A 2D coordination polymer assembled from a nickel(II) tetra­aza­macrocyclic cation and 4,4′-(di­methyl­silanedi­yl)diphthalate(3–) linker

The preformed nickel(II) com­plex of the 14-membered macrocyclic ligand 1,4,8,11-tetra­aza­cyclo­tetra­decane (cyclam, L), when treated with 4,4′-(di­methyl­silanedi­yl)diphthalic acid (H₄A) in a DMF/H₂O mixture (4:1 v/v) under heating, leads to [Ni(L)]₃(HA)₂·3DMF (I·DMF). Redissolution of this com­pound in a DMF/H₂O/MeOH mixture (4:1:30 v/v/v) with mild acidification under gentle heating results in the formation of a similar com­pound but containing water and methanol mol­ecules of crystallization, [Ni(L)]₃(HA)₂·5H₂O·2MeOH (II·H₂O). At lower temperature and concentration of reactants and longer reaction time, single crystals of com­position {[{Ni(L)}₃(HA)₂]·4CH₃OH}_n (II·MeOH) were isolated. Single-crystal X-ray diffraction analysis of this com­pound, which, according to PXRD is isostructural with II·H₂O but different from I·DMF, revealed its two-dimensional (2D) polymeric structure, i.e. poly[[bis­{μ₃-4-[(4-carb­oxy-3-carboxyl­atophen­yl)di­methyl­sil­yl]benzene-1,2-di­carboxyl­ato-κ³O¹:O²:O^3′}­tris­(1,4,8,11-tetra­aza­cyclo­tetra­decane-κ⁴N)trinickel(II)] methanol tetra­solvate], {[Ni₃(C₁₈H₁₃O₈Si)₂(C₁₀H₂₄N₄)₃]·4CH₃OH}_n. It is built up of the monoprotonated tricarboxyl­ate HA³⁻ ligand coordinated in a monodentate manner in the axial positions of two crystallographically independent Ni^II cations, one of which is located on a crystallographic inversion centre. Both metal ions adopt a slightly tetra­gonally elongated trans-N₄O₂ octa­hedral geometry. The com­pound has a lamellar structure with polymeric layers oriented parallel to the (10) plane, which are in turn linked via hydrogen bonds involving protonated carb­oxy­lic acid groups of the ligand. Bulk com­pounds I·DMF and II·H₂O were characterized by FT–IR and diffuse reflectance spectroscopy and thermogravimetry, which provide evidence of their structural differences.

Computing details

Data collection: CrysAlis PRO (Agilent, 2014); cell refinement: CrysAlis PRO (Agilent, 2014); data reduction: CrysAlis PRP (Agilent, 2014); program(s) used to solve structure: OLEX2 (Dolomanov et al., 2009); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: publCIF (Westrip, 2010) and PLATON (Spek, 2020).

Poly[[bis{µ₃-4-[(4-carboxy-3-carboxylatophenyl)dimethylsilyl]benzene-1,2-dicarboxylato-κ³O¹:O²:O^3'}-tris(1,4,8,11-tetraazacyclotetradecane-κ⁴N)trinickel(II)] methanol tetrasolvate]

Crystal data

[Ni3(C18H13O8Si)2(C10H24N4)3]·4CH4O	F(000) = 1780
Mr = 1676.04	Dx = 1.362 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 13.5400 (7) Å	Cell parameters from 3580 reflections
b = 14.0473 (6) Å	θ = 1.9–26.3°
c = 22.0478 (12) Å	µ = 0.79 mm^−1
β = 102.895 (5)°	T = 160 K
V = 4087.7 (4) Å^3	Irregular, light violet
Z = 2	0.25 × 0.10 × 0.03 mm

Data collection

Agilent Xcalibur Eos diffractometer	5410 reflections with I > 2σ(I)
Detector resolution: 8.0797 pixels mm^-1	Rint = 0.062
ω scans	θmax = 26.0°, θmin = 1.7°
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2014)	h = −16→16
Tmin = 0.898, Tmax = 1.000	k = −17→17
20822 measured reflections	l = −27→17
8041 independent reflections

Refinement

Refinement on F^2	141 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.068	H-atom parameters constrained
wR(F^2) = 0.130	w = 1/[σ^2(Fo^2) + (0.0379P)^2 + 4.0667P] where P = (Fo^2 + 2Fc^2)/3
S = 1.05	(Δ/σ)max < 0.001
8041 reflections	Δρmax = 0.64 e Å^−3
519 parameters	Δρmin = −0.41 e Å^−3

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.

Refinement. Crystallographic measurements were carried out with an Oxford-Diffraction Xcalibur E CCD diffractometer equipped with graphite-monochromated Mo-Ka radiation. The unit cell determination and data integration were carried out using the CrysAlis package of Oxford Diffraction. The structure was solved by direct methods using Olex2 and refined by full-matrix least-squares on F². Atomic displacements for non-hydrogen atoms were refined using an anisotropic model.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ni1	0.500000	0.500000	0.500000	0.01529 (18)
Ni2	−0.02509 (4)	0.24865 (4)	0.14648 (2)	0.02124 (15)
Si1	0.45189 (9)	0.02454 (7)	0.36702 (5)	0.0187 (3)
O1	0.5459 (2)	0.35919 (18)	0.48894 (13)	0.0223 (7)
O2	0.7037 (2)	0.3513 (2)	0.54473 (14)	0.0343 (8)
O3	0.8684 (2)	0.19926 (18)	0.56857 (12)	0.0229 (7)
C31	0.1371 (3)	0.2434 (3)	0.26931 (19)	0.0231 (10)
C2	0.5614 (4)	0.5186 (3)	0.6311 (2)	0.0377 (13)
H2A	0.527283	0.578512	0.634185	0.045*
H2B	0.610634	0.508034	0.669774	0.045*
O4	0.8792 (2)	0.2890 (2)	0.48579 (13)	0.0274 (7)
N2	0.6122 (3)	0.5221 (2)	0.57947 (15)	0.0245 (9)
H2	0.656765	0.466421	0.583870	0.029*
N1	0.4131 (3)	0.4540 (2)	0.55990 (16)	0.0280 (9)
H1	0.368437	0.506529	0.565598	0.034*
O5	0.0727 (2)	0.19903 (19)	0.22917 (13)	0.0299 (8)
C16	0.6313 (3)	0.3196 (3)	0.50553 (18)	0.0193 (9)
C7	0.1445 (9)	0.2664 (8)	0.0903 (8)	0.027 (4)	0.781 (3)
H7A	0.174283	0.258548	0.054451	0.032*	0.781 (3)
H7B	0.197020	0.255712	0.127459	0.032*	0.781 (3)
O10X	0.7373 (8)	0.4040 (8)	0.4033 (5)	0.0358 (12)*	0.48 (2)
H10X	0.771654	0.374972	0.432895	0.054*	0.48 (2)
O6	0.1691 (2)	0.3255 (2)	0.26436 (14)	0.0379 (9)
N3	0.0532 (3)	0.3723 (3)	0.14296 (19)	0.0255 (6)	0.781 (3)
H3	0.106903	0.373919	0.180989	0.031*	0.781 (3)
C30	0.1874 (3)	0.1883 (3)	0.32705 (19)	0.0201 (10)
C5	0.3493 (4)	0.3713 (3)	0.5383 (2)	0.0404 (13)
H5A	0.311335	0.354649	0.569198	0.049*
H5B	0.391985	0.317600	0.533610	0.049*
C12	−0.2009 (5)	0.2257 (5)	0.1937 (3)	0.0397 (18)	0.781 (3)
H12A	−0.249712	0.238567	0.155126	0.048*	0.781 (3)
H12B	−0.235158	0.231252	0.227702	0.048*	0.781 (3)
C23	0.5584 (3)	0.1779 (3)	0.44063 (17)	0.0164 (9)
H23	0.494855	0.205301	0.437256	0.020*
O8	0.0036 (3)	0.2773 (3)	0.34502 (16)	0.0547 (11)
C4	0.2763 (3)	0.3906 (3)	0.4768 (2)	0.0391 (13)
H4A	0.242931	0.450976	0.479881	0.047*
H4B	0.224545	0.341594	0.470073	0.047*
C3	0.6773 (3)	0.6059 (3)	0.5797 (2)	0.0353 (12)
H3A	0.731066	0.604979	0.617034	0.042*
H3B	0.637541	0.663123	0.580741	0.042*
C25	0.4601 (4)	0.0213 (3)	0.28406 (19)	0.0361 (12)
H25A	0.404628	−0.015249	0.260554	0.054*
H25B	0.522937	−0.007625	0.280780	0.054*
H25C	0.456913	0.084956	0.267961	0.054*
C28	0.2047 (3)	0.1289 (3)	0.43107 (19)	0.0233 (10)
H28	0.180937	0.124394	0.467407	0.028*
C27	0.2943 (3)	0.0831 (3)	0.42732 (19)	0.0253 (10)
H27	0.329588	0.048738	0.461375	0.030*
C17	0.6432 (3)	0.2261 (3)	0.47454 (18)	0.0173 (9)
C33	0.2767 (3)	0.1406 (3)	0.32442 (18)	0.0199 (9)
H33	0.300500	0.144355	0.288045	0.024*
C6	0.1043 (4)	0.3649 (4)	0.0911 (2)	0.0291 (14)	0.781 (3)
H6A	0.159366	0.410571	0.096377	0.035*	0.781 (3)
H6B	0.056920	0.378511	0.052079	0.035*	0.781 (3)
N4	0.0623 (3)	0.1956 (3)	0.0874 (2)	0.0255 (6)	0.781 (3)
H4	0.019763	0.199878	0.045252	0.031*	0.781 (3)
C29	0.1505 (3)	0.1811 (3)	0.38124 (19)	0.0199 (9)
O7	0.0295 (3)	0.2155 (3)	0.43904 (15)	0.0499 (10)
H7	−0.023085	0.243948	0.439673	0.075*
C26	0.3318 (3)	0.0875 (3)	0.37398 (18)	0.0186 (9)
N6	−0.1174 (3)	0.2954 (3)	0.20186 (19)	0.0255 (6)	0.781 (3)
H6	−0.078942	0.289576	0.244970	0.031*	0.781 (3)
C32	0.0538 (3)	0.2297 (3)	0.3849 (2)	0.0240 (10)
O9	0.3328 (7)	0.3757 (7)	0.2170 (6)	0.0674 (17)*	0.68 (4)
H9	0.293274	0.367023	0.239736	0.101*	0.68 (4)
C19	0.8356 (3)	0.2299 (3)	0.51494 (19)	0.0202 (9)
C24	0.4528 (3)	−0.0978 (3)	0.3994 (2)	0.0373 (12)
H24A	0.398831	−0.134264	0.374409	0.056*
H24B	0.443588	−0.094432	0.441319	0.056*
H24C	0.516488	−0.127749	0.399342	0.056*
C18	0.7381 (3)	0.1856 (3)	0.47911 (18)	0.0181 (9)
C20	0.7464 (3)	0.0995 (3)	0.44918 (19)	0.0241 (10)
H20	0.810144	0.073027	0.451680	0.029*
C22	0.5645 (3)	0.0906 (3)	0.41168 (18)	0.0184 (9)
C11	−0.1600 (6)	0.1274 (5)	0.1921 (3)	0.0366 (19)	0.781 (3)
H11A	−0.113528	0.112984	0.231289	0.044*	0.781 (3)
H11B	−0.214852	0.081480	0.185587	0.044*	0.781 (3)
N5	−0.1068 (3)	0.1223 (3)	0.1407 (2)	0.0255 (6)	0.781 (3)
H5	−0.158362	0.123963	0.101679	0.031*	0.781 (3)
C1	0.4855 (4)	0.4385 (3)	0.6197 (2)	0.0374 (12)
H1A	0.520227	0.378314	0.618742	0.045*
H1B	0.449587	0.436097	0.653102	0.045*
C21	0.6620 (3)	0.0527 (3)	0.41600 (19)	0.0252 (10)
H21	0.669602	−0.004425	0.396246	0.030*
C14	−0.0612 (7)	0.4600 (4)	0.1967 (4)	0.043 (2)	0.781 (3)
H14A	−0.011748	0.443902	0.234370	0.051*	0.781 (3)
H14B	−0.084050	0.524325	0.201951	0.051*	0.781 (3)
C13	−0.1487 (5)	0.3959 (4)	0.1925 (3)	0.0352 (17)	0.781 (3)
H13A	−0.194052	0.403007	0.151986	0.042*	0.781 (3)
H13B	−0.185579	0.414038	0.223766	0.042*	0.781 (3)
C9	0.0076 (5)	0.0287 (4)	0.0886 (3)	0.0377 (17)	0.781 (3)
H9A	−0.039755	0.042695	0.049630	0.045*	0.781 (3)
H9B	0.031393	−0.036033	0.085999	0.045*	0.781 (3)
C10	−0.0483 (6)	0.0339 (4)	0.1407 (3)	0.0317 (16)	0.781 (3)
H10A	−0.094128	−0.019916	0.137349	0.038*	0.781 (3)
H10B	0.000345	0.028587	0.180208	0.038*	0.781 (3)
C8	0.0974 (4)	0.0958 (4)	0.0954 (3)	0.0321 (15)	0.781 (3)
H8A	0.141564	0.087850	0.136290	0.039*	0.781 (3)
H8B	0.135853	0.080462	0.064506	0.039*	0.781 (3)
C34	0.3987 (13)	0.2921 (7)	0.2204 (10)	0.065 (3)*	0.68 (4)
H34A	0.359812	0.238897	0.200761	0.097*	0.68 (4)
H34B	0.427240	0.277048	0.263252	0.097*	0.68 (4)
H34C	0.452256	0.305512	0.199579	0.097*	0.68 (4)
C35X	0.7232 (12)	0.3482 (13)	0.3502 (5)	0.051 (2)*	0.48 (2)
H35A	0.677970	0.379938	0.316549	0.076*	0.48 (2)
H35B	0.694675	0.288005	0.357888	0.076*	0.48 (2)
H35C	0.787222	0.337907	0.339338	0.076*	0.48 (2)
N4X	0.0201 (11)	0.1303 (7)	0.1066 (6)	0.0255 (6)	0.219 (3)
H4X	−0.019083	0.128137	0.063519	0.031*	0.219 (3)
N3X	0.0984 (8)	0.3195 (9)	0.1288 (7)	0.0255 (6)	0.219 (3)
H3X	0.149315	0.319445	0.168130	0.031*	0.219 (3)
N6X	−0.0630 (11)	0.3656 (7)	0.1946 (6)	0.0255 (6)	0.219 (3)
H6X	−0.020204	0.361620	0.236711	0.031*	0.219 (3)
N5X	−0.1493 (9)	0.1931 (12)	0.1737 (7)	0.0255 (6)	0.219 (3)
H5X	−0.203788	0.194857	0.136068	0.031*	0.219 (3)
C15X	0.0851 (19)	0.4200 (11)	0.1095 (10)	0.035 (6)*	0.219 (3)
H15A	0.030887	0.423084	0.072469	0.042*	0.219 (3)
H15B	0.146599	0.440705	0.097864	0.042*	0.219 (3)
C8X	0.004 (2)	0.0390 (15)	0.1358 (14)	0.046 (7)*	0.219 (3)
H8XA	0.054247	0.031577	0.174365	0.056*	0.219 (3)
H8XB	0.012144	−0.012858	0.108325	0.056*	0.219 (3)
C14X	0.062 (2)	0.4892 (19)	0.1551 (13)	0.057 (8)*	0.219 (3)
H14C	0.057803	0.553008	0.137897	0.068*	0.219 (3)
H14D	0.115033	0.488245	0.192821	0.068*	0.219 (3)
C13X	−0.044 (3)	0.4604 (14)	0.1705 (15)	0.039 (9)*	0.219 (3)
H13C	−0.056843	0.506664	0.200382	0.046*	0.219 (3)
H13D	−0.094894	0.470089	0.132627	0.046*	0.219 (3)
C9X	−0.1043 (19)	0.0343 (18)	0.1495 (12)	0.039 (7)*	0.219 (3)
H9XA	−0.151109	0.043418	0.109622	0.047*	0.219 (3)
H9XB	−0.113088	−0.031044	0.161511	0.047*	0.219 (3)
C12X	−0.1684 (13)	0.3533 (18)	0.2014 (13)	0.036 (7)*	0.219 (3)
H12C	−0.181466	0.395671	0.233445	0.043*	0.219 (3)
H12D	−0.215185	0.369064	0.162573	0.043*	0.219 (3)
C11X	−0.183 (2)	0.2582 (18)	0.2176 (12)	0.039 (8)*	0.219 (3)
H11C	−0.254210	0.247424	0.216380	0.047*	0.219 (3)
H11D	−0.144873	0.245821	0.259541	0.047*	0.219 (3)
C10X	−0.142 (3)	0.0920 (13)	0.1927 (17)	0.046 (7)*	0.219 (3)
H10C	−0.097433	0.086340	0.233584	0.056*	0.219 (3)
H10D	−0.208581	0.069345	0.195522	0.056*	0.219 (3)
C7X	0.1229 (14)	0.162 (2)	0.1048 (14)	0.060 (8)*	0.219 (3)
H7XA	0.165630	0.152089	0.145957	0.072*	0.219 (3)
H7XB	0.147955	0.119703	0.076668	0.072*	0.219 (3)
C15	−0.0057 (6)	0.4615 (4)	0.1426 (3)	0.0365 (18)	0.781 (3)
H15C	−0.054644	0.467559	0.103307	0.044*	0.781 (3)
H15D	0.039585	0.515858	0.147069	0.044*	0.781 (3)
C6X	0.136 (4)	0.253 (3)	0.087 (3)	0.036 (15)*	0.219 (3)
H6XA	0.100185	0.263171	0.044684	0.043*	0.219 (3)
H6XB	0.207842	0.264945	0.089899	0.043*	0.219 (3)
C34X	0.423 (2)	0.3000 (19)	0.2420 (18)	0.065 (3)*	0.32 (4)
H34D	0.420272	0.237330	0.224267	0.097*	0.32 (4)
H34E	0.413227	0.295689	0.283762	0.097*	0.32 (4)
H34F	0.487360	0.328346	0.242411	0.097*	0.32 (4)
O9X	0.3422 (17)	0.3587 (19)	0.2046 (11)	0.0674 (17)*	0.32 (4)
H9X	0.299893	0.366154	0.226772	0.101*	0.32 (4)
O10	0.7548 (8)	0.4224 (7)	0.4134 (4)	0.0358 (12)*	0.52 (2)
H10	0.794450	0.390413	0.438930	0.054*	0.52 (2)
C35	0.7467 (11)	0.3841 (13)	0.3541 (5)	0.051 (2)*	0.52 (2)
H35D	0.738771	0.434726	0.324118	0.076*	0.52 (2)
H35E	0.688918	0.342753	0.344327	0.076*	0.52 (2)
H35F	0.806877	0.348627	0.353056	0.076*	0.52 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0109 (4)	0.0181 (4)	0.0156 (4)	0.0010 (3)	0.0003 (3)	−0.0051 (3)
Ni2	0.0139 (3)	0.0239 (3)	0.0236 (3)	0.0023 (3)	−0.0008 (2)	0.0066 (2)
Si1	0.0174 (6)	0.0192 (6)	0.0165 (6)	0.0000 (5)	−0.0024 (5)	−0.0034 (5)
O1	0.0123 (14)	0.0202 (14)	0.0316 (17)	0.0048 (13)	−0.0012 (13)	−0.0091 (13)
O2	0.0201 (17)	0.0324 (17)	0.043 (2)	0.0071 (15)	−0.0089 (15)	−0.0219 (15)
O3	0.0206 (16)	0.0264 (15)	0.0186 (16)	−0.0065 (14)	−0.0027 (13)	−0.0037 (13)
C31	0.020 (2)	0.024 (2)	0.023 (2)	0.005 (2)	−0.0006 (19)	0.0066 (19)
C2	0.033 (3)	0.054 (3)	0.022 (3)	0.014 (3)	−0.002 (2)	−0.010 (2)
O4	0.0184 (16)	0.0333 (17)	0.0291 (18)	0.0000 (14)	0.0026 (14)	0.0016 (14)
N2	0.0192 (19)	0.0255 (19)	0.025 (2)	0.0058 (17)	−0.0034 (16)	−0.0097 (16)
N1	0.023 (2)	0.031 (2)	0.031 (2)	0.0024 (18)	0.0099 (18)	0.0001 (17)
O5	0.0236 (17)	0.0259 (16)	0.0308 (18)	−0.0038 (14)	−0.0136 (15)	0.0085 (14)
C16	0.016 (2)	0.021 (2)	0.020 (2)	0.0002 (19)	0.0025 (19)	−0.0035 (18)
C7	0.022 (5)	0.038 (6)	0.022 (5)	−0.004 (4)	0.008 (3)	0.003 (3)
O6	0.045 (2)	0.0265 (17)	0.0320 (19)	−0.0087 (16)	−0.0140 (16)	0.0089 (14)
N3	0.0211 (13)	0.0298 (13)	0.0212 (12)	0.0014 (11)	−0.0047 (10)	0.0019 (10)
C30	0.021 (2)	0.0124 (19)	0.023 (2)	−0.0031 (19)	−0.0036 (19)	−0.0010 (17)
C5	0.029 (3)	0.038 (3)	0.057 (4)	−0.006 (2)	0.014 (3)	0.002 (3)
C12	0.031 (4)	0.055 (5)	0.033 (4)	0.006 (4)	0.008 (3)	−0.003 (4)
C23	0.012 (2)	0.018 (2)	0.018 (2)	0.0049 (18)	0.0027 (17)	−0.0007 (16)
O8	0.044 (2)	0.077 (3)	0.046 (2)	0.038 (2)	0.0169 (19)	0.026 (2)
C4	0.019 (3)	0.031 (3)	0.064 (4)	−0.011 (2)	0.003 (3)	−0.008 (2)
C3	0.023 (3)	0.031 (3)	0.045 (3)	0.002 (2)	−0.008 (2)	−0.018 (2)
C25	0.032 (3)	0.049 (3)	0.025 (3)	0.009 (2)	0.000 (2)	−0.009 (2)
C28	0.022 (2)	0.031 (2)	0.017 (2)	−0.002 (2)	0.0033 (19)	0.0016 (19)
C27	0.022 (2)	0.030 (2)	0.021 (2)	0.000 (2)	−0.002 (2)	0.0021 (19)
C17	0.016 (2)	0.015 (2)	0.020 (2)	0.0013 (18)	0.0029 (18)	−0.0010 (16)
C33	0.019 (2)	0.024 (2)	0.014 (2)	−0.005 (2)	−0.0006 (18)	0.0003 (18)
C6	0.025 (3)	0.025 (3)	0.035 (4)	−0.004 (3)	0.004 (3)	0.012 (3)
N4	0.0211 (13)	0.0298 (13)	0.0212 (12)	0.0014 (11)	−0.0047 (10)	0.0019 (10)
C29	0.015 (2)	0.021 (2)	0.021 (2)	−0.0027 (19)	−0.0024 (18)	−0.0035 (17)
O7	0.033 (2)	0.081 (3)	0.039 (2)	0.030 (2)	0.0160 (18)	0.0093 (19)
C26	0.015 (2)	0.017 (2)	0.020 (2)	−0.0014 (18)	−0.0047 (18)	−0.0013 (17)
N6	0.0211 (13)	0.0298 (13)	0.0212 (12)	0.0014 (11)	−0.0047 (10)	0.0019 (10)
C32	0.022 (2)	0.026 (2)	0.022 (2)	−0.001 (2)	0.001 (2)	−0.0058 (19)
C19	0.015 (2)	0.020 (2)	0.024 (2)	0.0072 (19)	0.0020 (19)	−0.0036 (18)
C24	0.030 (3)	0.029 (2)	0.049 (3)	−0.003 (2)	0.001 (3)	0.001 (2)
C18	0.017 (2)	0.020 (2)	0.016 (2)	0.0023 (19)	0.0005 (18)	−0.0021 (17)
C20	0.015 (2)	0.023 (2)	0.032 (3)	0.007 (2)	−0.001 (2)	−0.0060 (19)
C22	0.016 (2)	0.021 (2)	0.015 (2)	0.0035 (19)	−0.0025 (18)	−0.0007 (17)
C11	0.030 (4)	0.043 (5)	0.033 (4)	−0.016 (4)	−0.002 (3)	0.008 (4)
N5	0.0211 (13)	0.0298 (13)	0.0212 (12)	0.0014 (11)	−0.0047 (10)	0.0019 (10)
C1	0.041 (3)	0.054 (3)	0.021 (3)	0.002 (3)	0.015 (2)	0.008 (2)
C21	0.023 (2)	0.020 (2)	0.030 (3)	0.003 (2)	−0.001 (2)	−0.0134 (19)
C14	0.064 (6)	0.032 (4)	0.029 (4)	0.026 (4)	0.005 (4)	−0.010 (3)
C13	0.041 (4)	0.033 (4)	0.033 (4)	0.019 (4)	0.011 (3)	0.000 (3)
C9	0.036 (4)	0.020 (3)	0.053 (5)	0.002 (3)	0.001 (3)	−0.005 (3)
C10	0.033 (4)	0.025 (3)	0.036 (4)	0.002 (3)	0.004 (3)	0.007 (3)
C8	0.024 (3)	0.032 (3)	0.040 (4)	0.014 (3)	0.007 (3)	0.006 (3)
N4X	0.0211 (13)	0.0298 (13)	0.0212 (12)	0.0014 (11)	−0.0047 (10)	0.0019 (10)
N3X	0.0211 (13)	0.0298 (13)	0.0212 (12)	0.0014 (11)	−0.0047 (10)	0.0019 (10)
N6X	0.0211 (13)	0.0298 (13)	0.0212 (12)	0.0014 (11)	−0.0047 (10)	0.0019 (10)
N5X	0.0211 (13)	0.0298 (13)	0.0212 (12)	0.0014 (11)	−0.0047 (10)	0.0019 (10)
C15	0.050 (5)	0.014 (3)	0.037 (4)	0.003 (3)	−0.006 (4)	0.016 (3)

Geometric parameters (Å, º)

Ni1—N1^i	2.059 (4)	C19—C18	1.513 (5)
Ni1—N1	2.059 (4)	C24—H24A	0.9600
Ni1—N2^i	2.070 (3)	C24—H24B	0.9600
Ni1—N2	2.070 (3)	C24—H24C	0.9600
Ni1—O1^i	2.104 (2)	C18—C20	1.395 (5)
Ni1—O1	2.104 (2)	C20—C21	1.378 (5)
Ni2—N4X	2.037 (7)	C20—H20	0.9300
Ni2—N6	2.041 (4)	C22—C21	1.407 (5)
Ni2—N3	2.045 (4)	C11—N5	1.474 (6)
Ni2—N3X	2.057 (7)	C11—H11A	0.9700
Ni2—N5X	2.060 (8)	C11—H11B	0.9700
Ni2—N5	2.080 (4)	N5—C10	1.472 (5)
Ni2—N6X	2.081 (7)	N5—H5	0.9800
Ni2—N4	2.083 (4)	C1—H1A	0.9700
Ni2—O3^ii	2.112 (3)	C1—H1B	0.9700
Ni2—O5	2.118 (3)	C21—H21	0.9300
Si1—C25	1.858 (4)	C14—C13	1.475 (10)
Si1—C24	1.860 (4)	C14—C15	1.545 (10)
Si1—C22	1.867 (4)	C14—H14A	0.9700
Si1—C26	1.887 (4)	C14—H14B	0.9700
O1—C16	1.262 (4)	C13—H13A	0.9700
O2—C16	1.236 (4)	C13—H13B	0.9700
O3—C19	1.243 (4)	C9—C10	1.514 (9)
C31—O6	1.246 (5)	C9—C8	1.519 (8)
C31—O5	1.260 (5)	C9—H9A	0.9700
C31—C30	1.515 (5)	C9—H9B	0.9700
C2—N2	1.455 (5)	C10—H10A	0.9700
C2—C1	1.507 (6)	C10—H10B	0.9700
C2—H2A	0.9700	C8—H8A	0.9700
C2—H2B	0.9700	C8—H8B	0.9700
O4—C19	1.273 (5)	C34—H34A	0.9600
N2—C3	1.470 (5)	C34—H34B	0.9600
N2—H2	0.9800	C34—H34C	0.9600
N1—C5	1.462 (5)	C35X—H35A	0.9600
N1—C1	1.472 (5)	C35X—H35B	0.9600
N1—H1	0.9800	C35X—H35C	0.9600
C16—C17	1.506 (5)	N4X—C7X	1.469 (8)
C7—N4	1.483 (8)	N4X—C8X	1.473 (8)
C7—C6	1.489 (14)	N4X—H4X	0.9800
C7—H7A	0.9700	N3X—C15X	1.473 (8)
C7—H7B	0.9700	N3X—C6X	1.476 (8)
O10X—C35X	1.387 (8)	N3X—H3X	0.9800
O10X—H10X	0.8199	N6X—C13X	1.478 (8)
N3—C6	1.467 (5)	N6X—C12X	1.479 (8)
N3—C15	1.485 (5)	N6X—H6X	0.9800
N3—H3	0.9800	N5X—C11X	1.48 (3)
C30—C33	1.395 (5)	N5X—C10X	1.477 (8)
C30—C29	1.398 (6)	N5X—H5X	0.9800
C5—C4	1.513 (6)	C15X—C14X	1.48 (3)
C5—H5A	0.9700	C15X—H15A	0.9700
C5—H5B	0.9700	C15X—H15B	0.9700
C12—N6	1.476 (6)	C8X—C9X	1.56 (3)
C12—C11	1.490 (9)	C8X—H8XA	0.9700
C12—H12A	0.9700	C8X—H8XB	0.9700
C12—H12B	0.9700	C14X—C13X	1.59 (4)
C23—C22	1.393 (5)	C14X—H14C	0.9700
C23—C17	1.398 (5)	C14X—H14D	0.9700
C23—H23	0.9300	C13X—H13C	0.9700
O8—C32	1.190 (5)	C13X—H13D	0.9700
C4—C3^i	1.516 (7)	C9X—C10X	1.43 (4)
C4—H4A	0.9700	C9X—H9XA	0.9700
C4—H4B	0.9700	C9X—H9XB	0.9700
C3—H3A	0.9700	C12X—C11X	1.41 (3)
C3—H3B	0.9700	C12X—H12C	0.9700
C25—H25A	0.9600	C12X—H12D	0.9700
C25—H25B	0.9600	C11X—H11C	0.9700
C25—H25C	0.9600	C11X—H11D	0.9700
C28—C29	1.388 (5)	C10X—H10C	0.9700
C28—C27	1.391 (6)	C10X—H10D	0.9700
C28—H28	0.9300	C7X—C6X	1.37 (6)
C27—C26	1.383 (6)	C7X—H7XA	0.9700
C27—H27	0.9300	C7X—H7XB	0.9700
C17—C18	1.388 (5)	C15—H15C	0.9700
C33—C26	1.394 (5)	C15—H15D	0.9700
C33—H33	0.9300	C6X—H6XA	0.9700
C6—H6A	0.9700	C6X—H6XB	0.9700
C6—H6B	0.9700	C34X—O9X	1.466 (10)
N4—C8	1.479 (5)	C34X—H34D	0.9600
N4—H4	0.9800	C34X—H34E	0.9600
C29—C32	1.494 (6)	C34X—H34F	0.9600
O7—C32	1.321 (5)	O9X—H9X	0.8394
O7—H7	0.8200	O10—C35	1.396 (8)
N6—C13	1.475 (5)	O10—H10	0.8200
N6—H6	0.9800	C35—H35D	0.9600
O9—C34	1.467 (8)	C35—H35E	0.9600
O9—H9	0.8199	C35—H35F	0.9600
N1^i—Ni1—N1	180.0	C20—C18—C19	116.8 (3)
N1^i—Ni1—N2^i	85.45 (14)	C21—C20—C18	121.3 (4)
N1—Ni1—N2^i	94.56 (14)	C21—C20—H20	119.3
N1^i—Ni1—N2	94.56 (14)	C18—C20—H20	119.3
N1—Ni1—N2	85.44 (14)	C23—C22—C21	116.9 (4)
N2^i—Ni1—N2	180.0 (2)	C23—C22—Si1	123.7 (3)
N1^i—Ni1—O1^i	90.28 (13)	C21—C22—Si1	119.4 (3)
N1—Ni1—O1^i	89.72 (13)	N5—C11—C12	108.1 (5)
N2^i—Ni1—O1^i	93.42 (11)	N5—C11—H11A	110.1
N2—Ni1—O1^i	86.58 (11)	C12—C11—H11A	110.1
N1^i—Ni1—O1	89.72 (13)	N5—C11—H11B	110.1
N1—Ni1—O1	90.28 (13)	C12—C11—H11B	110.1
N2^i—Ni1—O1	86.58 (11)	H11A—C11—H11B	108.4
N2—Ni1—O1	93.42 (11)	C10—N5—C11	113.3 (5)
O1^i—Ni1—O1	180.0	C10—N5—Ni2	116.2 (4)
N6—Ni2—N3	98.11 (17)	C11—N5—Ni2	104.8 (3)
N4X—Ni2—N3X	88.7 (6)	C10—N5—H5	107.4
N4X—Ni2—N5X	99.2 (6)	C11—N5—H5	107.4
N3X—Ni2—N5X	171.6 (7)	Ni2—N5—H5	107.4
N6—Ni2—N5	85.61 (17)	N1—C1—C2	109.4 (4)
N3—Ni2—N5	174.42 (17)	N1—C1—H1A	109.8
N4X—Ni2—N6X	174.9 (6)	C2—C1—H1A	109.8
N3X—Ni2—N6X	91.0 (6)	N1—C1—H1B	109.8
N5X—Ni2—N6X	80.8 (6)	C2—C1—H1B	109.8
N6—Ni2—N4	176.65 (17)	H1A—C1—H1B	108.2
N3—Ni2—N4	84.73 (17)	C20—C21—C22	120.7 (4)
N5—Ni2—N4	91.43 (17)	C20—C21—H21	119.7
N6—Ni2—O3^ii	88.66 (14)	C22—C21—H21	119.7
N3—Ni2—O3^ii	86.59 (14)	C13—C14—C15	118.9 (6)
N5—Ni2—O3^ii	89.34 (14)	C13—C14—H14A	107.6
N4—Ni2—O3^ii	89.74 (14)	C15—C14—H14A	107.6
N4X—Ni2—O5	85.0 (4)	C13—C14—H14B	107.6
N6—Ni2—O5	86.54 (15)	C15—C14—H14B	107.6
N3—Ni2—O5	94.73 (14)	H14A—C14—H14B	107.0
N3X—Ni2—O5	86.8 (4)	C14—C13—N6	111.9 (5)
N5X—Ni2—O5	91.1 (4)	C14—C13—H13A	109.2
N5—Ni2—O5	89.64 (14)	N6—C13—H13A	109.2
N6X—Ni2—O5	89.9 (4)	C14—C13—H13B	109.2
N4—Ni2—O5	95.01 (15)	N6—C13—H13B	109.2
O3^ii—Ni2—O5	175.16 (12)	H13A—C13—H13B	107.9
C25—Si1—C24	111.0 (2)	C10—C9—C8	114.8 (6)
C25—Si1—C22	108.1 (2)	C10—C9—H9A	108.6
C24—Si1—C22	108.79 (19)	C8—C9—H9A	108.6
C25—Si1—C26	109.48 (19)	C10—C9—H9B	108.6
C24—Si1—C26	109.5 (2)	C8—C9—H9B	108.6
C22—Si1—C26	109.92 (17)	H9A—C9—H9B	107.6
C16—O1—Ni1	131.0 (2)	N5—C10—C9	113.6 (5)
C19—O3—Ni2^iii	133.4 (3)	N5—C10—H10A	108.8
O6—C31—O5	126.6 (4)	C9—C10—H10A	108.8
O6—C31—C30	116.5 (4)	N5—C10—H10B	108.8
O5—C31—C30	116.7 (4)	C9—C10—H10B	108.8
N2—C2—C1	108.6 (4)	H10A—C10—H10B	107.7
N2—C2—H2A	110.0	N4—C8—C9	110.4 (4)
C1—C2—H2A	110.0	N4—C8—H8A	109.6
N2—C2—H2B	110.0	C9—C8—H8A	109.6
C1—C2—H2B	110.0	N4—C8—H8B	109.6
H2A—C2—H2B	108.4	C9—C8—H8B	109.6
C2—N2—C3	114.3 (4)	H8A—C8—H8B	108.1
C2—N2—Ni1	105.7 (3)	O9—C34—H34A	109.5
C3—N2—Ni1	116.7 (3)	O9—C34—H34B	109.5
C2—N2—H2	106.5	H34A—C34—H34B	109.5
C3—N2—H2	106.5	O9—C34—H34C	109.5
Ni1—N2—H2	106.5	H34A—C34—H34C	109.5
C5—N1—C1	113.7 (3)	H34B—C34—H34C	109.5
C5—N1—Ni1	114.9 (3)	O10X—C35X—H35A	109.5
C1—N1—Ni1	105.0 (3)	O10X—C35X—H35B	109.5
C5—N1—H1	107.6	H35A—C35X—H35B	109.5
C1—N1—H1	107.6	O10X—C35X—H35C	109.5
Ni1—N1—H1	107.6	H35A—C35X—H35C	109.5
C31—O5—Ni2	130.1 (3)	H35B—C35X—H35C	109.5
O2—C16—O1	125.2 (4)	C7X—N4X—C8X	120.5 (19)
O2—C16—C17	118.9 (3)	C7X—N4X—Ni2	98.4 (13)
O1—C16—C17	115.9 (3)	C8X—N4X—Ni2	115.7 (15)
N4—C7—C6	110.6 (8)	C7X—N4X—H4X	107.1
N4—C7—H7A	109.5	C8X—N4X—H4X	107.1
C6—C7—H7A	109.5	Ni2—N4X—H4X	107.1
N4—C7—H7B	109.5	C15X—N3X—C6X	118 (3)
C6—C7—H7B	109.5	C15X—N3X—Ni2	117.8 (12)
H7A—C7—H7B	108.1	C6X—N3X—Ni2	102.9 (18)
C35X—O10X—H10X	109.7	C15X—N3X—H3X	105.8
C6—N3—C15	113.7 (5)	C6X—N3X—H3X	105.8
C6—N3—Ni2	108.0 (3)	Ni2—N3X—H3X	105.8
C15—N3—Ni2	115.8 (4)	C13X—N6X—C12X	113.3 (19)
C6—N3—H3	106.2	C13X—N6X—Ni2	116.4 (15)
C15—N3—H3	106.2	C12X—N6X—Ni2	108.2 (12)
Ni2—N3—H3	106.2	C13X—N6X—H6X	106.1
C33—C30—C29	118.6 (4)	C12X—N6X—H6X	106.1
C33—C30—C31	116.2 (4)	Ni2—N6X—H6X	106.1
C29—C30—C31	125.1 (4)	C11X—N5X—C10X	114.8 (19)
N1—C5—C4	111.7 (4)	C11X—N5X—Ni2	110.4 (13)
N1—C5—H5A	109.3	C10X—N5X—Ni2	116.1 (19)
C4—C5—H5A	109.3	C11X—N5X—H5X	104.7
N1—C5—H5B	109.3	C10X—N5X—H5X	104.7
C4—C5—H5B	109.3	Ni2—N5X—H5X	104.7
H5A—C5—H5B	107.9	N3X—C15X—C14X	118 (2)
N6—C12—C11	109.8 (5)	N3X—C15X—H15A	107.9
N6—C12—H12A	109.7	C14X—C15X—H15A	107.9
C11—C12—H12A	109.7	N3X—C15X—H15B	107.9
N6—C12—H12B	109.7	C14X—C15X—H15B	107.9
C11—C12—H12B	109.7	H15A—C15X—H15B	107.2
H12A—C12—H12B	108.2	N4X—C8X—C9X	111 (2)
C22—C23—C17	123.1 (4)	N4X—C8X—H8XA	109.4
C22—C23—H23	118.5	C9X—C8X—H8XA	109.4
C17—C23—H23	118.5	N4X—C8X—H8XB	109.4
C5—C4—C3^i	115.7 (4)	C9X—C8X—H8XB	109.4
C5—C4—H4A	108.4	H8XA—C8X—H8XB	108.0
C3^i—C4—H4A	108.4	C15X—C14X—C13X	108 (2)
C5—C4—H4B	108.4	C15X—C14X—H14C	110.0
C3^i—C4—H4B	108.4	C13X—C14X—H14C	110.0
H4A—C4—H4B	107.4	C15X—C14X—H14D	110.0
N2—C3—C4^i	112.4 (4)	C13X—C14X—H14D	110.0
N2—C3—H3A	109.1	H14C—C14X—H14D	108.4
C4^i—C3—H3A	109.1	N6X—C13X—C14X	123 (2)
N2—C3—H3B	109.1	N6X—C13X—H13C	106.6
C4^i—C3—H3B	109.1	C14X—C13X—H13C	106.6
H3A—C3—H3B	107.9	N6X—C13X—H13D	106.6
Si1—C25—H25A	109.5	C14X—C13X—H13D	106.6
Si1—C25—H25B	109.5	H13C—C13X—H13D	106.5
H25A—C25—H25B	109.5	C10X—C9X—C8X	126 (3)
Si1—C25—H25C	109.5	C10X—C9X—H9XA	105.7
H25A—C25—H25C	109.5	C8X—C9X—H9XA	105.7
H25B—C25—H25C	109.5	C10X—C9X—H9XB	105.7
C29—C28—C27	120.8 (4)	C8X—C9X—H9XB	105.7
C29—C28—H28	119.6	H9XA—C9X—H9XB	106.1
C27—C28—H28	119.6	C11X—C12X—N6X	109 (2)
C26—C27—C28	121.3 (4)	C11X—C12X—H12C	109.8
C26—C27—H27	119.3	N6X—C12X—H12C	109.8
C28—C27—H27	119.3	C11X—C12X—H12D	109.8
C18—C17—C23	118.5 (3)	N6X—C12X—H12D	109.8
C18—C17—C16	121.0 (3)	H12C—C12X—H12D	108.3
C23—C17—C16	120.5 (3)	C12X—C11X—N5X	110 (2)
C26—C33—C30	122.8 (4)	C12X—C11X—H11C	109.7
C26—C33—H33	118.6	N5X—C11X—H11C	109.7
C30—C33—H33	118.6	C12X—C11X—H11D	109.7
N3—C6—C7	108.1 (6)	N5X—C11X—H11D	109.7
N3—C6—H6A	110.1	H11C—C11X—H11D	108.2
C7—C6—H6A	110.1	C9X—C10X—N5X	111 (3)
N3—C6—H6B	110.1	C9X—C10X—H10C	109.3
C7—C6—H6B	110.1	N5X—C10X—H10C	109.3
H6A—C6—H6B	108.4	C9X—C10X—H10D	109.3
C8—N4—C7	114.3 (7)	N5X—C10X—H10D	109.3
C8—N4—Ni2	118.5 (3)	H10C—C10X—H10D	108.0
C7—N4—Ni2	105.1 (3)	C6X—C7X—N4X	118 (3)
C8—N4—H4	106.0	C6X—C7X—H7XA	107.7
C7—N4—H4	106.0	N4X—C7X—H7XA	107.7
Ni2—N4—H4	106.0	C6X—C7X—H7XB	107.7
C28—C29—C30	119.2 (4)	N4X—C7X—H7XB	107.7
C28—C29—C32	120.9 (4)	H7XA—C7X—H7XB	107.1
C30—C29—C32	119.9 (4)	N3—C15—C14	109.7 (5)
C32—O7—H7	109.5	N3—C15—H15C	109.7
C27—C26—C33	117.2 (4)	C14—C15—H15C	109.7
C27—C26—Si1	122.3 (3)	N3—C15—H15D	109.7
C33—C26—Si1	120.5 (3)	C14—C15—H15D	109.7
C13—N6—C12	115.4 (5)	H15C—C15—H15D	108.2
C13—N6—Ni2	114.9 (4)	C7X—C6X—N3X	109 (4)
C12—N6—Ni2	105.5 (4)	C7X—C6X—H6XA	109.8
C13—N6—H6	106.8	N3X—C6X—H6XA	109.8
C12—N6—H6	106.8	C7X—C6X—H6XB	109.8
Ni2—N6—H6	106.8	N3X—C6X—H6XB	109.8
O8—C32—O7	122.5 (4)	H6XA—C6X—H6XB	108.2
O8—C32—C29	125.4 (4)	O9X—C34X—H34D	109.5
O7—C32—C29	112.2 (4)	O9X—C34X—H34E	109.5
C34—O9—H9	108.8	H34D—C34X—H34E	109.5
O3—C19—O4	126.8 (4)	O9X—C34X—H34F	109.5
O3—C19—C18	116.0 (4)	H34D—C34X—H34F	109.5
O4—C19—C18	117.0 (4)	H34E—C34X—H34F	109.5
Si1—C24—H24A	109.5	C34X—O9X—H9X	105.1
Si1—C24—H24B	109.5	C35—O10—H10	109.5
H24A—C24—H24B	109.5	O10—C35—H35D	109.5
Si1—C24—H24C	109.5	O10—C35—H35E	109.5
H24A—C24—H24C	109.5	H35D—C35—H35E	109.5
H24B—C24—H24C	109.5	O10—C35—H35F	109.5
C17—C18—C20	119.5 (4)	H35D—C35—H35F	109.5
C17—C18—C19	123.7 (3)	H35E—C35—H35F	109.5
C1—C2—N2—C3	171.2 (4)	O3—C19—C18—C17	97.3 (5)
C1—C2—N2—Ni1	41.4 (4)	O4—C19—C18—C17	−87.7 (5)
O6—C31—O5—Ni2	−11.9 (7)	O3—C19—C18—C20	−83.0 (5)
C30—C31—O5—Ni2	173.8 (3)	O4—C19—C18—C20	91.9 (4)
Ni1—O1—C16—O2	17.1 (7)	C17—C18—C20—C21	−1.2 (6)
Ni1—O1—C16—C17	−163.4 (3)	C19—C18—C20—C21	179.2 (4)
O6—C31—C30—C33	−84.5 (5)	C17—C23—C22—C21	−2.1 (6)
O5—C31—C30—C33	90.4 (5)	C17—C23—C22—Si1	179.2 (3)
O6—C31—C30—C29	96.5 (5)	C25—Si1—C22—C23	114.2 (4)
O5—C31—C30—C29	−88.6 (5)	C24—Si1—C22—C23	−125.2 (4)
C1—N1—C5—C4	180.0 (4)	C26—Si1—C22—C23	−5.3 (4)
Ni1—N1—C5—C4	−59.0 (4)	C25—Si1—C22—C21	−64.5 (4)
N1—C5—C4—C3^i	73.3 (5)	C24—Si1—C22—C21	56.2 (4)
C2—N2—C3—C4^i	−176.7 (4)	C26—Si1—C22—C21	176.1 (3)
Ni1—N2—C3—C4^i	−52.6 (4)	N6—C12—C11—N5	−58.2 (7)
C29—C28—C27—C26	−0.4 (6)	C12—C11—N5—C10	170.3 (5)
C22—C23—C17—C18	0.6 (6)	C12—C11—N5—Ni2	42.6 (6)
C22—C23—C17—C16	−179.1 (4)	C5—N1—C1—C2	168.1 (4)
O2—C16—C17—C18	−13.7 (6)	Ni1—N1—C1—C2	41.8 (4)
O1—C16—C17—C18	166.8 (4)	N2—C2—C1—N1	−58.0 (5)
O2—C16—C17—C23	166.0 (4)	C18—C20—C21—C22	−0.4 (7)
O1—C16—C17—C23	−13.5 (6)	C23—C22—C21—C20	1.9 (6)
C29—C30—C33—C26	−1.3 (6)	Si1—C22—C21—C20	−179.3 (3)
C31—C30—C33—C26	179.6 (4)	C15—C14—C13—N6	73.3 (7)
C15—N3—C6—C7	−170.0 (7)	C12—N6—C13—C14	−175.5 (6)
Ni2—N3—C6—C7	−40.1 (7)	Ni2—N6—C13—C14	−52.4 (6)
N4—C7—C6—N3	55.0 (12)	C11—N5—C10—C9	−179.3 (6)
C6—C7—N4—C8	−171.7 (8)	Ni2—N5—C10—C9	−57.8 (6)
C6—C7—N4—Ni2	−40.2 (12)	C8—C9—C10—N5	70.8 (7)
C27—C28—C29—C30	−0.7 (6)	C7—N4—C8—C9	−177.1 (8)
C27—C28—C29—C32	179.5 (4)	Ni2—N4—C8—C9	58.1 (6)
C33—C30—C29—C28	1.5 (6)	C10—C9—C8—N4	−69.2 (7)
C31—C30—C29—C28	−179.5 (4)	C6X—N3X—C15X—C14X	−171 (3)
C33—C30—C29—C32	−178.7 (3)	Ni2—N3X—C15X—C14X	65 (2)
C31—C30—C29—C32	0.3 (6)	C7X—N4X—C8X—C9X	164 (2)
C28—C27—C26—C33	0.6 (6)	Ni2—N4X—C8X—C9X	46 (3)
C28—C27—C26—Si1	−179.0 (3)	N3X—C15X—C14X—C13X	−62 (3)
C30—C33—C26—C27	0.2 (6)	C12X—N6X—C13X—C14X	−176 (3)
C30—C33—C26—Si1	179.8 (3)	Ni2—N6X—C13X—C14X	−50 (3)
C25—Si1—C26—C27	165.7 (3)	C15X—C14X—C13X—N6X	57 (3)
C24—Si1—C26—C27	43.8 (4)	N4X—C8X—C9X—C10X	−66 (4)
C22—Si1—C26—C27	−75.7 (4)	C13X—N6X—C12X—C11X	173 (2)
C25—Si1—C26—C33	−13.9 (4)	Ni2—N6X—C12X—C11X	43 (2)
C24—Si1—C26—C33	−135.8 (3)	N6X—C12X—C11X—N5X	−51 (3)
C22—Si1—C26—C33	104.7 (3)	C10X—N5X—C11X—C12X	169 (2)
C11—C12—N6—C13	169.1 (5)	Ni2—N5X—C11X—C12X	35 (2)
C11—C12—N6—Ni2	41.1 (6)	C8X—C9X—C10X—N5X	66 (4)
C28—C29—C32—O8	178.5 (4)	C11X—N5X—C10X—C9X	−177 (2)
C30—C29—C32—O8	−1.3 (6)	Ni2—N5X—C10X—C9X	−46 (3)
C28—C29—C32—O7	−0.4 (5)	C8X—N4X—C7X—C6X	−169 (3)
C30—C29—C32—O7	179.7 (4)	Ni2—N4X—C7X—C6X	−42 (3)
Ni2^iii—O3—C19—O4	22.7 (6)	C6—N3—C15—C14	176.9 (5)
Ni2^iii—O3—C19—C18	−162.8 (2)	Ni2—N3—C15—C14	51.0 (6)
C23—C17—C18—C20	1.1 (6)	C13—C14—C15—N3	−72.0 (7)
C16—C17—C18—C20	−179.2 (4)	N4X—C7X—C6X—N3X	57 (6)
C23—C17—C18—C19	−179.3 (4)	C15X—N3X—C6X—C7X	−167 (3)
C16—C17—C18—C19	0.4 (6)	Ni2—N3X—C6X—C7X	−35 (5)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2···O2	0.98	2.00	2.882 (4)	148
N3—H3···O6	0.98	1.96	2.861 (5)	151
N4—H4···O4^ii	0.98	2.06	2.955 (5)	151
N5—H5···O2^ii	0.98	2.03	2.962 (5)	157
N6—H6···O8	0.98	2.25	3.225 (5)	178
O7—H7···O4^iv	0.82	1.95	2.684 (5)	150
N4—H4···O7^v	0.98	2.66	3.437 (6)	137
N1—H1···O10^i	0.98	2.08	3.021 (9)	160
O9—H9···O6	0.82	1.97	2.745 (11)	158
O10—H10···O4	0.82	1.97	2.775 (9)	166

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