A tetra­nuclear nickel(II) complex, [Ni₄(L)₄](ClO₄)₄·C₂H₃N·2H₂O, with an asymmetric Ni₄O₄ open-cubane-like core

A tetra­nuclear complex with an open-cubane like structure was synthesized from 2-meth­oxy-6-(pyridin-2-yl-hydrazonometh­yl)-phenol and characterized using micro-analytical and spectroscopic techniques, and single-crystal X-ray diffraction analysis.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.011 Å
• Disorder in solvent or counterion
• R factor = 0.048
• wR factor = 0.125
• Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D       H2BA     ..H1W1     .       2.09 Ang.
                                                      x,y,z  =      1_555 Check
PLAT417_ALERT_2_B Short Inter D-H..H-D       H2BA     ..H1W3     .       2.02 Ang.
                                                      x,y,z  =      1_555 Check
PLAT987_ALERT_1_B The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check

Alert level C
PLAT090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       7.56 Note
PLAT222_ALERT_3_C NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.5 Ratio
PLAT234_ALERT_4_C Large Hirshfeld Difference Cl4      --O44      .       0.19 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference Cl4      --O42A     .       0.18 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference Cl4      --O43A     .       0.18 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference Cl4      --O44A     .       0.21 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference Cl3      --O33A     .       0.20 Ang.
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of       C11S Check
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.1 Note
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.01124 Ang.
PLAT417_ALERT_2_C Short Inter D-H..H-D       H2BA     ..H1W4     .       2.12 Ang.
                                                      x,y,z  =      1_555 Check
PLAT480_ALERT_4_C Long H...A H-Bond Reported H8AA     ..O33      .       2.63 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H10B     ..O23A     .       2.64 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H3CA     ..O44      .       2.65 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1W2     ..O42      .       2.63 Ang.
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         40 Note
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         27 Report
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          4 Report
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       9.18 Why ?
PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records         20 Report
PLAT177_ALERT_4_G The CIF-Embedded .res File Contains DELU Records          3 Report
PLAT178_ALERT_4_G The CIF-Embedded .res File Contains SIMU Records          3 Report
PLAT186_ALERT_4_G The CIF-Embedded .res File Contains ISOR Records          4 Report
PLAT231_ALERT_4_G Hirshfeld Test (Solvent)   Cl4      --O42      .        6.3 s.u.
PLAT231_ALERT_4_G Hirshfeld Test (Solvent)   Cl3      --O32      .        7.1 s.u.
PLAT231_ALERT_4_G Hirshfeld Test (Solvent)   Cl3      --O33      .        9.5 s.u.
PLAT231_ALERT_4_G Hirshfeld Test (Solvent)   Cl3      --O32A     .        6.9 s.u.
PLAT244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl1 Check
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2  )        80% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  3  )        80% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  4  )        60% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  7  )       100% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  9  )       100% Note
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ..... (Resd  7  )       1.53 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ..... (Resd  9  )       1.47 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  O31      ..C10B             3.01 Ang.
                                          3/2-x,1/2+y,1/2+z  =      4_655 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  O32      ..C10D             2.97 Ang.
                                         3/2-x,-1/2+y,1/2+z  =      4_645 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  O43      ..C7D              2.81 Ang.
                                                      x,y,z  =      1_555 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  O41A     ..C5A              2.84 Ang.
                                             -1/2+x,3/2-y,z  =      3_465 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  O42A     ..C7D              2.77 Ang.
                                                      x,y,z  =      1_555 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  O43A     ..C8A              2.96 Ang.
                                             -1/2+x,3/2-y,z  =      3_465 Check
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........         39 Note
PLAT794_ALERT_5_G Tentative Bond Valency for Ni1       (II)      .       2.02 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Ni2       (II)      .       2.04 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Ni3       (II)      .       2.03 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Ni4       (II)      .       2.02 Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............        320 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          2 Note
PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          2 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   3 ALERT level B = A potentially serious problem, consider carefully
  17 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  35 ALERT level G = General information/check it is not something unexpected

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

---

Computing details

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXT (Sheldrick 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: SHELXTL (Sheldrick 2008); software used to prepare material for publication: SHELXTL (Sheldrick 2008).

cyclo-Tetrakis(µ-2-methoxy-6-{[2-(pyridin-2-yl)hydrazin-1-ylidene]methyl}phenolato)tetranickel(II) tetrakis(perchlorate) acetonitrile monosolvate dihydrate

Crystal data

[Ni4(C13H12N3O2)4](ClO4)4·C2H3N·2H2O	Dx = 1.785 Mg m^−3
Mr = 1678.75	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pna21	Cell parameters from 9461 reflections
a = 23.5976 (6) Å	θ = 2.4–26.3°
b = 11.8723 (3) Å	µ = 1.46 mm^−1
c = 22.2989 (6) Å	T = 100 K
V = 6247.2 (3) Å^3	Needle, green
Z = 4	0.25 × 0.11 × 0.09 mm
F(000) = 3432

Data collection

Bruker APEXII CCD diffractometer	11629 reflections with I > 2σ(I)
φ and ω scans	Rint = 0.068
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	θmax = 28.3°, θmin = 1.9°
Tmin = 0.554, Tmax = 0.765	h = −31→31
86241 measured reflections	k = −15→15
14617 independent reflections	l = −26→29

Refinement

Refinement on F^2	Hydrogen site location: mixed
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F^2 > 2σ(F^2)] = 0.048	w = 1/[σ^2(Fo^2) + (0.0571P)^2 + 9.1783P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.125	(Δ/σ)max = 0.001
S = 1.06	Δρmax = 0.84 e Å^−3
14617 reflections	Δρmin = −1.30 e Å^−3
1051 parameters	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
320 restraints	Extinction coefficient: 0.00135 (19)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack x determined using 4529 quotients [(I^+)-(I^-)]/[(I^+)+(I^-)] (Parsons et al., 2013)
Secondary atom site location: difference Fourier map	Absolute structure parameter: 0.024 (5)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ni1	0.73671 (3)	0.62167 (6)	0.50776 (4)	0.01973 (18)
Ni2	0.65087 (3)	0.46794 (6)	0.42646 (4)	0.01955 (17)
Ni3	0.58915 (3)	0.60905 (7)	0.53570 (4)	0.02116 (18)
Ni4	0.64341 (3)	0.75702 (6)	0.42586 (4)	0.02228 (18)
O1A	0.6789 (2)	0.7401 (4)	0.5065 (2)	0.0261 (10)
O2A	0.6144 (2)	0.9102 (4)	0.4796 (3)	0.0319 (12)
N1A	0.7519 (2)	0.6456 (5)	0.5919 (3)	0.0282 (13)
N2A	0.7897 (3)	0.5687 (5)	0.6153 (3)	0.0315 (13)
H2AA	0.797624	0.565969	0.653817	0.06 (3)*
N3A	0.7945 (2)	0.5026 (5)	0.5191 (3)	0.0251 (12)
C1A	0.6699 (3)	0.8175 (6)	0.5507 (3)	0.0259 (15)
C2A	0.6349 (3)	0.9109 (5)	0.5375 (4)	0.0284 (15)
C3A	0.6212 (4)	0.9884 (6)	0.5812 (4)	0.0383 (19)
H3AA	0.597016	1.049895	0.571891	0.046*
C4A	0.6423 (4)	0.9769 (7)	0.6381 (4)	0.045 (2)
H4AA	0.632679	1.030502	0.668040	0.054*
C5A	0.6775 (4)	0.8881 (7)	0.6523 (4)	0.0406 (19)
H5AA	0.692022	0.881058	0.691864	0.049*
C6A	0.6920 (3)	0.8081 (6)	0.6086 (3)	0.0302 (16)
C7A	0.5891 (4)	1.0134 (6)	0.4589 (4)	0.044 (2)
H7AA	0.612658	1.077293	0.471255	0.066*
H7AB	0.551164	1.021250	0.476297	0.066*
H7AC	0.586234	1.011904	0.415072	0.066*
C8A	0.7308 (3)	0.7216 (6)	0.6278 (3)	0.0311 (16)
H8AA	0.741612	0.719868	0.668851	0.037*
C9A	0.8139 (3)	0.4970 (6)	0.5750 (3)	0.0265 (15)
C10A	0.8565 (3)	0.4202 (7)	0.5921 (4)	0.0326 (17)
H10A	0.869548	0.417446	0.632430	0.039*
C11A	0.8782 (3)	0.3517 (7)	0.5509 (4)	0.0363 (18)
H11A	0.906120	0.298033	0.562076	0.044*
C12A	0.8601 (3)	0.3578 (6)	0.4908 (4)	0.0342 (17)
H12A	0.876312	0.310984	0.460768	0.041*
C13A	0.8179 (3)	0.4346 (6)	0.4770 (4)	0.0298 (15)
H13A	0.804979	0.439766	0.436785	0.036*
O1B	0.71137 (17)	0.5813 (3)	0.4250 (2)	0.0231 (9)
O2B	0.80171 (19)	0.7036 (4)	0.4463 (2)	0.0256 (10)
N1B	0.6495 (2)	0.4613 (5)	0.3398 (3)	0.0254 (13)
N2B	0.6028 (3)	0.4046 (5)	0.3185 (3)	0.0301 (13)
H2BA	0.594259	0.403529	0.280135	0.07 (4)*
N3B	0.5861 (2)	0.3646 (4)	0.4175 (3)	0.0252 (12)
C1B	0.7471 (3)	0.6010 (5)	0.3779 (3)	0.0239 (14)
C2B	0.7959 (3)	0.6656 (5)	0.3881 (3)	0.0240 (14)
C3B	0.8342 (3)	0.6893 (6)	0.3426 (3)	0.0272 (15)
H3BA	0.867365	0.732216	0.350462	0.033*
C4B	0.8230 (3)	0.6488 (6)	0.2849 (3)	0.0302 (15)
H4BA	0.849159	0.663339	0.253437	0.036*
C5B	0.7750 (3)	0.5886 (6)	0.2734 (3)	0.0282 (15)
H5BA	0.767612	0.563818	0.233670	0.034*
C6B	0.7361 (3)	0.5626 (6)	0.3195 (3)	0.0252 (14)
C7B	0.8561 (3)	0.7453 (7)	0.4645 (4)	0.0367 (18)
H7BA	0.865425	0.812932	0.441373	0.055*
H7BB	0.884944	0.687402	0.457407	0.055*
H7BC	0.855123	0.763956	0.507341	0.055*
C8B	0.6866 (3)	0.4975 (6)	0.3018 (3)	0.0260 (14)
H8BA	0.681397	0.480901	0.260520	0.031*
C9B	0.5706 (3)	0.3504 (6)	0.3597 (4)	0.0282 (15)
C10B	0.5229 (3)	0.2854 (6)	0.3442 (4)	0.0352 (17)
H10B	0.511292	0.278466	0.303583	0.042*
C11B	0.4938 (3)	0.2330 (6)	0.3886 (4)	0.0369 (19)
H11B	0.461388	0.188949	0.379192	0.044*
C12B	0.5115 (3)	0.2435 (6)	0.4488 (4)	0.0316 (16)
H12B	0.492177	0.204730	0.479900	0.038*
C13B	0.5568 (3)	0.3103 (5)	0.4614 (4)	0.0298 (16)
H13B	0.568312	0.319200	0.501973	0.036*
O1C	0.64418 (19)	0.4911 (4)	0.5149 (2)	0.0252 (10)
O2C	0.7018 (2)	0.3254 (4)	0.4662 (2)	0.0303 (11)
N1C	0.6018 (2)	0.5844 (5)	0.6203 (3)	0.0281 (13)
N2C	0.5735 (3)	0.6611 (5)	0.6559 (3)	0.0327 (14)
H2CA	0.575273	0.658689	0.695341	0.14 (6)*
N3C	0.5404 (2)	0.7317 (5)	0.5660 (3)	0.0270 (12)
C1C	0.6662 (3)	0.4124 (6)	0.5522 (3)	0.0253 (15)
C2C	0.6976 (3)	0.3228 (6)	0.5273 (4)	0.0299 (16)
C3C	0.7222 (3)	0.2412 (6)	0.5633 (4)	0.0367 (18)
H3CA	0.742965	0.181040	0.545793	0.044*
C4C	0.7164 (3)	0.2480 (7)	0.6254 (4)	0.0385 (19)
H4CA	0.733433	0.192783	0.650417	0.046*
C5C	0.6862 (3)	0.3341 (7)	0.6501 (4)	0.0364 (18)
H5CA	0.682536	0.337817	0.692492	0.044*
C6C	0.6602 (3)	0.4172 (6)	0.6149 (4)	0.0290 (15)
C7C	0.7241 (3)	0.2280 (6)	0.4358 (4)	0.041 (2)
H7CA	0.764599	0.220712	0.444534	0.062*
H7CB	0.718647	0.236542	0.392429	0.062*
H7CC	0.704131	0.160439	0.449638	0.062*
C8C	0.6291 (3)	0.5033 (6)	0.6458 (4)	0.0329 (17)
H8CA	0.628574	0.500392	0.688326	0.040*
C9C	0.5425 (3)	0.7411 (6)	0.6262 (4)	0.0315 (16)
C10C	0.5134 (3)	0.8263 (7)	0.6577 (4)	0.0387 (18)
H10C	0.516037	0.832498	0.700031	0.046*
C11C	0.4814 (4)	0.8989 (7)	0.6252 (5)	0.047 (2)
H11C	0.461404	0.957613	0.644892	0.056*
C12C	0.4776 (4)	0.8880 (7)	0.5629 (4)	0.0383 (18)
H12C	0.454778	0.938126	0.540173	0.046*
C13C	0.5076 (3)	0.8034 (6)	0.5351 (4)	0.0314 (15)
H13C	0.504959	0.795620	0.492831	0.038*
O1D	0.5854 (2)	0.6484 (4)	0.4489 (2)	0.0273 (11)
O2D	0.5083 (2)	0.5253 (4)	0.5041 (3)	0.0335 (11)
N1D	0.6176 (3)	0.7490 (5)	0.3430 (3)	0.0319 (14)
N2D	0.6544 (3)	0.7994 (6)	0.3044 (3)	0.0354 (15)
H2DA	0.650230	0.794969	0.265219	0.06 (3)*
N3D	0.7016 (3)	0.8547 (5)	0.3897 (3)	0.0287 (13)
C1D	0.5384 (3)	0.6181 (5)	0.4174 (4)	0.0278 (15)
C2D	0.4963 (3)	0.5530 (5)	0.4450 (3)	0.0276 (15)
C3D	0.4487 (3)	0.5165 (6)	0.4145 (4)	0.0330 (17)
H3DA	0.420861	0.472560	0.434478	0.040*
C4D	0.4418 (3)	0.5441 (7)	0.3551 (4)	0.0381 (18)
H4DA	0.408760	0.520128	0.334346	0.046*
C5D	0.4820 (3)	0.6059 (6)	0.3257 (4)	0.0365 (18)
H5DA	0.477119	0.623155	0.284384	0.044*
C6D	0.5309 (3)	0.6444 (6)	0.3562 (4)	0.0319 (16)
C7D	0.4621 (4)	0.4883 (7)	0.5406 (4)	0.045 (2)
H7DA	0.451192	0.411766	0.528798	0.067*
H7DB	0.429829	0.539144	0.535135	0.067*
H7DC	0.473691	0.488523	0.582776	0.067*
C8D	0.5718 (3)	0.7045 (6)	0.3210 (4)	0.0324 (16)
H8DA	0.564968	0.712128	0.279187	0.039*
C9D	0.6979 (3)	0.8568 (6)	0.3297 (4)	0.0333 (17)
C10D	0.7367 (4)	0.9166 (7)	0.2944 (4)	0.0397 (19)
H10D	0.734936	0.914895	0.251865	0.048*
C11D	0.7779 (4)	0.9786 (7)	0.3244 (5)	0.046 (2)
H11D	0.804852	1.020685	0.302010	0.056*
C12D	0.7801 (3)	0.9795 (6)	0.3863 (5)	0.042 (2)
H12D	0.807932	1.023129	0.406559	0.050*
C13D	0.7415 (3)	0.9164 (6)	0.4182 (4)	0.0342 (17)
H13D	0.742885	0.916202	0.460822	0.041*
Cl1	0.52002 (8)	0.25270 (17)	0.65520 (9)	0.0359 (4)
O11	0.4683 (2)	0.1969 (6)	0.6705 (3)	0.0526 (16)
O12	0.5136 (3)	0.3696 (5)	0.6678 (3)	0.0580 (18)
O13	0.5308 (4)	0.2377 (7)	0.5934 (3)	0.071 (2)
O14	0.5644 (3)	0.2096 (7)	0.6908 (3)	0.072 (2)
Cl2	0.64516 (10)	0.75422 (18)	0.80261 (10)	0.0462 (5)
O21	0.6408 (13)	0.711 (2)	0.8612 (9)	0.044 (6)	0.57 (6)
O22	0.6361 (18)	0.6641 (19)	0.7612 (13)	0.072 (8)	0.57 (6)
O23	0.6043 (10)	0.8369 (17)	0.7913 (11)	0.056 (6)	0.57 (6)
O24	0.7018 (7)	0.797 (3)	0.7964 (16)	0.097 (9)	0.57 (6)
O21A	0.6366 (17)	0.693 (3)	0.8554 (11)	0.053 (11)	0.43 (6)
O22A	0.6610 (18)	0.677 (2)	0.7558 (11)	0.053 (8)	0.43 (6)
O23A	0.5915 (12)	0.800 (5)	0.7822 (16)	0.081 (11)	0.43 (6)
O24A	0.685 (2)	0.838 (3)	0.8092 (13)	0.093 (12)	0.43 (6)
Cl3	0.86202 (15)	0.6242 (4)	0.76039 (17)	0.0898 (11)
O31	0.9121 (5)	0.6848 (11)	0.7412 (6)	0.144 (5)
O32	0.8498 (7)	0.5395 (12)	0.7231 (6)	0.064 (4)	0.512 (13)
O33	0.8143 (6)	0.7097 (13)	0.7581 (8)	0.074 (4)	0.512 (13)
O34	0.8732 (11)	0.598 (2)	0.8193 (7)	0.076 (5)	0.512 (13)
O32A	0.8836 (6)	0.4985 (11)	0.7347 (6)	0.057 (4)	0.488 (13)
O33A	0.8224 (7)	0.6441 (15)	0.7248 (7)	0.079 (4)	0.488 (13)
O34A	0.8626 (12)	0.610 (2)	0.8193 (7)	0.068 (5)	0.488 (13)
Cl4	0.32147 (12)	0.5162 (3)	0.59552 (15)	0.0719 (8)
O41	0.3017 (5)	0.4882 (10)	0.6510 (4)	0.076 (3)	0.806 (12)
O42	0.3541 (5)	0.6162 (7)	0.6010 (5)	0.063 (3)	0.806 (12)
O43	0.3553 (5)	0.4174 (9)	0.5809 (6)	0.092 (4)	0.806 (12)
O44	0.2846 (5)	0.5263 (11)	0.5485 (4)	0.087 (4)	0.806 (12)
O41A	0.2808 (14)	0.491 (4)	0.6390 (16)	0.099 (14)	0.194 (12)
O42A	0.3754 (9)	0.486 (4)	0.6243 (13)	0.106 (9)	0.194 (12)
O43A	0.3244 (17)	0.6325 (18)	0.5851 (18)	0.061 (8)	0.194 (12)
O44A	0.3147 (16)	0.457 (3)	0.5430 (13)	0.072 (9)	0.194 (12)
N1S	0.4678 (4)	0.9156 (9)	0.4038 (4)	0.075 (3)
C11S	0.4759 (4)	0.9363 (7)	0.3557 (5)	0.051 (2)
C12S	0.4883 (6)	0.9668 (10)	0.2935 (5)	0.071 (3)
H12E	0.529373	0.972979	0.288126	0.106*
H12F	0.470415	1.039174	0.284150	0.106*
H12G	0.473352	0.908563	0.266681	0.106*
O1W	0.5643 (5)	0.4311 (10)	0.2040 (5)	0.040 (4)	0.51 (2)
H1W1	0.538 (4)	0.468 (11)	0.2161 (18)	0.060*	0.51 (2)
H1W2	0.587 (6)	0.474 (11)	0.189 (9)	0.060*	0.51 (2)
O1WA	0.5995 (10)	0.3463 (16)	0.1981 (8)	0.096 (9)	0.49 (2)
H1W3	0.602 (13)	0.411 (14)	0.19 (2)	0.144*	0.49 (2)
H1W4	0.565 (3)	0.33 (2)	0.199 (5)	0.144*	0.49 (2)
O2W	0.6389 (3)	0.7126 (6)	0.1929 (3)	0.0547 (17)
H2W1	0.6042 (15)	0.712 (10)	0.185 (5)	0.082*
H2W2	0.651 (4)	0.670 (9)	0.167 (4)	0.082*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0225 (4)	0.0185 (4)	0.0181 (4)	0.0000 (3)	0.0010 (3)	−0.0011 (3)
Ni2	0.0213 (3)	0.0167 (3)	0.0207 (4)	−0.0003 (3)	0.0006 (4)	0.0004 (4)
Ni3	0.0231 (4)	0.0197 (4)	0.0206 (4)	0.0018 (3)	0.0008 (3)	0.0027 (3)
Ni4	0.0266 (4)	0.0175 (4)	0.0227 (4)	0.0018 (3)	0.0022 (4)	0.0019 (4)
O1A	0.031 (2)	0.018 (2)	0.029 (3)	0.0000 (18)	0.005 (2)	−0.003 (2)
O2A	0.034 (3)	0.020 (2)	0.042 (3)	0.008 (2)	0.005 (2)	0.004 (2)
N1A	0.027 (3)	0.029 (3)	0.029 (3)	−0.004 (2)	0.002 (2)	0.000 (3)
N2A	0.037 (3)	0.032 (3)	0.026 (3)	0.002 (3)	−0.002 (3)	0.005 (3)
N3A	0.026 (3)	0.024 (3)	0.025 (3)	−0.002 (2)	0.003 (2)	0.002 (2)
C1A	0.025 (3)	0.020 (3)	0.033 (4)	−0.003 (3)	0.006 (3)	−0.004 (3)
C2A	0.030 (3)	0.018 (3)	0.037 (4)	−0.006 (3)	0.010 (3)	−0.003 (3)
C3A	0.045 (4)	0.025 (4)	0.045 (5)	−0.004 (3)	0.014 (4)	−0.009 (3)
C4A	0.050 (5)	0.034 (4)	0.052 (6)	−0.006 (4)	0.016 (4)	−0.019 (4)
C5A	0.049 (5)	0.036 (4)	0.038 (5)	−0.007 (4)	0.008 (4)	−0.011 (4)
C6A	0.033 (4)	0.028 (3)	0.030 (4)	−0.006 (3)	0.005 (3)	−0.006 (3)
C7A	0.043 (4)	0.028 (4)	0.061 (6)	0.009 (3)	0.010 (4)	0.015 (4)
C8A	0.039 (4)	0.031 (4)	0.024 (4)	−0.008 (3)	0.002 (3)	−0.005 (3)
C9A	0.022 (3)	0.028 (3)	0.030 (4)	−0.008 (3)	0.004 (3)	0.004 (3)
C10A	0.025 (3)	0.038 (4)	0.035 (4)	0.002 (3)	−0.003 (3)	0.013 (3)
C11A	0.029 (4)	0.038 (4)	0.041 (5)	0.000 (3)	−0.006 (3)	0.011 (3)
C12A	0.034 (4)	0.027 (4)	0.042 (5)	0.002 (3)	0.002 (3)	−0.001 (3)
C13A	0.030 (4)	0.029 (4)	0.030 (4)	0.000 (3)	−0.002 (3)	0.002 (3)
O1B	0.026 (2)	0.024 (2)	0.019 (2)	0.0011 (17)	0.002 (2)	0.000 (2)
O2B	0.025 (2)	0.025 (2)	0.026 (3)	−0.0070 (19)	0.0051 (19)	−0.0003 (19)
N1B	0.027 (3)	0.022 (3)	0.028 (3)	−0.001 (2)	0.002 (2)	−0.001 (2)
N2B	0.029 (3)	0.036 (3)	0.025 (4)	−0.006 (3)	−0.001 (2)	0.000 (3)
N3B	0.028 (3)	0.018 (2)	0.030 (3)	0.003 (2)	0.002 (2)	0.000 (2)
C1B	0.024 (3)	0.019 (3)	0.029 (4)	0.003 (2)	0.004 (3)	−0.001 (3)
C2B	0.025 (3)	0.020 (3)	0.027 (4)	0.001 (3)	0.006 (3)	−0.002 (3)
C3B	0.029 (3)	0.029 (4)	0.024 (4)	0.000 (3)	0.005 (3)	−0.002 (3)
C4B	0.032 (4)	0.036 (4)	0.023 (4)	−0.001 (3)	0.010 (3)	0.003 (3)
C5B	0.035 (4)	0.029 (3)	0.020 (4)	−0.001 (3)	0.002 (3)	−0.004 (3)
C6B	0.031 (3)	0.021 (3)	0.024 (4)	0.000 (3)	0.003 (3)	0.002 (3)
C7B	0.029 (4)	0.043 (4)	0.038 (5)	−0.010 (3)	0.000 (3)	−0.010 (4)
C8B	0.031 (3)	0.023 (3)	0.025 (4)	0.003 (3)	0.003 (3)	−0.005 (3)
C9B	0.029 (3)	0.021 (3)	0.034 (4)	0.001 (3)	−0.001 (3)	−0.002 (3)
C10B	0.034 (4)	0.032 (4)	0.040 (5)	−0.004 (3)	−0.005 (3)	−0.011 (3)
C11B	0.024 (3)	0.025 (4)	0.062 (6)	−0.003 (3)	0.002 (4)	0.001 (4)
C12B	0.028 (3)	0.024 (3)	0.043 (5)	−0.001 (3)	−0.002 (3)	0.003 (3)
C13B	0.028 (3)	0.018 (3)	0.043 (5)	0.004 (3)	0.005 (3)	0.003 (3)
O1C	0.028 (2)	0.019 (2)	0.028 (3)	0.0025 (18)	−0.004 (2)	0.001 (2)
O2C	0.031 (3)	0.021 (2)	0.039 (3)	0.004 (2)	0.000 (2)	−0.002 (2)
N1C	0.028 (3)	0.026 (3)	0.030 (3)	−0.003 (2)	0.004 (3)	0.002 (3)
N2C	0.037 (3)	0.031 (3)	0.030 (4)	0.001 (3)	0.008 (3)	0.001 (3)
N3C	0.025 (3)	0.028 (3)	0.028 (3)	−0.003 (2)	0.003 (2)	0.001 (2)
C1C	0.021 (3)	0.025 (3)	0.031 (4)	−0.002 (2)	−0.002 (3)	0.005 (3)
C2C	0.025 (3)	0.025 (3)	0.040 (5)	−0.001 (3)	0.001 (3)	0.009 (3)
C3C	0.029 (4)	0.027 (4)	0.054 (5)	0.003 (3)	−0.001 (3)	0.008 (4)
C4C	0.038 (4)	0.035 (4)	0.043 (5)	0.000 (3)	−0.009 (4)	0.018 (4)
C5C	0.037 (4)	0.039 (4)	0.033 (4)	−0.004 (3)	−0.011 (3)	0.012 (3)
C6C	0.028 (3)	0.025 (3)	0.034 (4)	−0.007 (3)	−0.004 (3)	0.005 (3)
C7C	0.042 (4)	0.027 (4)	0.055 (6)	0.006 (3)	−0.002 (4)	−0.010 (4)
C8C	0.032 (4)	0.037 (4)	0.031 (4)	−0.010 (3)	−0.004 (3)	0.012 (3)
C9C	0.028 (3)	0.031 (4)	0.035 (5)	−0.004 (3)	0.005 (3)	0.004 (3)
C10C	0.044 (4)	0.042 (4)	0.031 (4)	0.010 (4)	0.016 (4)	0.000 (3)
C11C	0.039 (4)	0.047 (5)	0.053 (6)	0.012 (4)	0.015 (4)	−0.004 (4)
C12C	0.037 (4)	0.035 (4)	0.043 (5)	0.007 (3)	0.012 (4)	0.003 (4)
C13C	0.033 (4)	0.030 (4)	0.032 (4)	0.005 (3)	0.004 (3)	0.006 (3)
O1D	0.029 (2)	0.025 (2)	0.028 (3)	0.001 (2)	−0.005 (2)	0.002 (2)
O2D	0.030 (2)	0.032 (3)	0.038 (3)	−0.002 (2)	−0.002 (2)	0.006 (2)
N1D	0.038 (3)	0.028 (3)	0.030 (4)	0.004 (3)	0.006 (3)	0.006 (3)
N2D	0.037 (4)	0.043 (4)	0.027 (4)	0.000 (3)	0.003 (3)	0.009 (3)
N3D	0.039 (3)	0.018 (3)	0.030 (3)	0.004 (2)	0.004 (3)	0.001 (2)
C1D	0.030 (3)	0.021 (3)	0.032 (4)	0.008 (3)	−0.001 (3)	0.000 (3)
C2D	0.033 (4)	0.018 (3)	0.032 (4)	0.005 (3)	0.000 (3)	0.004 (3)
C3D	0.030 (3)	0.028 (3)	0.042 (5)	0.003 (3)	−0.005 (3)	−0.003 (3)
C4D	0.030 (4)	0.041 (4)	0.043 (5)	0.006 (3)	−0.009 (3)	−0.005 (4)
C5D	0.039 (4)	0.034 (4)	0.036 (5)	0.006 (3)	−0.013 (3)	0.002 (3)
C6D	0.036 (4)	0.025 (3)	0.034 (4)	0.005 (3)	−0.005 (3)	−0.002 (3)
C7D	0.045 (5)	0.037 (4)	0.053 (6)	−0.008 (4)	0.006 (4)	0.015 (4)
C8D	0.037 (4)	0.031 (4)	0.030 (4)	0.009 (3)	0.000 (3)	0.005 (3)
C9D	0.042 (4)	0.024 (3)	0.034 (4)	0.009 (3)	0.012 (3)	0.009 (3)
C10D	0.044 (5)	0.036 (4)	0.039 (5)	0.003 (4)	0.017 (4)	0.012 (4)
C11D	0.049 (5)	0.032 (4)	0.058 (6)	0.004 (4)	0.022 (4)	0.008 (4)
C12D	0.037 (4)	0.024 (4)	0.066 (6)	−0.001 (3)	0.007 (4)	−0.007 (4)
C13D	0.033 (4)	0.022 (3)	0.047 (5)	0.001 (3)	0.005 (4)	−0.004 (3)
Cl1	0.0321 (9)	0.0463 (10)	0.0294 (10)	0.0015 (8)	0.0001 (7)	0.0039 (8)
O11	0.037 (3)	0.063 (4)	0.058 (4)	−0.010 (3)	−0.002 (3)	0.007 (3)
O12	0.080 (5)	0.043 (3)	0.051 (4)	−0.009 (3)	−0.002 (4)	0.002 (3)
O13	0.091 (5)	0.081 (5)	0.040 (4)	0.010 (4)	0.022 (4)	−0.001 (4)
O14	0.039 (4)	0.099 (6)	0.076 (5)	0.015 (4)	−0.010 (3)	0.025 (4)
Cl2	0.0553 (12)	0.0398 (11)	0.0434 (13)	0.0063 (9)	0.0047 (10)	0.0041 (9)
O21	0.054 (12)	0.044 (9)	0.034 (9)	0.021 (8)	−0.004 (7)	−0.010 (7)
O22	0.114 (18)	0.054 (10)	0.049 (11)	0.039 (11)	−0.045 (11)	−0.015 (8)
O23	0.064 (10)	0.044 (9)	0.059 (11)	0.026 (7)	0.025 (8)	0.018 (7)
O24	0.066 (11)	0.115 (17)	0.110 (18)	−0.021 (11)	0.008 (10)	0.031 (14)
O21A	0.057 (15)	0.053 (16)	0.049 (16)	−0.011 (11)	−0.001 (12)	0.012 (13)
O22A	0.088 (18)	0.038 (10)	0.032 (10)	0.018 (10)	0.000 (11)	0.001 (7)
O23A	0.064 (13)	0.12 (2)	0.062 (15)	0.035 (15)	−0.011 (11)	0.040 (16)
O24A	0.15 (2)	0.074 (16)	0.056 (14)	−0.063 (16)	−0.006 (15)	−0.003 (11)
Cl3	0.076 (2)	0.126 (3)	0.067 (2)	−0.032 (2)	−0.0087 (16)	0.013 (2)
O31	0.114 (8)	0.178 (10)	0.139 (9)	−0.060 (8)	0.030 (7)	−0.013 (8)
O32	0.078 (7)	0.074 (7)	0.040 (6)	−0.002 (6)	−0.023 (6)	−0.005 (6)
O33	0.066 (7)	0.085 (8)	0.073 (8)	0.021 (7)	−0.024 (7)	−0.008 (7)
O34	0.080 (9)	0.085 (9)	0.062 (8)	−0.005 (8)	−0.043 (7)	−0.002 (7)
O32A	0.056 (7)	0.076 (8)	0.040 (7)	−0.010 (6)	−0.003 (6)	0.017 (6)
O33A	0.097 (8)	0.086 (8)	0.055 (7)	−0.004 (7)	−0.051 (6)	0.001 (6)
O34A	0.079 (10)	0.080 (8)	0.045 (7)	−0.005 (8)	−0.028 (7)	0.007 (6)
Cl4	0.0608 (15)	0.081 (2)	0.074 (2)	0.0103 (14)	0.0146 (14)	0.0152 (16)
O41	0.096 (8)	0.088 (6)	0.046 (6)	−0.016 (6)	−0.020 (5)	0.040 (5)
O42	0.087 (7)	0.044 (5)	0.060 (6)	−0.010 (5)	0.012 (5)	0.009 (4)
O43	0.101 (8)	0.068 (6)	0.108 (9)	0.017 (6)	0.031 (7)	0.010 (6)
O44	0.103 (8)	0.112 (9)	0.046 (6)	−0.010 (7)	−0.025 (6)	0.015 (6)
O41A	0.10 (2)	0.13 (2)	0.07 (2)	−0.014 (18)	0.021 (18)	0.032 (17)
O42A	0.118 (14)	0.098 (14)	0.103 (15)	0.008 (14)	−0.012 (14)	0.010 (13)
O43A	0.067 (15)	0.050 (14)	0.066 (15)	0.016 (13)	0.012 (14)	0.021 (12)
O44A	0.069 (15)	0.098 (16)	0.050 (14)	−0.005 (14)	−0.019 (13)	−0.014 (14)
N1S	0.091 (7)	0.084 (7)	0.050 (6)	−0.039 (6)	−0.019 (5)	0.029 (5)
C11S	0.060 (6)	0.035 (5)	0.058 (7)	−0.003 (4)	−0.017 (5)	−0.001 (4)
C12S	0.112 (10)	0.067 (7)	0.033 (6)	0.025 (7)	−0.003 (6)	−0.010 (5)
O1W	0.046 (7)	0.043 (7)	0.031 (7)	0.002 (5)	−0.003 (5)	0.001 (5)
O1WA	0.14 (2)	0.102 (17)	0.051 (12)	−0.052 (15)	0.027 (11)	−0.034 (11)
O2W	0.063 (4)	0.059 (4)	0.042 (4)	0.012 (4)	0.004 (3)	−0.012 (3)

Geometric parameters (Å, º)

Ni1—N1A	1.932 (7)	C1C—C6C	1.406 (11)
Ni1—O1A	1.960 (5)	C1C—C2C	1.410 (10)
Ni1—N3A	1.980 (6)	C2C—C3C	1.386 (10)
Ni1—O1B	1.998 (5)	C3C—C4C	1.393 (12)
Ni1—O2B	2.276 (4)	C3C—H3CA	0.9500
Ni2—N1B	1.935 (6)	C4C—C5C	1.363 (12)
Ni2—O1B	1.962 (4)	C4C—H4CA	0.9500
Ni2—N3B	1.971 (6)	C5C—C6C	1.401 (10)
Ni2—O1C	1.997 (5)	C5C—H5CA	0.9500
Ni2—O2C	2.257 (5)	C6C—C8C	1.434 (11)
Ni3—N1C	1.932 (7)	C7C—H7CA	0.9800
Ni3—O1C	1.965 (5)	C7C—H7CB	0.9800
Ni3—N3C	1.975 (6)	C7C—H7CC	0.9800
Ni3—O1D	1.993 (5)	C8C—H8CA	0.9500
Ni3—O2D	2.264 (5)	C9C—C10C	1.409 (11)
Ni4—N1D	1.948 (7)	C10C—C11C	1.355 (13)
Ni4—O1D	1.950 (5)	C10C—H10C	0.9500
Ni4—N3D	1.969 (6)	C11C—C12C	1.397 (13)
Ni4—O1A	1.993 (5)	C11C—H11C	0.9500
Ni4—O2A	2.283 (5)	C12C—C13C	1.375 (10)
O1A—C1A	1.365 (8)	C12C—H12C	0.9500
O2A—C2A	1.378 (10)	C13C—H13C	0.9500
O2A—C7A	1.439 (8)	O1D—C1D	1.360 (9)
N1A—C8A	1.305 (9)	O2D—C2D	1.387 (9)
N1A—N2A	1.377 (9)	O2D—C7D	1.429 (9)
N2A—C9A	1.364 (10)	N1D—C8D	1.300 (10)
N2A—H2AA	0.8800	N1D—N2D	1.362 (9)
N3A—C9A	1.330 (9)	N2D—C9D	1.355 (11)
N3A—C13A	1.356 (9)	N2D—H2DA	0.8800
C1A—C6A	1.396 (11)	N3D—C9D	1.341 (10)
C1A—C2A	1.414 (10)	N3D—C13D	1.351 (10)
C2A—C3A	1.379 (10)	C1D—C2D	1.403 (10)
C3A—C4A	1.370 (13)	C1D—C6D	1.410 (11)
C3A—H3AA	0.9500	C2D—C3D	1.383 (10)
C4A—C5A	1.378 (13)	C3D—C4D	1.373 (12)
C4A—H4AA	0.9500	C3D—H3DA	0.9500
C5A—C6A	1.403 (10)	C4D—C5D	1.368 (12)
C5A—H5AA	0.9500	C4D—H4DA	0.9500
C6A—C8A	1.441 (11)	C5D—C6D	1.416 (11)
C7A—H7AA	0.9800	C5D—H5DA	0.9500
C7A—H7AB	0.9800	C6D—C8D	1.433 (11)
C7A—H7AC	0.9800	C7D—H7DA	0.9800
C8A—H8AA	0.9500	C7D—H7DB	0.9800
C9A—C10A	1.411 (10)	C7D—H7DC	0.9800
C10A—C11A	1.330 (12)	C8D—H8DA	0.9500
C10A—H10A	0.9500	C9D—C10D	1.401 (11)
C11A—C12A	1.408 (12)	C10D—C11D	1.390 (13)
C11A—H11A	0.9500	C10D—H10D	0.9500
C12A—C13A	1.384 (10)	C11D—C12D	1.381 (14)
C12A—H12A	0.9500	C11D—H11D	0.9500
C13A—H13A	0.9500	C12D—C13D	1.380 (11)
O1B—C1B	1.367 (8)	C12D—H12D	0.9500
O2B—C2B	1.380 (8)	C13D—H13D	0.9500
O2B—C7B	1.435 (8)	Cl1—O14	1.409 (6)
N1B—C8B	1.292 (9)	Cl1—O13	1.413 (7)
N1B—N2B	1.377 (8)	Cl1—O12	1.424 (6)
N2B—C9B	1.353 (10)	Cl1—O11	1.429 (6)
N2B—H2BA	0.8800	Cl2—O24A	1.378 (18)
N3B—C9B	1.351 (10)	Cl2—O21A	1.397 (18)
N3B—C13B	1.360 (9)	Cl2—O23	1.399 (14)
C1B—C2B	1.402 (9)	Cl2—O21	1.405 (15)
C1B—C6B	1.404 (10)	Cl2—O22	1.430 (14)
C2B—C3B	1.387 (10)	Cl2—O22A	1.437 (17)
C3B—C4B	1.398 (10)	Cl2—O24	1.438 (14)
C3B—H3BA	0.9500	Cl2—O23A	1.449 (17)
C4B—C5B	1.364 (10)	Cl3—O33A	1.248 (12)
C4B—H4BA	0.9500	Cl3—O34A	1.326 (15)
C5B—C6B	1.414 (10)	Cl3—O32	1.336 (12)
C5B—H5BA	0.9500	Cl3—O34	1.377 (15)
C6B—C8B	1.453 (10)	Cl3—O31	1.448 (9)
C7B—H7BA	0.9800	Cl3—O33	1.517 (12)
C7B—H7BB	0.9800	Cl3—O32A	1.677 (14)
C7B—H7BC	0.9800	Cl4—O41	1.363 (9)
C8B—H8BA	0.9500	Cl4—O44	1.368 (9)
C9B—C10B	1.408 (10)	Cl4—O44A	1.38 (2)
C10B—C11B	1.356 (12)	Cl4—O41A	1.40 (2)
C10B—H10B	0.9500	Cl4—O43A	1.40 (2)
C11B—C12B	1.411 (12)	Cl4—O42	1.420 (9)
C11B—H11B	0.9500	Cl4—O43	1.457 (10)
C12B—C13B	1.360 (10)	Cl4—O42A	1.47 (2)
C12B—H12B	0.9500	N1S—C11S	1.117 (13)
C13B—H13B	0.9500	C11S—C12S	1.462 (15)
O1C—C1C	1.355 (8)	C12S—H12E	0.9800
O2C—C2C	1.368 (9)	C12S—H12F	0.9800
O2C—C7C	1.439 (9)	C12S—H12G	0.9800
N1C—C8C	1.290 (9)	O1W—H1W1	0.80 (3)
N1C—N2C	1.381 (9)	O1W—H1W2	0.82 (3)
N2C—C9C	1.371 (10)	O1WA—H1W3	0.82 (3)
N2C—H2CA	0.8800	O1WA—H1W4	0.82 (3)
N3C—C13C	1.341 (9)	O2W—H2W1	0.84 (3)
N3C—C9C	1.347 (10)	O2W—H2W2	0.83 (3)
N1A—Ni1—O1A	92.2 (2)	C8C—N1C—N2C	118.7 (7)
N1A—Ni1—N3A	81.6 (2)	C8C—N1C—Ni3	128.3 (6)
O1A—Ni1—N3A	173.5 (2)	N2C—N1C—Ni3	112.8 (5)
N1A—Ni1—O1B	171.2 (2)	C9C—N2C—N1C	115.9 (7)
O1A—Ni1—O1B	87.1 (2)	C9C—N2C—H2CA	122.1
N3A—Ni1—O1B	98.8 (2)	N1C—N2C—H2CA	122.1
N1A—Ni1—O2B	113.4 (2)	C13C—N3C—C9C	118.6 (6)
O1A—Ni1—O2B	98.83 (19)	C13C—N3C—Ni3	129.0 (5)
N3A—Ni1—O2B	85.3 (2)	C9C—N3C—Ni3	112.4 (5)
O1B—Ni1—O2B	75.39 (17)	O1C—C1C—C6C	123.0 (6)
N1B—Ni2—O1B	91.3 (2)	O1C—C1C—C2C	118.7 (7)
N1B—Ni2—N3B	82.0 (2)	C6C—C1C—C2C	118.3 (6)
O1B—Ni2—N3B	171.8 (2)	O2C—C2C—C3C	124.2 (7)
N1B—Ni2—O1C	172.1 (2)	O2C—C2C—C1C	114.4 (6)
O1B—Ni2—O1C	88.8 (2)	C3C—C2C—C1C	121.3 (8)
N3B—Ni2—O1C	97.1 (2)	C2C—C3C—C4C	119.6 (7)
N1B—Ni2—O2C	111.7 (2)	C2C—C3C—H3CA	120.2
O1B—Ni2—O2C	97.69 (18)	C4C—C3C—H3CA	120.2
N3B—Ni2—O2C	89.2 (2)	C5C—C4C—C3C	119.8 (7)
O1C—Ni2—O2C	76.02 (19)	C5C—C4C—H4CA	120.1
N1C—Ni3—O1C	91.2 (2)	C3C—C4C—H4CA	120.1
N1C—Ni3—N3C	82.4 (3)	C4C—C5C—C6C	122.0 (8)
O1C—Ni3—N3C	172.3 (2)	C4C—C5C—H5CA	119.0
N1C—Ni3—O1D	172.1 (2)	C6C—C5C—H5CA	119.0
O1C—Ni3—O1D	88.1 (2)	C5C—C6C—C1C	119.0 (7)
N3C—Ni3—O1D	97.7 (2)	C5C—C6C—C8C	117.2 (8)
N1C—Ni3—O2D	111.5 (2)	C1C—C6C—C8C	123.8 (7)
O1C—Ni3—O2D	99.81 (19)	O2C—C7C—H7CA	109.5
N3C—Ni3—O2D	86.5 (2)	O2C—C7C—H7CB	109.5
O1D—Ni3—O2D	76.3 (2)	H7CA—C7C—H7CB	109.5
N1D—Ni4—O1D	89.9 (2)	O2C—C7C—H7CC	109.5
N1D—Ni4—N3D	81.9 (3)	H7CA—C7C—H7CC	109.5
O1D—Ni4—N3D	170.6 (2)	H7CB—C7C—H7CC	109.5
N1D—Ni4—O1A	169.1 (2)	N1C—C8C—C6C	125.2 (7)
O1D—Ni4—O1A	89.5 (2)	N1C—C8C—H8CA	117.4
N3D—Ni4—O1A	97.8 (2)	C6C—C8C—H8CA	117.4
N1D—Ni4—O2A	116.3 (2)	N3C—C9C—N2C	116.4 (7)
O1D—Ni4—O2A	100.3 (2)	N3C—C9C—C10C	122.5 (7)
N3D—Ni4—O2A	87.4 (2)	N2C—C9C—C10C	121.1 (7)
O1A—Ni4—O2A	74.5 (2)	C11C—C10C—C9C	117.5 (8)
C1A—O1A—Ni1	125.5 (4)	C11C—C10C—H10C	121.3
C1A—O1A—Ni4	121.3 (4)	C9C—C10C—H10C	121.3
Ni1—O1A—Ni4	112.2 (2)	C10C—C11C—C12C	120.5 (8)
C2A—O2A—C7A	116.2 (6)	C10C—C11C—H11C	119.7
C2A—O2A—Ni4	113.0 (4)	C12C—C11C—H11C	119.7
C7A—O2A—Ni4	129.4 (5)	C13C—C12C—C11C	118.8 (8)
C8A—N1A—N2A	118.3 (7)	C13C—C12C—H12C	120.6
C8A—N1A—Ni1	128.8 (5)	C11C—C12C—H12C	120.6
N2A—N1A—Ni1	112.9 (5)	N3C—C13C—C12C	122.0 (8)
C9A—N2A—N1A	115.8 (6)	N3C—C13C—H13C	119.0
C9A—N2A—H2AA	122.1	C12C—C13C—H13C	119.0
N1A—N2A—H2AA	122.1	C1D—O1D—Ni4	127.6 (5)
C9A—N3A—C13A	118.5 (6)	C1D—O1D—Ni3	118.5 (4)
C9A—N3A—Ni1	113.1 (5)	Ni4—O1D—Ni3	112.3 (2)
C13A—N3A—Ni1	128.2 (5)	C2D—O2D—C7D	117.2 (6)
O1A—C1A—C6A	123.8 (6)	C2D—O2D—Ni3	111.3 (4)
O1A—C1A—C2A	117.9 (7)	C7D—O2D—Ni3	126.9 (5)
C6A—C1A—C2A	118.3 (6)	C8D—N1D—N2D	118.1 (7)
O2A—C2A—C3A	125.7 (7)	C8D—N1D—Ni4	129.7 (5)
O2A—C2A—C1A	113.3 (6)	N2D—N1D—Ni4	112.2 (5)
C3A—C2A—C1A	120.8 (8)	C9D—N2D—N1D	116.1 (7)
C4A—C3A—C2A	120.2 (8)	C9D—N2D—H2DA	121.9
C4A—C3A—H3AA	119.9	N1D—N2D—H2DA	121.9
C2A—C3A—H3AA	119.9	C9D—N3D—C13D	120.3 (7)
C3A—C4A—C5A	120.5 (8)	C9D—N3D—Ni4	112.0 (5)
C3A—C4A—H4AA	119.7	C13D—N3D—Ni4	127.7 (6)
C5A—C4A—H4AA	119.7	O1D—C1D—C2D	119.7 (7)
C4A—C5A—C6A	120.3 (9)	O1D—C1D—C6D	122.9 (6)
C4A—C5A—H5AA	119.8	C2D—C1D—C6D	117.2 (7)
C6A—C5A—H5AA	119.8	C3D—C2D—O2D	124.0 (6)
C1A—C6A—C5A	119.8 (7)	C3D—C2D—C1D	122.2 (7)
C1A—C6A—C8A	124.7 (6)	O2D—C2D—C1D	113.8 (6)
C5A—C6A—C8A	115.5 (7)	C4D—C3D—C2D	119.8 (7)
O2A—C7A—H7AA	109.5	C4D—C3D—H3DA	120.1
O2A—C7A—H7AB	109.5	C2D—C3D—H3DA	120.1
H7AA—C7A—H7AB	109.5	C5D—C4D—C3D	120.5 (7)
O2A—C7A—H7AC	109.5	C5D—C4D—H4DA	119.7
H7AA—C7A—H7AC	109.5	C3D—C4D—H4DA	119.7
H7AB—C7A—H7AC	109.5	C4D—C5D—C6D	120.5 (8)
N1A—C8A—C6A	123.6 (7)	C4D—C5D—H5DA	119.7
N1A—C8A—H8AA	118.2	C6D—C5D—H5DA	119.7
C6A—C8A—H8AA	118.2	C1D—C6D—C5D	119.8 (7)
N3A—C9A—N2A	116.2 (6)	C1D—C6D—C8D	123.8 (7)
N3A—C9A—C10A	122.2 (7)	C5D—C6D—C8D	116.4 (7)
N2A—C9A—C10A	121.6 (7)	O2D—C7D—H7DA	109.5
C11A—C10A—C9A	118.8 (8)	O2D—C7D—H7DB	109.5
C11A—C10A—H10A	120.6	H7DA—C7D—H7DB	109.5
C9A—C10A—H10A	120.6	O2D—C7D—H7DC	109.5
C10A—C11A—C12A	120.7 (7)	H7DA—C7D—H7DC	109.5
C10A—C11A—H11A	119.6	H7DB—C7D—H7DC	109.5
C12A—C11A—H11A	119.6	N1D—C8D—C6D	123.7 (7)
C13A—C12A—C11A	117.5 (7)	N1D—C8D—H8DA	118.2
C13A—C12A—H12A	121.2	C6D—C8D—H8DA	118.2
C11A—C12A—H12A	121.2	N3D—C9D—N2D	117.1 (7)
N3A—C13A—C12A	122.2 (7)	N3D—C9D—C10D	121.9 (8)
N3A—C13A—H13A	118.9	N2D—C9D—C10D	121.0 (8)
C12A—C13A—H13A	118.9	C11D—C10D—C9D	117.1 (8)
C1B—O1B—Ni2	125.4 (4)	C11D—C10D—H10D	121.5
C1B—O1B—Ni1	118.9 (4)	C9D—C10D—H10D	121.5
Ni2—O1B—Ni1	111.5 (2)	C12D—C11D—C10D	120.7 (8)
C2B—O2B—C7B	117.9 (5)	C12D—C11D—H11D	119.6
C2B—O2B—Ni1	111.1 (4)	C10D—C11D—H11D	119.6
C7B—O2B—Ni1	125.4 (4)	C13D—C12D—C11D	119.1 (8)
C8B—N1B—N2B	118.7 (6)	C13D—C12D—H12D	120.4
C8B—N1B—Ni2	129.1 (5)	C11D—C12D—H12D	120.4
N2B—N1B—Ni2	112.1 (4)	N3D—C13D—C12D	120.8 (9)
C9B—N2B—N1B	116.7 (6)	N3D—C13D—H13D	119.6
C9B—N2B—H2BA	121.7	C12D—C13D—H13D	119.6
N1B—N2B—H2BA	121.7	O14—Cl1—O13	111.7 (5)
C9B—N3B—C13B	119.4 (6)	O14—Cl1—O12	108.8 (5)
C9B—N3B—Ni2	112.6 (5)	O13—Cl1—O12	109.5 (4)
C13B—N3B—Ni2	128.0 (5)	O14—Cl1—O11	109.3 (4)
O1B—C1B—C2B	118.5 (6)	O13—Cl1—O11	109.1 (5)
O1B—C1B—C6B	122.7 (6)	O12—Cl1—O11	108.3 (4)
C2B—C1B—C6B	118.8 (6)	O24A—Cl2—O21A	112.5 (17)
O2B—C2B—C3B	123.8 (6)	O23—Cl2—O21	111.8 (11)
O2B—C2B—C1B	114.3 (6)	O23—Cl2—O22	107.8 (11)
C3B—C2B—C1B	121.8 (7)	O21—Cl2—O22	108.6 (13)
C2B—C3B—C4B	118.7 (7)	O24A—Cl2—O22A	111.1 (14)
C2B—C3B—H3BA	120.6	O21A—Cl2—O22A	108.6 (16)
C4B—C3B—H3BA	120.6	O23—Cl2—O24	112.1 (12)
C5B—C4B—C3B	120.7 (7)	O21—Cl2—O24	106.6 (13)
C5B—C4B—H4BA	119.7	O22—Cl2—O24	109.9 (12)
C3B—C4B—H4BA	119.7	O24A—Cl2—O23A	111.2 (15)
C4B—C5B—C6B	121.2 (7)	O21A—Cl2—O23A	109.4 (17)
C4B—C5B—H5BA	119.4	O22A—Cl2—O23A	103.7 (15)
C6B—C5B—H5BA	119.4	O33A—Cl3—O34A	131.5 (15)
C1B—C6B—C5B	118.8 (6)	O32—Cl3—O34	117.6 (13)
C1B—C6B—C8B	125.1 (6)	O33A—Cl3—O31	109.2 (10)
C5B—C6B—C8B	116.1 (6)	O34A—Cl3—O31	110.4 (13)
O2B—C7B—H7BA	109.5	O32—Cl3—O31	111.5 (9)
O2B—C7B—H7BB	109.5	O34—Cl3—O31	103.8 (12)
H7BA—C7B—H7BB	109.5	O32—Cl3—O33	108.8 (9)
O2B—C7B—H7BC	109.5	O34—Cl3—O33	109.1 (13)
H7BA—C7B—H7BC	109.5	O31—Cl3—O33	105.3 (8)
H7BB—C7B—H7BC	109.5	O33A—Cl3—O32A	100.3 (10)
N1B—C8B—C6B	122.9 (7)	O34A—Cl3—O32A	102.7 (13)
N1B—C8B—H8BA	118.6	O31—Cl3—O32A	95.4 (7)
C6B—C8B—H8BA	118.6	O41—Cl4—O44	120.0 (7)
N3B—C9B—N2B	115.9 (6)	O44A—Cl4—O41A	114 (2)
N3B—C9B—C10B	121.2 (7)	O44A—Cl4—O43A	111.8 (18)
N2B—C9B—C10B	122.9 (7)	O41A—Cl4—O43A	111 (2)
C11B—C10B—C9B	118.5 (8)	O41—Cl4—O42	108.1 (7)
C11B—C10B—H10B	120.7	O44—Cl4—O42	109.7 (7)
C9B—C10B—H10B	120.7	O41—Cl4—O43	101.2 (7)
C10B—C11B—C12B	120.2 (7)	O44—Cl4—O43	104.3 (8)
C10B—C11B—H11B	119.9	O42—Cl4—O43	113.3 (7)
C12B—C11B—H11B	119.9	O44A—Cl4—O42A	110.2 (17)
C13B—C12B—C11B	118.8 (7)	O41A—Cl4—O42A	104.0 (18)
C13B—C12B—H12B	120.6	O43A—Cl4—O42A	105.6 (18)
C11B—C12B—H12B	120.6	N1S—C11S—C12S	177.7 (12)
C12B—C13B—N3B	121.7 (8)	C11S—C12S—H12E	109.5
C12B—C13B—H13B	119.1	C11S—C12S—H12F	109.5
N3B—C13B—H13B	119.1	H12E—C12S—H12F	109.5
C1C—O1C—Ni3	126.9 (5)	C11S—C12S—H12G	109.5
C1C—O1C—Ni2	118.8 (4)	H12E—C12S—H12G	109.5
Ni3—O1C—Ni2	112.6 (2)	H12F—C12S—H12G	109.5
C2C—O2C—C7C	118.5 (6)	H1W1—O1W—H1W2	107 (5)
C2C—O2C—Ni2	111.7 (4)	H1W3—O1WA—H1W4	108 (5)
C7C—O2C—Ni2	127.8 (5)	H2W1—O2W—H2W2	102 (4)
C8A—N1A—N2A—C9A	−174.9 (6)	C8C—N1C—N2C—C9C	−176.2 (6)
Ni1—N1A—N2A—C9A	6.2 (7)	Ni3—N1C—N2C—C9C	−0.8 (7)
Ni1—O1A—C1A—C6A	−14.8 (9)	Ni3—O1C—C1C—C6C	−12.1 (9)
Ni4—O1A—C1A—C6A	177.7 (5)	Ni2—O1C—C1C—C6C	−175.5 (5)
Ni1—O1A—C1A—C2A	167.0 (4)	Ni3—O1C—C1C—C2C	169.2 (5)
Ni4—O1A—C1A—C2A	−0.5 (8)	Ni2—O1C—C1C—C2C	5.8 (8)
C7A—O2A—C2A—C3A	17.2 (10)	C7C—O2C—C2C—C3C	11.8 (10)
Ni4—O2A—C2A—C3A	−175.2 (6)	Ni2—O2C—C2C—C3C	176.9 (6)
C7A—O2A—C2A—C1A	−166.9 (6)	C7C—O2C—C2C—C1C	−169.2 (6)
Ni4—O2A—C2A—C1A	0.8 (7)	Ni2—O2C—C2C—C1C	−4.1 (7)
O1A—C1A—C2A—O2A	−0.2 (8)	O1C—C1C—C2C—O2C	−0.5 (9)
C6A—C1A—C2A—O2A	−178.6 (6)	C6C—C1C—C2C—O2C	−179.3 (6)
O1A—C1A—C2A—C3A	175.9 (6)	O1C—C1C—C2C—C3C	178.5 (6)
C6A—C1A—C2A—C3A	−2.4 (10)	C6C—C1C—C2C—C3C	−0.3 (10)
O2A—C2A—C3A—C4A	176.9 (7)	O2C—C2C—C3C—C4C	178.5 (7)
C1A—C2A—C3A—C4A	1.2 (11)	C1C—C2C—C3C—C4C	−0.5 (11)
C2A—C3A—C4A—C5A	0.1 (12)	C2C—C3C—C4C—C5C	0.6 (12)
C3A—C4A—C5A—C6A	−0.2 (12)	C3C—C4C—C5C—C6C	0.1 (12)
O1A—C1A—C6A—C5A	−175.9 (6)	C4C—C5C—C6C—C1C	−0.8 (11)
C2A—C1A—C6A—C5A	2.3 (10)	C4C—C5C—C6C—C8C	179.5 (7)
O1A—C1A—C6A—C8A	5.5 (11)	O1C—C1C—C6C—C5C	−177.8 (6)
C2A—C1A—C6A—C8A	−176.2 (6)	C2C—C1C—C6C—C5C	0.9 (10)
C4A—C5A—C6A—C1A	−1.1 (11)	O1C—C1C—C6C—C8C	1.8 (10)
C4A—C5A—C6A—C8A	177.6 (7)	C2C—C1C—C6C—C8C	−179.5 (6)
N2A—N1A—C8A—C6A	178.6 (6)	N2C—N1C—C8C—C6C	179.8 (6)
Ni1—N1A—C8A—C6A	−2.7 (11)	Ni3—N1C—C8C—C6C	5.2 (10)
C1A—C6A—C8A—N1A	3.8 (11)	C5C—C6C—C8C—N1C	−178.4 (7)
C5A—C6A—C8A—N1A	−174.8 (7)	C1C—C6C—C8C—N1C	1.9 (11)
C13A—N3A—C9A—N2A	178.7 (6)	C13C—N3C—C9C—N2C	175.7 (6)
Ni1—N3A—C9A—N2A	2.9 (7)	Ni3—N3C—C9C—N2C	−4.9 (8)
C13A—N3A—C9A—C10A	−2.2 (10)	C13C—N3C—C9C—C10C	−2.6 (10)
Ni1—N3A—C9A—C10A	−178.0 (5)	Ni3—N3C—C9C—C10C	176.8 (6)
N1A—N2A—C9A—N3A	−6.0 (9)	N1C—N2C—C9C—N3C	3.9 (9)
N1A—N2A—C9A—C10A	174.9 (6)	N1C—N2C—C9C—C10C	−177.8 (7)
N3A—C9A—C10A—C11A	0.4 (11)	N3C—C9C—C10C—C11C	1.4 (12)
N2A—C9A—C10A—C11A	179.4 (7)	N2C—C9C—C10C—C11C	−176.8 (7)
C9A—C10A—C11A—C12A	1.9 (11)	C9C—C10C—C11C—C12C	0.4 (13)
C10A—C11A—C12A—C13A	−2.2 (11)	C10C—C11C—C12C—C13C	−1.0 (13)
C9A—N3A—C13A—C12A	1.8 (10)	C9C—N3C—C13C—C12C	2.0 (10)
Ni1—N3A—C13A—C12A	176.9 (5)	Ni3—N3C—C13C—C12C	−177.3 (6)
C11A—C12A—C13A—N3A	0.4 (11)	C11C—C12C—C13C—N3C	−0.3 (12)
C8B—N1B—N2B—C9B	168.2 (6)	C8D—N1D—N2D—C9D	172.1 (6)
Ni2—N1B—N2B—C9B	−8.9 (7)	Ni4—N1D—N2D—C9D	−7.5 (8)
Ni2—O1B—C1B—C2B	−165.5 (4)	Ni4—O1D—C1D—C2D	−169.2 (4)
Ni1—O1B—C1B—C2B	−10.6 (7)	Ni3—O1D—C1D—C2D	−5.0 (8)
Ni2—O1B—C1B—C6B	16.7 (9)	Ni4—O1D—C1D—C6D	14.1 (9)
Ni1—O1B—C1B—C6B	171.7 (5)	Ni3—O1D—C1D—C6D	178.3 (5)
C7B—O2B—C2B—C3B	−16.1 (10)	C7D—O2D—C2D—C3D	−20.3 (10)
Ni1—O2B—C2B—C3B	−171.2 (5)	Ni3—O2D—C2D—C3D	−178.1 (5)
C7B—O2B—C2B—C1B	164.7 (6)	C7D—O2D—C2D—C1D	162.5 (6)
Ni1—O2B—C2B—C1B	9.6 (7)	Ni3—O2D—C2D—C1D	4.7 (7)
O1B—C1B—C2B—O2B	−0.7 (9)	O1D—C1D—C2D—C3D	−177.7 (6)
C6B—C1B—C2B—O2B	177.2 (6)	C6D—C1D—C2D—C3D	−0.8 (9)
O1B—C1B—C2B—C3B	−179.9 (6)	O1D—C1D—C2D—O2D	−0.4 (9)
C6B—C1B—C2B—C3B	−2.1 (10)	C6D—C1D—C2D—O2D	176.5 (6)
O2B—C2B—C3B—C4B	−178.2 (6)	O2D—C2D—C3D—C4D	−177.0 (7)
C1B—C2B—C3B—C4B	1.0 (10)	C1D—C2D—C3D—C4D	0.0 (10)
C2B—C3B—C4B—C5B	1.0 (11)	C2D—C3D—C4D—C5D	1.0 (11)
C3B—C4B—C5B—C6B	−1.9 (11)	C3D—C4D—C5D—C6D	−1.3 (12)
O1B—C1B—C6B—C5B	178.9 (6)	O1D—C1D—C6D—C5D	177.3 (6)
C2B—C1B—C6B—C5B	1.1 (10)	C2D—C1D—C6D—C5D	0.5 (10)
O1B—C1B—C6B—C8B	−0.5 (10)	O1D—C1D—C6D—C8D	0.6 (11)
C2B—C1B—C6B—C8B	−178.3 (6)	C2D—C1D—C6D—C8D	−176.2 (6)
C4B—C5B—C6B—C1B	0.8 (11)	C4D—C5D—C6D—C1D	0.5 (11)
C4B—C5B—C6B—C8B	−179.7 (7)	C4D—C5D—C6D—C8D	177.5 (7)
N2B—N1B—C8B—C6B	177.2 (6)	N2D—N1D—C8D—C6D	177.0 (7)
Ni2—N1B—C8B—C6B	−6.3 (10)	Ni4—N1D—C8D—C6D	−3.5 (11)
C1B—C6B—C8B—N1B	−5.2 (11)	C1D—C6D—C8D—N1D	−6.1 (11)
C5B—C6B—C8B—N1B	175.3 (6)	C5D—C6D—C8D—N1D	177.1 (7)
C13B—N3B—C9B—N2B	−178.2 (6)	C13D—N3D—C9D—N2D	−175.4 (6)
Ni2—N3B—C9B—N2B	2.5 (7)	Ni4—N3D—C9D—N2D	3.8 (8)
C13B—N3B—C9B—C10B	3.5 (10)	C13D—N3D—C9D—C10D	3.8 (10)
Ni2—N3B—C9B—C10B	−175.8 (5)	Ni4—N3D—C9D—C10D	−177.0 (6)
N1B—N2B—C9B—N3B	4.2 (9)	N1D—N2D—C9D—N3D	2.5 (10)
N1B—N2B—C9B—C10B	−177.5 (6)	N1D—N2D—C9D—C10D	−176.8 (7)
N3B—C9B—C10B—C11B	−2.8 (11)	N3D—C9D—C10D—C11D	−3.0 (11)
N2B—C9B—C10B—C11B	179.1 (7)	N2D—C9D—C10D—C11D	176.2 (7)
C9B—C10B—C11B—C12B	−0.2 (11)	C9D—C10D—C11D—C12D	0.4 (12)
C10B—C11B—C12B—C13B	2.4 (11)	C10D—C11D—C12D—C13D	1.2 (12)
C11B—C12B—C13B—N3B	−1.6 (10)	C9D—N3D—C13D—C12D	−2.1 (10)
C9B—N3B—C13B—C12B	−1.3 (9)	Ni4—N3D—C13D—C12D	178.9 (5)
Ni2—N3B—C13B—C12B	177.9 (5)	C11D—C12D—C13D—N3D	−0.4 (11)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C7B—H7BB···N1S^i	0.98	2.60	3.523 (11)	157
C13B—H13B···O13	0.95	2.42	3.126 (9)	131
C13C—H13C···N1S	0.95	2.59	3.348 (11)	137
N2D—H2DA···O2W	0.88	1.91	2.720 (9)	152
C7D—H7DC···O12	0.98	2.56	3.389 (10)	142
C12S—H12G···O14^ii	0.98	2.37	3.335 (12)	168
O2W—H2W1···O11^ii	0.84 (3)	2.12 (7)	2.795 (8)	138 (9)
O2W—H2W2···Cl4^ii	0.83 (3)	2.78 (3)	3.599 (6)	170 (9)

Symmetry codes: (i) x+1/2, −y+3/2, z; (ii) −x+1, −y+1, z−1/2.