.202.865 (8)134
N22—H22A···N110.862.363.111 (6)146
N22—H22B···O31iii0.862.483.225 (6)145
N22—H22B···O32iii0.862.162.975 (6)157
N24—H24A···O10.862.142.913 (6)149
N24—H24B···O4Wv0.862.132.893 (8)148
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1/2, y+1/2, z+3/2; (iii) x+1/2, y+1/2, z+1/2; (iv) x+1, y+1, z+1; (v) x1, y, z.
 

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