Diaqua­bis[(1R,2R)-(+)–1,2-diphenyl­ethyl­enediamine-κ2N,N′]nickel(II) dichloride–dichloridobis(1,10-phen­anthroline-κ2N,N′)nickel(II) (1/2)

Zhang, Y.-Z.; Chen, Z.-L.; Ng, S.W.

doi:10.1107/S1600536807033296

Buy article online - an online subscription or single-article purchase is required to access this article.

Diaquabis[(1R,2R)-(+)–1,2-diphenylethylenediamine-κ²N,N′]nickel(II) dichloride–dichloridobis(1,10-phenanthroline-κ²N,N′)nickel(II) (1/2)

Y.-Z. Zhang, Z.-L. Chen and S. W. Ng

In the title compound, [Ni(C₁₄H₁₆N₂)₂(H₂O)₂]Cl₂·2[NiCl₂(C₁₂H₈N₂)₂], the dication, whose Ni atom is chelated by a chiral ligand, lies about a pseudo-inversion site. The dication uses its coordinated water molecules to form hydrogen bonds to the chloride counterion as well as to a coordinated Cl atom of the neutral complex. The three Ni atoms exist in octahedral geometries.

Read article Similar articles

Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807033296/xu2291sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807033296/xu2291Isup2.hkl Contains datablock I

CCDC reference: 657566

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.013 Å
R factor = 0.056
wR factor = 0.165
Data-to-parameter ratio = 17.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry .....        100 PerFi
PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem...          n

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT113_ALERT_2_C ADDSYM Suggests Possible Pseudo/New Spacegroup .      P21/c
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.05 Ratio
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.24 Ratio
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C43
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C49
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C22
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C56
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C33
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C41
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C47
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C50
PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ...         13
PLAT420_ALERT_2_C D-H Without Acceptor       N5     -   H5B    ...          ?
PLAT420_ALERT_2_C D-H Without Acceptor       N7     -   H7A    ...          ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          4
PLAT731_ALERT_1_C Bond    Calc   1.338(14), Rep    1.338(5) ......       2.80 su-Ra
              N1   -C9      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.358(11), Rep    1.358(4) ......       2.75 su-Ra
              N1   -C1      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.333(13), Rep    1.332(5) ......       2.60 su-Ra
              N2   -C12     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.365(11), Rep    1.365(4) ......       2.75 su-Ra
              N2   -C6      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.337(12), Rep    1.339(5) ......       2.40 su-Ra
              N3   -C21     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc    1.360(9), Rep    1.360(4) ......       2.25 su-Ra
              N3   -C13     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.338(12), Rep    1.340(5) ......       2.40 su-Ra
              N4   -C24     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.463(11), Rep    1.464(5) ......       2.20 su-Ra
              N7   -C39     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.335(14), Rep    1.334(5) ......       2.80 su-Ra
              N9   -C61     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.364(11), Rep    1.364(4) ......       2.75 su-Ra
              N9   -C53     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.337(15), Rep    1.337(5) ......       3.00 su-Ra
              N10  -C64     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.364(11), Rep    1.364(4) ......       2.75 su-Ra
              N10  -C58     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.343(13), Rep    1.342(5) ......       2.60 su-Ra
              N11  -C73     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.365(10), Rep    1.365(4) ......       2.50 su-Ra
              N11  -C65     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.340(13), Rep    1.340(5) ......       2.60 su-Ra
              N12  -C76     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.391(11), Rep    1.390(5) ......       2.20 su-Ra
              C2   -C7      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.386(11), Rep    1.386(5) ......       2.20 su-Ra
              C5   -C10     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.376(16), Rep    1.376(5) ......       3.20 su-Ra
              C7   -C8      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.387(16), Rep    1.386(5) ......       3.20 su-Ra
              C8   -C9      1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.385(17), Rep    1.384(5) ......       3.40 su-Ra
              C10  -C11     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.395(16), Rep    1.396(5) ......       3.20 su-Ra
              C11  -C12     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.403(11), Rep    1.403(5) ......       2.20 su-Ra
              C14  -C19     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.397(12), Rep    1.397(5) ......       2.40 su-Ra
              C17  -C22     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.385(14), Rep    1.384(5) ......       2.80 su-Ra
              C19  -C20     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.387(13), Rep    1.387(5) ......       2.60 su-Ra
              C20  -C21     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.380(14), Rep    1.380(5) ......       2.80 su-Ra
              C22  -C23     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.393(15), Rep    1.393(5) ......       3.00 su-Ra
              C23  -C24     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc    1.514(9), Rep    1.515(4) ......       2.25 su-Ra
              C25  -C27     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.514(10), Rep    1.514(4) ......       2.50 su-Ra
              C26  -C33     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.390(11), Rep    1.391(5) ......       2.20 su-Ra
              C54  -C59     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.390(11), Rep    1.389(5) ......       2.20 su-Ra
              C57  -C62     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.378(18), Rep    1.377(5) ......       3.60 su-Ra
              C59  -C60     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.388(17), Rep    1.388(5) ......       3.40 su-Ra
              C60  -C61     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.381(16), Rep    1.381(5) ......       3.20 su-Ra
              C62  -C63     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.395(17), Rep    1.395(5) ......       3.40 su-Ra
              C63  -C64     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.397(12), Rep    1.395(5) ......       2.40 su-Ra
              C66  -C71     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.398(12), Rep    1.398(5) ......       2.40 su-Ra
              C69  -C74     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.378(15), Rep    1.379(5) ......       3.00 su-Ra
              C71  -C72     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.386(14), Rep    1.387(5) ......       2.80 su-Ra
              C72  -C73     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.377(14), Rep    1.377(5) ......       2.80 su-Ra
              C74  -C75     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc   1.392(16), Rep    1.393(5) ......       3.20 su-Ra
              C75  -C76     1.555   1.555

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           27.50
           From the CIF: _reflns_number_total              14184
           Count of symmetry unique reflns         8518
           Completeness (_total/calc)            166.52%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      5666
           Fraction of Friedel pairs measured     0.665
           Are heavy atom types Z>Si present        yes
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C25    = .          R
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C26    = .          R
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C39    = .          R
PLAT791_ALERT_1_G Confirm the Absolute Configuration of C40    = .          R
PLAT794_ALERT_5_G Check Predicted Bond Valency for Ni1         (2)       2.05
PLAT794_ALERT_5_G Check Predicted Bond Valency for Ni3         (2)       2.11
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......        590

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
  57 ALERT level C = Check and explain
  10 ALERT level G = General alerts; check

  48 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  14 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

Comment top

1,2-Diphenylethylenediamine, which can exist in the meso and the optically active R,R and S,S forms, behaves like ethylenediamine in a number of metal complexes; several nickel(II) complexes have been characterized by crystallography. These have the ligand functioning in the expected chelating mode, as noted in the nitrite/perchlorate, nitrite/chloride (Finney et al., 1981), dichloride (García-Granda & Gómez-Beltrán, 1984; Murmann & Barnes, 2004) and acetate (García-Granda et al., 1990) derivatives. The dichloride complexes are ionic and there is no direct interaction between the four-coordinate cation and the halide.

The attempt to synthesize a similar, mixed-ligand complex, by adding a molar equivalent of 1,10-phenanthroline yielded a cocrystal of dichlorobis(phenanthroline)nickel and diaquabis(diphenylethylenediamine)nickel dichloride (Fig. 1). The trinuclear compound lies on a false inversion site. The nickel atom of the diaquabis(diphenylethylenediamine)nickel cation lies on this site, which also relates the two neutral dichlorobis(phenanthroline)nickel to each other. The cation uses its water molecules to form hydrogen bonds to the free chlorine anion as well as to the chlorine atom of the neutral molecule. The three nickel atoms exist in octahedral geometries.

Related literature top

For the nickel complexes of meso-, R,R- and S,S -1,2-diphenylethylenediamine, see: Finney et al. (1981); García-Granda & Gómez-Beltrán (1984); García-Granda et al. (1990); Murmann & Barnes (2004).

Experimental top

Nickel chloride hexahydrate (0.237 g, 1 mmol), (1R,2R)-(+)–1,2-diphenylethylenediamine (0.212 g, 1 mmol) and 1,10-phenanthroline (0.198 g, 1 mmol) were placed in a 23-ml, Teflon-lined, Parr bomb along with ethanol (12 ml). The bomb was heated at 413 K for 72 h, and then cooled over 24 h. Green crystals were isolated in 40% yield.

Structure description top

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

Figures top

Fig. 1. Thermal ellipsoid plot of the cocrystal. Displacement ellipsoids are drawn at the 50% probability level, and H atoms as spheres of arbitrary radii. The dashed lines denote the intermolecular hydrogen bonds.

Diaquabis[(1R,2R)-(+)–1,2-diphenylethylenediamine- κ²N,N']nickel(II) dichloride–dichloridobis(1,10-phenanthroline- κ²N,N')nickel(II) (1/2) top

Crystal data top

[Ni(C₁₄H₁₆N₂)₂(H₂O)₂]Cl₂·2[NiCl₂(C₁₂H₈N₂)₂]	F(000) = 1620
M_r = 1570.25	D_x = 1.461 Mg m⁻³
Monoclinic, P2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2yb	Cell parameters from 3615 reflections
a = 12.390 (2) Å	θ = 2.3–24.4°
b = 13.819 (2) Å	µ = 1.06 mm⁻¹
c = 21.261 (3) Å	T = 293 K
β = 101.348 (2)°	Block, green
V = 3569.1 (9) Å³	0.48 × 0.23 × 0.18 mm
Z = 2

Data collection top

Bruker APEX area-detector diffractometer	14184 independent reflections
Radiation source: fine-focus sealed tube	7201 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.046
φ and ω scans	θ_max = 27.5°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −16→14
T_min = 0.629, T_max = 0.832	k = −15→17
22161 measured reflections	l = −27→27

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.056	H-atom parameters constrained
wR(F²) = 0.165	w = 1/[σ²(F_o²) + (0.0657P)²] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.002
14184 reflections	Δρ_max = 0.73 e Å⁻³
796 parameters	Δρ_min = −0.50 e Å⁻³
590 restraints	Absolute structure: Flack (1983), 5767 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.07 (3)

Crystal data top

[Ni(C₁₄H₁₆N₂)₂(H₂O)₂]Cl₂·2[NiCl₂(C₁₂H₈N₂)₂]	V = 3569.1 (9) Å³
M_r = 1570.25	Z = 2
Monoclinic, P2₁	Mo Kα radiation
a = 12.390 (2) Å	µ = 1.06 mm⁻¹
b = 13.819 (2) Å	T = 293 K
c = 21.261 (3) Å	0.48 × 0.23 × 0.18 mm
β = 101.348 (2)°

Data collection top

Bruker APEX area-detector diffractometer	14184 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	7201 reflections with I > 2σ(I)
T_min = 0.629, T_max = 0.832	R_int = 0.046
22161 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.056	H-atom parameters constrained
wR(F²) = 0.165	Δρ_max = 0.73 e Å⁻³
S = 1.02	Δρ_min = −0.50 e Å⁻³
14184 reflections	Absolute structure: Flack (1983), 5767 Friedel pairs
796 parameters	Absolute structure parameter: −0.07 (3)
590 restraints

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Ni1	0.29514 (10)	0.5000 (1)	0.49741 (6)	0.0299 (4)
Ni2	0.25490 (14)	0.5183 (2)	0.75226 (8)	0.0338 (2)
Ni3	0.20348 (10)	0.53816 (7)	1.00447 (6)	0.0316 (4)
Cl1	0.2252 (2)	0.6289 (3)	0.55598 (13)	0.0430 (8)
Cl2	0.4373 (2)	0.4691 (3)	0.58756 (13)	0.0421 (9)
Cl3	0.2784 (3)	0.4096 (3)	0.94865 (13)	0.0456 (9)
Cl4	0.0615 (2)	0.5664 (3)	0.91330 (13)	0.0424 (9)
Cl5	0.2419 (3)	0.2174 (3)	0.73513 (16)	0.0572 (11)
Cl6	0.2600 (3)	0.8237 (3)	0.76323 (16)	0.0553 (10)
O1W	0.1792 (6)	0.4053 (7)	0.7986 (3)	0.044 (2)
H1W1	0.1761	0.4221	0.8352	0.065*
H1W2	0.2159	0.3556	0.8000	0.065*
O2W	0.3293 (6)	0.6312 (7)	0.7052 (3)	0.044 (2)
H2W1	0.3028	0.6307	0.6667	0.066*
H2W2	0.3175	0.6838	0.7204	0.066*
N1	0.3601 (6)	0.3954 (7)	0.4420 (4)	0.038 (3)
N2	0.3986 (6)	0.5863 (6)	0.4543 (4)	0.034 (3)
N3	0.1607 (5)	0.5282 (6)	0.4219 (3)	0.030 (2)
N4	0.1767 (5)	0.4016 (7)	0.5181 (3)	0.032 (2)
N5	0.1297 (5)	0.4921 (7)	0.6732 (4)	0.035 (2)
H5A	0.1451	0.5194	0.6397	0.042*
H5B	0.1230	0.4310	0.6661	0.042*
N6	0.1413 (6)	0.6165 (7)	0.7728 (3)	0.035 (2)
H6A	0.1134	0.5957	0.8042	0.042*
H6B	0.1731	0.6710	0.7838	0.042*
N7	0.3814 (6)	0.5373 (7)	0.8346 (4)	0.042 (2)
H7A	0.4106	0.5936	0.8335	0.051*
H7B	0.3539	0.5339	0.8686	0.051*
N8	0.3740 (5)	0.4240 (7)	0.7278 (4)	0.035 (2)
H8A	0.3543	0.3650	0.7320	0.042*
H8B	0.3785	0.4329	0.6884	0.042*
N9	0.1349 (6)	0.6434 (7)	1.0580 (4)	0.038 (3)
N10	0.1035 (7)	0.4532 (7)	1.0484 (4)	0.039 (3)
N11	0.3398 (5)	0.5123 (7)	1.0794 (4)	0.034 (2)
N12	0.3175 (5)	0.6347 (7)	0.9814 (3)	0.033 (2)
C1	0.4366 (5)	0.4348 (6)	0.4119 (3)	0.037 (3)
C2	0.4929 (7)	0.3789 (5)	0.3745 (4)	0.056 (4)
C3	0.5649 (6)	0.4225 (8)	0.3406 (3)	0.076 (5)
H3	0.6025	0.3851	0.3156	0.092*
C4	0.5806 (5)	0.5221 (8)	0.3441 (3)	0.070 (4)
H4	0.6288	0.5513	0.3214	0.084*
C5	0.5244 (7)	0.5780 (5)	0.3814 (4)	0.054 (4)
C6	0.4524 (5)	0.5344 (6)	0.4153 (3)	0.040 (3)
C7	0.4764 (10)	0.2793 (6)	0.3723 (6)	0.072 (5)
H7	0.5165	0.2402	0.3496	0.086*
C8	0.4004 (9)	0.2388 (9)	0.4037 (5)	0.066 (4)
H8	0.3877	0.1725	0.4025	0.079*
C9	0.3432 (10)	0.2998 (7)	0.4373 (5)	0.054 (4)
H9	0.2904	0.2729	0.4576	0.065*
C10	0.5338 (10)	0.6777 (6)	0.3872 (6)	0.070 (4)
H10	0.5800	0.7101	0.3647	0.084*
C11	0.4768 (9)	0.7308 (10)	0.4253 (5)	0.071 (5)
H11	0.4836	0.7978	0.4277	0.086*
C12	0.4090 (9)	0.6821 (7)	0.4600 (5)	0.049 (3)
H12	0.3716	0.7160	0.4869	0.059*
C13	0.0692 (5)	0.4766 (5)	0.4267 (3)	0.031 (3)
C14	−0.0298 (6)	0.4863 (5)	0.3832 (3)	0.034 (3)
C15	−0.1196 (4)	0.4293 (7)	0.3894 (3)	0.055 (4)
H15	−0.1858	0.4358	0.3602	0.066*
C16	−0.1104 (5)	0.3626 (6)	0.4390 (4)	0.048 (3)
H16	−0.1704	0.3244	0.4432	0.057*
C17	−0.0114 (6)	0.3529 (5)	0.4826 (3)	0.041 (3)
C18	0.0784 (4)	0.4099 (6)	0.4764 (3)	0.033 (3)
C19	−0.0362 (8)	0.5558 (7)	0.3345 (4)	0.046 (3)
H19	−0.1014	0.5652	0.3049	0.055*
C20	0.0565 (7)	0.6102 (9)	0.3315 (5)	0.049 (4)
H20	0.0538	0.6570	0.2998	0.059*
C21	0.1533 (8)	0.5951 (8)	0.3758 (4)	0.045 (3)
H21	0.2148	0.6324	0.3732	0.054*
C22	0.0032 (9)	0.2872 (8)	0.5335 (4)	0.061 (4)
H22	−0.0558	0.2487	0.5389	0.073*
C23	0.1023 (7)	0.2777 (9)	0.5760 (5)	0.046 (3)
H23	0.1114	0.2333	0.6095	0.055*
C24	0.1879 (8)	0.3376 (8)	0.5662 (4)	0.040 (3)
H24	0.2555	0.3330	0.5943	0.048*
C25	0.0271 (5)	0.5315 (5)	0.6866 (3)	0.042 (2)
H25	0.0064	0.4906	0.7200	0.051*
C26	0.0539 (5)	0.6301 (5)	0.7160 (3)	0.041 (2)
H26	0.0874	0.6664	0.6852	0.049*
C27	−0.0695 (5)	0.5310 (6)	0.6305 (3)	0.042 (3)
C28	−0.1636 (6)	0.4801 (6)	0.6368 (3)	0.068 (3)
H28	−0.1660	0.4473	0.6747	0.082*
C29	−0.2541 (5)	0.4781 (6)	0.5864 (4)	0.072 (3)
H29	−0.3170	0.4440	0.5906	0.086*
C30	−0.2505 (5)	0.5271 (7)	0.5297 (3)	0.067 (3)
H30	−0.3110	0.5258	0.4960	0.081*
C31	−0.1564 (6)	0.5780 (6)	0.5235 (3)	0.064 (3)
H31	−0.1540	0.6108	0.4856	0.077*
C32	−0.0659 (5)	0.5800 (6)	0.5739 (3)	0.056 (3)
H32	−0.0030	0.6140	0.5697	0.067*
C33	−0.0425 (5)	0.6905 (6)	0.7272 (4)	0.037 (3)
C34	−0.1180 (6)	0.6580 (5)	0.7629 (3)	0.062 (3)
H34	−0.1112	0.5962	0.7806	0.074*
C35	−0.2038 (5)	0.7177 (7)	0.7721 (3)	0.072 (3)
H35	−0.2544	0.6959	0.7959	0.086*
C36	−0.2141 (6)	0.8101 (6)	0.7456 (4)	0.074 (4)
H36	−0.2715	0.8500	0.7518	0.089*
C37	−0.1386 (7)	0.8426 (5)	0.7100 (4)	0.062 (3)
H37	−0.1455	0.9044	0.6923	0.075*
C38	−0.0528 (5)	0.7829 (6)	0.7008 (3)	0.062 (3)
H38	−0.0023	0.8047	0.6769	0.074*
C39	0.4657 (5)	0.4626 (6)	0.8365 (3)	0.040 (2)
H39	0.4373	0.4035	0.8529	0.048*
C40	0.4817 (5)	0.4411 (6)	0.7691 (3)	0.042 (2)
H40	0.5130	0.4990	0.7531	0.050*
C41	0.5703 (5)	0.4891 (6)	0.8827 (3)	0.046 (3)
C42	0.6388 (7)	0.5615 (6)	0.8674 (3)	0.091 (4)
H42	0.6197	0.5946	0.8288	0.109*
C43	0.7357 (6)	0.5843 (6)	0.9100 (4)	0.113 (5)
H43	0.7815	0.6327	0.8998	0.136*
C44	0.7641 (5)	0.5349 (7)	0.9678 (4)	0.079 (4)
H44	0.8290	0.5502	0.9963	0.095*
C45	0.6957 (6)	0.4625 (6)	0.9831 (3)	0.073 (4)
H45	0.7147	0.4294	1.0217	0.087*
C46	0.5988 (6)	0.4396 (5)	0.9405 (3)	0.056 (3)
H46	0.5530	0.3912	0.9507	0.067*
C47	0.5609 (5)	0.3586 (5)	0.7668 (4)	0.041 (3)
C48	0.6560 (6)	0.3785 (5)	0.7438 (4)	0.079 (4)
H48	0.6689	0.4409	0.7305	0.095*
C49	0.7318 (5)	0.3054 (7)	0.7407 (4)	0.098 (5)
H49	0.7955	0.3188	0.7253	0.117*
C50	0.7125 (6)	0.2123 (6)	0.7606 (4)	0.064 (3)
H50	0.7632	0.1634	0.7585	0.077*
C51	0.6174 (7)	0.1923 (5)	0.7836 (3)	0.064 (4)
H51	0.6045	0.1300	0.7969	0.077*
C52	0.5416 (5)	0.2654 (6)	0.7867 (3)	0.055 (3)
H52	0.4779	0.2520	0.8021	0.066*
C53	0.0607 (5)	0.6031 (6)	1.0899 (3)	0.041 (3)
C54	0.0013 (7)	0.6585 (5)	1.1258 (4)	0.056 (4)
C55	−0.0704 (6)	0.6138 (7)	1.1595 (3)	0.066 (4)
H55	−0.1101	0.6508	1.1836	0.079*
C56	−0.0827 (5)	0.5138 (8)	1.1572 (3)	0.076 (4)
H56	−0.1307	0.4839	1.1797	0.091*
C57	−0.0233 (7)	0.4585 (5)	1.1212 (4)	0.054 (4)
C58	0.0484 (5)	0.5031 (6)	1.0876 (3)	0.041 (3)
C59	0.0182 (10)	0.7580 (6)	1.1268 (6)	0.076 (5)
H59	−0.0218	0.7974	1.1493	0.091*
C60	0.0933 (10)	0.7992 (10)	1.0949 (6)	0.077 (5)
H60	0.1048	0.8657	1.0959	0.092*
C61	0.1513 (10)	0.7389 (7)	1.0612 (5)	0.054 (4)
H61	0.2033	0.7658	1.0403	0.065*
C62	−0.0342 (10)	0.3584 (6)	1.1188 (6)	0.070 (4)
H62	−0.0775	0.3266	1.1434	0.083*
C63	0.0209 (9)	0.3075 (9)	1.0789 (5)	0.062 (4)
H63	0.0136	0.2407	1.0753	0.075*
C64	0.0877 (10)	0.3575 (8)	1.0442 (6)	0.056 (4)
H64	0.1230	0.3224	1.0169	0.067*
C65	0.4298 (5)	0.5649 (5)	1.0721 (3)	0.032 (3)
C66	0.5300 (6)	0.5571 (5)	1.1147 (3)	0.044 (3)
C67	0.6183 (4)	0.6146 (7)	1.1068 (3)	0.049 (3)
H67	0.6854	0.6094	1.1354	0.059*
C68	0.6065 (5)	0.6800 (6)	1.0563 (4)	0.059 (4)
H68	0.6656	0.7186	1.0510	0.071*
C69	0.5063 (6)	0.6879 (6)	1.0136 (3)	0.039 (3)
C70	0.4180 (4)	0.6303 (6)	1.0215 (3)	0.031 (3)
C71	0.5383 (9)	0.4863 (7)	1.1623 (5)	0.057 (4)
H71	0.6055	0.4764	1.1899	0.069*
C72	0.4489 (7)	0.4308 (9)	1.1691 (5)	0.053 (4)
H72	0.4548	0.3836	1.2008	0.064*
C73	0.3498 (8)	0.4475 (8)	1.1273 (4)	0.042 (3)
H73	0.2880	0.4126	1.1325	0.050*
C74	0.4920 (8)	0.7537 (8)	0.9627 (4)	0.042 (3)
H74	0.5492	0.7938	0.9565	0.050*
C75	0.3907 (8)	0.7573 (10)	0.9221 (5)	0.056 (4)
H75	0.3798	0.7985	0.8868	0.067*
C76	0.3046 (9)	0.6995 (8)	0.9336 (5)	0.044 (3)
H76	0.2356	0.7061	0.9072	0.053*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0295 (7)	0.0305 (11)	0.0294 (7)	−0.0009 (7)	0.0051 (6)	0.0016 (8)
Ni2	0.0321 (5)	0.0401 (5)	0.0297 (4)	−0.0037 (4)	0.0073 (3)	−0.0004 (4)
Ni3	0.0335 (8)	0.0357 (12)	0.0258 (7)	0.0005 (7)	0.0063 (6)	0.0007 (8)
Cl1	0.0495 (18)	0.039 (2)	0.0415 (17)	0.0118 (15)	0.0121 (14)	−0.0011 (16)
Cl2	0.0401 (17)	0.046 (2)	0.0370 (16)	0.0067 (15)	0.0005 (13)	0.0036 (16)
Cl3	0.057 (2)	0.045 (2)	0.0348 (17)	0.0134 (17)	0.0100 (14)	−0.0015 (16)
Cl4	0.0397 (17)	0.050 (3)	0.0343 (16)	0.0065 (15)	0.0002 (13)	0.0008 (16)
Cl5	0.061 (2)	0.059 (3)	0.0510 (18)	−0.0211 (19)	0.0089 (16)	−0.007 (2)
Cl6	0.070 (2)	0.043 (3)	0.0504 (18)	−0.0181 (19)	0.0063 (17)	−0.0025 (19)
O1W	0.045 (4)	0.053 (5)	0.036 (4)	−0.004 (4)	0.015 (3)	0.008 (4)
O2W	0.054 (4)	0.040 (5)	0.041 (4)	−0.004 (4)	0.015 (4)	0.000 (4)
N1	0.042 (5)	0.042 (6)	0.030 (5)	0.000 (4)	0.006 (4)	−0.005 (4)
N2	0.032 (4)	0.042 (6)	0.029 (4)	−0.010 (4)	0.003 (4)	0.007 (4)
N3	0.038 (4)	0.026 (5)	0.027 (4)	−0.004 (4)	0.005 (3)	0.002 (4)
N4	0.038 (5)	0.030 (5)	0.031 (5)	−0.006 (4)	0.010 (4)	−0.002 (4)
N5	0.028 (4)	0.035 (5)	0.043 (4)	0.003 (3)	0.007 (3)	−0.002 (4)
N6	0.032 (4)	0.043 (5)	0.029 (4)	−0.008 (4)	0.004 (3)	−0.006 (4)
N7	0.040 (4)	0.052 (6)	0.038 (4)	−0.004 (4)	0.012 (3)	−0.006 (4)
N8	0.033 (4)	0.042 (5)	0.033 (4)	0.001 (4)	0.012 (4)	0.004 (4)
N9	0.042 (5)	0.039 (6)	0.033 (5)	0.006 (4)	0.004 (4)	0.002 (4)
N10	0.033 (5)	0.044 (6)	0.037 (5)	−0.001 (4)	0.006 (4)	0.002 (5)
N11	0.038 (4)	0.038 (6)	0.025 (4)	0.005 (5)	0.004 (3)	0.003 (5)
N12	0.038 (5)	0.036 (6)	0.023 (4)	0.002 (4)	0.002 (4)	0.002 (4)
C1	0.027 (5)	0.050 (7)	0.033 (5)	0.008 (5)	0.004 (4)	−0.002 (5)
C2	0.046 (6)	0.079 (8)	0.040 (6)	0.007 (6)	0.004 (5)	−0.005 (6)
C3	0.053 (7)	0.125 (9)	0.052 (7)	0.016 (7)	0.013 (6)	−0.014 (7)
C4	0.042 (6)	0.132 (9)	0.043 (6)	−0.008 (7)	0.022 (5)	0.013 (7)
C5	0.034 (5)	0.085 (8)	0.039 (6)	−0.008 (6)	−0.005 (5)	0.002 (6)
C6	0.031 (5)	0.065 (7)	0.026 (5)	0.001 (5)	0.009 (4)	0.005 (5)
C7	0.072 (7)	0.090 (9)	0.049 (6)	0.028 (6)	0.004 (6)	−0.022 (6)
C8	0.082 (7)	0.053 (7)	0.058 (7)	0.022 (6)	0.005 (6)	−0.013 (6)
C9	0.063 (6)	0.052 (8)	0.045 (6)	0.003 (6)	0.006 (5)	−0.004 (6)
C10	0.056 (7)	0.108 (9)	0.044 (6)	−0.026 (6)	0.004 (5)	0.021 (6)
C11	0.073 (7)	0.062 (8)	0.070 (7)	−0.027 (6)	−0.007 (6)	0.025 (6)
C12	0.048 (6)	0.041 (7)	0.053 (6)	−0.019 (5)	−0.004 (5)	0.005 (5)
C13	0.032 (5)	0.030 (6)	0.030 (5)	−0.003 (4)	0.006 (4)	−0.004 (5)
C14	0.029 (5)	0.036 (6)	0.034 (5)	0.000 (4)	−0.002 (4)	−0.004 (5)
C15	0.042 (6)	0.064 (7)	0.055 (6)	0.002 (6)	0.000 (5)	−0.014 (6)
C16	0.032 (5)	0.047 (7)	0.060 (6)	−0.014 (5)	0.002 (5)	−0.008 (5)
C17	0.042 (6)	0.040 (7)	0.044 (6)	−0.011 (5)	0.013 (5)	−0.002 (5)
C18	0.029 (5)	0.035 (6)	0.034 (5)	−0.007 (5)	0.009 (4)	−0.009 (5)
C19	0.046 (6)	0.056 (7)	0.029 (5)	0.007 (5)	−0.010 (4)	0.002 (5)
C20	0.053 (6)	0.047 (7)	0.044 (6)	0.006 (5)	−0.001 (5)	0.017 (6)
C21	0.053 (6)	0.049 (7)	0.033 (5)	0.005 (5)	0.009 (5)	0.005 (5)
C22	0.058 (6)	0.060 (8)	0.069 (7)	−0.031 (6)	0.025 (6)	−0.017 (6)
C23	0.068 (6)	0.038 (6)	0.036 (5)	−0.010 (5)	0.019 (5)	0.005 (5)
C24	0.045 (5)	0.044 (7)	0.029 (5)	0.010 (5)	0.003 (4)	0.000 (5)
C25	0.036 (4)	0.050 (5)	0.037 (4)	−0.002 (4)	−0.001 (3)	−0.002 (4)
C26	0.034 (4)	0.051 (5)	0.034 (4)	0.003 (4)	−0.002 (4)	0.002 (4)
C27	0.036 (5)	0.059 (6)	0.030 (4)	−0.003 (4)	0.003 (4)	−0.008 (4)
C28	0.056 (6)	0.091 (8)	0.050 (6)	−0.022 (5)	−0.009 (5)	0.008 (5)
C29	0.046 (5)	0.089 (7)	0.072 (6)	−0.029 (5)	−0.012 (5)	0.008 (6)
C30	0.055 (6)	0.085 (7)	0.051 (6)	0.000 (5)	−0.016 (5)	0.002 (5)
C31	0.063 (6)	0.067 (7)	0.057 (6)	0.004 (5)	0.000 (5)	0.008 (5)
C32	0.050 (5)	0.057 (6)	0.053 (6)	−0.009 (5)	−0.005 (5)	−0.007 (5)
C33	0.028 (4)	0.052 (6)	0.030 (4)	0.003 (4)	0.004 (4)	−0.001 (4)
C34	0.059 (6)	0.057 (6)	0.071 (6)	−0.002 (5)	0.016 (5)	0.018 (5)
C35	0.050 (5)	0.094 (8)	0.076 (6)	−0.008 (5)	0.024 (5)	0.015 (6)
C36	0.065 (7)	0.089 (8)	0.069 (7)	0.030 (6)	0.013 (6)	−0.006 (6)
C37	0.063 (6)	0.053 (7)	0.075 (7)	0.006 (5)	0.021 (5)	0.017 (6)
C38	0.057 (6)	0.060 (7)	0.073 (6)	0.015 (5)	0.023 (5)	0.010 (5)
C39	0.039 (4)	0.043 (5)	0.035 (4)	0.003 (4)	−0.001 (4)	−0.002 (4)
C40	0.031 (4)	0.053 (5)	0.039 (5)	0.000 (4)	0.004 (4)	−0.002 (4)
C41	0.041 (5)	0.060 (6)	0.034 (5)	−0.002 (4)	0.004 (4)	−0.003 (5)
C42	0.088 (7)	0.121 (9)	0.057 (6)	−0.057 (6)	−0.004 (5)	0.024 (6)
C43	0.100 (8)	0.141 (10)	0.093 (8)	−0.056 (7)	0.005 (7)	0.014 (7)
C44	0.056 (6)	0.098 (8)	0.070 (7)	−0.006 (6)	−0.020 (5)	−0.013 (6)
C45	0.077 (7)	0.067 (7)	0.065 (6)	0.003 (5)	−0.008 (5)	−0.004 (5)
C46	0.051 (5)	0.067 (6)	0.045 (5)	−0.009 (5)	−0.003 (4)	−0.001 (5)
C47	0.032 (5)	0.056 (6)	0.031 (5)	−0.006 (4)	0.000 (4)	0.000 (4)
C48	0.070 (6)	0.070 (7)	0.108 (8)	0.013 (5)	0.042 (6)	0.033 (6)
C49	0.090 (7)	0.097 (8)	0.120 (8)	0.017 (6)	0.055 (7)	0.032 (7)
C50	0.049 (6)	0.077 (7)	0.069 (6)	0.022 (5)	0.018 (5)	0.018 (6)
C51	0.075 (6)	0.059 (7)	0.060 (6)	0.016 (5)	0.017 (5)	0.010 (6)
C52	0.063 (6)	0.056 (7)	0.055 (5)	0.006 (5)	0.032 (5)	0.003 (5)
C53	0.034 (5)	0.068 (8)	0.021 (5)	0.007 (5)	0.002 (4)	0.000 (5)
C54	0.044 (6)	0.084 (8)	0.040 (6)	0.020 (6)	0.010 (5)	−0.008 (6)
C55	0.038 (6)	0.120 (9)	0.046 (6)	0.014 (6)	0.021 (5)	−0.011 (6)
C56	0.048 (6)	0.133 (9)	0.046 (6)	−0.009 (7)	0.010 (5)	0.004 (7)
C57	0.040 (6)	0.086 (8)	0.038 (6)	−0.013 (6)	0.013 (5)	0.012 (6)
C58	0.031 (5)	0.058 (7)	0.033 (5)	−0.001 (5)	0.001 (4)	0.005 (5)
C59	0.067 (7)	0.097 (9)	0.063 (7)	0.035 (7)	0.010 (6)	−0.021 (7)
C60	0.096 (8)	0.065 (8)	0.070 (7)	0.017 (7)	0.015 (6)	−0.014 (7)
C61	0.070 (7)	0.047 (7)	0.046 (6)	0.007 (6)	0.011 (5)	−0.012 (6)
C62	0.051 (6)	0.093 (8)	0.059 (7)	−0.034 (6)	−0.002 (5)	0.021 (6)
C63	0.063 (7)	0.052 (7)	0.065 (7)	−0.024 (6)	−0.004 (6)	0.012 (6)
C64	0.058 (7)	0.059 (8)	0.048 (6)	−0.009 (6)	0.006 (5)	−0.001 (6)
C65	0.028 (5)	0.034 (6)	0.035 (5)	0.006 (4)	0.007 (4)	−0.008 (5)
C66	0.044 (6)	0.041 (7)	0.046 (6)	0.007 (5)	0.002 (5)	−0.013 (5)
C67	0.027 (5)	0.050 (7)	0.065 (6)	0.004 (5)	−0.003 (5)	−0.007 (6)
C68	0.050 (6)	0.058 (7)	0.074 (7)	−0.011 (6)	0.021 (6)	−0.009 (6)
C69	0.034 (5)	0.044 (7)	0.040 (5)	−0.002 (5)	0.005 (4)	−0.003 (5)
C70	0.035 (5)	0.028 (6)	0.028 (5)	0.005 (5)	0.001 (4)	0.001 (5)
C71	0.050 (6)	0.064 (8)	0.055 (6)	0.016 (6)	0.003 (5)	−0.011 (6)
C72	0.064 (7)	0.051 (7)	0.039 (6)	0.013 (6)	−0.002 (5)	0.013 (6)
C73	0.046 (6)	0.039 (6)	0.039 (5)	0.001 (5)	0.003 (5)	0.005 (5)
C74	0.048 (6)	0.037 (6)	0.042 (5)	−0.012 (5)	0.011 (5)	0.008 (5)
C75	0.078 (7)	0.042 (7)	0.049 (6)	−0.012 (6)	0.011 (6)	0.006 (6)
C76	0.050 (6)	0.039 (7)	0.042 (6)	−0.011 (5)	0.007 (5)	0.003 (5)

Geometric parameters (Å, º) top

Ni1—N2	2.090 (9)	C25—H25	0.9800
Ni1—N4	2.109 (8)	C26—C33	1.514 (4)
Ni1—N3	2.109 (7)	C26—H26	0.9800
Ni1—N1	2.120 (10)	C27—C28	1.3900
Ni1—Cl2	2.372 (3)	C27—C32	1.3900
Ni1—Cl1	2.429 (3)	C28—C29	1.3900
Ni2—N6	2.064 (9)	C28—H28	0.9300
Ni2—N5	2.082 (8)	C29—C30	1.3900
Ni2—N8	2.108 (9)	C29—H29	0.9300
Ni2—N7	2.123 (8)	C30—C31	1.3900
Ni2—O1W	2.157 (8)	C30—H30	0.9300
Ni2—O2W	2.156 (8)	C31—C32	1.3900
Ni3—N10	2.059 (10)	C31—H31	0.9300
Ni3—N12	2.071 (9)	C32—H32	0.9300
Ni3—N11	2.112 (7)	C33—C34	1.3900
Ni3—N9	2.125 (10)	C33—C38	1.3900
Ni3—Cl4	2.380 (3)	C34—C35	1.3900
Ni3—Cl3	2.421 (4)	C34—H34	0.9300
O1W—H1W1	0.8200	C35—C36	1.3900
O1W—H1W2	0.8200	C35—H35	0.9300
O2W—H2W1	0.8200	C36—C37	1.3900
O2W—H2W2	0.8200	C36—H36	0.9300
N1—C9	1.338 (5)	C37—C38	1.3900
N1—C1	1.358 (4)	C37—H37	0.9300
N2—C12	1.332 (5)	C38—H38	0.9300
N2—C6	1.365 (4)	C39—C41	1.509 (5)
N3—C21	1.339 (5)	C39—C40	1.515 (5)
N3—C13	1.360 (4)	C39—H39	0.9800
N4—C24	1.340 (5)	C40—C47	1.511 (5)
N4—C18	1.362 (4)	C40—H40	0.9800
N5—C25	1.462 (5)	C41—C42	1.3900
N5—H5A	0.8600	C41—C46	1.3900
N5—H5B	0.8600	C42—C43	1.3900
N6—C26	1.466 (5)	C42—H42	0.9300
N6—H6A	0.8600	C43—C44	1.3900
N6—H6B	0.8600	C43—H43	0.9300
N7—C39	1.464 (5)	C44—C45	1.3900
N7—H7A	0.8600	C44—H44	0.9300
N7—H7B	0.8600	C45—C46	1.3900
N8—C40	1.464 (5)	C45—H45	0.9300
N8—H8A	0.8600	C46—H46	0.9300
N8—H8B	0.8600	C47—C48	1.3900
N9—C61	1.334 (5)	C47—C52	1.3900
N9—C53	1.364 (4)	C48—C49	1.3900
N10—C64	1.337 (5)	C48—H48	0.9300
N10—C58	1.364 (4)	C49—C50	1.3900
N11—C73	1.342 (5)	C49—H49	0.9300
N11—C65	1.365 (4)	C50—C51	1.3900
N12—C76	1.340 (5)	C50—H50	0.9300
N12—C70	1.365 (4)	C51—C52	1.3900
C1—C2	1.3900	C51—H51	0.9300
C1—C6	1.3900	C52—H52	0.9300
C2—C7	1.390 (5)	C53—C54	1.3900
C2—C3	1.3900	C53—C58	1.3900
C3—C4	1.3900	C54—C55	1.3900
C3—H3	0.9300	C54—C59	1.391 (5)
C4—C5	1.3900	C55—C56	1.3900
C4—H4	0.9300	C55—H55	0.9300
C5—C10	1.386 (5)	C56—C57	1.3900
C5—C6	1.3900	C56—H56	0.9300
C7—C8	1.376 (5)	C57—C62	1.389 (5)
C7—H7	0.9300	C57—C58	1.3900
C8—C9	1.386 (5)	C59—C60	1.377 (5)
C8—H8	0.9300	C59—H59	0.9300
C9—H9	0.9300	C60—C61	1.388 (5)
C10—C11	1.384 (5)	C60—H60	0.9300
C10—H10	0.9300	C61—H61	0.9300
C11—C12	1.396 (5)	C62—C63	1.381 (5)
C11—H11	0.9300	C62—H62	0.9300
C12—H12	0.9300	C63—C64	1.395 (5)
C13—C14	1.3900	C63—H63	0.9300
C13—C18	1.3900	C64—H64	0.9300
C14—C15	1.3900	C65—C66	1.3900
C14—C19	1.403 (5)	C65—C70	1.3900
C15—C16	1.3900	C66—C67	1.3900
C15—H15	0.9300	C66—C71	1.395 (5)
C16—C17	1.3900	C67—C68	1.3900
C16—H16	0.9300	C67—H67	0.9300
C17—C18	1.3900	C68—C69	1.3900
C17—C22	1.397 (5)	C68—H68	0.9300
C19—C20	1.384 (5)	C69—C70	1.3900
C19—H19	0.9300	C69—C74	1.398 (5)
C20—C21	1.387 (5)	C71—C72	1.379 (5)
C20—H20	0.9300	C71—H71	0.9300
C21—H21	0.9300	C72—C73	1.387 (5)
C22—C23	1.380 (5)	C72—H72	0.9300
C22—H22	0.9300	C73—H73	0.9300
C23—C24	1.393 (5)	C74—C75	1.377 (5)
C23—H23	0.9300	C74—H74	0.9300
C24—H24	0.9300	C75—C76	1.393 (5)
C25—C26	1.508 (5)	C75—H75	0.9300
C25—C27	1.515 (4)	C76—H76	0.9300

N2—Ni1—N4	166.2 (3)	C23—C24—H24	118.7
N2—Ni1—N3	91.2 (3)	N5—C25—C26	106.7 (6)
N4—Ni1—N3	78.4 (3)	N5—C25—C27	115.3 (6)
N2—Ni1—N1	79.2 (3)	C26—C25—C27	114.0 (6)
N4—Ni1—N1	91.9 (3)	N5—C25—H25	106.8
N3—Ni1—N1	91.9 (4)	C26—C25—H25	106.8
N2—Ni1—Cl2	92.0 (2)	C27—C25—H25	106.8
N4—Ni1—Cl2	98.76 (18)	N6—C26—C25	107.0 (6)
N3—Ni1—Cl2	175.8 (2)	N6—C26—C33	114.8 (6)
N1—Ni1—Cl2	91.4 (3)	C25—C26—C33	116.6 (6)
N2—Ni1—Cl1	96.8 (2)	N6—C26—H26	105.9
N4—Ni1—Cl1	91.9 (3)	C25—C26—H26	105.9
N3—Ni1—Cl1	86.9 (3)	C33—C26—H26	105.9
N1—Ni1—Cl1	175.8 (2)	C28—C27—C32	120.0
Cl2—Ni1—Cl1	90.04 (12)	C28—C27—C25	118.3 (5)
N6—Ni2—N5	81.6 (3)	C32—C27—C25	121.7 (6)
N6—Ni2—N8	176.7 (5)	C27—C28—C29	120.0
N5—Ni2—N8	98.1 (3)	C27—C28—H28	120.0
N6—Ni2—N7	99.7 (3)	C29—C28—H28	120.0
N5—Ni2—N7	177.0 (5)	C30—C29—C28	120.0
N8—Ni2—N7	80.8 (3)	C30—C29—H29	120.0
N6—Ni2—O1W	90.2 (3)	C28—C29—H29	120.0
N5—Ni2—O1W	85.5 (3)	C29—C30—C31	120.0
N8—Ni2—O1W	93.1 (3)	C29—C30—H30	120.0
N7—Ni2—O1W	91.7 (3)	C31—C30—H30	120.0
N6—Ni2—O2W	89.6 (4)	C32—C31—C30	120.0
N5—Ni2—O2W	94.0 (3)	C32—C31—H31	120.0
N8—Ni2—O2W	87.1 (3)	C30—C31—H31	120.0
N7—Ni2—O2W	88.8 (3)	C31—C32—C27	120.0
O1W—Ni2—O2W	179.5 (4)	C31—C32—H32	120.0
N10—Ni3—N12	166.9 (3)	C27—C32—H32	120.0
N10—Ni3—N11	91.4 (3)	C34—C33—C38	120.0
N12—Ni3—N11	78.8 (3)	C34—C33—C26	122.9 (6)
N10—Ni3—N9	78.9 (3)	C38—C33—C26	117.1 (6)
N12—Ni3—N9	92.8 (3)	C35—C34—C33	120.0
N11—Ni3—N9	93.2 (4)	C35—C34—H34	120.0
N10—Ni3—Cl4	92.8 (3)	C33—C34—H34	120.0
N12—Ni3—Cl4	97.50 (18)	C34—C35—C36	120.0
N11—Ni3—Cl4	174.6 (2)	C34—C35—H35	120.0
N9—Ni3—Cl4	90.8 (3)	C36—C35—H35	120.0
N10—Ni3—Cl3	97.3 (2)	C37—C36—C35	120.0
N12—Ni3—Cl3	90.6 (3)	C37—C36—H36	120.0
N11—Ni3—Cl3	85.4 (3)	C35—C36—H36	120.0
N9—Ni3—Cl3	175.9 (2)	C36—C37—C38	120.0
Cl4—Ni3—Cl3	90.83 (11)	C36—C37—H37	120.0
Ni2—O1W—H1W1	109.5	C38—C37—H37	120.0
Ni2—O1W—H1W2	109.5	C37—C38—C33	120.0
H1W1—O1W—H1W2	109.5	C37—C38—H38	120.0
Ni2—O2W—H2W1	109.5	C33—C38—H38	120.0
Ni2—O2W—H2W2	109.5	N7—C39—C41	111.4 (6)
H2W1—O2W—H2W2	109.5	N7—C39—C40	109.7 (6)
C9—N1—C1	118.3 (10)	C41—C39—C40	114.1 (6)
C9—N1—Ni1	130.1 (7)	N7—C39—H39	107.1
C1—N1—Ni1	111.4 (7)	C41—C39—H39	107.1
C12—N2—C6	121.8 (10)	C40—C39—H39	107.1
C12—N2—Ni1	125.7 (7)	N8—C40—C47	112.4 (6)
C6—N2—Ni1	112.4 (7)	N8—C40—C39	109.0 (5)
C21—N3—C13	118.6 (8)	C47—C40—C39	112.6 (6)
C21—N3—Ni1	128.0 (6)	N8—C40—H40	107.5
C13—N3—Ni1	113.1 (5)	C47—C40—H40	107.5
C24—N4—C18	119.8 (8)	C39—C40—H40	107.5
C24—N4—Ni1	127.8 (6)	C42—C41—C46	120.0
C18—N4—Ni1	112.4 (5)	C42—C41—C39	120.5 (6)
C25—N5—Ni2	108.4 (5)	C46—C41—C39	119.5 (6)
C25—N5—H5A	110.0	C43—C42—C41	120.0
Ni2—N5—H5A	110.0	C43—C42—H42	120.0
C25—N5—H5B	110.0	C41—C42—H42	120.0
Ni2—N5—H5B	110.0	C42—C43—C44	120.0
H5A—N5—H5B	108.4	C42—C43—H43	120.0
C26—N6—Ni2	109.5 (5)	C44—C43—H43	120.0
C26—N6—H6A	109.8	C45—C44—C43	120.0
Ni2—N6—H6A	109.8	C45—C44—H44	120.0
C26—N6—H6B	109.8	C43—C44—H44	120.0
Ni2—N6—H6B	109.8	C46—C45—C44	120.0
H6A—N6—H6B	108.2	C46—C45—H45	120.0
C39—N7—Ni2	110.1 (5)	C44—C45—H45	120.0
C39—N7—H7A	109.6	C45—C46—C41	120.0
Ni2—N7—H7A	109.6	C45—C46—H46	120.0
C39—N7—H7B	109.6	C41—C46—H46	120.0
Ni2—N7—H7B	109.6	C48—C47—C52	120.0
H7A—N7—H7B	108.2	C48—C47—C40	117.5 (6)
C40—N8—Ni2	110.6 (5)	C52—C47—C40	122.5 (6)
C40—N8—H8A	109.5	C47—C48—C49	120.0
Ni2—N8—H8A	109.5	C47—C48—H48	120.0
C40—N8—H8B	109.5	C49—C48—H48	120.0
Ni2—N8—H8B	109.5	C50—C49—C48	120.0
H8A—N8—H8B	108.1	C50—C49—H49	120.0
C61—N9—C53	119.3 (10)	C48—C49—H49	120.0
C61—N9—Ni3	129.1 (7)	C49—C50—C51	120.0
C53—N9—Ni3	111.5 (7)	C49—C50—H50	120.0
C64—N10—C58	117.1 (10)	C51—C50—H50	120.0
C64—N10—Ni3	128.9 (7)	C52—C51—C50	120.0
C58—N10—Ni3	114.0 (7)	C52—C51—H51	120.0
C73—N11—C65	119.1 (8)	C50—C51—H51	120.0
C73—N11—Ni3	128.7 (6)	C51—C52—C47	120.0
C65—N11—Ni3	111.9 (5)	C51—C52—H52	120.0
C76—N12—C70	117.5 (8)	C47—C52—H52	120.0
C76—N12—Ni3	128.7 (6)	N9—C53—C54	122.0 (8)
C70—N12—Ni3	113.8 (6)	N9—C53—C58	118.0 (8)
N1—C1—C2	121.4 (8)	C54—C53—C58	120.0
N1—C1—C6	118.4 (8)	C55—C54—C53	120.0
C2—C1—C6	120.0	C55—C54—C59	122.8 (9)
C7—C2—C1	118.9 (9)	C53—C54—C59	117.2 (9)
C7—C2—C3	121.1 (9)	C54—C55—C56	120.0
C1—C2—C3	120.0	C54—C55—H55	120.0
C4—C3—C2	120.0	C56—C55—H55	120.0
C4—C3—H3	120.0	C57—C56—C55	120.0
C2—C3—H3	120.0	C57—C56—H56	120.0
C3—C4—C5	120.0	C55—C56—H56	120.0
C3—C4—H4	120.0	C62—C57—C56	120.7 (9)
C5—C4—H4	120.0	C62—C57—C58	119.3 (9)
C10—C5—C6	115.9 (9)	C56—C57—C58	120.0
C10—C5—C4	124.1 (9)	N10—C58—C57	122.5 (8)
C6—C5—C4	120.0	N10—C58—C53	117.4 (8)
N2—C6—C5	121.8 (8)	C57—C58—C53	120.0
N2—C6—C1	118.2 (8)	C60—C59—C54	121.1 (12)
C5—C6—C1	120.0	C60—C59—H59	119.5
C8—C7—C2	119.7 (11)	C54—C59—H59	119.5
C8—C7—H7	120.2	C59—C60—C61	118.3 (13)
C2—C7—H7	120.2	C59—C60—H60	120.8
C7—C8—C9	118.1 (13)	C61—C60—H60	120.8
C7—C8—H8	121.0	N9—C61—C60	122.1 (13)
C9—C8—H8	121.0	N9—C61—H61	119.0
N1—C9—C8	123.5 (13)	C60—C61—H61	119.0
N1—C9—H9	118.3	C63—C62—C57	118.3 (11)
C8—C9—H9	118.3	C63—C62—H62	120.9
C11—C10—C5	122.4 (11)	C57—C62—H62	120.9
C11—C10—H10	118.8	C62—C63—C64	119.3 (12)
C5—C10—H10	118.8	C62—C63—H63	120.4
C10—C11—C12	118.9 (12)	C64—C63—H63	120.4
C10—C11—H11	120.6	N10—C64—C63	123.3 (12)
C12—C11—H11	120.6	N10—C64—H64	118.3
N2—C12—C11	119.2 (12)	C63—C64—H64	118.3
N2—C12—H12	120.4	N11—C65—C66	121.9 (6)
C11—C12—H12	120.4	N11—C65—C70	118.1 (6)
N3—C13—C14	122.6 (6)	C66—C65—C70	120.0
N3—C13—C18	117.3 (6)	C65—C66—C67	120.0
C14—C13—C18	120.0	C65—C66—C71	117.2 (7)
C13—C14—C15	120.0	C67—C66—C71	122.7 (7)
C13—C14—C19	118.1 (6)	C66—C67—C68	120.0
C15—C14—C19	121.8 (6)	C66—C67—H67	120.0
C16—C15—C14	120.0	C68—C67—H67	120.0
C16—C15—H15	120.0	C69—C68—C67	120.0
C14—C15—H15	120.0	C69—C68—H68	120.0
C15—C16—C17	120.0	C67—C68—H68	120.0
C15—C16—H16	120.0	C68—C69—C70	120.0
C17—C16—H16	120.0	C68—C69—C74	121.1 (7)
C18—C17—C16	120.0	C70—C69—C74	118.9 (7)
C18—C17—C22	117.2 (6)	N12—C70—C69	122.8 (6)
C16—C17—C22	122.8 (6)	N12—C70—C65	117.2 (6)
N4—C18—C17	121.4 (6)	C69—C70—C65	120.0
N4—C18—C13	118.6 (6)	C72—C71—C66	121.3 (10)
C17—C18—C13	120.0	C72—C71—H71	119.3
C20—C19—C14	118.6 (9)	C66—C71—H71	119.3
C20—C19—H19	120.7	C71—C72—C73	117.9 (11)
C14—C19—H19	120.7	C71—C72—H72	121.1
C19—C20—C21	120.1 (10)	C73—C72—H72	121.1
C19—C20—H20	119.9	N11—C73—C72	122.3 (10)
C21—C20—H20	119.9	N11—C73—H73	118.8
N3—C21—C20	121.8 (10)	C72—C73—H73	118.8
N3—C21—H21	119.1	C75—C74—C69	118.1 (9)
C20—C21—H21	119.1	C75—C74—H74	121.0
C23—C22—C17	122.1 (9)	C69—C74—H74	121.0
C23—C22—H22	118.9	C74—C75—C76	120.3 (11)
C17—C22—H22	118.9	C74—C75—H75	119.9
C22—C23—C24	116.8 (10)	C76—C75—H75	119.9
C22—C23—H23	121.6	N12—C76—C75	122.3 (10)
C24—C23—H23	121.6	N12—C76—H76	118.8
N4—C24—C23	122.6 (10)	C75—C76—H76	118.8
N4—C24—H24	118.7

N2—Ni1—N1—C9	177.9 (11)	C13—C14—C19—C20	1.0 (13)
N4—Ni1—N1—C9	−12.7 (11)	C15—C14—C19—C20	179.8 (8)
N3—Ni1—N1—C9	−91.1 (11)	C14—C19—C20—C21	0.4 (18)
Cl2—Ni1—N1—C9	86.2 (11)	C13—N3—C21—C20	−2.6 (16)
N2—Ni1—N1—C1	3.7 (6)	Ni1—N3—C21—C20	−175.3 (9)
N4—Ni1—N1—C1	173.1 (6)	C19—C20—C21—N3	0.3 (18)
N3—Ni1—N1—C1	94.6 (6)	C18—C17—C22—C23	−0.7 (15)
Cl2—Ni1—N1—C1	−88.1 (6)	C16—C17—C22—C23	179.3 (10)
N4—Ni1—N2—C12	125.7 (13)	C17—C22—C23—C24	0.6 (19)
N3—Ni1—N2—C12	84.5 (10)	C18—N4—C24—C23	0.2 (17)
N1—Ni1—N2—C12	176.1 (10)	Ni1—N4—C24—C23	178.4 (9)
Cl2—Ni1—N2—C12	−92.9 (9)	C22—C23—C24—N4	−0.4 (19)
Cl1—Ni1—N2—C12	−2.6 (10)	Ni2—N5—C25—C26	44.3 (7)
N4—Ni1—N2—C6	−50.8 (16)	Ni2—N5—C25—C27	172.0 (5)
N3—Ni1—N2—C6	−92.1 (6)	Ni2—N6—C26—C25	41.4 (8)
N1—Ni1—N2—C6	−0.4 (6)	Ni2—N6—C26—C33	172.4 (6)
Cl2—Ni1—N2—C6	90.6 (6)	N5—C25—C26—N6	−56.9 (8)
Cl1—Ni1—N2—C6	−179.2 (6)	C27—C25—C26—N6	174.7 (6)
N2—Ni1—N3—C21	−12.3 (9)	N5—C25—C26—C33	173.2 (6)
N4—Ni1—N3—C21	176.9 (10)	C27—C25—C26—C33	44.7 (9)
N1—Ni1—N3—C21	−91.6 (9)	N5—C25—C27—C28	120.6 (7)
Cl1—Ni1—N3—C21	84.4 (9)	C26—C25—C27—C28	−115.4 (6)
N2—Ni1—N3—C13	174.6 (7)	N5—C25—C27—C32	−59.6 (9)
N4—Ni1—N3—C13	3.8 (6)	C26—C25—C27—C32	64.4 (8)
N1—Ni1—N3—C13	95.4 (7)	C32—C27—C28—C29	0.0
Cl1—Ni1—N3—C13	−88.7 (6)	C25—C27—C28—C29	179.8 (7)
N2—Ni1—N4—C24	136.4 (12)	C27—C28—C29—C30	0.0
N3—Ni1—N4—C24	178.7 (10)	C28—C29—C30—C31	0.0
N1—Ni1—N4—C24	87.2 (10)	C29—C30—C31—C32	0.0
Cl2—Ni1—N4—C24	−4.5 (9)	C30—C31—C32—C27	0.0
Cl1—Ni1—N4—C24	−94.8 (9)	C28—C27—C32—C31	0.0
N2—Ni1—N4—C18	−45.3 (17)	C25—C27—C32—C31	−179.8 (7)
N3—Ni1—N4—C18	−3.0 (6)	N6—C26—C33—C34	−70.8 (8)
N1—Ni1—N4—C18	−94.5 (7)	C25—C26—C33—C34	55.4 (8)
Cl2—Ni1—N4—C18	173.8 (6)	N6—C26—C33—C38	108.3 (7)
Cl1—Ni1—N4—C18	83.5 (6)	C25—C26—C33—C38	−125.6 (6)
N6—Ni2—N5—C25	−17.4 (6)	C38—C33—C34—C35	0.0
N8—Ni2—N5—C25	166.0 (6)	C26—C33—C34—C35	179.1 (7)
O1W—Ni2—N5—C25	73.5 (6)	C33—C34—C35—C36	0.0
O2W—Ni2—N5—C25	−106.4 (6)	C34—C35—C36—C37	0.0
N5—Ni2—N6—C26	−13.7 (6)	C35—C36—C37—C38	0.0
N7—Ni2—N6—C26	169.0 (6)	C36—C37—C38—C33	0.0
O1W—Ni2—N6—C26	−99.2 (6)	C34—C33—C38—C37	0.0
O2W—Ni2—N6—C26	80.3 (6)	C26—C33—C38—C37	−179.1 (6)
N6—Ni2—N7—C39	170.6 (6)	Ni2—N7—C39—C41	164.2 (5)
N8—Ni2—N7—C39	−12.7 (6)	Ni2—N7—C39—C40	36.9 (8)
O1W—Ni2—N7—C39	80.1 (6)	Ni2—N8—C40—C47	163.6 (5)
O2W—Ni2—N7—C39	−100.0 (6)	Ni2—N8—C40—C39	38.0 (8)
N5—Ni2—N8—C40	168.5 (6)	N7—C39—C40—N8	−49.8 (9)
N7—Ni2—N8—C40	−14.4 (6)	C41—C39—C40—N8	−175.6 (7)
O1W—Ni2—N8—C40	−105.6 (6)	N7—C39—C40—C47	−175.2 (7)
O2W—Ni2—N8—C40	74.9 (6)	C41—C39—C40—C47	59.0 (9)
N10—Ni3—N9—C61	−179.0 (11)	N7—C39—C41—C42	−73.0 (8)
N12—Ni3—N9—C61	11.2 (11)	C40—C39—C41—C42	51.8 (8)
N11—Ni3—N9—C61	90.2 (11)	N7—C39—C41—C46	107.8 (7)
Cl4—Ni3—N9—C61	−86.3 (10)	C40—C39—C41—C46	−127.3 (6)
N10—Ni3—N9—C53	−2.5 (6)	C46—C41—C42—C43	0.0
N12—Ni3—N9—C53	−172.2 (6)	C39—C41—C42—C43	−179.1 (8)
N11—Ni3—N9—C53	−93.3 (6)	C41—C42—C43—C44	0.0
Cl4—Ni3—N9—C53	90.2 (6)	C42—C43—C44—C45	0.0
N12—Ni3—N10—C64	−127.8 (14)	C43—C44—C45—C46	0.0
N11—Ni3—N10—C64	−86.4 (11)	C44—C45—C46—C41	0.0
N9—Ni3—N10—C64	−179.4 (11)	C42—C41—C46—C45	0.0
Cl4—Ni3—N10—C64	90.3 (10)	C39—C41—C46—C45	179.1 (7)
Cl3—Ni3—N10—C64	−0.9 (11)	N8—C40—C47—C48	117.7 (6)
N12—Ni3—N10—C58	51.0 (17)	C39—C40—C47—C48	−118.8 (6)
N11—Ni3—N10—C58	92.3 (7)	N8—C40—C47—C52	−62.3 (8)
N9—Ni3—N10—C58	−0.7 (6)	C39—C40—C47—C52	61.2 (8)
Cl4—Ni3—N10—C58	−91.0 (6)	C52—C47—C48—C49	0.0
Cl3—Ni3—N10—C58	177.8 (6)	C40—C47—C48—C49	180.0 (6)
N10—Ni3—N11—C73	11.2 (10)	C47—C48—C49—C50	0.0
N12—Ni3—N11—C73	−177.6 (10)	C48—C49—C50—C51	0.0
N9—Ni3—N11—C73	90.2 (10)	C49—C50—C51—C52	0.0
Cl3—Ni3—N11—C73	−86.0 (10)	C50—C51—C52—C47	0.0
N10—Ni3—N11—C65	−175.0 (7)	C48—C47—C52—C51	0.0
N12—Ni3—N11—C65	−3.8 (6)	C40—C47—C52—C51	−180.0 (7)
N9—Ni3—N11—C65	−96.0 (7)	C61—N9—C53—C54	−0.1 (13)
Cl3—Ni3—N11—C65	87.8 (6)	Ni3—N9—C53—C54	−177.0 (3)
N10—Ni3—N12—C76	−134.3 (13)	C61—N9—C53—C58	−177.7 (8)
N11—Ni3—N12—C76	−176.6 (11)	Ni3—N9—C53—C58	5.4 (8)
N9—Ni3—N12—C76	−83.9 (10)	N9—C53—C54—C55	−177.5 (7)
Cl4—Ni3—N12—C76	7.3 (10)	C58—C53—C54—C55	0.0
Cl3—Ni3—N12—C76	98.3 (10)	N9—C53—C54—C59	1.8 (9)
N10—Ni3—N12—C70	45.0 (18)	C58—C53—C54—C59	179.3 (9)
N11—Ni3—N12—C70	2.7 (6)	C53—C54—C55—C56	0.0
N9—Ni3—N12—C70	95.4 (7)	C59—C54—C55—C56	−179.3 (10)
Cl4—Ni3—N12—C70	−173.4 (6)	C54—C55—C56—C57	0.0
Cl3—Ni3—N12—C70	−82.4 (6)	C55—C56—C57—C62	179.6 (10)
C9—N1—C1—C2	2.9 (12)	C55—C56—C57—C58	0.0
Ni1—N1—C1—C2	177.9 (4)	C64—N10—C58—C57	−1.3 (12)
C9—N1—C1—C6	178.4 (8)	Ni3—N10—C58—C57	179.8 (3)
Ni1—N1—C1—C6	−6.7 (8)	C64—N10—C58—C53	−177.3 (8)
N1—C1—C2—C7	−5.1 (9)	Ni3—N10—C58—C53	3.8 (8)
C6—C1—C2—C7	179.5 (9)	C62—C57—C58—N10	4.6 (9)
N1—C1—C2—C3	175.4 (7)	C56—C57—C58—N10	−175.8 (7)
C6—C1—C2—C3	0.0	C62—C57—C58—C53	−179.6 (9)
C7—C2—C3—C4	−179.5 (10)	C56—C57—C58—C53	0.0
C1—C2—C3—C4	0.0	N9—C53—C58—N10	−6.3 (9)
C2—C3—C4—C5	0.0	C54—C53—C58—N10	176.0 (7)
C3—C4—C5—C10	−179.2 (10)	N9—C53—C58—C57	177.6 (7)
C3—C4—C5—C6	0.0	C54—C53—C58—C57	0.0
C12—N2—C6—C5	2.6 (12)	C55—C54—C59—C60	177.4 (10)
Ni1—N2—C6—C5	179.3 (3)	C53—C54—C59—C60	−1.9 (16)
C12—N2—C6—C1	−179.7 (8)	C54—C59—C60—C61	0 (2)
Ni1—N2—C6—C1	−3.0 (8)	C53—N9—C61—C60	−1.5 (18)
C10—C5—C6—N2	−3.1 (9)	Ni3—N9—C61—C60	174.8 (9)
C4—C5—C6—N2	177.6 (7)	C59—C60—C61—N9	1 (2)
C10—C5—C6—C1	179.3 (9)	C56—C57—C62—C63	175.7 (8)
C4—C5—C6—C1	0.0	C58—C57—C62—C63	−4.7 (14)
N1—C1—C6—N2	6.7 (9)	C57—C62—C63—C64	1.9 (18)
C2—C1—C6—N2	−177.7 (7)	C58—N10—C64—C63	−1.7 (18)
N1—C1—C6—C5	−175.5 (7)	Ni3—N10—C64—C63	177.0 (8)
C2—C1—C6—C5	0.0	C62—C63—C64—N10	1.4 (19)
C1—C2—C7—C8	3.8 (15)	C73—N11—C65—C66	−3.5 (12)
C3—C2—C7—C8	−176.7 (9)	Ni3—N11—C65—C66	−178.0 (4)
C2—C7—C8—C9	−0.5 (18)	C73—N11—C65—C70	178.9 (8)
C1—N1—C9—C8	0.6 (18)	Ni3—N11—C65—C70	4.4 (8)
Ni1—N1—C9—C8	−173.3 (8)	N11—C65—C66—C67	−177.6 (8)
C7—C8—C9—N1	−1.8 (19)	C70—C65—C66—C67	0.0
C6—C5—C10—C11	1.2 (15)	N11—C65—C66—C71	5.9 (9)
C4—C5—C10—C11	−179.6 (9)	C70—C65—C66—C71	−176.5 (8)
C5—C10—C11—C12	1.2 (19)	C65—C66—C67—C68	0.0
C6—N2—C12—C11	0.0 (17)	C71—C66—C67—C68	176.3 (8)
Ni1—N2—C12—C11	−176.3 (7)	C66—C67—C68—C69	0.0
C10—C11—C12—N2	−1.8 (18)	C67—C68—C69—C70	0.0
C21—N3—C13—C14	4.2 (12)	C67—C68—C69—C74	179.4 (8)
Ni1—N3—C13—C14	177.9 (4)	C76—N12—C70—C69	−1.8 (12)
C21—N3—C13—C18	−178.0 (8)	Ni3—N12—C70—C69	178.9 (4)
Ni1—N3—C13—C18	−4.2 (8)	C76—N12—C70—C65	178.1 (8)
N3—C13—C14—C15	177.8 (8)	Ni3—N12—C70—C65	−1.2 (8)
C18—C13—C14—C15	0.0	C68—C69—C70—N12	179.9 (8)
N3—C13—C14—C19	−3.4 (9)	C74—C69—C70—N12	0.5 (9)
C18—C13—C14—C19	178.8 (8)	C68—C69—C70—C65	0.0
C13—C14—C15—C16	0.0	C74—C69—C70—C65	−179.4 (8)
C19—C14—C15—C16	−178.7 (8)	N11—C65—C70—N12	−2.2 (9)
C14—C15—C16—C17	0.0	C66—C65—C70—N12	−179.9 (8)
C15—C16—C17—C18	0.0	N11—C65—C70—C69	177.7 (8)
C15—C16—C17—C22	180.0 (9)	C66—C65—C70—C69	0.0
C24—N4—C18—C17	−0.2 (12)	C65—C66—C71—C72	−4.0 (14)
Ni1—N4—C18—C17	−178.7 (4)	C67—C66—C71—C72	179.6 (9)
C24—N4—C18—C13	−179.8 (8)	C66—C71—C72—C73	−0.2 (18)
Ni1—N4—C18—C13	1.8 (8)	C65—N11—C73—C72	−1.1 (16)
C16—C17—C18—N4	−179.6 (8)	Ni3—N11—C73—C72	172.4 (9)
C22—C17—C18—N4	0.4 (9)	C71—C72—C73—N11	2.8 (18)
C16—C17—C18—C13	0.0	C68—C69—C74—C75	179.7 (9)
C22—C17—C18—C13	180.0 (8)	C70—C69—C74—C75	−0.9 (14)
N3—C13—C18—N4	1.7 (9)	C69—C74—C75—C76	2.6 (19)
C14—C13—C18—N4	179.6 (8)	C70—N12—C76—C75	3.5 (18)
N3—C13—C18—C17	−177.9 (8)	Ni3—N12—C76—C75	−177.2 (9)
C14—C13—C18—C17	0.0	C74—C75—C76—N12	−4 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W1···Cl3	0.82	2.50	3.185 (8)	142
O1W—H1W2···Cl5	0.82	2.41	3.095 (10)	141
O2W—H2W1···Cl1	0.82	2.36	3.182 (8)	180
O2W—H2W2···Cl6	0.82	2.31	3.123 (10)	172

Experimental details

Crystal data
Chemical formula	[Ni(C₁₄H₁₆N₂)₂(H₂O)₂]Cl₂·2[NiCl₂(C₁₂H₈N₂)₂]
M_r	1570.25
Crystal system, space group	Monoclinic, P2₁
Temperature (K)	293
a, b, c (Å)	12.390 (2), 13.819 (2), 21.261 (3)
β (°)	101.348 (2)
V (Å³)	3569.1 (9)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	1.06
Crystal size (mm)	0.48 × 0.23 × 0.18

Data collection
Diffractometer	Bruker APEX area-detector
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.629, 0.832
No. of measured, independent and observed [I > 2σ(I)] reflections	22161, 14184, 7201
R_int	0.046
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.056, 0.165, 1.02
No. of reflections	14184
No. of parameters	796
No. of restraints	590
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.73, −0.50
Absolute structure	Flack (1983), 5767 Friedel pairs
Absolute structure parameter	−0.07 (3)

Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1W1···Cl3	0.82	2.50	3.185 (8)	142
O1W—H1W2···Cl5	0.82	2.41	3.095 (10)	141
O2W—H2W1···Cl1	0.82	2.36	3.182 (8)	180
O2W—H2W2···Cl6	0.82	2.31	3.123 (10)	172

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.

E-mail address*
Repeat e-mail address* (for error checking)

Format*	PDF (US $40)
	HTML (US $40)
	PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number (non-UK EC countries only)
Country*

Terms and conditions of use
Contact us

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Text
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page