Three novel topologically different metal–organic frameworks built from 3-nitro-4-(pyridin-4-yl)benzoic acid

Qin, T.; Zhang, S.; Wang, Y.; Hou, T.; Zhu, D.; Jing, S.

doi:10.1107/S2053229618018211

Three novel topologically different metal–organic frameworks built from 3-nitro-4-(pyridin-4-yl)benzoic acid

T. Qin, S. Zhang, Y. Wang, T. Hou, D. Zhu and S. Jing

The design and synthesis of metal–organic frameworks (MOFs) have attracted much interest due to the intriguing diversity of their architectures and topologies. However, building MOFs with different topological structures from the same ligand is still a challenge. Using 3-nitro-4-(pyridin-4-yl)benzoic acid (HL) as a new ligand, three novel MOFs, namely poly[[(N,N-dimethylformamide-κO)bis[μ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ³O,O′:N]cadmium(II)] N,N-dimethylformamide monosolvate methanol monosolvate], {[Cd(C₁₂H₇N₂O₄)₂(C₃H₇NO)]·C₃H₇NO·CH₃OH}_n, (1), poly[[(μ₂-acetato-κ²O:O′)[μ₃-3-nitro-4-(pyridin-4-yl)benzoato-κ³O:O′:N]bis[μ₃-3-nitro-4-(pyridin-4-yl)benzoato-κ⁴O,O′:O′:N]dicadmium(II)] N,N-dimethylacetamide disolvate monohydrate], {[Cd₂(C₁₂H₇N₂O₄)₃(CH₃CO₂)]·2C₄H₉NO·H₂O}_n, (2), and catena-poly[[[diaquanickel(II)]-bis[μ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:N]] N,N-dimethylacetamide disolvate], {[Ni(C₁₂H₇N₂O₄)₂(H₂O)₂]·2C₄H₉NO}_n, (3), have been prepared. Single-crystal structure analysis shows that the Cd^II atom in MOF (1) has a distorted pentagonal bipyramidal [CdN₂O₅] coordination geometry. The [CdN₂O₅] units as 4-connected nodes are interconnected by L⁻ ligands to form a fourfold interpenetrating three-dimensional (3D) framework with a dia topology. In MOF (2), there are two crystallographically different Cd^II ions showing a distorted pentagonal bipyramidal [CdNO₆] and a distorted octahedral [CdN₂O₄] coordination geometry, respectively. Two Cd^II ions are connected by three carboxylate groups to form a binuclear [Cd₂(COO)₃] cluster. Each binuclear cluster as a 6-connected node is further linked by acetate groups and L⁻ ligands to produce a non-interpenetrating 3D framework with a pcu topology. MOF (3) contains two crystallographically distinct Ni^II ions on special positions. Each Ni^II ion adopts an elongated octahedral [NiN₂O₄] geometry. Each Ni^II ion as a 4-connected node is linked by L⁻ ligands to generate a two-dimensional network with an sql topology, which is further stabilized by two types of intermolecular OW—HW

O hydrogen bonds to form a 3D supramolecular framework. MOFs (1)–(3) were also characterized by powder X-ray diffraction, IR spectroscopy and thermogravimetic analysis. Furthermore, the solid-state photoluminescence of HL and MOFs (1) and (2) have been investigated. The photoluminescence of MOFs (1) and (2) are enhanced and red-shifted with respect to free HL. The gas adsorption investigation of MOF (2) indicates a good separation selectivity (71) of CO₂/N₂ at 273 K (i.e. the amount of CO₂ adsorption is 71 times higher than N₂ at the same pressure).

Keywords: topology; three-dimensional MOF; 3-nitro-4-(pyridin-4-yl)benzoic acid; crystal structure; photoluminescence; gas adsorption.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618018211/sk3712sup1.cif Contains datablocks 1845689, 1831564, 1845690, global
	Structure factor file (CIF format) https://doi.org/10.1107/S2053229618018211/sk37121845689sup2.hkl Contains datablock 1845689
	Structure factor file (CIF format) https://doi.org/10.1107/S2053229618018211/sk37121831564sup3.hkl Contains datablock 1831564
	Structure factor file (CIF format) https://doi.org/10.1107/S2053229618018211/sk37121845690sup4.hkl Contains datablock 1845690
	Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618018211/sk3712sup5.pdf Reaction scheme, spectra (PXRD, FT-IR, TGA and emission) and additional geometry

CCDC references: 1845690; 1831564; 1845689

Computing details top

For all structures, data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS2018 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015b); molecular graphics: SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2010); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Poly[[(N,N-dimethylformamide-κO)bis[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ³O,O':N]cadmium(II)] N,N-dimethylformamide monosolvate methanol monosolvate] (1845689) top

Crystal data top

[Cd(C₁₂H₇N₂O₄)₂(C₃H₇NO)]·C₃H₇NO·CH₄O	F(000) = 1352
M_r = 671.89	D_x = 1.249 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 12.829 (5) Å	Cell parameters from 5739 reflections
b = 15.854 (6) Å	θ = 2.3–27.1°
c = 20.769 (6) Å	µ = 0.66 mm⁻¹
β = 122.215 (18)°	T = 150 K
V = 3574 (2) Å³	Block, pale yellow
Z = 4	0.23 × 0.21 × 0.20 mm

Data collection top

Bruker D8 Venture diffractometer	5765 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.039
ω scans	θ_max = 26.0°, θ_min = 3.0°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −15→15
T_min = 0.863, T_max = 0.879	k = −19→19
37455 measured reflections	l = −25→25
6942 independent reflections

Refinement top

Refinement on F²	157 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.056	H-atom parameters constrained
wR(F²) = 0.136	w = 1/[σ²(F_o²) + (0.0393P)² + 9.3747P] where P = (F_o² + 2F_c²)/3
S = 1.14	(Δ/σ)_max = 0.001
6942 reflections	Δρ_max = 2.10 e Å⁻³
407 parameters	Δρ_min = −1.10 e Å⁻³

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cd1	0.39798 (3)	0.52414 (2)	0.22861 (2)	0.04032 (12)
O1	0.5140 (4)	0.4138 (2)	0.3263 (2)	0.0753 (11)
O2	0.3145 (4)	0.4122 (2)	0.2630 (2)	0.0748 (10)
O3	0.6701 (5)	0.1328 (3)	0.5592 (3)	0.1142 (18)
O4	0.7464 (5)	0.2559 (4)	0.5651 (3)	0.126 (2)
O5	1.3191 (3)	0.8574 (2)	0.6401 (2)	0.0689 (10)
O6	1.1926 (3)	0.9557 (3)	0.6306 (2)	0.0816 (12)
O7	0.9997 (6)	0.6001 (4)	0.4008 (4)	0.145 (2)
O8	1.1370 (6)	0.5846 (3)	0.5157 (4)	0.148 (3)
O9	0.3605 (7)	0.6051 (4)	0.3111 (4)	0.139 (2)
N1	0.4284 (4)	0.0538 (2)	0.6440 (2)	0.0534 (9)
N2	0.6613 (5)	0.2050 (4)	0.5390 (3)	0.0786 (13)
N3	0.5850 (3)	0.5945 (2)	0.2950 (2)	0.0503 (9)
N4	1.0563 (5)	0.6244 (3)	0.4655 (4)	0.101 (2)
N5	0.3679 (15)	0.5395 (8)	0.4189 (9)	0.212 (4)
C1	0.4748 (5)	0.1314 (3)	0.6606 (3)	0.0631 (13)
H1A	0.505878	0.152505	0.710446	0.076*
C2	0.4799 (5)	0.1824 (3)	0.6090 (3)	0.0696 (14)
H2A	0.513217	0.237611	0.623344	0.084*
C3	0.4369 (5)	0.1537 (3)	0.5369 (3)	0.0586 (12)
C4	0.3893 (6)	0.0739 (4)	0.5195 (3)	0.0767 (17)
H4A	0.358176	0.051444	0.470093	0.092*
C5	0.3868 (6)	0.0263 (3)	0.5742 (3)	0.0719 (16)
H5A	0.353549	−0.029095	0.561130	0.086*
C6	0.4352 (5)	0.2088 (3)	0.4780 (3)	0.0583 (12)
C7	0.5381 (5)	0.2369 (3)	0.4806 (3)	0.0585 (11)
C8	0.5336 (5)	0.2935 (3)	0.4289 (3)	0.0577 (11)
H8A	0.607535	0.311982	0.433265	0.069*
C9	0.4226 (5)	0.3230 (3)	0.3714 (2)	0.0520 (10)
C10	0.3169 (5)	0.2956 (4)	0.3665 (3)	0.0761 (16)
H10A	0.238927	0.315052	0.326286	0.091*
C11	0.3233 (5)	0.2398 (4)	0.4200 (4)	0.0852 (19)
H11A	0.249614	0.222563	0.416669	0.102*
C12	0.4161 (5)	0.3873 (3)	0.3162 (3)	0.0577 (11)
C13	0.6705 (5)	0.5682 (4)	0.3637 (3)	0.0812 (19)
H13A	0.658520	0.515333	0.380352	0.097*
C14	0.7757 (5)	0.6125 (4)	0.4124 (3)	0.0838 (19)
H14A	0.832316	0.591897	0.462166	0.101*
C15	0.7980 (4)	0.6868 (3)	0.3884 (3)	0.0536 (11)
C16	0.7116 (5)	0.7141 (3)	0.3165 (3)	0.0690 (15)
H16A	0.723872	0.765052	0.297331	0.083*
C17	0.6066 (4)	0.6665 (3)	0.2722 (3)	0.0606 (13)
H17A	0.546855	0.686668	0.222837	0.073*
C18	0.9077 (4)	0.7380 (3)	0.4407 (3)	0.0554 (11)
C19	1.0264 (4)	0.7082 (3)	0.4814 (3)	0.0580 (12)
C20	1.1254 (4)	0.7553 (3)	0.5358 (3)	0.0564 (11)
H20A	1.206025	0.731969	0.562101	0.068*
C21	1.1064 (4)	0.8354 (3)	0.5514 (3)	0.0543 (11)
C22	0.9893 (5)	0.8687 (3)	0.5113 (4)	0.0783 (18)
H22A	0.975007	0.924717	0.520886	0.094*
C23	0.8917 (4)	0.8198 (3)	0.4564 (3)	0.0772 (17)
H23A	0.811422	0.843694	0.428823	0.093*
C24	1.2131 (4)	0.8857 (3)	0.6112 (3)	0.0579 (11)
C25	0.303 (2)	0.5777 (14)	0.3405 (12)	0.171 (3)	0.558 (12)
H25A	0.216120	0.581242	0.312223	0.205*	0.558 (12)
C25A	0.393 (3)	0.588 (2)	0.3730 (13)	0.194 (5)	0.442 (12)
H25B	0.466305	0.618474	0.405429	0.233*	0.442 (12)
C26	0.504 (2)	0.5604 (13)	0.4556 (12)	0.214 (6)	0.558 (12)
H26A	0.519247	0.580357	0.416564	0.320*	0.558 (12)
H26B	0.527793	0.604443	0.494073	0.320*	0.558 (12)
H26C	0.553685	0.509640	0.479859	0.320*	0.558 (12)
C26A	0.3825 (11)	0.491 (2)	0.4844 (14)	0.214 (6)	0.442 (12)
H26D	0.302132	0.469387	0.471683	0.321*	0.442 (12)
H26E	0.439110	0.443893	0.495954	0.321*	0.442 (12)
H26F	0.415853	0.528165	0.528932	0.321*	0.442 (12)
C27	0.284 (3)	0.5088 (19)	0.4401 (18)	0.209 (5)	0.558 (12)
H27A	0.331845	0.484792	0.491446	0.313*	0.558 (12)
H27B	0.233754	0.555511	0.439267	0.313*	0.558 (12)
H27C	0.231179	0.465204	0.404019	0.313*	0.558 (12)
C27A	0.228 (2)	0.545 (2)	0.3564 (14)	0.203 (5)	0.442 (12)
H27D	0.180466	0.514209	0.373396	0.305*	0.442 (12)
H27E	0.202087	0.604297	0.347645	0.305*	0.442 (12)
H27F	0.212958	0.520128	0.309071	0.305*	0.442 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.04007 (18)	0.03512 (17)	0.03677 (17)	0.00016 (11)	0.01445 (13)	0.00110 (11)
O1	0.084 (2)	0.067 (2)	0.0543 (19)	−0.0084 (16)	0.0233 (18)	0.0321 (14)
O2	0.098 (3)	0.056 (2)	0.072 (2)	0.0002 (17)	0.047 (2)	0.0255 (18)
O3	0.109 (4)	0.098 (4)	0.133 (4)	0.046 (3)	0.063 (3)	0.052 (3)
O4	0.070 (3)	0.162 (5)	0.109 (4)	−0.011 (3)	0.023 (3)	0.034 (4)
O5	0.0439 (16)	0.064 (2)	0.064 (2)	−0.0109 (15)	0.0054 (16)	−0.0100 (17)
O6	0.052 (2)	0.080 (3)	0.090 (3)	−0.0184 (18)	0.023 (2)	−0.038 (2)
O7	0.113 (4)	0.128 (4)	0.144 (5)	0.003 (3)	0.036 (3)	−0.078 (4)
O8	0.128 (4)	0.074 (3)	0.163 (5)	0.041 (3)	0.024 (4)	−0.012 (3)
O9	0.206 (5)	0.119 (4)	0.170 (5)	−0.015 (4)	0.153 (4)	−0.049 (3)
N1	0.065 (2)	0.050 (2)	0.0447 (18)	0.0019 (18)	0.0295 (18)	0.0064 (16)
N2	0.070 (3)	0.099 (4)	0.068 (3)	0.013 (3)	0.038 (2)	0.021 (3)
N3	0.0446 (19)	0.045 (2)	0.0400 (18)	−0.0056 (15)	0.0084 (15)	0.0026 (15)
N4	0.062 (3)	0.066 (3)	0.125 (5)	0.002 (3)	0.017 (3)	−0.036 (3)
N5	0.249 (7)	0.207 (6)	0.212 (6)	−0.028 (6)	0.145 (6)	−0.020 (5)
C1	0.073 (3)	0.060 (3)	0.047 (3)	−0.009 (2)	0.026 (2)	0.005 (2)
C2	0.084 (4)	0.057 (3)	0.063 (3)	−0.017 (3)	0.036 (3)	0.000 (2)
C3	0.067 (3)	0.057 (3)	0.059 (3)	0.002 (2)	0.038 (2)	0.011 (2)
C4	0.121 (5)	0.062 (3)	0.052 (3)	−0.016 (3)	0.049 (3)	−0.003 (2)
C5	0.115 (5)	0.049 (3)	0.060 (3)	−0.018 (3)	0.052 (3)	−0.003 (2)
C6	0.070 (3)	0.055 (3)	0.051 (3)	−0.002 (2)	0.033 (2)	0.011 (2)
C7	0.066 (3)	0.059 (3)	0.053 (3)	0.004 (2)	0.034 (2)	0.011 (2)
C8	0.064 (3)	0.062 (3)	0.058 (3)	−0.007 (2)	0.039 (2)	0.002 (2)
C9	0.074 (3)	0.042 (2)	0.045 (2)	−0.004 (2)	0.036 (2)	0.0015 (18)
C10	0.064 (3)	0.094 (4)	0.065 (3)	0.007 (3)	0.031 (3)	0.030 (3)
C11	0.058 (3)	0.109 (5)	0.087 (4)	0.001 (3)	0.037 (3)	0.044 (4)
C12	0.093 (3)	0.037 (2)	0.048 (2)	−0.012 (2)	0.040 (2)	−0.0058 (18)
C13	0.059 (3)	0.061 (3)	0.064 (3)	−0.021 (2)	−0.007 (2)	0.023 (3)
C14	0.068 (3)	0.068 (3)	0.059 (3)	−0.020 (3)	−0.005 (3)	0.018 (3)
C15	0.042 (2)	0.041 (2)	0.052 (2)	−0.0059 (18)	0.0075 (19)	−0.0003 (18)
C16	0.058 (3)	0.056 (3)	0.058 (3)	−0.018 (2)	0.007 (2)	0.015 (2)
C17	0.050 (3)	0.057 (3)	0.044 (2)	−0.015 (2)	0.003 (2)	0.010 (2)
C18	0.045 (2)	0.043 (2)	0.053 (3)	−0.0046 (18)	0.009 (2)	0.0011 (19)
C19	0.048 (2)	0.045 (2)	0.062 (3)	−0.0049 (19)	0.017 (2)	−0.009 (2)
C20	0.042 (2)	0.054 (3)	0.059 (3)	−0.004 (2)	0.017 (2)	−0.003 (2)
C21	0.041 (2)	0.050 (3)	0.055 (3)	−0.0090 (19)	0.014 (2)	−0.006 (2)
C22	0.050 (3)	0.045 (3)	0.099 (4)	−0.001 (2)	0.013 (3)	−0.015 (3)
C23	0.040 (2)	0.050 (3)	0.090 (4)	0.003 (2)	0.000 (3)	−0.005 (3)
C24	0.049 (2)	0.055 (3)	0.051 (3)	−0.016 (2)	0.014 (2)	−0.005 (2)
C25	0.219 (7)	0.177 (7)	0.198 (6)	−0.032 (6)	0.166 (5)	−0.034 (6)
C25A	0.230 (7)	0.181 (7)	0.205 (7)	−0.018 (6)	0.140 (6)	−0.036 (6)
C26	0.238 (9)	0.203 (8)	0.213 (8)	−0.009 (8)	0.129 (7)	−0.039 (8)
C26A	0.251 (9)	0.215 (9)	0.207 (9)	−0.024 (8)	0.143 (8)	−0.007 (8)
C27	0.243 (8)	0.216 (8)	0.211 (8)	−0.029 (8)	0.150 (7)	−0.007 (7)
C27A	0.236 (8)	0.207 (8)	0.211 (8)	−0.028 (7)	0.148 (7)	−0.017 (7)

Geometric parameters (Å, º) top

Cd1—N3	2.318 (4)	C7—C8	1.377 (6)
Cd1—O6ⁱ	2.339 (4)	C8—C9	1.363 (7)
Cd1—N1ⁱⁱ	2.344 (4)	C8—H8A	0.9500
Cd1—O2	2.372 (3)	C9—C10	1.376 (7)
Cd1—O9	2.386 (5)	C9—C12	1.503 (6)
Cd1—O5ⁱ	2.438 (3)	C10—C11	1.388 (7)
Cd1—O1	2.484 (3)	C10—H10A	0.9500
Cd1—C24ⁱ	2.729 (4)	C11—H11A	0.9500
Cd1—C12	2.759 (5)	C13—C14	1.373 (7)
O1—C12	1.232 (6)	C13—H13A	0.9500
O2—C12	1.241 (6)	C14—C15	1.367 (7)
O3—N2	1.204 (7)	C14—H14A	0.9500
O4—N2	1.227 (7)	C15—C16	1.372 (6)
O5—C24	1.240 (6)	C15—C18	1.480 (6)
O6—C24	1.255 (6)	C16—C17	1.381 (6)
O7—N4	1.200 (8)	C16—H16A	0.9500
O8—N4	1.187 (7)	C17—H17A	0.9500
O9—C25A	1.154 (17)	C18—C19	1.373 (6)
O9—C25	1.255 (15)	C18—C23	1.378 (7)
N1—C5	1.324 (6)	C19—C20	1.385 (6)
N1—C1	1.330 (6)	C20—C21	1.365 (7)
N2—C7	1.477 (7)	C20—H20A	0.9500
N3—C13	1.321 (6)	C21—C22	1.376 (7)
N3—C17	1.321 (6)	C21—C24	1.496 (6)
N4—C19	1.469 (7)	C22—C23	1.395 (7)
N5—C25A	1.387 (17)	C22—H22A	0.9500
N5—C27	1.442 (16)	C23—H23A	0.9500
N5—C26A	1.485 (16)	C25—H25A	0.9500
N5—C25	1.504 (17)	C25A—H25B	0.9500
N5—C26	1.528 (17)	C26—H26A	0.9800
N5—C27A	1.560 (17)	C26—H26B	0.9800
C1—C2	1.370 (7)	C26—H26C	0.9800
C1—H1A	0.9500	C26A—H26D	0.9800
C2—C3	1.369 (7)	C26A—H26E	0.9800
C2—H2A	0.9500	C26A—H26F	0.9800
C3—C4	1.367 (7)	C27—H27A	0.9800
C3—C6	1.495 (6)	C27—H27B	0.9800
C4—C5	1.379 (7)	C27—H27C	0.9800
C4—H4A	0.9500	C27A—H27D	0.9800
C5—H5A	0.9500	C27A—H27E	0.9800
C6—C7	1.366 (7)	C27A—H27F	0.9800
C6—C11	1.382 (7)

N3—Cd1—O6ⁱ	141.28 (13)	C8—C9—C10	119.0 (4)
N3—Cd1—N1ⁱⁱ	99.57 (14)	C8—C9—C12	120.6 (5)
O6ⁱ—Cd1—N1ⁱⁱ	88.85 (16)	C10—C9—C12	120.4 (5)
N3—Cd1—O2	132.17 (13)	C9—C10—C11	120.5 (5)
O6ⁱ—Cd1—O2	83.37 (14)	C9—C10—H10A	119.8
N1ⁱⁱ—Cd1—O2	96.54 (14)	C11—C10—H10A	119.8
N3—Cd1—O9	81.6 (2)	C6—C11—C10	121.0 (5)
O6ⁱ—Cd1—O9	89.2 (2)	C6—C11—H11A	119.5
N1ⁱⁱ—Cd1—O9	178.0 (2)	C10—C11—H11A	119.5
O2—Cd1—O9	83.69 (19)	O1—C12—O2	122.4 (4)
N3—Cd1—O5ⁱ	87.70 (12)	O1—C12—C9	117.6 (5)
O6ⁱ—Cd1—O5ⁱ	54.27 (13)	O2—C12—C9	119.9 (5)
N1ⁱⁱ—Cd1—O5ⁱ	90.53 (14)	O1—C12—Cd1	64.2 (2)
O2—Cd1—O5ⁱ	136.94 (13)	O2—C12—Cd1	59.0 (2)
O9—Cd1—O5ⁱ	88.0 (2)	C9—C12—Cd1	170.7 (3)
N3—Cd1—O1	82.73 (13)	N3—C13—C14	124.0 (5)
O6ⁱ—Cd1—O1	135.55 (13)	N3—C13—H13A	118.0
N1ⁱⁱ—Cd1—O1	88.53 (14)	C14—C13—H13A	118.0
O2—Cd1—O1	52.94 (14)	C15—C14—C13	119.2 (5)
O9—Cd1—O1	93.2 (2)	C15—C14—H14A	120.4
O5ⁱ—Cd1—O1	170.09 (12)	C13—C14—H14A	120.4
N3—Cd1—C24ⁱ	114.21 (15)	C14—C15—C16	117.6 (4)
O6ⁱ—Cd1—C24ⁱ	27.31 (14)	C14—C15—C18	120.5 (4)
N1ⁱⁱ—Cd1—C24ⁱ	91.11 (15)	C16—C15—C18	121.8 (4)
O2—Cd1—C24ⁱ	110.13 (16)	C15—C16—C17	119.2 (4)
O9—Cd1—C24ⁱ	87.0 (2)	C15—C16—H16A	120.4
O5ⁱ—Cd1—C24ⁱ	27.03 (14)	C17—C16—H16A	120.4
O1—Cd1—C24ⁱ	162.84 (15)	N3—C17—C16	123.4 (4)
N3—Cd1—C12	106.82 (15)	N3—C17—H17A	118.3
O6ⁱ—Cd1—C12	109.96 (16)	C16—C17—H17A	118.3
N1ⁱⁱ—Cd1—C12	95.18 (14)	C19—C18—C23	115.8 (4)
O2—Cd1—C12	26.64 (15)	C19—C18—C15	124.9 (4)
O9—Cd1—C12	85.9 (2)	C23—C18—C15	119.1 (4)
O5ⁱ—Cd1—C12	163.20 (15)	C18—C19—C20	123.4 (4)
O1—Cd1—C12	26.51 (14)	C18—C19—N4	120.7 (4)
C24ⁱ—Cd1—C12	136.75 (17)	C20—C19—N4	115.8 (4)
C12—O1—Cd1	89.3 (3)	C21—C20—C19	119.5 (4)
C12—O2—Cd1	94.4 (3)	C21—C20—H20A	120.2
C24—O5—Cd1ⁱⁱⁱ	89.7 (3)	C19—C20—H20A	120.2
C24—O6—Cd1ⁱⁱⁱ	93.9 (3)	C20—C21—C22	119.2 (4)
C25A—O9—Cd1	125 (2)	C20—C21—C24	119.5 (4)
C25—O9—Cd1	123.8 (11)	C22—C21—C24	121.3 (5)
C5—N1—C1	116.9 (4)	C21—C22—C23	119.8 (5)
C5—N1—Cd1^iv	121.1 (3)	C21—C22—H22A	120.1
C1—N1—Cd1^iv	121.6 (3)	C23—C22—H22A	120.1
O3—N2—O4	125.1 (6)	C18—C23—C22	122.2 (5)
O3—N2—C7	118.2 (6)	C18—C23—H23A	118.9
O4—N2—C7	116.7 (5)	C22—C23—H23A	118.9
C13—N3—C17	116.6 (4)	O5—C24—O6	121.8 (4)
C13—N3—Cd1	119.4 (3)	O5—C24—C21	119.4 (5)
C17—N3—Cd1	123.5 (3)	O6—C24—C21	118.8 (5)
O8—N4—O7	122.5 (6)	O5—C24—Cd1ⁱⁱⁱ	63.3 (2)
O8—N4—C19	119.6 (6)	O6—C24—Cd1ⁱⁱⁱ	58.7 (2)
O7—N4—C19	117.9 (6)	C21—C24—Cd1ⁱⁱⁱ	174.5 (4)
C25A—N5—C26A	162.3 (19)	O9—C25—N5	122.7 (18)
C27—N5—C25	113.4 (18)	O9—C25—H25A	118.6
C27—N5—C26	139.5 (18)	N5—C25—H25A	118.6
C25—N5—C26	106.0 (13)	O9—C25A—N5	145 (3)
C25A—N5—C27A	89 (2)	O9—C25A—H25B	107.5
C26A—N5—C27A	108.5 (13)	N5—C25A—H25B	107.5
N1—C1—C2	123.0 (5)	N5—C26—H26A	109.5
N1—C1—H1A	118.5	N5—C26—H26B	109.5
C2—C1—H1A	118.5	H26A—C26—H26B	109.5
C3—C2—C1	120.0 (5)	N5—C26—H26C	109.5
C3—C2—H2A	120.0	H26A—C26—H26C	109.5
C1—C2—H2A	120.0	H26B—C26—H26C	109.5
C4—C3—C2	117.4 (5)	N5—C26A—H26D	109.5
C4—C3—C6	121.0 (5)	N5—C26A—H26E	109.5
C2—C3—C6	121.5 (5)	H26D—C26A—H26E	109.5
C3—C4—C5	119.5 (5)	N5—C26A—H26F	109.5
C3—C4—H4A	120.3	H26D—C26A—H26F	109.5
C5—C4—H4A	120.3	H26E—C26A—H26F	109.5
N1—C5—C4	123.3 (5)	N5—C27—H27A	109.5
N1—C5—H5A	118.3	N5—C27—H27B	109.5
C4—C5—H5A	118.3	H27A—C27—H27B	109.5
C7—C6—C11	116.8 (4)	N5—C27—H27C	109.5
C7—C6—C3	124.5 (5)	H27A—C27—H27C	109.5
C11—C6—C3	118.4 (5)	H27B—C27—H27C	109.5
C6—C7—C8	122.9 (5)	N5—C27A—H27D	109.5
C6—C7—N2	120.6 (4)	N5—C27A—H27E	109.5
C8—C7—N2	116.4 (5)	H27D—C27A—H27E	109.5
C9—C8—C7	119.8 (5)	N5—C27A—H27F	109.5
C9—C8—H8A	120.1	H27D—C27A—H27F	109.5
C7—C8—H8A	120.1	H27E—C27A—H27F	109.5

C5—N1—C1—C2	0.5 (8)	C13—C14—C15—C16	1.2 (10)
Cd1^iv—N1—C1—C2	−171.8 (4)	C13—C14—C15—C18	177.2 (6)
N1—C1—C2—C3	−0.6 (9)	C14—C15—C16—C17	0.7 (9)
C1—C2—C3—C4	0.4 (9)	C18—C15—C16—C17	−175.2 (5)
C1—C2—C3—C6	177.0 (5)	C13—N3—C17—C16	−0.6 (9)
C2—C3—C4—C5	−0.2 (9)	Cd1—N3—C17—C16	171.0 (5)
C6—C3—C4—C5	−176.8 (6)	C15—C16—C17—N3	−1.1 (9)
C1—N1—C5—C4	−0.2 (9)	C14—C15—C18—C19	52.4 (8)
Cd1^iv—N1—C5—C4	172.1 (5)	C16—C15—C18—C19	−131.7 (6)
C3—C4—C5—N1	0.1 (11)	C14—C15—C18—C23	−121.3 (7)
C4—C3—C6—C7	−115.7 (7)	C16—C15—C18—C23	54.5 (8)
C2—C3—C6—C7	67.9 (8)	C23—C18—C19—C20	1.0 (8)
C4—C3—C6—C11	70.0 (8)	C15—C18—C19—C20	−173.0 (5)
C2—C3—C6—C11	−106.4 (7)	C23—C18—C19—N4	−175.2 (6)
C11—C6—C7—C8	0.2 (8)	C15—C18—C19—N4	10.8 (9)
C3—C6—C7—C8	−174.2 (5)	O8—N4—C19—C18	−147.9 (7)
C11—C6—C7—N2	−177.9 (6)	O7—N4—C19—C18	34.4 (10)
C3—C6—C7—N2	7.7 (8)	O8—N4—C19—C20	35.6 (10)
O3—N2—C7—C6	34.2 (8)	O7—N4—C19—C20	−142.1 (7)
O4—N2—C7—C6	−143.2 (6)	C18—C19—C20—C21	0.6 (8)
O3—N2—C7—C8	−144.1 (6)	N4—C19—C20—C21	176.9 (5)
O4—N2—C7—C8	38.6 (8)	C19—C20—C21—C22	−1.6 (8)
C6—C7—C8—C9	−0.9 (8)	C19—C20—C21—C24	178.9 (5)
N2—C7—C8—C9	177.2 (5)	C20—C21—C22—C23	1.1 (9)
C7—C8—C9—C10	0.3 (8)	C24—C21—C22—C23	−179.4 (6)
C7—C8—C9—C12	177.7 (4)	C19—C18—C23—C22	−1.4 (10)
C8—C9—C10—C11	0.9 (9)	C15—C18—C23—C22	172.9 (6)
C12—C9—C10—C11	−176.4 (6)	C21—C22—C23—C18	0.4 (11)
C7—C6—C11—C10	1.0 (10)	Cd1ⁱⁱⁱ—O5—C24—O6	5.7 (5)
C3—C6—C11—C10	175.8 (6)	Cd1ⁱⁱⁱ—O5—C24—C21	−174.6 (4)
C9—C10—C11—C6	−1.6 (11)	Cd1ⁱⁱⁱ—O6—C24—O5	−5.9 (6)
Cd1—O1—C12—O2	9.8 (5)	Cd1ⁱⁱⁱ—O6—C24—C21	174.3 (4)
Cd1—O1—C12—C9	−169.8 (4)	C20—C21—C24—O5	7.6 (8)
Cd1—O2—C12—O1	−10.3 (5)	C22—C21—C24—O5	−171.9 (6)
Cd1—O2—C12—C9	169.3 (4)	C20—C21—C24—O6	−172.7 (5)
C8—C9—C12—O1	−2.1 (7)	C22—C21—C24—O6	7.9 (8)
C10—C9—C12—O1	175.2 (5)	Cd1—O9—C25—N5	94 (2)
C8—C9—C12—O2	178.3 (5)	C27—N5—C25—O9	−177 (2)
C10—C9—C12—O2	−4.4 (7)	C26—N5—C25—O9	12 (3)
C17—N3—C13—C14	2.7 (10)	Cd1—O9—C25A—N5	−82 (6)
Cd1—N3—C13—C14	−169.2 (6)	C26A—N5—C25A—O9	156 (6)
N3—C13—C14—C15	−3.1 (12)	C27A—N5—C25A—O9	−29 (6)

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

Poly[[(µ₂-acetato-κ²O:O')[µ₃-3-nitro-4-(pyridin-4-yl)benzoato-κ³O:O':N]bis[µ₃-3-nitro-4-(pyridin-4-yl)benzoato-κ⁴O,O':O':N]dicadmium(II)] N,N-dimethylacetamide disolvate monohydrate] (1831564) top

Crystal data top

[Cd₂(C₁₂H₇N₂O₄)₃(C₂H₃O₂)]·2C₄H₉NO·H₂O	Z = 2
M_r = 1013.43	F(000) = 1004
Triclinic, P1	D_x = 1.257 Mg m⁻³
a = 8.342 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 13.903 (6) Å	Cell parameters from 3383 reflections
c = 23.568 (10) Å	θ = 2.4–26.8°
α = 86.840 (6)°	µ = 0.85 mm⁻¹
β = 89.264 (6)°	T = 296 K
γ = 78.826 (6)°	Needle, colorless
V = 2678 (2) Å³	0.25 × 0.12 × 0.10 mm

Data collection top

Bruker APEXII CCD diffractometer	5864 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.064
ω scans	θ_max = 25.5°, θ_min = 0.9°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −10→8
T_min = 0.816, T_max = 0.920	k = −16→16
19339 measured reflections	l = −28→28
9673 independent reflections

Refinement top

Refinement on F²	43 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.068	H-atom parameters constrained
wR(F²) = 0.168	w = 1/[σ²(F_o²) + (0.0899P)²] where P = (F_o² + 2F_c²)/3
S = 0.92	(Δ/σ)_max < 0.001
9673 reflections	Δρ_max = 2.47 e Å⁻³
542 parameters	Δρ_min = −1.40 e Å⁻³

Special details top

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

	x	y	z	U_iso*/U_eq
Cd1	0.14848 (6)	0.39801 (4)	0.25248 (2)	0.03564 (17)
Cd2	0.58087 (6)	0.29285 (4)	0.25474 (2)	0.03282 (17)
O1	0.5705 (6)	0.4585 (3)	0.2500 (2)	0.0446 (13)
O2	0.2986 (6)	0.5166 (3)	0.2466 (2)	0.0451 (13)
O3	0.9204 (9)	0.7147 (7)	0.2344 (4)	0.120 (3)
O4	0.8411 (10)	0.8193 (7)	0.2932 (5)	0.135 (4)
O5	0.6035 (7)	0.2934 (4)	0.3567 (2)	0.0560 (15)
O6	0.3557 (7)	0.3230 (4)	0.3234 (2)	0.0529 (14)
O7	0.6635 (10)	0.3956 (8)	0.5551 (4)	0.123 (3)
O8	0.5107 (9)	0.3274 (7)	0.6121 (3)	0.106 (3)
O9	0.3424 (7)	0.3183 (4)	0.1859 (2)	0.0569 (15)
O10	0.5922 (6)	0.2976 (4)	0.1543 (2)	0.0513 (14)
O11	0.5117 (9)	0.3371 (6)	−0.1041 (3)	0.103 (3)
O12	0.6622 (10)	0.3982 (7)	−0.0495 (3)	0.115 (3)
O13	0.8562 (8)	0.2748 (5)	0.2537 (3)	0.0736 (19)
O14	1.1062 (10)	0.2465 (6)	0.2710 (4)	0.125 (3)
C1	0.4715 (14)	1.0874 (7)	0.2944 (4)	0.089 (4)
H1A	0.419775	1.125696	0.322910	0.107*
C2	0.4566 (15)	0.9920 (7)	0.2958 (4)	0.091 (4)
H2A	0.393948	0.968087	0.324205	0.109*
C3	0.5325 (10)	0.9299 (5)	0.2559 (4)	0.048 (2)
C4	0.6150 (13)	0.9727 (7)	0.2159 (4)	0.081 (3)
H4A	0.667508	0.934800	0.187288	0.097*
C5	0.6253 (15)	1.0731 (6)	0.2153 (4)	0.090 (4)
H5A	0.682748	1.099857	0.186390	0.108*
C6	0.5156 (10)	0.8261 (5)	0.2547 (3)	0.0457 (19)
C7	0.6457 (9)	0.7479 (5)	0.2544 (3)	0.045 (2)
C8	0.6257 (9)	0.6507 (5)	0.2516 (3)	0.0394 (18)
H8A	0.716696	0.600128	0.251074	0.047*
C9	0.4716 (8)	0.6302 (5)	0.2498 (3)	0.0325 (16)
C10	0.3384 (9)	0.7069 (5)	0.2500 (3)	0.046 (2)
H10A	0.233277	0.694309	0.247658	0.056*
C11	0.3617 (9)	0.8033 (6)	0.2538 (4)	0.052 (2)
H11A	0.270674	0.853643	0.255663	0.062*
C12	0.4449 (9)	0.5263 (5)	0.2485 (3)	0.0361 (17)
C13	0.1425 (9)	0.5448 (6)	0.6554 (3)	0.047 (2)
H13A	0.177900	0.596846	0.671081	0.057*
C14	0.2276 (9)	0.5006 (6)	0.6102 (3)	0.050 (2)
H14A	0.321436	0.521777	0.597357	0.060*
C15	0.1775 (9)	0.4261 (6)	0.5839 (3)	0.0425 (19)
C16	0.0390 (11)	0.3955 (6)	0.6076 (3)	0.055 (2)
H16A	0.000241	0.344135	0.592321	0.065*
C17	−0.0385 (10)	0.4410 (6)	0.6529 (3)	0.050 (2)
H17A	−0.129936	0.419142	0.667553	0.060*
C18	0.2537 (11)	0.3867 (6)	0.5304 (3)	0.052 (2)
C19	0.4242 (10)	0.3661 (6)	0.5198 (3)	0.049 (2)
C20	0.4853 (10)	0.3418 (6)	0.4678 (3)	0.048 (2)
H20A	0.598002	0.327871	0.462660	0.058*
C21	0.3836 (10)	0.3373 (5)	0.4217 (3)	0.047 (2)
C22	0.2162 (10)	0.3534 (6)	0.4321 (3)	0.048 (2)
H22A	0.145266	0.347257	0.403001	0.057*
C23	0.1538 (9)	0.3783 (6)	0.4849 (3)	0.047 (2)
H23A	0.041160	0.389869	0.490216	0.056*
C24	0.4531 (11)	0.3167 (5)	0.3642 (3)	0.044 (2)
C25	0.1403 (9)	0.5463 (6)	−0.1583 (3)	0.0446 (19)
H25A	0.175434	0.598206	−0.178053	0.053*
C26	0.2251 (9)	0.5056 (6)	−0.1117 (3)	0.051 (2)
H26A	0.316211	0.528922	−0.100283	0.061*
C27	0.1745 (9)	0.4276 (6)	−0.0805 (3)	0.0433 (19)
C28	0.0410 (10)	0.3968 (6)	−0.1009 (3)	0.050 (2)
H28A	0.005523	0.343808	−0.082486	0.061*
C29	−0.0404 (9)	0.4421 (5)	−0.1474 (3)	0.0438 (19)
H29A	−0.133626	0.421179	−0.158965	0.053*
C30	0.2521 (10)	0.3881 (6)	−0.0251 (3)	0.0448 (19)
C31	0.4202 (10)	0.3675 (6)	−0.0131 (3)	0.050 (2)
C32	0.4816 (10)	0.3433 (6)	0.0407 (3)	0.049 (2)
H32A	0.593790	0.331484	0.046804	0.058*
C33	0.3756 (9)	0.3367 (5)	0.0857 (3)	0.0383 (17)
C34	0.2097 (9)	0.3524 (6)	0.0753 (3)	0.049 (2)
H34A	0.137646	0.346814	0.105162	0.059*
C35	0.1504 (9)	0.3758 (6)	0.0217 (3)	0.048 (2)
H35A	0.038455	0.384029	0.015766	0.058*
C36	0.4416 (11)	0.3172 (5)	0.1459 (3)	0.045 (2)
C37	0.9741 (12)	0.2203 (7)	0.2677 (5)	0.078 (3)
C38	0.9694 (17)	0.1119 (10)	0.2870 (8)	0.181 (6)
H38A	0.916450	0.082685	0.258367	0.271*
H38B	0.909941	0.110404	0.322049	0.271*
H38C	1.078938	0.075724	0.292373	0.271*
N1	0.5531 (8)	1.1297 (4)	0.2560 (3)	0.0457 (16)
N2	0.8123 (10)	0.7629 (5)	0.2586 (4)	0.071 (2)
N3	0.0088 (7)	0.5148 (4)	0.6775 (2)	0.0385 (14)
N4	0.5415 (11)	0.3618 (8)	0.5653 (4)	0.085 (3)
N5	0.0090 (7)	0.5168 (4)	−0.1777 (2)	0.0397 (15)
N6	0.5403 (10)	0.3666 (7)	−0.0588 (3)	0.076 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0353 (3)	0.0412 (3)	0.0333 (3)	−0.0140 (2)	0.0020 (2)	−0.0049 (2)
Cd2	0.0411 (3)	0.0278 (3)	0.0333 (3)	−0.0153 (2)	0.0013 (2)	−0.0041 (2)
O1	0.047 (3)	0.028 (3)	0.062 (4)	−0.014 (2)	0.006 (3)	−0.007 (2)
O2	0.034 (3)	0.037 (3)	0.069 (4)	−0.016 (2)	−0.003 (3)	−0.006 (3)
O3	0.046 (5)	0.122 (7)	0.207 (10)	−0.040 (5)	0.033 (5)	−0.056 (7)
O4	0.095 (6)	0.106 (6)	0.219 (10)	−0.043 (5)	−0.035 (6)	−0.050 (6)
O5	0.039 (3)	0.062 (4)	0.068 (4)	−0.012 (3)	0.018 (3)	−0.013 (3)
O6	0.068 (4)	0.052 (3)	0.035 (3)	−0.002 (3)	−0.004 (3)	−0.006 (3)
O7	0.069 (6)	0.197 (10)	0.113 (7)	−0.033 (6)	−0.029 (5)	−0.049 (6)
O8	0.084 (5)	0.157 (7)	0.064 (4)	0.007 (5)	−0.009 (4)	−0.006 (5)
O9	0.077 (4)	0.054 (3)	0.033 (3)	0.004 (3)	−0.004 (3)	−0.001 (3)
O10	0.037 (3)	0.049 (3)	0.072 (4)	−0.019 (3)	−0.008 (3)	0.004 (3)
O11	0.075 (5)	0.166 (8)	0.053 (4)	0.017 (5)	0.007 (4)	−0.018 (5)
O12	0.060 (5)	0.198 (10)	0.093 (6)	−0.047 (6)	0.022 (4)	0.020 (6)
O13	0.067 (5)	0.082 (5)	0.070 (4)	−0.017 (4)	0.001 (4)	0.014 (4)
O14	0.093 (5)	0.094 (5)	0.198 (7)	−0.050 (5)	−0.008 (5)	0.016 (5)
C1	0.141 (10)	0.046 (6)	0.091 (8)	−0.046 (6)	0.050 (7)	−0.020 (5)
C2	0.138 (10)	0.057 (6)	0.087 (8)	−0.045 (7)	0.058 (7)	−0.019 (6)
C3	0.052 (5)	0.029 (4)	0.067 (6)	−0.013 (4)	0.001 (4)	−0.004 (4)
C4	0.114 (7)	0.053 (5)	0.082 (6)	−0.029 (5)	0.040 (5)	−0.025 (5)
C5	0.164 (10)	0.032 (5)	0.084 (7)	−0.040 (6)	0.040 (7)	−0.013 (5)
C6	0.048 (5)	0.029 (4)	0.064 (5)	−0.016 (4)	−0.002 (4)	−0.007 (4)
C7	0.035 (4)	0.034 (4)	0.069 (6)	−0.017 (4)	−0.005 (4)	0.004 (4)
C8	0.034 (4)	0.023 (3)	0.059 (5)	−0.002 (3)	0.000 (4)	−0.005 (3)
C9	0.038 (4)	0.029 (4)	0.034 (4)	−0.014 (3)	0.004 (3)	−0.002 (3)
C10	0.032 (4)	0.038 (4)	0.071 (6)	−0.012 (3)	0.004 (4)	0.000 (4)
C11	0.036 (5)	0.037 (4)	0.083 (6)	−0.004 (4)	−0.001 (4)	−0.010 (4)
C12	0.035 (4)	0.035 (4)	0.040 (4)	−0.012 (4)	0.007 (3)	0.003 (3)
C13	0.037 (5)	0.065 (5)	0.045 (5)	−0.017 (4)	−0.003 (4)	−0.017 (4)
C14	0.032 (4)	0.073 (6)	0.049 (5)	−0.019 (4)	0.001 (4)	−0.009 (4)
C15	0.049 (5)	0.059 (5)	0.021 (4)	−0.011 (4)	0.003 (3)	−0.005 (3)
C16	0.070 (6)	0.058 (5)	0.044 (5)	−0.026 (5)	0.007 (4)	−0.018 (4)
C17	0.051 (5)	0.066 (6)	0.036 (4)	−0.021 (4)	0.011 (4)	−0.009 (4)
C18	0.067 (6)	0.055 (5)	0.039 (5)	−0.017 (4)	−0.006 (4)	−0.011 (4)
C19	0.043 (5)	0.068 (6)	0.034 (4)	−0.005 (4)	0.003 (4)	−0.015 (4)
C20	0.042 (5)	0.058 (5)	0.047 (5)	−0.013 (4)	0.003 (4)	−0.012 (4)
C21	0.061 (6)	0.040 (4)	0.041 (5)	−0.011 (4)	0.004 (4)	−0.012 (4)
C22	0.059 (6)	0.061 (5)	0.026 (4)	−0.019 (4)	−0.007 (4)	0.001 (4)
C23	0.038 (5)	0.060 (5)	0.045 (5)	−0.016 (4)	0.005 (4)	−0.008 (4)
C24	0.076 (6)	0.030 (4)	0.030 (4)	−0.018 (4)	0.000 (4)	−0.001 (3)
C25	0.039 (5)	0.057 (5)	0.041 (5)	−0.020 (4)	−0.004 (4)	0.006 (4)
C26	0.040 (5)	0.073 (6)	0.046 (5)	−0.026 (4)	−0.005 (4)	0.003 (4)
C27	0.041 (5)	0.063 (5)	0.025 (4)	−0.009 (4)	0.001 (3)	0.004 (4)
C28	0.058 (5)	0.050 (5)	0.049 (5)	−0.025 (4)	−0.008 (4)	0.005 (4)
C29	0.046 (5)	0.053 (5)	0.038 (4)	−0.023 (4)	−0.007 (4)	0.003 (4)
C30	0.051 (5)	0.050 (5)	0.034 (4)	−0.010 (4)	0.000 (4)	−0.001 (4)
C31	0.049 (5)	0.071 (6)	0.032 (4)	−0.016 (4)	0.007 (4)	−0.006 (4)
C32	0.044 (5)	0.063 (5)	0.039 (5)	−0.012 (4)	−0.002 (4)	0.001 (4)
C33	0.043 (5)	0.045 (4)	0.026 (4)	−0.006 (4)	0.002 (3)	−0.010 (3)
C34	0.039 (5)	0.063 (5)	0.046 (5)	−0.017 (4)	0.004 (4)	0.006 (4)
C35	0.035 (4)	0.067 (5)	0.042 (5)	−0.009 (4)	0.006 (4)	−0.007 (4)
C36	0.074 (6)	0.039 (4)	0.021 (4)	−0.015 (4)	0.006 (4)	−0.004 (3)
C37	0.045 (6)	0.046 (5)	0.145 (10)	−0.019 (5)	−0.009 (6)	0.014 (6)
C38	0.110 (11)	0.138 (12)	0.283 (16)	−0.013 (9)	−0.046 (11)	0.058 (12)
N1	0.056 (4)	0.032 (3)	0.052 (4)	−0.015 (3)	0.006 (3)	−0.002 (3)
N2	0.044 (5)	0.039 (4)	0.137 (8)	−0.021 (4)	−0.003 (5)	−0.015 (5)
N3	0.032 (3)	0.045 (4)	0.041 (4)	−0.011 (3)	−0.002 (3)	−0.007 (3)
N4	0.051 (6)	0.147 (9)	0.051 (5)	0.001 (6)	−0.012 (5)	−0.024 (5)
N5	0.035 (4)	0.044 (4)	0.040 (4)	−0.010 (3)	0.005 (3)	−0.004 (3)
N6	0.054 (6)	0.118 (8)	0.048 (5)	0.001 (5)	0.002 (4)	0.006 (5)

Geometric parameters (Å, º) top

Cd1—O14ⁱ	2.221 (8)	C13—N3	1.353 (9)
Cd1—O2	2.253 (5)	C13—C14	1.377 (10)
Cd1—N5ⁱⁱ	2.337 (6)	C13—H13A	0.9300
Cd1—N3ⁱⁱⁱ	2.337 (6)	C14—C15	1.370 (10)
Cd1—O9	2.397 (6)	C14—H14A	0.9300
Cd1—O6	2.460 (5)	C15—C16	1.405 (11)
Cd2—O13	2.262 (7)	C15—C18	1.489 (10)
Cd2—O1	2.284 (5)	C16—C17	1.363 (10)
Cd2—N1^iv	2.323 (6)	C16—H16A	0.9300
Cd2—O10	2.365 (6)	C17—N3	1.332 (9)
Cd2—O5	2.412 (6)	C17—H17A	0.9300
Cd2—O6	2.452 (5)	C18—C23	1.390 (10)
Cd2—O9	2.542 (5)	C18—C19	1.417 (11)
O1—C12	1.266 (8)	C19—C20	1.355 (10)
O2—C12	1.255 (8)	C19—N4	1.453 (10)
O3—N2	1.176 (9)	C20—C21	1.400 (10)
O4—N2	1.219 (10)	C20—H20A	0.9300
O5—C24	1.247 (9)	C21—C22	1.391 (11)
O6—C24	1.255 (9)	C21—C24	1.488 (10)
O7—N4	1.217 (11)	C22—C23	1.377 (10)
O8—N4	1.221 (10)	C22—H22A	0.9300
O9—C36	1.245 (9)	C23—H23A	0.9300
O10—C36	1.249 (9)	C25—N5	1.337 (9)
O11—N6	1.209 (9)	C25—C26	1.351 (10)
O12—N6	1.210 (10)	C25—H25A	0.9300
O13—C37	1.158 (10)	C26—C27	1.405 (10)
O14—C37	1.230 (11)	C26—H26A	0.9300
C1—N1	1.308 (10)	C27—C28	1.370 (10)
C1—C2	1.354 (12)	C27—C30	1.496 (9)
C1—H1A	0.9300	C28—C29	1.356 (10)
C2—C3	1.376 (12)	C28—H28A	0.9300
C2—H2A	0.9300	C29—N5	1.354 (9)
C3—C4	1.341 (11)	C29—H29A	0.9300
C3—C6	1.479 (10)	C30—C35	1.404 (10)
C4—C5	1.414 (12)	C30—C31	1.405 (11)
C4—H4A	0.9300	C31—C32	1.373 (10)
C5—N1	1.337 (11)	C31—N6	1.460 (11)
C5—H5A	0.9300	C32—C33	1.383 (10)
C6—C7	1.379 (10)	C32—H32A	0.9300
C6—C11	1.382 (10)	C33—C34	1.382 (10)
C7—C8	1.398 (9)	C33—C36	1.519 (9)
C7—N2	1.451 (10)	C34—C35	1.362 (10)
C8—C9	1.371 (9)	C34—H34A	0.9300
C8—H8A	0.9300	C35—H35A	0.9300
C9—C10	1.383 (10)	C37—C38	1.559 (13)
C9—C12	1.506 (9)	C38—H38A	0.9600
C10—C11	1.399 (10)	C38—H38B	0.9600
C10—H10A	0.9300	C38—H38C	0.9600
C11—H11A	0.9300

O14ⁱ—Cd1—O2	155.0 (3)	C16—C15—C18	121.7 (7)
O14ⁱ—Cd1—N5ⁱⁱ	114.0 (3)	C17—C16—C15	120.1 (8)
O2—Cd1—N5ⁱⁱ	87.56 (19)	C17—C16—H16A	120.0
O14ⁱ—Cd1—N3ⁱⁱⁱ	102.2 (3)	C15—C16—H16A	120.0
O2—Cd1—N3ⁱⁱⁱ	88.1 (2)	N3—C17—C16	124.0 (8)
N5ⁱⁱ—Cd1—N3ⁱⁱⁱ	93.8 (2)	N3—C17—H17A	118.0
O14ⁱ—Cd1—O9	82.8 (3)	C16—C17—H17A	118.0
O2—Cd1—O9	84.7 (2)	C23—C18—C19	116.2 (7)
N5ⁱⁱ—Cd1—O9	90.26 (19)	C23—C18—C15	119.1 (8)
N3ⁱⁱⁱ—Cd1—O9	171.6 (2)	C19—C18—C15	124.4 (7)
O14ⁱ—Cd1—O6	74.5 (3)	C20—C19—C18	121.6 (7)
O2—Cd1—O6	82.78 (18)	C20—C19—N4	116.9 (8)
N5ⁱⁱ—Cd1—O6	169.2 (2)	C18—C19—N4	121.3 (7)
N3ⁱⁱⁱ—Cd1—O6	90.80 (18)	C19—C20—C21	121.8 (8)
O9—Cd1—O6	83.96 (17)	C19—C20—H20A	119.1
O13—Cd2—O1	87.2 (2)	C21—C20—H20A	119.1
O13—Cd2—N1^iv	100.5 (2)	C22—C21—C20	117.1 (7)
O1—Cd2—N1^iv	172.0 (2)	C22—C21—C24	122.1 (7)
O13—Cd2—O10	87.3 (2)	C20—C21—C24	120.8 (8)
O1—Cd2—O10	88.41 (18)	C23—C22—C21	121.1 (7)
N1^iv—Cd2—O10	89.8 (2)	C23—C22—H22A	119.4
O13—Cd2—O5	85.8 (2)	C21—C22—H22A	119.4
O1—Cd2—O5	88.75 (18)	C22—C23—C18	122.1 (8)
N1^iv—Cd2—O5	93.9 (2)	C22—C23—H23A	118.9
O10—Cd2—O5	172.65 (18)	C18—C23—H23A	118.9
O13—Cd2—O6	138.6 (2)	O5—C24—O6	120.9 (7)
O1—Cd2—O6	86.88 (18)	O5—C24—C21	121.1 (7)
N1^iv—Cd2—O6	88.7 (2)	O6—C24—C21	118.0 (8)
O10—Cd2—O6	133.40 (18)	N5—C25—C26	124.1 (7)
O5—Cd2—O6	53.14 (18)	N5—C25—H25A	117.9
O13—Cd2—O9	139.7 (2)	C26—C25—H25A	117.9
O1—Cd2—O9	89.32 (18)	C25—C26—C27	119.4 (7)
N1^iv—Cd2—O9	83.4 (2)	C25—C26—H26A	120.3
O10—Cd2—O9	52.45 (18)	C27—C26—H26A	120.3
O5—Cd2—O9	134.28 (19)	C28—C27—C26	116.4 (7)
O6—Cd2—O9	81.14 (18)	C28—C27—C30	122.1 (7)
C12—O1—Cd2	127.9 (4)	C26—C27—C30	121.2 (7)
C12—O2—Cd1	140.1 (5)	C29—C28—C27	121.2 (7)
C24—O5—Cd2	93.9 (5)	C29—C28—H28A	119.4
C24—O6—Cd2	91.8 (5)	C27—C28—H28A	119.4
C24—O6—Cd1	159.1 (5)	N5—C29—C28	122.4 (7)
Cd2—O6—Cd1	94.94 (18)	N5—C29—H29A	118.8
C36—O9—Cd1	153.7 (5)	C28—C29—H29A	118.8
C36—O9—Cd2	88.8 (5)	C35—C30—C31	115.0 (7)
Cd1—O9—Cd2	94.22 (18)	C35—C30—C27	118.5 (7)
C36—O10—Cd2	97.0 (5)	C31—C30—C27	126.3 (7)
C37—O13—Cd2	141.9 (7)	C32—C31—C30	123.0 (7)
C37—O14—Cd1^v	125.6 (7)	C32—C31—N6	116.2 (7)
N1—C1—C2	125.0 (9)	C30—C31—N6	120.7 (7)
N1—C1—H1A	117.5	C31—C32—C33	119.6 (7)
C2—C1—H1A	117.5	C31—C32—H32A	120.2
C1—C2—C3	121.0 (9)	C33—C32—H32A	120.2
C1—C2—H2A	119.5	C34—C33—C32	119.0 (7)
C3—C2—H2A	119.5	C34—C33—C36	121.0 (7)
C4—C3—C2	114.6 (8)	C32—C33—C36	119.9 (7)
C4—C3—C6	122.3 (8)	C35—C34—C33	120.8 (7)
C2—C3—C6	123.0 (8)	C35—C34—H34A	119.6
C3—C4—C5	122.7 (9)	C33—C34—H34A	119.6
C3—C4—H4A	118.7	C34—C35—C30	122.4 (7)
C5—C4—H4A	118.7	C34—C35—H35A	118.8
N1—C5—C4	120.5 (9)	C30—C35—H35A	118.8
N1—C5—H5A	119.8	O9—C36—O10	121.4 (7)
C4—C5—H5A	119.8	O9—C36—C33	118.5 (8)
C7—C6—C11	116.3 (7)	O10—C36—C33	120.1 (7)
C7—C6—C3	124.1 (7)	O13—C37—O14	121.8 (9)
C11—C6—C3	119.6 (7)	O13—C37—C38	121.0 (9)
C6—C7—C8	122.7 (7)	O14—C37—C38	117.1 (10)
C6—C7—N2	120.9 (7)	C37—C38—H38A	109.5
C8—C7—N2	116.3 (7)	C37—C38—H38B	109.5
C9—C8—C7	119.8 (7)	H38A—C38—H38B	109.5
C9—C8—H8A	120.1	C37—C38—H38C	109.5
C7—C8—H8A	120.1	H38A—C38—H38C	109.5
C8—C9—C10	119.0 (6)	H38B—C38—H38C	109.5
C8—C9—C12	121.4 (6)	C1—N1—C5	116.2 (7)
C10—C9—C12	119.6 (6)	C1—N1—Cd2^vi	124.7 (6)
C9—C10—C11	120.1 (7)	C5—N1—Cd2^vi	119.1 (5)
C9—C10—H10A	120.0	O3—N2—O4	120.0 (9)
C11—C10—H10A	120.0	O3—N2—C7	121.6 (8)
C6—C11—C10	122.1 (7)	O4—N2—C7	117.9 (9)
C6—C11—H11A	119.0	C17—N3—C13	116.6 (7)
C10—C11—H11A	119.0	C17—N3—Cd1ⁱⁱⁱ	121.9 (5)
O2—C12—O1	127.0 (7)	C13—N3—Cd1ⁱⁱⁱ	121.0 (5)
O2—C12—C9	115.7 (6)	O7—N4—O8	123.5 (9)
O1—C12—C9	117.3 (6)	O7—N4—C19	117.8 (9)
N3—C13—C14	122.1 (7)	O8—N4—C19	118.6 (10)
N3—C13—H13A	119.0	C25—N5—C29	116.4 (6)
C14—C13—H13A	119.0	C25—N5—Cd1ⁱⁱ	122.0 (5)
C15—C14—C13	121.6 (7)	C29—N5—Cd1ⁱⁱ	121.0 (5)
C15—C14—H14A	119.2	O11—N6—O12	123.3 (9)
C13—C14—H14A	119.2	O11—N6—C31	118.9 (9)
C14—C15—C16	115.6 (7)	O12—N6—C31	117.7 (9)
C14—C15—C18	122.4 (7)

N1—C1—C2—C3	2 (2)	C20—C21—C24—O6	−173.1 (7)
C1—C2—C3—C4	−2.1 (17)	N5—C25—C26—C27	−0.5 (13)
C1—C2—C3—C6	−178.1 (10)	C25—C26—C27—C28	1.1 (12)
C2—C3—C4—C5	1.1 (16)	C25—C26—C27—C30	−172.7 (7)
C6—C3—C4—C5	177.0 (9)	C26—C27—C28—C29	−2.4 (12)
C3—C4—C5—N1	0.8 (18)	C30—C27—C28—C29	171.4 (8)
C4—C3—C6—C7	58.0 (13)	C27—C28—C29—N5	3.1 (13)
C2—C3—C6—C7	−126.4 (11)	C28—C27—C30—C35	−42.7 (11)
C4—C3—C6—C11	−122.0 (10)	C26—C27—C30—C35	130.8 (8)
C2—C3—C6—C11	53.6 (13)	C28—C27—C30—C31	142.1 (9)
C11—C6—C7—C8	1.7 (13)	C26—C27—C30—C31	−44.4 (12)
C3—C6—C7—C8	−178.2 (7)	C35—C30—C31—C32	−4.0 (12)
C11—C6—C7—N2	−176.4 (8)	C27—C30—C31—C32	171.4 (8)
C3—C6—C7—N2	3.7 (13)	C35—C30—C31—N6	173.1 (8)
C6—C7—C8—C9	−0.8 (12)	C27—C30—C31—N6	−11.6 (13)
N2—C7—C8—C9	177.4 (7)	C30—C31—C32—C33	1.2 (13)
C7—C8—C9—C10	0.8 (11)	N6—C31—C32—C33	−176.0 (8)
C7—C8—C9—C12	−178.4 (7)	C31—C32—C33—C34	1.5 (12)
C8—C9—C10—C11	−1.9 (11)	C31—C32—C33—C36	−175.6 (7)
C12—C9—C10—C11	177.3 (7)	C32—C33—C34—C35	−1.2 (12)
C7—C6—C11—C10	−2.9 (13)	C36—C33—C34—C35	175.9 (7)
C3—C6—C11—C10	177.1 (8)	C33—C34—C35—C30	−1.9 (13)
C9—C10—C11—C6	3.1 (13)	C31—C30—C35—C34	4.3 (12)
Cd1—O2—C12—O1	7.2 (13)	C27—C30—C35—C34	−171.4 (8)
Cd1—O2—C12—C9	−171.7 (5)	Cd1—O9—C36—O10	103.3 (12)
Cd2—O1—C12—O2	−3.4 (11)	Cd2—O9—C36—O10	6.2 (7)
Cd2—O1—C12—C9	175.5 (4)	Cd1—O9—C36—C33	−78.9 (14)
C8—C9—C12—O2	−179.7 (7)	Cd2—O9—C36—C33	−176.0 (6)
C10—C9—C12—O2	1.1 (10)	Cd2—O10—C36—O9	−6.7 (8)
C8—C9—C12—O1	1.2 (10)	Cd2—O10—C36—C33	175.5 (6)
C10—C9—C12—O1	−178.0 (7)	C34—C33—C36—O9	−1.9 (11)
N3—C13—C14—C15	2.6 (12)	C32—C33—C36—O9	175.1 (7)
C13—C14—C15—C16	−2.8 (12)	C34—C33—C36—O10	175.9 (7)
C13—C14—C15—C18	171.4 (7)	C32—C33—C36—O10	−7.0 (11)
C14—C15—C16—C17	1.6 (12)	Cd2—O13—C37—O14	−162.7 (8)
C18—C15—C16—C17	−172.6 (8)	Cd2—O13—C37—C38	13 (2)
C15—C16—C17—N3	−0.2 (13)	Cd1^v—O14—C37—O13	0.6 (19)
C14—C15—C18—C23	−129.5 (8)	Cd1^v—O14—C37—C38	−175.5 (10)
C16—C15—C18—C23	44.4 (11)	C2—C1—N1—C5	0.4 (17)
C14—C15—C18—C19	43.5 (12)	C2—C1—N1—Cd2^vi	−179.1 (9)
C16—C15—C18—C19	−142.6 (8)	C4—C5—N1—C1	−1.5 (16)
C23—C18—C19—C20	1.5 (12)	C4—C5—N1—Cd2^vi	178.0 (8)
C15—C18—C19—C20	−171.7 (8)	C6—C7—N2—O3	−144.9 (10)
C23—C18—C19—N4	−173.2 (8)	C8—C7—N2—O3	36.8 (14)
C15—C18—C19—N4	13.6 (13)	C6—C7—N2—O4	43.5 (13)
C18—C19—C20—C21	0.9 (13)	C8—C7—N2—O4	−134.8 (9)
N4—C19—C20—C21	175.8 (8)	C16—C17—N3—C13	−0.1 (11)
C19—C20—C21—C22	−3.5 (12)	C16—C17—N3—Cd1ⁱⁱⁱ	172.1 (6)
C19—C20—C21—C24	176.1 (7)	C14—C13—N3—C17	−1.0 (11)
C20—C21—C22—C23	3.6 (11)	C14—C13—N3—Cd1ⁱⁱⁱ	−173.4 (6)
C24—C21—C22—C23	−175.9 (7)	C20—C19—N4—O7	43.7 (14)
C21—C22—C23—C18	−1.3 (12)	C18—C19—N4—O7	−141.3 (10)
C19—C18—C23—C22	−1.3 (12)	C20—C19—N4—O8	−138.4 (9)
C15—C18—C23—C22	172.3 (7)	C18—C19—N4—O8	36.5 (14)
Cd2—O5—C24—O6	5.2 (7)	C26—C25—N5—C29	1.0 (12)
Cd2—O5—C24—C21	−175.2 (6)	C26—C25—N5—Cd1ⁱⁱ	173.0 (6)
Cd2—O6—C24—O5	−5.1 (7)	C28—C29—N5—C25	−2.3 (11)
Cd1—O6—C24—O5	−114.0 (14)	C28—C29—N5—Cd1ⁱⁱ	−174.3 (6)
Cd2—O6—C24—C21	175.3 (6)	C32—C31—N6—O11	142.2 (9)
Cd1—O6—C24—C21	66.3 (17)	C30—C31—N6—O11	−35.0 (13)
C22—C21—C24—O5	−173.2 (7)	C32—C31—N6—O12	−39.8 (13)
C20—C21—C24—O5	7.2 (11)	C30—C31—N6—O12	142.9 (9)
C22—C21—C24—O6	6.4 (11)

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

catena-Poly[[[diaquanickel(II)]-bis[µ₂-3-nitro-4-(pyridin-4-yl)benzoato-κ²O:N]] N,N-dimethylacetamide disolvate] (1845690) top

Crystal data top

[Ni(C₁₂H₇N₂O₄)₂(H₂O)₂]·2C₄H₉NO	Z = 2
M_r = 755.38	F(000) = 788
Triclinic, P1	D_x = 1.388 Mg m⁻³
a = 11.866 (7) Å	Mo Kα radiation, λ = 0.71073 Å
b = 12.259 (7) Å	Cell parameters from 4686 reflections
c = 14.248 (14) Å	θ = 2.3–27.1°
α = 98.341 (9)°	µ = 0.61 mm⁻¹
β = 93.604 (9)°	T = 296 K
γ = 117.018 (6)°	Block, light green
V = 1807 (2) Å³	0.20 × 0.18 × 0.12 mm

Data collection top

Bruker APEXII CCD diffractometer	5054 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.024
ω scans	θ_max = 25.0°, θ_min = 1.5°
Absorption correction: multi-scan (SADABS; Bruker, 2005)	h = −13→14
T_min = 0.889, T_max = 0.931	k = −14→14
12864 measured reflections	l = −16→16
6294 independent reflections

Refinement top

Refinement on F²	82 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.047	H-atom parameters constrained
wR(F²) = 0.136	w = 1/[σ²(F_o²) + (0.0739P)² + 0.983P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max < 0.001
6294 reflections	Δρ_max = 0.85 e Å⁻³
537 parameters	Δρ_min = −0.46 e Å⁻³

Special details top

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Ni1	0.000000	0.000000	0.000000	0.02411 (15)
Ni2	0.000000	1.000000	0.500000	0.02426 (15)
O1	−0.0510 (2)	0.82674 (18)	0.42739 (13)	0.0335 (5)
O1W	−0.1279 (2)	−0.1305 (2)	0.06831 (15)	0.0443 (6)
H1WA	−0.082098	−0.120880	0.120212	0.053*
H1WB	−0.206198	−0.172200	0.074282	0.053*
O2W	0.12087 (19)	1.07030 (19)	0.40066 (14)	0.0346 (5)
H2WA	0.128744	1.141065	0.393885	0.042*
H2WB	0.092074	1.020775	0.346545	0.042*
O2	−0.1332 (3)	0.7053 (2)	0.53437 (15)	0.0500 (6)
O3	−0.018 (3)	0.614 (2)	0.1026 (10)	0.103 (6)	0.86 (6)
O3A	0.048 (5)	0.653 (4)	0.127 (4)	0.051 (13)	0.14 (6)
O4	0.126 (7)	0.593 (3)	0.145 (4)	0.078 (10)	0.43 (16)
O4A	0.158 (4)	0.587 (3)	0.169 (4)	0.083 (6)	0.57 (16)
O5	0.14968 (18)	0.01671 (18)	0.09383 (13)	0.0309 (4)
O6	0.05986 (19)	−0.07410 (19)	0.21454 (13)	0.0348 (5)
O7	0.6737 (6)	0.0451 (8)	0.1233 (5)	0.090 (3)	0.594 (9)
O7A	0.6954 (13)	0.1306 (13)	0.1786 (10)	0.121 (4)	0.406 (9)
O8	0.6216 (8)	0.1896 (8)	0.1182 (6)	0.130 (3)	0.594 (9)
O8A	0.5760 (10)	0.0653 (11)	0.0499 (8)	0.117 (4)	0.406 (9)
O9	0.3862 (10)	0.234 (2)	−0.0433 (10)	0.075 (4)	0.50 (5)
O9A	0.3826 (10)	0.281 (2)	−0.0539 (7)	0.072 (4)	0.50 (5)
O10	0.6588 (4)	0.2897 (4)	0.5251 (3)	0.1091 (13)
N1	−0.0148 (2)	0.1448 (2)	0.09002 (16)	0.0321 (5)
N2	0.0442 (5)	0.5906 (3)	0.1650 (3)	0.0653 (12)
N3	0.8449 (2)	−0.0019 (2)	0.41517 (16)	0.0319 (5)
N4	0.5990 (4)	0.0777 (5)	0.1351 (3)	0.0905 (14)
N5	0.5640 (7)	0.3824 (7)	0.0429 (6)	0.161 (3)
N6	0.5084 (19)	0.3347 (16)	0.5422 (17)	0.108 (6)	0.52 (3)
N6A	0.5489 (17)	0.3784 (19)	0.5933 (15)	0.095 (6)	0.48 (3)
C1	−0.0469 (3)	0.2227 (3)	0.0532 (2)	0.0385 (7)
H1A	−0.060522	0.212539	−0.013183	0.046*
C2	−0.0610 (3)	0.3169 (3)	0.1069 (2)	0.0406 (8)
H2A	−0.085650	0.366824	0.077048	0.049*
C3	−0.0381 (3)	0.3371 (3)	0.2068 (2)	0.0353 (7)
C4	−0.0045 (4)	0.2575 (3)	0.2452 (2)	0.0466 (9)
H4A	0.011571	0.266755	0.311364	0.056*
C5	0.0055 (3)	0.1638 (3)	0.1855 (2)	0.0418 (8)
H5A	0.027730	0.110977	0.213495	0.050*
C6	−0.0533 (3)	0.4363 (3)	0.2689 (2)	0.0358 (7)
C7	−0.0190 (3)	0.5537 (3)	0.2486 (2)	0.0366 (7)
C8	−0.0360 (3)	0.6443 (3)	0.3054 (2)	0.0347 (7)
H8A	−0.014840	0.720158	0.286946	0.042*
C9	−0.0849 (3)	0.6216 (3)	0.3905 (2)	0.0317 (6)
C10	−0.1219 (3)	0.5042 (3)	0.4127 (2)	0.0437 (8)
H10A	−0.156807	0.486576	0.468700	0.052*
C11	−0.1076 (4)	0.4137 (3)	0.3527 (2)	0.0453 (8)
H11A	−0.134992	0.335500	0.368555	0.054*
C12	−0.0921 (3)	0.7248 (3)	0.4567 (2)	0.0314 (6)
C13	0.7882 (3)	0.0644 (3)	0.4515 (2)	0.0411 (8)
H13A	0.823027	0.115928	0.511616	0.049*
C14	0.6810 (3)	0.0598 (3)	0.4041 (2)	0.0468 (8)
H14A	0.644975	0.107377	0.432262	0.056*
C15	0.6270 (3)	−0.0154 (3)	0.3146 (2)	0.0389 (7)
C16	0.6863 (3)	−0.0830 (3)	0.2753 (2)	0.0448 (8)
H16A	0.654125	−0.133978	0.214782	0.054*
C17	0.7933 (3)	−0.0731 (3)	0.3273 (2)	0.0391 (7)
H17A	0.832160	−0.118437	0.300035	0.047*
C18	0.5050 (3)	−0.0252 (3)	0.2689 (2)	0.0404 (7)
C19	0.4903 (3)	0.0212 (4)	0.1873 (2)	0.0476 (8)
C20	0.3777 (3)	0.0192 (3)	0.1540 (2)	0.0461 (8)
H20A	0.372086	0.050986	0.099502	0.055*
C21	0.2741 (3)	−0.0295 (3)	0.2013 (2)	0.0316 (6)
C22	0.2845 (3)	−0.0781 (3)	0.2814 (2)	0.0418 (8)
H22A	0.214577	−0.112297	0.313732	0.050*
C23	0.3974 (3)	−0.0763 (3)	0.3138 (2)	0.0457 (8)
H23A	0.401564	−0.110336	0.367280	0.055*
C24	0.1510 (3)	−0.0289 (2)	0.16763 (19)	0.0284 (6)
C25	0.3793 (6)	0.3378 (7)	0.1171 (5)	0.129 (3)
H25A	0.419866	0.326593	0.172686	0.194*
H25B	0.291278	0.274960	0.103292	0.194*
H25C	0.383888	0.418963	0.129210	0.194*
C26	0.4480 (7)	0.3265 (7)	0.0306 (6)	0.124 (2)
C27	0.6281 (6)	0.3548 (9)	−0.0403 (6)	0.172 (4)
H27A	0.571320	0.329628	−0.099356	0.257*
H27B	0.647656	0.288870	−0.031087	0.257*
H27C	0.705581	0.428483	−0.042769	0.257*
C28	0.6440 (8)	0.4610 (10)	0.1384 (7)	0.213 (5)
H28A	0.611284	0.515905	0.164074	0.320*
H28B	0.731144	0.509412	0.129115	0.320*
H28C	0.640022	0.407294	0.182255	0.320*
C29	0.4406 (7)	0.2434 (7)	0.4449 (7)	0.184 (4)
H29A	0.411841	0.159097	0.453619	0.276*
H29B	0.499386	0.261492	0.399105	0.276*
H29C	0.368502	0.253153	0.421972	0.276*
C30	0.6183 (16)	0.3516 (13)	0.5725 (12)	0.074 (7)	0.52 (3)
C30A	0.5519 (16)	0.3027 (12)	0.5188 (15)	0.068 (6)	0.48 (3)
C31	0.6761 (9)	0.4459 (9)	0.6649 (5)	0.164 (4)
H31A	0.747637	0.439978	0.694320	0.246*
H31B	0.613156	0.429598	0.707466	0.246*
H31C	0.704344	0.528303	0.651906	0.246*
C32	0.4347 (7)	0.3936 (9)	0.5959 (7)	0.179 (4)
H32A	0.486919	0.482495	0.612408	0.268*
H32B	0.413581	0.360783	0.653234	0.268*
H32C	0.357584	0.374089	0.555438	0.268*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0279 (3)	0.0299 (3)	0.0202 (3)	0.0198 (2)	0.00001 (19)	0.00119 (19)
Ni2	0.0295 (3)	0.0287 (3)	0.0198 (3)	0.0203 (2)	−0.00107 (19)	−0.00088 (19)
O1	0.0483 (13)	0.0312 (10)	0.0258 (10)	0.0255 (10)	0.0000 (9)	−0.0014 (8)
O1W	0.0305 (12)	0.0581 (14)	0.0397 (12)	0.0155 (10)	−0.0001 (10)	0.0166 (11)
O2W	0.0413 (12)	0.0384 (11)	0.0280 (10)	0.0232 (10)	0.0052 (8)	0.0020 (8)
O2	0.0814 (18)	0.0440 (13)	0.0345 (12)	0.0367 (13)	0.0213 (12)	0.0062 (10)
O3	0.194 (17)	0.110 (8)	0.056 (4)	0.103 (11)	0.047 (7)	0.047 (5)
O3A	0.07 (2)	0.061 (16)	0.034 (16)	0.037 (14)	0.025 (11)	0.019 (11)
O4	0.066 (17)	0.098 (9)	0.064 (14)	0.031 (9)	0.036 (12)	0.015 (8)
O4A	0.064 (9)	0.110 (6)	0.078 (12)	0.039 (6)	0.035 (8)	0.020 (7)
O5	0.0311 (11)	0.0410 (11)	0.0270 (10)	0.0228 (9)	−0.0003 (8)	0.0066 (9)
O6	0.0325 (11)	0.0505 (12)	0.0270 (11)	0.0243 (10)	0.0032 (8)	0.0073 (9)
O7	0.061 (4)	0.155 (7)	0.120 (5)	0.083 (4)	0.056 (4)	0.087 (5)
O7A	0.114 (5)	0.127 (5)	0.117 (5)	0.049 (3)	0.017 (3)	0.035 (3)
O8	0.122 (4)	0.131 (4)	0.150 (4)	0.061 (3)	0.026 (3)	0.055 (3)
O8A	0.108 (5)	0.136 (5)	0.101 (5)	0.050 (3)	0.025 (3)	0.028 (3)
O9	0.059 (4)	0.083 (6)	0.068 (5)	0.025 (4)	0.002 (3)	0.004 (4)
O9A	0.049 (4)	0.079 (7)	0.069 (4)	0.016 (4)	−0.009 (3)	0.011 (4)
O10	0.121 (4)	0.095 (3)	0.137 (4)	0.069 (3)	0.049 (3)	0.020 (2)
N1	0.0447 (15)	0.0367 (13)	0.0242 (12)	0.0291 (12)	0.0016 (11)	0.0007 (10)
N2	0.113 (4)	0.0363 (17)	0.053 (2)	0.036 (2)	0.045 (2)	0.0115 (16)
N3	0.0331 (14)	0.0422 (14)	0.0267 (13)	0.0247 (11)	−0.0006 (10)	0.0029 (11)
N4	0.053 (2)	0.158 (4)	0.086 (3)	0.053 (3)	0.019 (2)	0.082 (3)
N5	0.108 (5)	0.182 (7)	0.177 (7)	0.067 (5)	−0.017 (5)	0.007 (6)
N6	0.090 (10)	0.093 (10)	0.132 (13)	0.040 (7)	0.012 (9)	0.006 (9)
N6A	0.103 (14)	0.106 (11)	0.108 (12)	0.073 (10)	0.045 (9)	0.021 (9)
C1	0.060 (2)	0.0404 (17)	0.0250 (15)	0.0338 (16)	0.0013 (14)	0.0015 (13)
C2	0.061 (2)	0.0389 (17)	0.0342 (17)	0.0352 (16)	0.0023 (15)	0.0050 (13)
C3	0.0485 (19)	0.0316 (15)	0.0317 (16)	0.0250 (14)	0.0064 (14)	0.0013 (12)
C4	0.079 (3)	0.052 (2)	0.0236 (16)	0.0465 (19)	0.0011 (15)	0.0021 (14)
C5	0.068 (2)	0.0478 (18)	0.0270 (16)	0.0438 (18)	−0.0008 (15)	0.0024 (13)
C6	0.052 (2)	0.0318 (15)	0.0288 (15)	0.0259 (15)	0.0058 (14)	0.0007 (12)
C7	0.050 (2)	0.0335 (16)	0.0301 (16)	0.0226 (15)	0.0118 (14)	0.0032 (12)
C8	0.0438 (18)	0.0287 (14)	0.0341 (16)	0.0195 (13)	0.0048 (14)	0.0053 (12)
C9	0.0388 (17)	0.0309 (15)	0.0293 (15)	0.0207 (13)	0.0050 (13)	0.0019 (12)
C10	0.068 (2)	0.0363 (17)	0.0365 (18)	0.0297 (16)	0.0199 (16)	0.0101 (14)
C11	0.075 (3)	0.0325 (16)	0.0390 (18)	0.0313 (17)	0.0185 (17)	0.0114 (14)
C12	0.0355 (16)	0.0322 (15)	0.0294 (15)	0.0209 (13)	−0.0008 (12)	−0.0011 (12)
C13	0.0431 (19)	0.0540 (19)	0.0353 (17)	0.0357 (16)	−0.0048 (14)	−0.0047 (14)
C14	0.045 (2)	0.062 (2)	0.045 (2)	0.0406 (18)	−0.0030 (16)	−0.0025 (16)
C15	0.0343 (17)	0.0545 (19)	0.0364 (17)	0.0282 (15)	−0.0007 (13)	0.0103 (14)
C16	0.044 (2)	0.065 (2)	0.0306 (17)	0.0349 (17)	−0.0074 (14)	−0.0028 (15)
C17	0.0416 (18)	0.0550 (19)	0.0296 (16)	0.0344 (16)	−0.0026 (13)	−0.0033 (14)
C18	0.0362 (18)	0.0533 (19)	0.0381 (17)	0.0273 (16)	−0.0034 (14)	0.0099 (15)
C19	0.0378 (19)	0.076 (2)	0.0424 (19)	0.0354 (18)	0.0052 (14)	0.0191 (17)
C20	0.0409 (19)	0.075 (2)	0.0367 (18)	0.0353 (18)	0.0076 (15)	0.0249 (17)
C21	0.0320 (16)	0.0378 (16)	0.0273 (15)	0.0201 (13)	−0.0005 (12)	0.0026 (12)
C22	0.0315 (17)	0.058 (2)	0.0401 (18)	0.0223 (15)	0.0034 (14)	0.0187 (16)
C23	0.0413 (19)	0.065 (2)	0.0423 (19)	0.0303 (17)	0.0039 (15)	0.0255 (17)
C24	0.0325 (15)	0.0317 (14)	0.0232 (14)	0.0199 (12)	−0.0015 (11)	−0.0024 (11)
C25	0.101 (5)	0.132 (5)	0.113 (5)	0.035 (4)	0.019 (4)	−0.031 (4)
C26	0.080 (5)	0.112 (5)	0.173 (7)	0.035 (4)	0.030 (5)	0.042 (5)
C27	0.075 (4)	0.297 (12)	0.144 (6)	0.080 (6)	0.048 (4)	0.059 (7)
C28	0.125 (7)	0.261 (12)	0.161 (8)	0.057 (7)	−0.071 (6)	−0.077 (8)
C29	0.126 (7)	0.115 (6)	0.233 (10)	0.024 (5)	−0.085 (7)	−0.041 (6)
C30	0.065 (10)	0.067 (8)	0.089 (10)	0.025 (7)	0.016 (7)	0.033 (8)
C30A	0.054 (9)	0.039 (6)	0.091 (11)	0.008 (5)	0.000 (7)	0.003 (6)
C31	0.185 (9)	0.216 (9)	0.093 (5)	0.121 (8)	−0.039 (5)	−0.032 (6)
C32	0.107 (6)	0.200 (9)	0.289 (12)	0.110 (6)	0.074 (7)	0.074 (8)

Geometric parameters (Å, º) top

Ni1—O1W	2.059 (2)	C4—C5	1.382 (4)
Ni1—O1Wⁱ	2.059 (2)	C4—H4A	0.9300
Ni1—O5ⁱ	2.068 (2)	C5—H5A	0.9300
Ni1—O5	2.068 (2)	C6—C7	1.388 (4)
Ni1—N1	2.116 (2)	C6—C11	1.396 (4)
Ni1—N1ⁱ	2.116 (2)	C7—C8	1.375 (4)
Ni2—O1	2.016 (2)	C8—C9	1.387 (4)
Ni2—O1ⁱⁱ	2.016 (2)	C8—H8A	0.9300
Ni2—O2Wⁱⁱ	2.071 (2)	C9—C10	1.392 (4)
Ni2—O2W	2.071 (2)	C9—C12	1.504 (4)
Ni2—N3ⁱⁱⁱ	2.126 (3)	C10—C11	1.380 (4)
Ni2—N3^iv	2.126 (2)	C10—H10A	0.9300
O1—C12	1.264 (3)	C11—H11A	0.9300
O1W—H1WA	0.8499	C13—C14	1.376 (4)
O1W—H1WB	0.8501	C13—H13A	0.9300
O2W—H2WA	0.8499	C14—C15	1.380 (5)
O2W—H2WB	0.8499	C14—H14A	0.9300
O2—C12	1.248 (4)	C15—C16	1.392 (5)
O3—N2	1.27 (2)	C15—C18	1.496 (4)
O3A—N2	0.99 (4)	C16—C17	1.375 (4)
O4—N2	1.02 (7)	C16—H16A	0.9300
O4A—N2	1.36 (5)	C17—H17A	0.9300
O5—C24	1.263 (3)	C18—C23	1.387 (5)
O6—C24	1.256 (3)	C18—C19	1.401 (5)
O7—N4	1.138 (6)	C19—C20	1.377 (4)
O7A—N4	1.109 (13)	C20—C21	1.370 (4)
O8—N4	1.335 (9)	C20—H20A	0.9300
O8A—N4	1.200 (11)	C21—C22	1.385 (4)
O9—C26	1.314 (12)	C21—C24	1.512 (4)
O9A—C26	1.288 (11)	C22—C23	1.378 (4)
O10—C30	1.219 (15)	C22—H22A	0.9300
O10—C30A	1.348 (16)	C23—H23A	0.9300
N1—C5	1.333 (4)	C25—C26	1.544 (8)
N1—C1	1.336 (4)	C25—H25A	0.9600
N2—C7	1.465 (5)	C25—H25B	0.9600
N3—C13	1.342 (4)	C25—H25C	0.9600
N3—C17	1.344 (4)	C27—H27A	0.9600
N4—C19	1.467 (5)	C27—H27B	0.9600
N5—C26	1.214 (8)	C27—H27C	0.9600
N5—C28	1.519 (9)	C28—H28A	0.9600
N5—C27	1.525 (9)	C28—H28B	0.9600
N6—C30	1.26 (3)	C28—H28C	0.9600
N6—C32	1.539 (16)	C29—C30A	1.45 (2)
N6—C29	1.55 (2)	C29—H29A	0.9600
N6A—C30A	1.32 (4)	C29—H29B	0.9600
N6A—C32	1.451 (17)	C29—H29C	0.9600
N6A—C31	1.56 (2)	C30—C31	1.51 (2)
C1—C2	1.371 (4)	C31—H31A	0.9600
C1—H1A	0.9300	C31—H31B	0.9600
C2—C3	1.395 (4)	C31—H31C	0.9600
C2—H2A	0.9300	C32—H32A	0.9600
C3—C4	1.375 (4)	C32—H32B	0.9600
C3—C6	1.484 (4)	C32—H32C	0.9600

O1W—Ni1—O1Wⁱ	180.0	C11—C10—C9	120.9 (3)
O1W—Ni1—O5ⁱ	90.13 (9)	C11—C10—H10A	119.6
O1Wⁱ—Ni1—O5ⁱ	89.87 (9)	C9—C10—H10A	119.6
O1W—Ni1—O5	89.87 (9)	C10—C11—C6	121.8 (3)
O1Wⁱ—Ni1—O5	90.13 (9)	C10—C11—H11A	119.1
O5ⁱ—Ni1—O5	180.0	C6—C11—H11A	119.1
O1W—Ni1—N1	90.62 (10)	O2—C12—O1	126.2 (3)
O1Wⁱ—Ni1—N1	89.38 (11)	O2—C12—C9	119.3 (3)
O5ⁱ—Ni1—N1	87.91 (9)	O1—C12—C9	114.5 (3)
O5—Ni1—N1	92.09 (9)	N3—C13—C14	123.1 (3)
O1W—Ni1—N1ⁱ	89.38 (10)	N3—C13—H13A	118.4
O1Wⁱ—Ni1—N1ⁱ	90.62 (10)	C14—C13—H13A	118.4
O5ⁱ—Ni1—N1ⁱ	92.09 (9)	C13—C14—C15	120.0 (3)
O5—Ni1—N1ⁱ	87.91 (9)	C13—C14—H14A	120.0
N1—Ni1—N1ⁱ	180.0	C15—C14—H14A	120.0
O1—Ni2—O1ⁱⁱ	180.00 (10)	C14—C15—C16	117.5 (3)
O1—Ni2—O2Wⁱⁱ	91.64 (9)	C14—C15—C18	118.2 (3)
O1ⁱⁱ—Ni2—O2Wⁱⁱ	88.36 (9)	C16—C15—C18	124.3 (3)
O1—Ni2—O2W	88.36 (9)	C17—C16—C15	119.0 (3)
O1ⁱⁱ—Ni2—O2W	91.64 (9)	C17—C16—H16A	120.5
O2Wⁱⁱ—Ni2—O2W	180.00 (12)	C15—C16—H16A	120.5
O1—Ni2—N3ⁱⁱⁱ	91.20 (9)	N3—C17—C16	123.9 (3)
O1ⁱⁱ—Ni2—N3ⁱⁱⁱ	88.80 (9)	N3—C17—H17A	118.1
O2Wⁱⁱ—Ni2—N3ⁱⁱⁱ	91.58 (10)	C16—C17—H17A	118.1
O2W—Ni2—N3ⁱⁱⁱ	88.42 (11)	C23—C18—C19	115.7 (3)
O1—Ni2—N3^iv	88.80 (9)	C23—C18—C15	118.3 (3)
O1ⁱⁱ—Ni2—N3^iv	91.20 (9)	C19—C18—C15	125.9 (3)
O2Wⁱⁱ—Ni2—N3^iv	88.42 (11)	C20—C19—C18	122.8 (3)
O2W—Ni2—N3^iv	91.58 (10)	C20—C19—N4	117.5 (3)
N3ⁱⁱⁱ—Ni2—N3^iv	180.0	C18—C19—N4	119.7 (3)
C12—O1—Ni2	129.71 (19)	C21—C20—C19	120.0 (3)
Ni1—O1W—H1WA	102.4	C21—C20—H20A	120.0
Ni1—O1W—H1WB	145.4	C19—C20—H20A	120.0
H1WA—O1W—H1WB	108.8	C20—C21—C22	118.8 (3)
Ni2—O2W—H2WA	110.7	C20—C21—C24	120.7 (3)
Ni2—O2W—H2WB	110.6	C22—C21—C24	120.5 (3)
H2WA—O2W—H2WB	108.8	C23—C22—C21	120.7 (3)
C24—O5—Ni1	131.40 (18)	C23—C22—H22A	119.6
C5—N1—C1	115.8 (2)	C21—C22—H22A	119.6
C5—N1—Ni1	123.15 (19)	C22—C23—C18	122.0 (3)
C1—N1—Ni1	121.01 (19)	C22—C23—H23A	119.0
O4—N2—O3	114 (5)	C18—C23—H23A	119.0
O3A—N2—O4A	109 (3)	O6—C24—O5	126.1 (3)
O3A—N2—C7	130.9 (18)	O6—C24—C21	117.6 (2)
O4—N2—C7	131 (5)	O5—C24—C21	116.3 (2)
O3—N2—C7	114.9 (10)	C26—C25—H25A	109.5
O4A—N2—C7	112 (2)	C26—C25—H25B	109.5
C13—N3—C17	116.5 (3)	H25A—C25—H25B	109.5
C13—N3—Ni2^v	119.8 (2)	C26—C25—H25C	109.5
C17—N3—Ni2^v	123.50 (19)	H25A—C25—H25C	109.5
O7A—N4—O8A	125.7 (9)	H25B—C25—H25C	109.5
O7—N4—O8	119.0 (6)	N5—C26—O9A	121.8 (9)
O7A—N4—C19	116.9 (8)	N5—C26—O9	120.1 (9)
O7—N4—C19	125.8 (5)	N5—C26—C25	117.6 (8)
O8A—N4—C19	117.4 (6)	O9A—C26—C25	119.1 (8)
O8—N4—C19	113.8 (5)	O9—C26—C25	119.7 (8)
C26—N5—C28	123.5 (9)	N5—C27—H27A	109.5
C26—N5—C27	115.7 (7)	N5—C27—H27B	109.5
C28—N5—C27	120.2 (7)	H27A—C27—H27B	109.5
C30—N6—C32	125 (2)	N5—C27—H27C	109.5
C30—N6—C29	117.2 (17)	H27A—C27—H27C	109.5
C32—N6—C29	117.7 (16)	H27B—C27—H27C	109.5
C30A—N6A—C32	118 (2)	N5—C28—H28A	109.5
C30A—N6A—C31	113.2 (14)	N5—C28—H28B	109.5
C32—N6A—C31	128.9 (16)	H28A—C28—H28B	109.5
N1—C1—C2	124.3 (3)	N5—C28—H28C	109.5
N1—C1—H1A	117.9	H28A—C28—H28C	109.5
C2—C1—H1A	117.9	H28B—C28—H28C	109.5
C1—C2—C3	119.5 (3)	N6—C29—H29A	109.5
C1—C2—H2A	120.3	N6—C29—H29B	109.5
C3—C2—H2A	120.3	H29A—C29—H29B	109.5
C4—C3—C2	116.5 (3)	N6—C29—H29C	109.5
C4—C3—C6	121.3 (3)	H29A—C29—H29C	109.5
C2—C3—C6	122.1 (3)	H29B—C29—H29C	109.5
C3—C4—C5	120.0 (3)	O10—C30—N6	117 (2)
C3—C4—H4A	120.0	O10—C30—C31	131.1 (14)
C5—C4—H4A	120.0	N6—C30—C31	112.1 (15)
N1—C5—C4	123.8 (3)	N6A—C30A—O10	113.4 (19)
N1—C5—H5A	118.1	N6A—C30A—C29	116.7 (16)
C4—C5—H5A	118.1	O10—C30A—C29	129.9 (15)
C7—C6—C11	115.6 (3)	C30—C31—H31A	109.5
C7—C6—C3	124.1 (3)	C30—C31—H31B	109.5
C11—C6—C3	120.3 (3)	H31A—C31—H31B	109.5
C8—C7—C6	123.8 (3)	C30—C31—H31C	109.5
C8—C7—N2	115.4 (3)	H31A—C31—H31C	109.5
C6—C7—N2	120.7 (3)	H31B—C31—H31C	109.5
C7—C8—C9	119.5 (3)	N6—C32—H32A	109.5
C7—C8—H8A	120.2	N6—C32—H32B	109.5
C9—C8—H8A	120.2	H32A—C32—H32B	109.5
C8—C9—C10	118.3 (3)	N6—C32—H32C	109.5
C8—C9—C12	119.3 (3)	H32A—C32—H32C	109.5
C10—C9—C12	122.4 (3)	H32B—C32—H32C	109.5

C5—N1—C1—C2	−0.9 (5)	C13—N3—C17—C16	−1.5 (5)
Ni1—N1—C1—C2	178.5 (3)	Ni2^v—N3—C17—C16	174.3 (3)
N1—C1—C2—C3	1.6 (5)	C15—C16—C17—N3	0.3 (5)
C1—C2—C3—C4	−1.2 (5)	C14—C15—C18—C23	−63.1 (4)
C1—C2—C3—C6	−179.2 (3)	C16—C15—C18—C23	113.0 (4)
C2—C3—C4—C5	0.2 (5)	C14—C15—C18—C19	112.0 (4)
C6—C3—C4—C5	178.2 (3)	C16—C15—C18—C19	−71.9 (5)
C1—N1—C5—C4	−0.2 (5)	C23—C18—C19—C20	1.3 (6)
Ni1—N1—C5—C4	−179.6 (3)	C15—C18—C19—C20	−173.8 (3)
C3—C4—C5—N1	0.6 (6)	C23—C18—C19—N4	179.7 (4)
C4—C3—C6—C7	143.6 (4)	C15—C18—C19—N4	4.5 (6)
C2—C3—C6—C7	−38.5 (5)	O7A—N4—C19—C20	144.0 (11)
C4—C3—C6—C11	−37.9 (5)	O7—N4—C19—C20	−144.7 (8)
C2—C3—C6—C11	140.0 (4)	O8A—N4—C19—C20	−34.3 (9)
C11—C6—C7—C8	0.0 (5)	O8—N4—C19—C20	48.8 (7)
C3—C6—C7—C8	178.5 (3)	O7A—N4—C19—C18	−34.5 (12)
C11—C6—C7—N2	177.2 (4)	O7—N4—C19—C18	36.9 (10)
C3—C6—C7—N2	−4.3 (5)	O8A—N4—C19—C18	147.3 (8)
O3A—N2—C7—C8	−27 (5)	O8—N4—C19—C18	−129.6 (5)
O4—N2—C7—C8	122 (3)	C18—C19—C20—C21	0.0 (6)
O3—N2—C7—C8	−65.1 (12)	N4—C19—C20—C21	−178.3 (4)
O4A—N2—C7—C8	117.4 (14)	C19—C20—C21—C22	−1.1 (5)
O3A—N2—C7—C6	156 (5)	C19—C20—C21—C24	178.2 (3)
O4—N2—C7—C6	−56 (3)	C20—C21—C22—C23	0.7 (5)
O3—N2—C7—C6	117.4 (11)	C24—C21—C22—C23	−178.5 (3)
O4A—N2—C7—C6	−60.1 (15)	C21—C22—C23—C18	0.7 (5)
C6—C7—C8—C9	2.9 (5)	C19—C18—C23—C22	−1.7 (5)
N2—C7—C8—C9	−174.5 (3)	C15—C18—C23—C22	173.9 (3)
C7—C8—C9—C10	−3.6 (5)	Ni1—O5—C24—O6	−17.5 (4)
C7—C8—C9—C12	174.5 (3)	Ni1—O5—C24—C21	162.00 (18)
C8—C9—C10—C11	1.5 (5)	C20—C21—C24—O6	−179.4 (3)
C12—C9—C10—C11	−176.5 (3)	C22—C21—C24—O6	−0.2 (4)
C9—C10—C11—C6	1.4 (6)	C20—C21—C24—O5	1.0 (4)
C7—C6—C11—C10	−2.2 (5)	C22—C21—C24—O5	−179.7 (3)
C3—C6—C11—C10	179.3 (3)	C28—N5—C26—O9A	166.6 (17)
Ni2—O1—C12—O2	14.6 (5)	C27—N5—C26—O9A	−21.9 (19)
Ni2—O1—C12—C9	−163.34 (19)	C28—N5—C26—O9	−161.0 (17)
C8—C9—C12—O2	−178.3 (3)	C27—N5—C26—O9	10.5 (19)
C10—C9—C12—O2	−0.3 (5)	C28—N5—C26—C25	0.7 (13)
C8—C9—C12—O1	−0.2 (4)	C27—N5—C26—C25	172.2 (7)
C10—C9—C12—O1	177.8 (3)	C32—N6—C30—O10	173.9 (13)
C17—N3—C13—C14	1.4 (5)	C29—N6—C30—O10	−3.7 (19)
Ni2^v—N3—C13—C14	−174.5 (3)	C32—N6—C30—C31	−5 (2)
N3—C13—C14—C15	−0.2 (5)	C29—N6—C30—C31	177.5 (11)
C13—C14—C15—C16	−1.0 (5)	C32—N6A—C30A—O10	−176.8 (10)
C13—C14—C15—C18	175.4 (3)	C31—N6A—C30A—O10	6.5 (15)
C14—C15—C16—C17	0.9 (5)	C32—N6A—C30A—C29	1.2 (17)
C18—C15—C16—C17	−175.2 (3)	C31—N6A—C30A—C29	−175.5 (10)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···O6	0.85	1.89	2.717 (4)	163
O1W—H1WB···O9ⁱ	0.85	1.91	2.707 (18)	156
O2W—H2WA···O2ⁱⁱ	0.85	1.98	2.706 (4)	142
O2W—H2WB···O6^vi	0.85	1.98	2.815 (4)	168
C1—H1A···O3^vii	0.93	2.48	3.104 (19)	125
C4—H4A···O2^viii	0.93	2.44	3.317 (5)	157
C5—H5A···O6	0.93	2.47	3.334 (4)	155
C14—H14A···O10	0.93	2.36	3.210 (7)	153
C16—H16A···O9^ix	0.93	2.48	3.393 (15)	167
C27—H27B···O8	0.96	2.57	3.227 (13)	126
C28—H28C···O8	0.96	2.60	3.183 (15)	120
C32—H32C···O2^viii	0.96	2.56	3.505 (11)	170

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

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