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The title compound, [Ni(C2H8N2)3]Cl2·2H2O or [Ni(en)3]Cl2·2H2O, where en is 1,2-ethanediamine, contains three [Ni(en)3]2+ cations, six Cl anions and six water mol­ecules in the asymmetric unit. The crystal structure is supported by O—H...Cl, N—H...Cl, O—H...O and N—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806017570/ac2009sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806017570/ac2009Isup2.hkl
Contains datablock I

CCDC reference: 610673

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](Wave) = 0.000 Å
  • R factor = 0.034
  • wR factor = 0.099
  • Data-to-parameter ratio = 8.7

checkCIF/PLATON results

No syntax errors found



Alert level C REFNR01_ALERT_3_C Ratio of reflections to parameters is < 10 for a non-centrosymmetric structure, where ZMAX > 18 sine(theta)/lambda 0.6002 Proportion of unique data used 0.8041 Ratio reflections to parameters 8.7387
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 25.25 From the CIF: _reflns_number_total 5282 Count of symmetry unique reflns 4247 Completeness (_total/calc) 124.37% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1035 Fraction of Friedel pairs measured 0.244 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Tris(1,2-ethanediamine-N,N')nickel(II) dichloride dihydrate top
Crystal data top
[Ni(C2H8N2)3]Cl2·2H2OF(000) = 2208.0
Mr = 345.93Dx = 1.471 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2ycCell parameters from 1679 reflections
a = 26.186 (2) Åθ = 1.4–23.7°
b = 13.8917 (9) ŵ = 1.59 mm1
c = 12.8986 (8) ÅT = 293 K
β = 93.197 (2)°Block, colourless
V = 4684.8 (6) Å30.30 × 0.30 × 0.30 mm
Z = 12
Data collection top
Bruker SMART CCD area detector
diffractometer
5282 independent reflections
Radiation source: fine-focus sealed tube4247 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
φ and ω scansθmax = 25.3°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 2231
Tmin = 0.627, Tmax = 0.627k = 1615
12308 measured reflectionsl = 1515
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)] = 0.034H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.099 w = 1/[σ2(Fo2) + (0.0519P)2 + 4.1952P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max < 0.001
4247 reflectionsΔρmax = 0.80 e Å3
486 parametersΔρmin = 0.45 e Å3
20 restraintsAbsolute structure: Flack (1983), with how many Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.00 (2)
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
Ni10.250270 (17)0.77240 (6)0.51366 (3)0.0263 (3)
Ni20.41627 (3)0.72688 (4)0.99565 (9)0.02602 (18)
Ni30.58250 (3)0.77185 (4)0.49404 (7)0.02559 (19)
O10.2484 (2)0.6837 (3)0.0442 (4)0.0548 (15)
O20.2536 (2)0.6103 (4)0.2479 (4)0.0593 (14)
O60.5860 (2)0.3156 (4)0.4579 (4)0.0565 (14)*
O30.4103 (2)0.1064 (4)0.7575 (4)0.0671 (15)
O40.4181 (2)0.1825 (3)0.9599 (4)0.0576 (13)
O50.5874 (2)0.3926 (5)0.2618 (4)0.0653 (14)*
C130.5556 (3)0.5679 (5)0.4823 (7)0.044 (2)
H13A0.54360.51260.44200.052*
H13B0.54180.56380.55030.052*
C140.6128 (3)0.5668 (5)0.4932 (6)0.0378 (18)
H14A0.62460.51020.53150.045*
H14B0.62690.56540.42530.045*
C30.2789 (3)0.8624 (7)0.3198 (7)0.046 (2)
H3A0.28950.85580.24930.056*
H3B0.29400.92070.34910.056*
C40.2215 (3)0.8694 (7)0.3186 (6)0.050 (2)
H4A0.21000.92650.28100.059*
H4B0.20620.81360.28390.059*
C110.4461 (3)0.9311 (5)0.9974 (6)0.0370 (17)
H11A0.46180.93150.93110.044*
H11B0.45720.98821.03570.044*
C120.3892 (3)0.9309 (5)0.9808 (7)0.044 (2)
H12A0.37370.93591.04710.052*
H12B0.37830.98580.93880.052*
C70.4421 (3)0.6312 (7)1.1944 (6)0.0446 (19)
H7A0.45730.68791.22730.053*
H7B0.45310.57521.23470.053*
C80.3841 (3)0.6390 (6)1.1903 (7)0.049 (2)
H8A0.36870.58121.16000.059*
H8B0.37220.64691.25970.059*
C90.4496 (3)0.6276 (6)0.8094 (6)0.0452 (19)
H9A0.46470.57120.84310.054*
H9B0.46160.63140.73970.054*
C100.3920 (3)0.6196 (7)0.8046 (6)0.0446 (18)
H10A0.37710.67340.76570.053*
H10B0.38150.56060.76920.053*
C150.6165 (3)0.8667 (6)0.6901 (6)0.046 (2)
H15A0.62910.92270.72830.056*
H15B0.63220.80970.72130.056*
C160.5593 (3)0.8606 (7)0.6931 (7)0.056 (2)
H16A0.54970.85360.76430.068*
H16B0.54370.91890.66470.068*
C170.6066 (3)0.8735 (7)0.3020 (6)0.047 (2)
H17A0.61520.86990.23000.057*
H17B0.62250.93060.33260.057*
C180.5487 (3)0.8796 (7)0.3081 (6)0.0505 (19)
H18A0.53600.93850.27550.061*
H18B0.53250.82550.27170.061*
C10.2790 (3)0.8784 (7)0.7042 (6)0.048 (2)
H1A0.29090.93630.73990.057*
H1B0.29370.82310.74090.057*
C20.2212 (3)0.8734 (8)0.7008 (7)0.050 (2)
H2A0.20950.87230.77080.060*
H2B0.20670.92940.66530.060*
C50.2221 (3)0.5693 (5)0.5148 (6)0.041 (2)
H5A0.21040.51160.47840.049*
H6B0.20700.57070.58170.049*
C60.2801 (3)0.5674 (5)0.5305 (6)0.0343 (18)
H6A0.29070.51350.57450.041*
H5B0.29540.55980.46420.041*
Cl10.25234 (8)0.09788 (16)0.50712 (17)0.0516 (6)
Cl50.58309 (10)0.09717 (9)0.4979 (2)0.0473 (4)
Cl40.41631 (11)0.59980 (9)0.4993 (2)0.0506 (3)
Cl20.24875 (10)0.38611 (15)0.31461 (16)0.0469 (4)
Cl30.42028 (8)0.11590 (14)1.19457 (14)0.0523 (4)
Cl60.58160 (8)0.61568 (14)0.19103 (14)0.0472 (4)
N130.5376 (2)0.6572 (4)0.4301 (4)0.0282 (13)
HA130.50430.66710.44070.034*
HB130.54120.65300.36120.034*
N140.6294 (2)0.6548 (4)0.5494 (5)0.0350 (14)
HA140.66240.66720.53860.042*
HB140.62630.64680.61800.042*
N30.2967 (2)0.7787 (4)0.3819 (5)0.0343 (15)
HA30.32990.78580.40280.041*
HB30.29320.72440.34430.041*
N40.2057 (2)0.8740 (5)0.4252 (5)0.0364 (15)
HA40.17220.85980.42730.044*
HB40.21090.93360.45110.044*
N110.4615 (2)0.8440 (4)1.0564 (5)0.0356 (15)
HA110.45630.85231.12420.043*
HB110.49490.83181.04980.043*
N120.3724 (2)0.8406 (4)0.9280 (4)0.0298 (13)
HA120.37730.84450.85960.036*
HB120.33890.83040.93610.036*
N70.4584 (2)0.6225 (5)1.0874 (4)0.0390 (15)
HA70.45180.56291.06280.047*
HB70.49210.63371.08560.047*
N80.3699 (3)0.7230 (4)1.1261 (5)0.0409 (17)
HA80.37450.77721.16370.049*
HB80.33670.71931.10440.049*
N90.4648 (2)0.7148 (4)0.8684 (5)0.0335 (14)
HA90.46130.76710.82730.040*
HB90.49770.71040.89200.040*
N100.3737 (2)0.6194 (5)0.9115 (4)0.0363 (14)
HA100.37880.56140.94130.044*
HB100.34000.63290.91010.044*
N150.6291 (2)0.8743 (5)0.5784 (5)0.0390 (15)
HA150.66240.86130.57150.047*
HB150.62260.93410.55430.047*
N160.5416 (3)0.7776 (5)0.6320 (5)0.0403 (17)
HB160.50790.78280.61570.048*
HA160.54700.72330.66900.048*
N170.6256 (2)0.7865 (4)0.3588 (5)0.0350 (15)
HA170.65910.79290.37720.042*
HB170.62150.73410.31820.042*
N180.5361 (2)0.8780 (5)0.4180 (5)0.0373 (14)
HA180.50280.86380.42330.045*
HB180.54230.93600.44710.045*
N10.2945 (2)0.8791 (5)0.5964 (5)0.0392 (15)
HB10.32800.86580.59440.047*
HA10.28860.93750.56770.047*
N20.2053 (3)0.7858 (5)0.6456 (5)0.0387 (16)
HB20.17190.78930.62530.046*
HA20.21000.73430.68730.046*
N60.2969 (2)0.6580 (5)0.5792 (5)0.0391 (16)
HA60.33000.66890.56770.047*
HB60.29380.65500.64830.047*
N50.2060 (2)0.6547 (4)0.4543 (5)0.0325 (14)
HB50.17250.66610.46070.039*
HA50.21130.64560.38670.039*
H1E0.243 (2)0.672 (3)0.0202 (17)0.039*
H1F0.2352 (16)0.7380 (19)0.057 (3)0.039*
H2E0.252 (2)0.632 (2)0.186 (2)0.039*
H2F0.251 (2)0.5495 (14)0.244 (3)0.039*
H6E0.5555 (9)0.308 (3)0.433 (3)0.039*
H6F0.5847 (18)0.340 (3)0.518 (2)0.039*
H3E0.4091 (17)0.131 (2)0.6969 (19)0.039*
H3F0.415 (2)0.0462 (14)0.751 (3)0.039*
H4E0.4367 (12)0.196 (4)1.014 (3)0.039*
H4F0.3874 (8)0.197 (4)0.972 (3)0.039*
H5E0.5686 (14)0.442 (2)0.251 (3)0.039*
H5F0.6025 (16)0.399 (3)0.321 (2)0.039*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0256 (4)0.0273 (5)0.0260 (6)0.0006 (3)0.0011 (5)0.0004 (3)
Ni20.0249 (3)0.0265 (3)0.0265 (4)0.0010 (4)0.0002 (3)0.0002 (3)
Ni30.0257 (3)0.0251 (3)0.0260 (5)0.0007 (4)0.0013 (3)0.0003 (3)
O10.102 (4)0.034 (2)0.028 (2)0.001 (2)0.006 (2)0.0046 (15)
O20.096 (4)0.048 (2)0.034 (2)0.004 (2)0.007 (2)0.0107 (18)
O30.102 (4)0.061 (3)0.039 (2)0.008 (3)0.005 (3)0.006 (2)
O40.066 (3)0.055 (3)0.051 (2)0.001 (2)0.002 (2)0.0054 (19)
C130.060 (5)0.023 (3)0.048 (4)0.008 (3)0.003 (4)0.004 (3)
C140.024 (4)0.036 (4)0.053 (5)0.005 (3)0.005 (3)0.007 (3)
C30.055 (4)0.052 (5)0.033 (4)0.003 (4)0.010 (3)0.015 (3)
C40.065 (5)0.045 (5)0.038 (4)0.006 (4)0.003 (4)0.010 (4)
C110.031 (4)0.035 (3)0.045 (4)0.003 (3)0.007 (3)0.001 (3)
C120.061 (5)0.022 (3)0.048 (4)0.008 (3)0.001 (4)0.004 (3)
C70.047 (4)0.049 (4)0.037 (4)0.001 (4)0.007 (3)0.011 (3)
C80.048 (4)0.051 (5)0.048 (4)0.005 (4)0.009 (4)0.016 (4)
C90.051 (4)0.044 (4)0.041 (4)0.006 (3)0.007 (3)0.012 (3)
C100.051 (4)0.044 (4)0.038 (4)0.002 (4)0.005 (3)0.012 (3)
C150.055 (4)0.049 (4)0.035 (4)0.007 (4)0.009 (3)0.011 (3)
C160.067 (5)0.058 (6)0.046 (4)0.006 (4)0.009 (4)0.014 (4)
C170.063 (5)0.042 (4)0.037 (4)0.013 (4)0.008 (3)0.012 (3)
C180.064 (5)0.046 (4)0.040 (4)0.007 (4)0.006 (3)0.011 (4)
C10.055 (5)0.048 (5)0.039 (4)0.004 (4)0.011 (4)0.012 (4)
C20.050 (5)0.062 (5)0.038 (4)0.011 (4)0.004 (3)0.014 (4)
C50.057 (5)0.022 (3)0.045 (4)0.005 (3)0.011 (4)0.005 (3)
C60.027 (4)0.035 (4)0.041 (4)0.005 (3)0.006 (3)0.001 (3)
Cl10.0435 (11)0.0396 (12)0.0723 (16)0.0018 (11)0.0099 (10)0.0035 (10)
Cl50.0406 (7)0.0359 (7)0.0659 (10)0.0015 (12)0.0073 (6)0.0008 (12)
Cl40.0456 (7)0.0365 (6)0.0710 (9)0.0010 (13)0.0146 (6)0.0018 (13)
Cl20.0541 (10)0.0507 (9)0.0360 (9)0.0059 (11)0.0030 (8)0.0078 (10)
Cl30.0578 (9)0.0585 (9)0.0405 (8)0.0075 (9)0.0034 (8)0.0090 (9)
Cl60.0509 (9)0.0532 (9)0.0373 (8)0.0048 (9)0.0005 (7)0.0080 (9)
N130.026 (3)0.031 (3)0.027 (3)0.003 (2)0.000 (2)0.004 (2)
N140.031 (3)0.037 (3)0.037 (3)0.001 (2)0.001 (2)0.001 (2)
N30.029 (3)0.036 (3)0.038 (4)0.003 (2)0.005 (2)0.001 (2)
N40.033 (3)0.035 (4)0.041 (3)0.000 (3)0.000 (2)0.001 (3)
N110.031 (3)0.039 (3)0.036 (3)0.004 (2)0.002 (2)0.002 (2)
N120.028 (3)0.035 (3)0.027 (3)0.001 (2)0.001 (2)0.006 (2)
N70.038 (3)0.032 (3)0.047 (4)0.004 (3)0.003 (3)0.005 (3)
N80.041 (4)0.050 (4)0.033 (3)0.002 (3)0.004 (3)0.004 (2)
N90.028 (3)0.037 (3)0.037 (3)0.001 (2)0.006 (2)0.003 (2)
N100.032 (3)0.037 (3)0.039 (3)0.000 (3)0.005 (2)0.003 (3)
N150.041 (3)0.032 (3)0.044 (3)0.006 (3)0.000 (3)0.006 (3)
N160.043 (4)0.049 (4)0.030 (3)0.005 (3)0.008 (3)0.003 (2)
N170.032 (3)0.037 (3)0.037 (4)0.005 (3)0.007 (3)0.004 (2)
N180.035 (3)0.033 (3)0.044 (3)0.000 (3)0.003 (2)0.002 (3)
N10.037 (3)0.033 (3)0.048 (4)0.005 (3)0.002 (3)0.000 (3)
N20.042 (4)0.046 (4)0.029 (3)0.006 (3)0.002 (3)0.002 (3)
N60.035 (3)0.044 (4)0.038 (4)0.006 (3)0.003 (3)0.004 (3)
N50.032 (3)0.034 (3)0.032 (3)0.003 (2)0.003 (2)0.006 (2)
Geometric parameters (Å, º) top
Ni1—N52.122 (6)C15—N151.500 (11)
Ni1—N42.123 (6)C15—C161.502 (12)
Ni1—N12.130 (6)C15—H15A0.9700
Ni1—N22.131 (7)C15—H15B0.9700
Ni1—N32.146 (6)C16—N161.457 (11)
Ni1—N62.149 (6)C16—H16A0.9700
Ni2—N122.114 (5)C16—H16B0.9700
Ni2—N102.125 (6)C17—N171.485 (10)
Ni2—N82.130 (7)C17—C181.525 (12)
Ni2—N112.135 (6)C17—H17A0.9700
Ni2—N92.137 (6)C17—H17B0.9700
Ni2—N72.138 (6)C18—N181.472 (10)
Ni3—N182.116 (6)C18—H18A0.9700
Ni3—N132.119 (5)C18—H18B0.9700
Ni3—N162.129 (7)C1—N11.469 (10)
Ni3—N152.133 (6)C1—C21.513 (10)
Ni3—N142.136 (6)C1—H1A0.9700
Ni3—N172.140 (6)C1—H1B0.9700
O1—H1E0.850 (19)C2—N21.460 (11)
O1—H1F0.850 (18)C2—H2A0.9700
O2—H2E0.850 (19)C2—H2B0.9700
O2—H2F0.850 (18)C5—N51.468 (9)
O6—H6E0.850 (18)C5—C61.520 (11)
O6—H6F0.850 (19)C5—H5A0.9700
O3—H3E0.850 (18)C5—H6B0.9700
O3—H3F0.850 (18)C6—N61.465 (9)
O4—H4E0.850 (19)C6—H6A0.9700
O4—H4F0.850 (19)C6—H5B0.9700
O5—H5E0.850 (18)N13—HA130.9000
O5—H5F0.850 (18)N13—HB130.9000
C13—N131.476 (9)N14—HA140.9000
C13—C141.497 (8)N14—HB140.9000
C13—H13A0.9700N3—HA30.9000
C13—H13B0.9700N3—HB30.9000
C14—N141.473 (9)N4—HA40.9000
C14—H14A0.9700N4—HB40.9000
C14—H14B0.9700N11—HA110.9000
C3—N31.473 (10)N11—HB110.9000
C3—C41.504 (11)N12—HA120.9000
C3—H3A0.9700N12—HB120.9000
C3—H3B0.9700N7—HA70.9000
C4—N41.459 (10)N7—HB70.9000
C4—H4A0.9700N8—HA80.9000
C4—H4B0.9700N8—HB80.9000
C11—N111.475 (9)N9—HA90.9000
C11—C121.494 (8)N9—HB90.9000
C11—H11A0.9700N10—HA100.9000
C11—H11B0.9700N10—HB100.9000
C12—N121.482 (9)N15—HA150.9000
C12—H12A0.9700N15—HB150.9000
C12—H12B0.9700N16—HB160.9000
C7—N71.473 (10)N16—HA160.9000
C7—C81.521 (11)N17—HA170.9000
C7—H7A0.9700N17—HB170.9000
C7—H7B0.9700N18—HA180.9000
C8—N81.467 (10)N18—HB180.9000
C8—H8A0.9700N1—HB10.9000
C8—H8B0.9700N1—HA10.9000
C9—N91.474 (10)N2—HB20.9000
C9—C101.508 (11)N2—HA20.9000
C9—H9A0.9700N6—HA60.9000
C9—H9B0.9700N6—HB60.9000
C10—N101.486 (10)N5—HB50.9000
C10—H10A0.9700N5—HA50.9000
C10—H10B0.9700
N5—Ni1—N492.6 (3)H18A—C18—H18B108.3
N5—Ni1—N1170.9 (2)N1—C1—C2107.5 (6)
N4—Ni1—N194.2 (2)N1—C1—H1A110.2
N5—Ni1—N292.3 (2)C2—C1—H1A110.2
N4—Ni1—N293.4 (2)N1—C1—H1B110.2
N1—Ni1—N281.3 (2)C2—C1—H1B110.2
N5—Ni1—N393.9 (2)H1A—C1—H1B108.5
N4—Ni1—N382.3 (2)N2—C2—C1108.1 (8)
N1—Ni1—N393.0 (2)N2—C2—H2A110.1
N2—Ni1—N3172.6 (2)C1—C2—H2A110.1
N5—Ni1—N681.9 (2)N2—C2—H2B110.1
N4—Ni1—N6170.6 (3)C1—C2—H2B110.1
N1—Ni1—N692.1 (3)H2A—C2—H2B108.4
N2—Ni1—N694.5 (3)N5—C5—C6109.9 (6)
N3—Ni1—N690.4 (2)N5—C5—H5A109.7
N12—Ni2—N1093.2 (3)C6—C5—H5A109.7
N12—Ni2—N891.4 (2)N5—C5—H6B109.7
N10—Ni2—N894.6 (2)C6—C5—H6B109.7
N12—Ni2—N1181.95 (15)H5A—C5—H6B108.2
N10—Ni2—N11170.8 (2)N6—C6—C5108.5 (6)
N8—Ni2—N1193.3 (3)N6—C6—H6A110.0
N12—Ni2—N994.2 (2)C5—C6—H6A110.0
N10—Ni2—N982.5 (2)N6—C6—H5B110.0
N8—Ni2—N9173.82 (17)C5—C6—H5B110.0
N11—Ni2—N990.0 (2)H6A—C6—H5B108.4
N12—Ni2—N7170.8 (2)C13—N13—Ni3107.3 (4)
N10—Ni2—N792.65 (15)C13—N13—HA13110.3
N8—Ni2—N781.1 (2)Ni3—N13—HA13110.3
N11—Ni2—N793.2 (3)C13—N13—HB13110.3
N9—Ni2—N793.6 (2)Ni3—N13—HB13110.3
N18—Ni3—N1392.9 (3)HA13—N13—HB13108.5
N18—Ni3—N1693.4 (3)C14—N14—Ni3108.6 (4)
N13—Ni3—N1693.4 (2)C14—N14—HA14110.0
N18—Ni3—N1593.95 (16)Ni3—N14—HA14110.0
N13—Ni3—N15171.6 (3)C14—N14—HB14110.0
N16—Ni3—N1581.3 (3)Ni3—N14—HB14110.0
N18—Ni3—N14171.7 (2)HA14—N14—HB14108.3
N13—Ni3—N1481.60 (15)C3—N3—Ni1106.7 (5)
N16—Ni3—N1493.2 (2)C3—N3—HA3110.4
N15—Ni3—N1492.1 (3)Ni1—N3—HA3110.4
N18—Ni3—N1782.6 (2)C3—N3—HB3110.4
N13—Ni3—N1793.5 (2)Ni1—N3—HB3110.4
N16—Ni3—N17172.18 (17)HA3—N3—HB3108.6
N15—Ni3—N1792.2 (2)C4—N4—Ni1107.5 (5)
N14—Ni3—N1791.5 (2)C4—N4—HA4110.2
H1E—O1—H1F108 (2)Ni1—N4—HA4110.2
H2E—O2—H2F108 (2)C4—N4—HB4110.2
H6E—O6—H6F108 (2)Ni1—N4—HB4110.2
H3E—O3—H3F108 (2)HA4—N4—HB4108.5
H4E—O4—H4F108 (3)C11—N11—Ni2107.8 (4)
H5E—O5—H5F108 (2)C11—N11—HA11110.1
N13—C13—C14110.1 (7)Ni2—N11—HA11110.1
N13—C13—H13A109.6C11—N11—HB11110.1
C14—C13—H13A109.6Ni2—N11—HB11110.1
N13—C13—H13B109.6HA11—N11—HB11108.5
C14—C13—H13B109.6C12—N12—Ni2107.6 (4)
H13A—C13—H13B108.2C12—N12—HA12110.2
N14—C14—C13107.7 (6)Ni2—N12—HA12110.2
N14—C14—H14A110.2C12—N12—HB12110.2
C13—C14—H14A110.2Ni2—N12—HB12110.2
N14—C14—H14B110.2HA12—N12—HB12108.5
C13—C14—H14B110.2C7—N7—Ni2107.2 (5)
H14A—C14—H14B108.5C7—N7—HA7110.3
N3—C3—C4110.0 (7)Ni2—N7—HA7110.3
N3—C3—H3A109.7C7—N7—HB7110.3
C4—C3—H3A109.7Ni2—N7—HB7110.3
N3—C3—H3B109.7HA7—N7—HB7108.5
C4—C3—H3B109.7C8—N8—Ni2109.1 (5)
H3A—C3—H3B108.2C8—N8—HA8109.9
N4—C4—C3109.2 (6)Ni2—N8—HA8109.9
N4—C4—H4A109.8C8—N8—HB8109.9
C3—C4—H4A109.8Ni2—N8—HB8109.9
N4—C4—H4B109.8HA8—N8—HB8108.3
C3—C4—H4B109.8C9—N9—Ni2107.8 (5)
H4A—C4—H4B108.3C9—N9—HA9110.1
N11—C11—C12108.3 (6)Ni2—N9—HA9110.1
N11—C11—H11A110.0C9—N9—HB9110.1
C12—C11—H11A110.0Ni2—N9—HB9110.1
N11—C11—H11B110.0HA9—N9—HB9108.5
C12—C11—H11B110.0C10—N10—Ni2106.6 (5)
H11A—C11—H11B108.4C10—N10—HA10110.4
N12—C12—C11109.6 (6)Ni2—N10—HA10110.4
N12—C12—H12A109.7C10—N10—HB10110.4
C11—C12—H12A109.7Ni2—N10—HB10110.4
N12—C12—H12B109.7HA10—N10—HB10108.6
C11—C12—H12B109.7C15—N15—Ni3107.0 (5)
H12A—C12—H12B108.2C15—N15—HA15110.3
N7—C7—C8108.3 (6)Ni3—N15—HA15110.3
N7—C7—H7A110.0C15—N15—HB15110.3
C8—C7—H7A110.0Ni3—N15—HB15110.3
N7—C7—H7B110.0HA15—N15—HB15108.6
C8—C7—H7B110.0C16—N16—Ni3108.8 (5)
H7A—C7—H7B108.4C16—N16—HB16109.9
N8—C8—C7107.3 (7)Ni3—N16—HB16109.9
N8—C8—H8A110.3C16—N16—HA16109.9
C7—C8—H8A110.3Ni3—N16—HA16109.9
N8—C8—H8B110.3HB16—N16—HA16108.3
C7—C8—H8B110.3C17—N17—Ni3107.6 (5)
H8A—C8—H8B108.5C17—N17—HA17110.2
N9—C9—C10108.8 (7)Ni3—N17—HA17110.2
N9—C9—H9A109.9C17—N17—HB17110.2
C10—C9—H9A109.9Ni3—N17—HB17110.2
N9—C9—H9B109.9HA17—N17—HB17108.5
C10—C9—H9B109.9C18—N18—Ni3107.7 (5)
H9A—C9—H9B108.3C18—N18—HA18110.2
N10—C10—C9109.6 (6)Ni3—N18—HA18110.2
N10—C10—H10A109.7C18—N18—HB18110.2
C9—C10—H10A109.7Ni3—N18—HB18110.2
N10—C10—H10B109.7HA18—N18—HB18108.5
C9—C10—H10B109.7C1—N1—Ni1107.4 (5)
H10A—C10—H10B108.2C1—N1—HB1110.2
N15—C15—C16107.7 (6)Ni1—N1—HB1110.2
N15—C15—H15A110.2C1—N1—HA1110.2
C16—C15—H15A110.2Ni1—N1—HA1110.2
N15—C15—H15B110.2HB1—N1—HA1108.5
C16—C15—H15B110.2C2—N2—Ni1107.9 (5)
H15A—C15—H15B108.5C2—N2—HB2110.1
N16—C16—C15108.5 (7)Ni1—N2—HB2110.1
N16—C16—H16A110.0C2—N2—HA2110.1
C15—C16—H16A110.0Ni1—N2—HA2110.1
N16—C16—H16B110.0HB2—N2—HA2108.4
C15—C16—H16B110.0C6—N6—Ni1108.4 (4)
H16A—C16—H16B108.4C6—N6—HA6110.0
N17—C17—C18109.1 (7)Ni1—N6—HA6110.0
N17—C17—H17A109.9C6—N6—HB6110.0
C18—C17—H17A109.9Ni1—N6—HB6110.0
N17—C17—H17B109.9HA6—N6—HB6108.4
C18—C17—H17B109.9C5—N5—Ni1107.2 (4)
H17A—C17—H17B108.3C5—N5—HB5110.3
N18—C18—C17108.9 (6)Ni1—N5—HB5110.3
N18—C18—H18A109.9C5—N5—HA5110.3
C17—C18—H18A109.9Ni1—N5—HA5110.3
N18—C18—H18B109.9HB5—N5—HA5108.5
C17—C18—H18B109.9
N13—C13—C14—N1456.1 (7)N10—Ni2—N9—C912.8 (5)
N3—C3—C4—N456.2 (11)N8—Ni2—N9—C950 (3)
N11—C11—C12—N1256.2 (7)N11—Ni2—N9—C9172.6 (5)
N7—C7—C8—N858.1 (10)N7—Ni2—N9—C979.4 (5)
N9—C9—C10—N1056.3 (10)C9—C10—N10—Ni242.7 (9)
N15—C15—C16—N1657.9 (10)N12—Ni2—N10—C1077.7 (5)
N17—C17—C18—N1855.5 (10)N8—Ni2—N10—C10169.3 (5)
N1—C1—C2—N259.3 (10)N11—Ni2—N10—C1020 (2)
N5—C5—C6—N655.6 (8)N9—Ni2—N10—C1016.1 (5)
C14—C13—N13—Ni342.4 (6)N7—Ni2—N10—C10109.4 (5)
N18—Ni3—N13—C13171.2 (5)C16—C15—N15—Ni344.0 (8)
N16—Ni3—N13—C1377.6 (5)N18—Ni3—N15—C15109.7 (5)
N15—Ni3—N13—C1327 (2)N13—Ni3—N15—C1535 (2)
N14—Ni3—N13—C1315.1 (5)N16—Ni3—N15—C1516.9 (5)
N17—Ni3—N13—C13106.1 (5)N14—Ni3—N15—C1576.0 (5)
C13—C14—N14—Ni340.2 (7)N17—Ni3—N15—C15167.5 (5)
N18—Ni3—N14—C1435 (2)C15—C16—N16—Ni341.7 (9)
N13—Ni3—N14—C1414.0 (5)N18—Ni3—N16—C1680.1 (6)
N16—Ni3—N14—C14107.0 (5)N13—Ni3—N16—C16173.2 (6)
N15—Ni3—N14—C14171.6 (5)N15—Ni3—N16—C1613.4 (6)
N17—Ni3—N14—C1479.3 (5)N14—Ni3—N16—C16105.0 (6)
C4—C3—N3—Ni139.2 (8)N17—Ni3—N16—C1621 (3)
N5—Ni1—N3—C3104.6 (5)C18—C17—N17—Ni338.3 (8)
N4—Ni1—N3—C312.5 (5)N18—Ni3—N17—C1711.9 (5)
N1—Ni1—N3—C381.3 (5)N13—Ni3—N17—C17104.4 (5)
N2—Ni1—N3—C342 (2)N16—Ni3—N17—C1747 (3)
N6—Ni1—N3—C3173.4 (5)N15—Ni3—N17—C1781.8 (5)
C3—C4—N4—Ni142.3 (9)N14—Ni3—N17—C17173.9 (5)
N5—Ni1—N4—C477.3 (5)C17—C18—N18—Ni343.0 (9)
N1—Ni1—N4—C4108.8 (5)N13—Ni3—N18—C1876.0 (6)
N2—Ni1—N4—C4169.8 (5)N16—Ni3—N18—C18169.6 (6)
N3—Ni1—N4—C416.3 (5)N15—Ni3—N18—C18108.9 (6)
N6—Ni1—N4—C423 (2)N14—Ni3—N18—C1827 (2)
C12—C11—N11—Ni241.3 (7)N17—Ni3—N18—C1817.2 (6)
N12—Ni2—N11—C1114.9 (5)C2—C1—N1—Ni144.4 (9)
N10—Ni2—N11—C1143.7 (19)N5—Ni1—N1—C129 (2)
N8—Ni2—N11—C11105.8 (5)N4—Ni1—N1—C1109.6 (6)
N9—Ni2—N11—C1179.4 (5)N2—Ni1—N1—C116.8 (5)
N7—Ni2—N11—C11172.9 (5)N3—Ni1—N1—C1167.9 (5)
C11—C12—N12—Ni241.4 (7)N6—Ni1—N1—C177.4 (6)
N10—Ni2—N12—C12173.7 (5)C1—C2—N2—Ni142.7 (8)
N8—Ni2—N12—C1279.0 (5)N5—Ni1—N2—C2172.1 (5)
N11—Ni2—N12—C1214.2 (5)N4—Ni1—N2—C279.3 (5)
N9—Ni2—N12—C12103.6 (5)N1—Ni1—N2—C214.4 (5)
N7—Ni2—N12—C1244.2 (18)N3—Ni1—N2—C225 (2)
C8—C7—N7—Ni244.8 (8)N6—Ni1—N2—C2105.8 (5)
N12—Ni2—N7—C717.9 (19)C5—C6—N6—Ni138.2 (7)
N10—Ni2—N7—C7111.6 (5)N5—Ni1—N6—C612.2 (5)
N8—Ni2—N7—C717.4 (5)N4—Ni1—N6—C643 (2)
N11—Ni2—N7—C775.5 (5)N1—Ni1—N6—C6174.7 (5)
N9—Ni2—N7—C7165.7 (5)N2—Ni1—N6—C6103.9 (5)
C7—C8—N8—Ni241.0 (8)N3—Ni1—N6—C681.7 (5)
N12—Ni2—N8—C8171.8 (6)C6—C5—N5—Ni143.1 (7)
N10—Ni2—N8—C878.5 (6)N4—Ni1—N5—C5170.8 (5)
N11—Ni2—N8—C8106.2 (6)N1—Ni1—N5—C532.3 (19)
N9—Ni2—N8—C817 (3)N2—Ni1—N5—C577.3 (5)
N7—Ni2—N8—C813.5 (5)N3—Ni1—N5—C5106.8 (5)
C10—C9—N9—Ni239.5 (8)N6—Ni1—N5—C516.9 (5)
N12—Ni2—N9—C9105.5 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2—H2E···O10.85 (4)1.97 (2)2.815 (9)179 (5)
O2—H2F···Cl20.85 (4)2.45 (2)3.236 (8)155 (3)
O4—H4E···Cl30.85 (4)2.64 (4)3.163 (8)121 (4)
O5—H5E···Cl60.85 (4)2.56 (2)3.231 (9)136 (3)
O5—H5F···O60.85 (4)2.17 (2)2.749 (4)125 (4)
N3—HB3···O20.902.233.086 (5)158
N5—HA5···O20.902.213.064 (4)158
N6—HA6···Cl40.902.653.443 (3)147
N13—HA13···Cl40.902.643.440 (6)149
N13—HB13···Cl60.902.543.401 (5)160
N17—HB17···Cl60.902.503.371 (4)161
 

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