[Bis[tris­(3,5-dimethyl­pyrazol­yl)­methane]­nickel(II)][tetra­chloro­nickelate(II)]–methanol–water (1/1/1)

Michaud, A.; Fontaine, F.-G.; Zargarian, D.

doi:10.1107/S1600536805011128

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[Bis[tris(3,5-dimethylpyrazolyl)methane]nickel(II)][tetrachloronickelate(II)]-methanol-water (1/1/1)

A. Michaud, F.-G. Fontaine and D. Zargarian

The title complex, [Ni(HC(3,5-Me₂pz)₃)₂][NiCl₄]·CH₃OH·H₂O, where HC(3,5-Me₂pz)₃ is tris(3,5-dimethylpyrazolyl)methane (C₁₆H₂₂N₆), contains two octahedral nickel(II) cationic complexes, each having $\overline{1}$ symmetry. The Ni atom in each cation is coordinated by six pyrazolyl rings of two chelating HC(3,5-Me₂pz)₃ ligands, with Ni-N distances between 2.0870 (16) Å and 2.1094 (16) Å. The anion consists of nickel(II) surrounded tetrahedrally by four Cl^- anions, with Ni-Cl distances between 2.2547 (7) Å and 2.2847 (7) Å. There is also one methanol molecule and one disordered water molecule in the asymmetric unit.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805011128/lh6402sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536805011128/lh6402Isup2.hkl Contains datablock I

CCDC reference: 272021

checkCIF report

Key indicators

Single-crystal X-ray study
T = 220 K
Mean (C-C) = 0.003 Å
R factor = 0.051
wR factor = 0.156
Data-to-parameter ratio = 17.0

checkCIF/PLATON results

No syntax errors found



Alert level C
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.99 <> 1.01
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight           906.07
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   33.00  396.36
           H         1.01   48.00   48.38
           N        14.01   12.00  168.08
           Cl       35.45    4.00  141.81
           Ni       58.69    2.00  117.38
           O        16.00    1.00   16.00
           Calculated formula weight              888.02
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................     906.07
PLAT044_ALERT_1_C Calculated and Reported Dx Differ ..............          ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large .............       0.79
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.78
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Ni3
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of .      56.00 A   3  

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:C33 H50 Cl4 N12 Ni2 O2
            Atom count from the _atom_site data:  C33 H48 Cl4 N12 Ni2 O1
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: Large difference may be due to a
            symmetry error - see SYMMG tests
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  C33 H50 Cl4 N12 Ni2 O2
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        132.00    132.00    0.00
           H        200.00    192.00    8.00
           Cl        16.00     16.00    0.00
           N         48.00     48.00    0.00
           Ni         8.00      8.00    0.00
           O          8.00      4.00    4.00

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

   6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 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, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: UdMX (local program).

[Bis[tris(3,5-dimethylpyrazolyl)methane]nickel(II)][tetrachloronickel(II)] methanol water solvate top

Crystal data top

[Ni(C₁₆H₂₂N₆)₂][NiCl₄]·CH₄O·H₂O	F(000) = 1899
M_r = 906.07	D_x = 1.447 Mg m⁻³
Monoclinic, P2₁/c	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: -P 2ybc	Cell parameters from 36297 reflections
a = 10.2998 (2) Å	θ = 2.4–72.6°
b = 18.5245 (3) Å	µ = 3.85 mm⁻¹
c = 21.9660 (3) Å	T = 220 K
β = 94.118 (1)°	Plate, blue
V = 4180.26 (12) Å³	0.30 × 0.30 × 0.08 mm
Z = 4

Data collection top

Bruker SMART 2K/Platform CCD area-detector diffractometer	8242 independent reflections
Radiation source: sealed tube	7048 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.091
Detector resolution: 5.5 pixels mm^-1	θ_max = 72.6°, θ_min = 3.1°
ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −22→21
T_min = 0.287, T_max = 0.740	l = −27→26
49482 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.051	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.156	H-atom parameters constrained
S = 1.13	w = 1/[σ²(F_o²) + (0.1017P)² + 0.294P] where P = (F_o² + 2F_c²)/3
8242 reflections	(Δ/σ)_max = 0.001
485 parameters	Δρ_max = 1.05 e Å⁻³
2 restraints	Δρ_min = −0.57 e Å⁻³

Special details top

Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8 Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis. The structure contains 34 electrons displaced on four different sites of 53 Å³ , which were attributed to four disordered water molecules per unit cell. The PLATON/Squeeze (Spek, 2003) operation has been carried out to model these molecules and solve the disorder issue.

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.

Hydrogen bond details:

H97D.·Cl2 2.505 O97.·Cl2 3.332 (3) O97—H97D.·Cl2 173.9

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

	x	y	z	U_iso*/U_eq
Ni1	1.0000	0.5000	0.5000	0.02969 (10)
N1	0.84141 (15)	0.44415 (9)	0.45692 (7)	0.0361 (4)
N2	0.75964 (14)	0.41052 (8)	0.49442 (7)	0.0320 (3)
N3	0.97738 (14)	0.59002 (9)	0.44310 (7)	0.0365 (4)
N4	1.08906 (14)	0.61892 (8)	0.42337 (7)	0.0317 (3)
N5	1.13211 (15)	0.46284 (8)	0.43795 (7)	0.0364 (4)
N6	1.21832 (14)	0.51278 (8)	0.41874 (7)	0.0311 (3)
C1	0.8539 (3)	0.45594 (17)	0.34510 (10)	0.0682 (8)
H1A	0.9355	0.4799	0.3572	0.102*
H1B	0.7962	0.4895	0.3227	0.102*
H1C	0.8704	0.4149	0.3193	0.102*
C2	0.7919 (2)	0.43049 (12)	0.40067 (9)	0.0441 (5)
C3	0.6785 (2)	0.38900 (12)	0.40213 (9)	0.0455 (5)
H3	0.6253	0.3728	0.3683	0.055*
C4	0.66017 (17)	0.37659 (11)	0.46202 (9)	0.0375 (4)
C5	0.5570 (2)	0.33501 (14)	0.49058 (11)	0.0559 (6)
H5A	0.5971	0.2994	0.5184	0.084*
H5B	0.5024	0.3108	0.4591	0.084*
H5C	0.5043	0.3677	0.5130	0.084*
C6	1.0915 (3)	0.33253 (12)	0.42014 (14)	0.0629 (7)
H6A	1.0200	0.3417	0.4455	0.094*
H6B	1.1495	0.2969	0.4397	0.094*
H6C	1.0576	0.3145	0.3807	0.094*
C7	1.1650 (2)	0.40132 (11)	0.41166 (10)	0.0424 (5)
C8	1.2721 (2)	0.41145 (11)	0.37708 (9)	0.0418 (5)
H8	1.3136	0.3761	0.3547	0.050*
C9	1.30475 (18)	0.48283 (11)	0.38218 (8)	0.0358 (4)
C10	1.4092 (2)	0.52464 (13)	0.35493 (11)	0.0525 (6)
H10A	1.3712	0.5657	0.3328	0.079*
H10B	1.4531	0.4940	0.3271	0.079*
H10C	1.4713	0.5415	0.3871	0.079*
C11	0.7432 (2)	0.61966 (16)	0.43184 (14)	0.0678 (8)
H11A	0.7298	0.5685	0.4383	0.102*
H11B	0.6878	0.6356	0.3968	0.102*
H11C	0.7214	0.6463	0.4678	0.102*
C12	0.8825 (2)	0.63294 (12)	0.42041 (10)	0.0444 (5)
C13	0.9332 (2)	0.68830 (12)	0.38660 (10)	0.0490 (5)
H13	0.8857	0.7253	0.3659	0.059*
C14	1.0652 (2)	0.67893 (10)	0.38914 (8)	0.0385 (4)
C15	1.1701 (3)	0.71997 (12)	0.36165 (12)	0.0564 (6)
H15A	1.2313	0.7379	0.3938	0.085*
H15B	1.1324	0.7603	0.3384	0.085*
H15C	1.2151	0.6885	0.3348	0.085*
C16	1.21270 (16)	0.58590 (9)	0.44066 (8)	0.0293 (4)
H16	1.2806	0.6139	0.4214	0.035*
Ni2	1.0000	0.5000	0.0000	0.03056 (10)
N21	0.99622 (14)	0.45153 (9)	0.08592 (7)	0.0349 (3)
N22	1.11431 (14)	0.43399 (8)	0.11478 (7)	0.0327 (3)
N23	1.15014 (15)	0.56432 (8)	0.04077 (7)	0.0355 (4)
N24	1.24117 (14)	0.53040 (8)	0.07845 (7)	0.0326 (3)
N25	0.85380 (15)	0.57610 (9)	0.01538 (7)	0.0359 (4)
N26	0.75850 (14)	0.58431 (8)	−0.03054 (7)	0.0339 (3)
C21	0.7660 (2)	0.43614 (15)	0.10752 (12)	0.0551 (6)
H21A	0.7371	0.4821	0.1229	0.083*
H21B	0.7200	0.3972	0.1263	0.083*
H21C	0.7480	0.4344	0.0636	0.083*
C22	0.90868 (18)	0.42801 (11)	0.12266 (9)	0.0378 (4)
C23	0.9693 (2)	0.39611 (12)	0.17472 (9)	0.0416 (5)
H23	0.9281	0.3759	0.2075	0.050*
C24	1.1004 (2)	0.39999 (11)	0.16884 (8)	0.0384 (4)
C25	1.2136 (2)	0.37426 (15)	0.20925 (11)	0.0615 (7)
H25A	1.2688	0.3440	0.1860	0.092*
H25B	1.1825	0.3466	0.2428	0.092*
H25C	1.2632	0.4154	0.2253	0.092*
C26	1.1081 (2)	0.69081 (12)	0.00798 (12)	0.0537 (6)
H26A	1.0920	0.6758	−0.0342	0.081*
H26B	1.1566	0.7357	0.0096	0.081*
H26C	1.0257	0.6978	0.0260	0.081*
C27	1.1847 (2)	0.63414 (11)	0.04262 (9)	0.0394 (4)
C28	1.2973 (2)	0.64331 (11)	0.08114 (10)	0.0433 (5)
H28	1.3407	0.6871	0.0901	0.052*
C29	1.33216 (18)	0.57706 (11)	0.10331 (9)	0.0379 (4)
C30	1.4421 (2)	0.55469 (13)	0.14730 (12)	0.0541 (6)
H30A	1.4081	0.5285	0.1810	0.081*
H30B	1.4885	0.5972	0.1628	0.081*
H30C	1.5011	0.5238	0.1267	0.081*
C31	0.8930 (3)	0.62224 (14)	0.12066 (10)	0.0580 (6)
H31A	0.9708	0.5928	0.1198	0.087*
H31B	0.8414	0.6057	0.1532	0.087*
H31C	0.9176	0.6722	0.1278	0.087*
C32	0.8154 (2)	0.61600 (11)	0.06126 (9)	0.0414 (5)
C33	0.6957 (2)	0.64820 (13)	0.04463 (10)	0.0482 (5)
H33	0.6481	0.6785	0.0691	0.058*
C34	0.66092 (19)	0.62771 (11)	−0.01338 (10)	0.0437 (5)
C35	0.5422 (2)	0.64314 (17)	−0.05376 (14)	0.0706 (8)
H35A	0.5633	0.6769	−0.0853	0.106*
H35B	0.4760	0.6639	−0.0298	0.106*
H35C	0.5098	0.5986	−0.0725	0.106*
C36	0.76798 (17)	0.54663 (10)	−0.08759 (8)	0.0317 (4)
H36	0.6935	0.5616	−0.1158	0.038*
Ni3	0.42641 (4)	0.77631 (2)	0.245018 (15)	0.04356 (9)
Cl1	0.49993 (7)	0.71671 (4)	0.33024 (3)	0.07339 (19)
Cl2	0.21731 (6)	0.75424 (4)	0.20784 (3)	0.06300 (17)
Cl3	0.55720 (6)	0.75212 (3)	0.16896 (3)	0.05183 (14)
Cl4	0.43912 (6)	0.89555 (3)	0.26514 (3)	0.05340 (14)
C97	0.0810 (3)	0.56757 (17)	0.25579 (12)	0.0685 (8)
H97A	0.1145	0.5600	0.2977	0.103*
H97B	0.0296	0.5261	0.2419	0.103*
H97C	0.0268	0.6105	0.2534	0.103*
O97	0.1815 (3)	0.57619 (15)	0.22006 (15)	0.1196 (10)
H97D	0.1956	0.6199	0.2155	0.179*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.03121 (19)	0.0318 (2)	0.0265 (2)	−0.00488 (15)	0.00538 (16)	0.00149 (15)
N1	0.0388 (7)	0.0447 (8)	0.0256 (7)	−0.0136 (6)	0.0069 (6)	0.0010 (6)
N2	0.0344 (7)	0.0372 (7)	0.0251 (7)	−0.0080 (6)	0.0070 (6)	−0.0009 (6)
N3	0.0317 (7)	0.0405 (8)	0.0378 (8)	−0.0006 (6)	0.0058 (6)	0.0084 (6)
N4	0.0364 (7)	0.0305 (7)	0.0290 (7)	−0.0016 (6)	0.0079 (6)	0.0030 (6)
N5	0.0422 (7)	0.0313 (7)	0.0368 (8)	−0.0063 (6)	0.0109 (6)	−0.0030 (6)
N6	0.0366 (7)	0.0302 (7)	0.0278 (7)	−0.0019 (6)	0.0095 (6)	−0.0004 (6)
C1	0.0777 (15)	0.099 (2)	0.0281 (10)	−0.0350 (15)	0.0081 (11)	0.0000 (12)
C2	0.0499 (10)	0.0562 (12)	0.0265 (9)	−0.0123 (9)	0.0041 (8)	−0.0030 (8)
C3	0.0441 (10)	0.0595 (12)	0.0325 (10)	−0.0139 (9)	0.0007 (8)	−0.0108 (9)
C4	0.0340 (8)	0.0424 (10)	0.0364 (9)	−0.0066 (7)	0.0050 (7)	−0.0083 (8)
C5	0.0475 (10)	0.0738 (15)	0.0472 (12)	−0.0265 (10)	0.0097 (9)	−0.0085 (11)
C6	0.0824 (16)	0.0306 (10)	0.0781 (17)	−0.0112 (11)	0.0229 (14)	−0.0087 (10)
C7	0.0533 (11)	0.0316 (9)	0.0431 (11)	−0.0019 (8)	0.0083 (9)	−0.0043 (8)
C8	0.0520 (10)	0.0378 (9)	0.0363 (10)	0.0078 (8)	0.0092 (8)	−0.0058 (8)
C9	0.0382 (8)	0.0405 (9)	0.0293 (9)	0.0049 (8)	0.0073 (7)	−0.0010 (7)
C10	0.0524 (11)	0.0543 (12)	0.0544 (13)	−0.0021 (10)	0.0291 (10)	−0.0053 (10)
C11	0.0374 (10)	0.0856 (18)	0.0807 (18)	0.0135 (11)	0.0060 (11)	0.0276 (15)
C12	0.0400 (9)	0.0502 (11)	0.0428 (11)	0.0057 (9)	0.0020 (8)	0.0088 (9)
C13	0.0561 (11)	0.0483 (11)	0.0431 (11)	0.0165 (9)	0.0067 (9)	0.0123 (9)
C14	0.0561 (11)	0.0314 (8)	0.0290 (8)	0.0030 (8)	0.0112 (8)	0.0040 (7)
C15	0.0771 (14)	0.0420 (11)	0.0536 (13)	0.0046 (11)	0.0294 (11)	0.0168 (9)
C16	0.0332 (8)	0.0306 (8)	0.0249 (8)	−0.0046 (6)	0.0080 (6)	−0.0005 (6)
Ni2	0.03101 (19)	0.0343 (2)	0.0262 (2)	0.00491 (16)	0.00076 (17)	−0.00090 (15)
N21	0.0304 (7)	0.0428 (8)	0.0313 (8)	0.0027 (6)	0.0007 (6)	0.0017 (6)
N22	0.0340 (7)	0.0368 (8)	0.0270 (7)	−0.0005 (6)	−0.0012 (6)	−0.0002 (6)
N23	0.0379 (7)	0.0346 (8)	0.0334 (8)	0.0026 (6)	−0.0020 (6)	0.0006 (6)
N24	0.0329 (7)	0.0315 (7)	0.0329 (7)	0.0014 (6)	−0.0004 (6)	0.0000 (6)
N25	0.0388 (7)	0.0399 (8)	0.0287 (7)	0.0083 (6)	0.0004 (6)	−0.0029 (6)
N26	0.0309 (7)	0.0360 (8)	0.0347 (8)	0.0051 (6)	0.0021 (6)	−0.0019 (6)
C21	0.0372 (10)	0.0735 (15)	0.0560 (13)	−0.0015 (10)	0.0138 (9)	0.0031 (12)
C22	0.0376 (9)	0.0418 (10)	0.0348 (9)	−0.0009 (8)	0.0080 (7)	−0.0041 (8)
C23	0.0506 (10)	0.0486 (11)	0.0264 (9)	−0.0091 (9)	0.0079 (8)	−0.0028 (7)
C24	0.0480 (10)	0.0417 (10)	0.0252 (8)	−0.0054 (8)	0.0010 (7)	−0.0002 (7)
C25	0.0630 (13)	0.0804 (17)	0.0389 (11)	−0.0104 (12)	−0.0114 (10)	0.0195 (11)
C26	0.0668 (13)	0.0377 (10)	0.0555 (13)	0.0040 (10)	−0.0030 (11)	0.0034 (10)
C27	0.0481 (10)	0.0350 (9)	0.0356 (10)	0.0007 (8)	0.0050 (8)	−0.0006 (7)
C28	0.0523 (10)	0.0375 (9)	0.0399 (10)	−0.0092 (8)	0.0025 (9)	−0.0027 (8)
C29	0.0380 (9)	0.0401 (10)	0.0353 (9)	−0.0047 (8)	0.0008 (8)	−0.0025 (8)
C30	0.0494 (11)	0.0505 (12)	0.0594 (14)	−0.0091 (10)	−0.0160 (10)	0.0014 (10)
C31	0.0783 (15)	0.0649 (14)	0.0299 (10)	0.0197 (12)	−0.0027 (10)	−0.0112 (10)
C32	0.0531 (11)	0.0404 (10)	0.0314 (9)	0.0091 (8)	0.0077 (8)	−0.0040 (8)
C33	0.0507 (11)	0.0507 (11)	0.0443 (11)	0.0120 (9)	0.0112 (9)	−0.0094 (9)
C34	0.0367 (9)	0.0437 (10)	0.0511 (12)	0.0099 (8)	0.0067 (8)	−0.0067 (9)
C35	0.0481 (11)	0.0858 (18)	0.0758 (17)	0.0327 (12)	−0.0094 (12)	−0.0213 (14)
C36	0.0316 (7)	0.0340 (8)	0.0290 (8)	0.0019 (7)	−0.0002 (6)	0.0008 (7)
Ni3	0.0580 (2)	0.04482 (19)	0.02817 (17)	−0.00942 (16)	0.00548 (15)	0.00153 (13)
Cl1	0.0811 (4)	0.0822 (4)	0.0555 (3)	−0.0005 (3)	−0.0041 (3)	0.0297 (3)
Cl2	0.0620 (3)	0.0824 (4)	0.0447 (3)	−0.0229 (3)	0.0042 (3)	0.0039 (3)
Cl3	0.0698 (3)	0.0452 (3)	0.0426 (3)	−0.0082 (2)	0.0183 (2)	−0.00509 (19)
Cl4	0.0662 (3)	0.0486 (3)	0.0452 (3)	−0.0028 (2)	0.0031 (2)	−0.0095 (2)
C97	0.0834 (17)	0.0806 (18)	0.0416 (13)	−0.0146 (14)	0.0045 (13)	−0.0075 (12)
O97	0.1276 (19)	0.0930 (17)	0.147 (2)	0.0082 (15)	0.0738 (18)	0.0250 (17)

Geometric parameters (Å, º) top

Ni1—N3	2.0870 (16)	Ni2—N25ⁱⁱ	2.1077 (15)
Ni1—N3ⁱ	2.0870 (16)	N21—C22	1.326 (2)
Ni1—N1ⁱ	2.1004 (15)	N21—N22	1.370 (2)
Ni1—N1	2.1004 (15)	N22—C24	1.361 (2)
Ni1—N5ⁱ	2.1094 (16)	N22—C36ⁱⁱ	1.435 (2)
Ni1—N5	2.1094 (16)	N23—C27	1.341 (3)
N1—C2	1.327 (2)	N23—N24	1.359 (2)
N1—N2	1.369 (2)	N24—C29	1.360 (2)
N2—C4	1.359 (2)	N24—C36ⁱⁱ	1.445 (2)
N2—C16ⁱ	1.436 (2)	N25—C32	1.332 (2)
N3—C12	1.328 (2)	N25—N26	1.365 (2)
N3—N4	1.367 (2)	N26—C34	1.361 (2)
N4—C14	1.355 (2)	N26—C36	1.444 (2)
N4—C16	1.439 (2)	C21—C22	1.491 (3)
N5—C7	1.332 (2)	C21—H21A	0.9700
N5—N6	1.370 (2)	C21—H21B	0.9700
N6—C9	1.359 (2)	C21—H21C	0.9700
N6—C16	1.440 (2)	C22—C23	1.395 (3)
C1—C2	1.494 (3)	C23—C24	1.368 (3)
C1—H1A	0.9700	C23—H23	0.9400
C1—H1B	0.9700	C24—C25	1.492 (3)
C1—H1C	0.9700	C25—H25A	0.9700
C2—C3	1.400 (3)	C25—H25B	0.9700
C3—C4	1.362 (3)	C25—H25C	0.9700
C3—H3	0.9400	C26—C27	1.489 (3)
C4—C5	1.487 (3)	C26—H26A	0.9700
C5—H5A	0.9700	C26—H26B	0.9700
C5—H5B	0.9700	C26—H26C	0.9700
C5—H5C	0.9700	C27—C28	1.396 (3)
C6—C7	1.501 (3)	C28—C29	1.359 (3)
C6—H6A	0.9700	C28—H28	0.9400
C6—H6B	0.9700	C29—C30	1.494 (3)
C6—H6C	0.9700	C30—H30A	0.9700
C7—C8	1.397 (3)	C30—H30B	0.9700
C8—C9	1.367 (3)	C30—H30C	0.9700
C8—H8	0.9400	C31—C32	1.485 (3)
C9—C10	1.486 (3)	C31—H31A	0.9700
C10—H10A	0.9700	C31—H31B	0.9700
C10—H10B	0.9700	C31—H31C	0.9700
C10—H10C	0.9700	C32—C33	1.394 (3)
C11—C12	1.496 (3)	C33—C34	1.353 (3)
C11—H11A	0.9700	C33—H33	0.9400
C11—H11B	0.9700	C34—C35	1.486 (3)
C11—H11C	0.9700	C35—H35A	0.9700
C12—C13	1.390 (3)	C35—H35B	0.9700
C13—C14	1.368 (3)	C35—H35C	0.9700
C13—H13	0.9400	C36—N22ⁱⁱ	1.435 (2)
C14—C15	1.484 (3)	C36—N24ⁱⁱ	1.445 (2)
C15—H15A	0.9700	C36—H36	0.9900
C15—H15B	0.9700	Ni3—Cl4	2.2547 (7)
C15—H15C	0.9700	Ni3—Cl1	2.2568 (7)
C16—N2ⁱ	1.436 (2)	Ni3—Cl3	2.2649 (7)
C16—H16	0.9900	Ni3—Cl2	2.2847 (7)
Ni2—N21	2.0929 (16)	C97—O97	1.353 (4)
Ni2—N21ⁱⁱ	2.0929 (16)	C97—H97A	0.9700
Ni2—N23ⁱⁱ	2.1010 (15)	C97—H97B	0.9700
Ni2—N23	2.1010 (15)	C97—H97C	0.9700
Ni2—N25	2.1076 (15)	O97—H97D	0.8300

N3—Ni1—N3ⁱ	180	N21ⁱⁱ—Ni2—N25	85.26 (6)
N3—Ni1—N1ⁱ	85.76 (6)	N23ⁱⁱ—Ni2—N25	86.28 (6)
N3ⁱ—Ni1—N1ⁱ	94.24 (6)	N23—Ni2—N25	93.72 (6)
N3—Ni1—N1	94.24 (6)	N21—Ni2—N25ⁱⁱ	85.26 (6)
N3ⁱ—Ni1—N1	85.76 (6)	N21ⁱⁱ—Ni2—N25ⁱⁱ	94.74 (6)
N1ⁱ—Ni1—N1	180	N23ⁱⁱ—Ni2—N25ⁱⁱ	93.71 (6)
N3—Ni1—N5ⁱ	94.40 (6)	N23—Ni2—N25ⁱⁱ	86.28 (6)
N3ⁱ—Ni1—N5ⁱ	85.60 (6)	N25—Ni2—N25ⁱⁱ	180
N1ⁱ—Ni1—N5ⁱ	93.73 (6)	C22—N21—N22	105.09 (15)
N1—Ni1—N5ⁱ	86.27 (6)	C22—N21—Ni2	138.35 (13)
N3—Ni1—N5	85.59 (6)	N22—N21—Ni2	116.47 (11)
N3ⁱ—Ni1—N5	94.40 (6)	C24—N22—N21	111.62 (15)
N1ⁱ—Ni1—N5	86.27 (6)	C24—N22—C36ⁱⁱ	128.59 (15)
N1—Ni1—N5	93.73 (6)	N21—N22—C36ⁱⁱ	119.78 (14)
N5ⁱ—Ni1—N5	180	C27—N23—N24	104.91 (15)
C2—N1—N2	105.14 (15)	C27—N23—Ni2	138.19 (13)
C2—N1—Ni1	138.43 (13)	N24—N23—Ni2	116.86 (11)
N2—N1—Ni1	116.43 (11)	N23—N24—C29	112.08 (15)
C4—N2—N1	111.63 (15)	N23—N24—C36ⁱⁱ	119.48 (14)
C4—N2—C16ⁱ	129.05 (15)	C29—N24—C36ⁱⁱ	128.44 (15)
N1—N2—C16ⁱ	119.32 (14)	C32—N25—N26	105.11 (15)
C12—N3—N4	105.03 (15)	C32—N25—Ni2	138.29 (13)
C12—N3—Ni1	138.63 (14)	N26—N25—Ni2	116.12 (11)
N4—N3—Ni1	116.26 (11)	C34—N26—N25	111.55 (16)
C14—N4—N3	111.97 (15)	C34—N26—C36	128.55 (16)
C14—N4—C16	128.10 (16)	N25—N26—C36	119.86 (14)
N3—N4—C16	119.91 (14)	C22—C21—H21A	109.5
C7—N5—N6	104.70 (15)	C22—C21—H21B	109.5
C7—N5—Ni1	139.02 (14)	H21A—C21—H21B	109.5
N6—N5—Ni1	116.18 (11)	C22—C21—H21C	109.5
C9—N6—N5	111.89 (15)	H21A—C21—H21C	109.5
C9—N6—C16	128.69 (15)	H21B—C21—H21C	109.5
N5—N6—C16	119.33 (14)	N21—C22—C23	110.74 (17)
C2—C1—H1A	109.5	N21—C22—C21	122.25 (18)
C2—C1—H1B	109.5	C23—C22—C21	127.01 (19)
H1A—C1—H1B	109.5	C24—C23—C22	106.71 (17)
C2—C1—H1C	109.5	C24—C23—H23	126.6
H1A—C1—H1C	109.5	C22—C23—H23	126.6
H1B—C1—H1C	109.5	N22—C24—C23	105.85 (17)
N1—C2—C3	110.43 (18)	N22—C24—C25	122.73 (19)
N1—C2—C1	122.81 (19)	C23—C24—C25	131.42 (19)
C3—C2—C1	126.75 (19)	C24—C25—H25A	109.5
C4—C3—C2	106.76 (17)	C24—C25—H25B	109.5
C4—C3—H3	126.6	H25A—C25—H25B	109.5
C2—C3—H3	126.6	C24—C25—H25C	109.5
N2—C4—C3	106.04 (16)	H25A—C25—H25C	109.5
N2—C4—C5	123.59 (18)	H25B—C25—H25C	109.5
C3—C4—C5	130.37 (18)	C27—C26—H26A	109.5
C4—C5—H5A	109.5	C27—C26—H26B	109.5
C4—C5—H5B	109.5	H26A—C26—H26B	109.5
H5A—C5—H5B	109.5	C27—C26—H26C	109.5
C4—C5—H5C	109.5	H26A—C26—H26C	109.5
H5A—C5—H5C	109.5	H26B—C26—H26C	109.5
H5B—C5—H5C	109.5	N23—C27—C28	110.04 (17)
C7—C6—H6A	109.5	N23—C27—C26	122.31 (18)
C7—C6—H6B	109.5	C28—C27—C26	127.64 (19)
H6A—C6—H6B	109.5	C29—C28—C27	107.10 (18)
C7—C6—H6C	109.5	C29—C28—H28	126.4
H6A—C6—H6C	109.5	C27—C28—H28	126.4
H6B—C6—H6C	109.5	C28—C29—N24	105.85 (17)
N5—C7—C8	110.86 (18)	C28—C29—C30	130.62 (19)
N5—C7—C6	121.8 (2)	N24—C29—C30	123.50 (18)
C8—C7—C6	127.4 (2)	C29—C30—H30A	109.5
C9—C8—C7	106.54 (17)	C29—C30—H30B	109.5
C9—C8—H8	126.7	H30A—C30—H30B	109.5
C7—C8—H8	126.7	C29—C30—H30C	109.5
N6—C9—C8	106.00 (17)	H30A—C30—H30C	109.5
N6—C9—C10	123.29 (18)	H30B—C30—H30C	109.5
C8—C9—C10	130.71 (18)	C32—C31—H31A	109.5
C9—C10—H10A	109.5	C32—C31—H31B	109.5
C9—C10—H10B	109.5	H31A—C31—H31B	109.5
H10A—C10—H10B	109.5	C32—C31—H31C	109.5
C9—C10—H10C	109.5	H31A—C31—H31C	109.5
H10A—C10—H10C	109.5	H31B—C31—H31C	109.5
H10B—C10—H10C	109.5	N25—C32—C33	110.11 (18)
C12—C11—H11A	109.5	N25—C32—C31	122.51 (19)
C12—C11—H11B	109.5	C33—C32—C31	127.37 (19)
H11A—C11—H11B	109.5	C34—C33—C32	107.23 (18)
C12—C11—H11C	109.5	C34—C33—H33	126.4
H11A—C11—H11C	109.5	C32—C33—H33	126.4
H11B—C11—H11C	109.5	C33—C34—N26	105.99 (18)
N3—C12—C13	110.37 (18)	C33—C34—C35	131.2 (2)
N3—C12—C11	121.8 (2)	N26—C34—C35	122.7 (2)
C13—C12—C11	127.8 (2)	C34—C35—H35A	109.5
C14—C13—C12	107.14 (18)	C34—C35—H35B	109.5
C14—C13—H13	126.4	H35A—C35—H35B	109.5
C12—C13—H13	126.4	C34—C35—H35C	109.5
N4—C14—C13	105.48 (17)	H35A—C35—H35C	109.5
N4—C14—C15	122.54 (19)	H35B—C35—H35C	109.5
C13—C14—C15	131.97 (19)	N22ⁱⁱ—C36—N26	110.62 (14)
C14—C15—H15A	109.5	N22ⁱⁱ—C36—N24ⁱⁱ	111.74 (14)
C14—C15—H15B	109.5	N26—C36—N24ⁱⁱ	110.34 (15)
H15A—C15—H15B	109.5	N22ⁱⁱ—C36—H36	108.0
C14—C15—H15C	109.5	N26—C36—H36	108.0
H15A—C15—H15C	109.5	N24ⁱⁱ—C36—H36	108.0
H15B—C15—H15C	109.5	Cl4—Ni3—Cl1	107.78 (3)
N2ⁱ—C16—N4	110.57 (14)	Cl4—Ni3—Cl3	108.01 (2)
N2ⁱ—C16—N6	111.44 (14)	Cl1—Ni3—Cl3	109.46 (3)
N4—C16—N6	111.57 (14)	Cl4—Ni3—Cl2	106.58 (3)
N2ⁱ—C16—H16	107.7	Cl1—Ni3—Cl2	117.42 (3)
N4—C16—H16	107.7	Cl3—Ni3—Cl2	107.24 (3)
N6—C16—H16	107.7	O97—C97—H97A	109.5
N21—Ni2—N21ⁱⁱ	180	O97—C97—H97B	109.5
N21—Ni2—N23ⁱⁱ	94.60 (6)	H97A—C97—H97B	109.5
N21ⁱⁱ—Ni2—N23ⁱⁱ	85.40 (6)	O97—C97—H97C	109.5
N21—Ni2—N23	85.39 (6)	H97A—C97—H97C	109.5
N21ⁱⁱ—Ni2—N23	94.61 (6)	H97B—C97—H97C	109.5
N23ⁱⁱ—Ni2—N23	180	C97—O97—H97D	109.5
N21—Ni2—N25	94.74 (6)

N3—Ni1—N1—C2	43.6 (2)	C9—N6—C16—N4	122.73 (18)
N3ⁱ—Ni1—N1—C2	−136.4 (2)	N5—N6—C16—N4	−61.0 (2)
N5ⁱ—Ni1—N1—C2	137.7 (2)	N23ⁱⁱ—Ni2—N21—C22	−41.2 (2)
N5—Ni1—N1—C2	−42.3 (2)	N23—Ni2—N21—C22	138.8 (2)
N3—Ni1—N1—N2	−136.12 (13)	N25—Ni2—N21—C22	45.5 (2)
N3ⁱ—Ni1—N1—N2	43.88 (13)	N25ⁱⁱ—Ni2—N21—C22	−134.5 (2)
N5ⁱ—Ni1—N1—N2	−41.98 (13)	N23ⁱⁱ—Ni2—N21—N22	134.82 (13)
N5—Ni1—N1—N2	138.03 (13)	N23—Ni2—N21—N22	−45.18 (13)
C2—N1—N2—C4	−0.2 (2)	N25—Ni2—N21—N22	−138.54 (13)
Ni1—N1—N2—C4	179.54 (12)	N25ⁱⁱ—Ni2—N21—N22	41.46 (13)
C2—N1—N2—C16ⁱ	179.16 (17)	C22—N21—N22—C24	0.0 (2)
Ni1—N1—N2—C16ⁱ	−1.1 (2)	Ni2—N21—N22—C24	−177.25 (12)
N1ⁱ—Ni1—N3—C12	−133.9 (2)	C22—N21—N22—C36ⁱⁱ	−178.72 (16)
N1—Ni1—N3—C12	46.1 (2)	Ni2—N21—N22—C36ⁱⁱ	4.0 (2)
N5ⁱ—Ni1—N3—C12	−40.4 (2)	N21—Ni2—N23—C27	−134.8 (2)
N5—Ni1—N3—C12	139.6 (2)	N21ⁱⁱ—Ni2—N23—C27	45.2 (2)
N1ⁱ—Ni1—N3—N4	42.24 (13)	N25—Ni2—N23—C27	−40.3 (2)
N1—Ni1—N3—N4	−137.76 (13)	N25ⁱⁱ—Ni2—N23—C27	139.7 (2)
N5ⁱ—Ni1—N3—N4	135.66 (13)	N21—Ni2—N23—N24	42.61 (13)
N5—Ni1—N3—N4	−44.34 (13)	N21ⁱⁱ—Ni2—N23—N24	−137.39 (13)
C12—N3—N4—C14	0.2 (2)	N25—Ni2—N23—N24	137.07 (13)
Ni1—N3—N4—C14	−177.12 (12)	N25ⁱⁱ—Ni2—N23—N24	−42.93 (13)
C12—N3—N4—C16	179.07 (16)	C27—N23—N24—C29	−0.6 (2)
Ni1—N3—N4—C16	1.7 (2)	Ni2—N23—N24—C29	−178.77 (12)
N3—Ni1—N5—C7	−140.3 (2)	C27—N23—N24—C36ⁱⁱ	179.35 (16)
N3ⁱ—Ni1—N5—C7	39.7 (2)	Ni2—N23—N24—C36ⁱⁱ	1.1 (2)
N1ⁱ—Ni1—N5—C7	133.7 (2)	N21—Ni2—N25—C32	36.7 (2)
N1—Ni1—N5—C7	−46.3 (2)	N21ⁱⁱ—Ni2—N25—C32	−143.3 (2)
N3—Ni1—N5—N6	44.03 (12)	N23ⁱⁱ—Ni2—N25—C32	131.0 (2)
N3ⁱ—Ni1—N5—N6	−135.97 (12)	N23—Ni2—N25—C32	−49.0 (2)
N1ⁱ—Ni1—N5—N6	−41.99 (12)	N21—Ni2—N25—N26	−133.78 (13)
N1—Ni1—N5—N6	138.01 (12)	N21ⁱⁱ—Ni2—N25—N26	46.22 (13)
C7—N5—N6—C9	−1.1 (2)	N23ⁱⁱ—Ni2—N25—N26	−39.46 (13)
Ni1—N5—N6—C9	175.94 (12)	N23—Ni2—N25—N26	140.54 (13)
C7—N5—N6—C16	−177.99 (16)	C32—N25—N26—C34	−1.0 (2)
Ni1—N5—N6—C16	−0.90 (19)	Ni2—N25—N26—C34	172.49 (13)
N2—N1—C2—C3	0.6 (2)	C32—N25—N26—C36	−178.77 (16)
Ni1—N1—C2—C3	−179.13 (16)	Ni2—N25—N26—C36	−5.3 (2)
N2—N1—C2—C1	−178.3 (2)	N22—N21—C22—C23	0.4 (2)
Ni1—N1—C2—C1	2.0 (4)	Ni2—N21—C22—C23	176.63 (15)
N1—C2—C3—C4	−0.7 (3)	N22—N21—C22—C21	−179.50 (19)
C1—C2—C3—C4	178.1 (2)	Ni2—N21—C22—C21	−3.2 (3)
N1—N2—C4—C3	−0.2 (2)	N21—C22—C23—C24	−0.6 (2)
C16ⁱ—N2—C4—C3	−179.51 (18)	C21—C22—C23—C24	179.3 (2)
N1—N2—C4—C5	179.40 (19)	N21—N22—C24—C23	−0.3 (2)
C16ⁱ—N2—C4—C5	0.1 (3)	C36ⁱⁱ—N22—C24—C23	178.23 (17)
C2—C3—C4—N2	0.5 (2)	N21—N22—C24—C25	179.31 (19)
C2—C3—C4—C5	−179.0 (2)	C36ⁱⁱ—N22—C24—C25	−2.1 (3)
N6—N5—C7—C8	1.1 (2)	C22—C23—C24—N22	0.5 (2)
Ni1—N5—C7—C8	−174.92 (15)	C22—C23—C24—C25	−179.1 (2)
N6—N5—C7—C6	−178.7 (2)	N24—N23—C27—C28	0.3 (2)
Ni1—N5—C7—C6	5.3 (4)	Ni2—N23—C27—C28	177.90 (15)
N5—C7—C8—C9	−0.7 (2)	N24—N23—C27—C26	−178.92 (19)
C6—C7—C8—C9	179.1 (2)	Ni2—N23—C27—C26	−1.3 (3)
N5—N6—C9—C8	0.8 (2)	N23—C27—C28—C29	0.1 (2)
C16—N6—C9—C8	177.22 (17)	C26—C27—C28—C29	179.2 (2)
N5—N6—C9—C10	−179.96 (18)	C27—C28—C29—N24	−0.4 (2)
C16—N6—C9—C10	−3.5 (3)	C27—C28—C29—C30	−178.4 (2)
C7—C8—C9—N6	−0.1 (2)	N23—N24—C29—C28	0.6 (2)
C7—C8—C9—C10	−179.3 (2)	C36ⁱⁱ—N24—C29—C28	−179.29 (18)
N4—N3—C12—C13	0.1 (2)	N23—N24—C29—C30	178.81 (19)
Ni1—N3—C12—C13	176.51 (17)	C36ⁱⁱ—N24—C29—C30	−1.1 (3)
N4—N3—C12—C11	−179.9 (2)	N26—N25—C32—C33	0.9 (2)
Ni1—N3—C12—C11	−3.5 (4)	Ni2—N25—C32—C33	−170.26 (16)
N3—C12—C13—C14	−0.4 (3)	N26—N25—C32—C31	−179.7 (2)
C11—C12—C13—C14	179.6 (2)	Ni2—N25—C32—C31	9.1 (4)
N3—N4—C14—C13	−0.5 (2)	N25—C32—C33—C34	−0.5 (3)
C16—N4—C14—C13	−179.21 (18)	C31—C32—C33—C34	−179.9 (2)
N3—N4—C14—C15	−179.27 (19)	C32—C33—C34—N26	−0.1 (3)
C16—N4—C14—C15	2.0 (3)	C32—C33—C34—C35	177.6 (3)
C12—C13—C14—N4	0.5 (2)	N25—N26—C34—C33	0.7 (2)
C12—C13—C14—C15	179.2 (2)	C36—N26—C34—C33	178.20 (19)
C14—N4—C16—N2ⁱ	115.04 (19)	N25—N26—C34—C35	−177.3 (2)
N3—N4—C16—N2ⁱ	−63.6 (2)	C36—N26—C34—C35	0.2 (3)
C14—N4—C16—N6	−120.34 (19)	C34—N26—C36—N22ⁱⁱ	124.1 (2)
N3—N4—C16—N6	61.0 (2)	N25—N26—C36—N22ⁱⁱ	−58.5 (2)
C9—N6—C16—N2ⁱ	−113.14 (19)	C34—N26—C36—N24ⁱⁱ	−111.7 (2)
N5—N6—C16—N2ⁱ	63.10 (19)	N25—N26—C36—N24ⁱⁱ	65.7 (2)

Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+2, −y+1, −z.

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