Characterization and gas adsorption of a novel three-dimensional metal–organic framework (MOF) generated from a new polydentate fluorene-bridged ligand

A polydentate ligand bridged by a fluorene group, namely 9,9-bis­(2-hy­droxy­eth­yl)-2,7-bis­(pyridin-4-yl)fluorene (L), has been prepared under solvothermal conditions in aceto­nitrile. Crystals of the three-dimensional metal–organic frame­work (MOF) poly[[[μ₃-9,9-bis­(2-hy­droxy­eth­yl)-2,7-bis­(pyridin-4-yl)fluorene-κ³N:N′:O]bis­(methanol-κO)(μ-sulfato-κ²O:O′)nickel(II)] methanol disolvate], {[Ni(SO₄)(C₂₇H₂₄N₂O₂)(CH₃OH)]·2CH₃OH}_n, (I), were obtained by the solvothermal reaction of L and NiSO₄ in methanol. The ligand L forms a two-dimensional network in the crystallographic bc plane via two groups of O—H...N hydrogen bonds and neighbouring two-dimensional planes are completely parallel and stack to form a three-dimensional structure. In (I), the Ni^II ions are linked by sulfate ions through Ni—O bonds to form inorganic chains and these Ni-containing chains are linked into a three-dimensional framework via Ni—O and Ni—N bonds involving the polydentate ligand L. With one of the hy­droxy groups of L coordinating to the Ni^II atom, the torsion angle of the hy­droxy­ethyl group changes from that of the uncoordinated mol­ecule. In addition, the adsorption properties of (I) with carbon dioxide were investigated.

Computing details

For both structures, data collection: CrysAlis PRO (Rigaku OD, 2015); cell refinement: CrysAlis PRO (Rigaku OD, 2015); data reduction: CrysAlis PRO (Rigaku OD, 2015); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

9,9-Bis(2-hydroxyethyl)-2,7-bis(pyridin-4-yl)fluorene (L)

Crystal data

C27H24N2O2	Dx = 1.289 Mg m^−3
Mr = 408.48	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pbca	Cell parameters from 7179 reflections
a = 18.4485 (4) Å	θ = 3.7–28.8°
b = 11.6452 (3) Å	µ = 0.08 mm^−1
c = 19.5931 (5) Å	T = 128 K
V = 4209.31 (18) Å^3	Block, clear light yellow
Z = 8	0.36 × 0.33 × 0.24 mm
F(000) = 1728

Data collection

Rigaku Oxford Diffraction SuperNova Dual Source diffractometer with an Eos detector	Rint = 0.024
ω scans	θmax = 25.7°, θmin = 3.0°
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015)	h = −22→22
Tmin = 0.863, Tmax = 1.000	k = −14→14
14992 measured reflections	l = −22→23
3985 independent reflections	17227 standard reflections every 1.00 reflections
3508 reflections with I > 2σ(I)

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.037	H-atom parameters constrained
wR(F^2) = 0.093	w = 1/[σ^2(Fo^2) + (0.0345P)^2 + 2.4368P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.001
3985 reflections	Δρmax = 0.24 e Å^−3
282 parameters	Δρmin = −0.21 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.

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

	x	y	z	Uiso*/Ueq
C1	0.68936 (8)	−0.40557 (13)	0.17107 (7)	0.0224 (3)
H1A	0.6828	−0.4847	0.1732	0.027*
C2	0.65573 (8)	−0.33842 (12)	0.21970 (7)	0.0194 (3)
H2A	0.6274	−0.3722	0.2534	0.023*
C3	0.66449 (7)	−0.21956 (12)	0.21792 (7)	0.0169 (3)
C4	0.70571 (8)	−0.17496 (13)	0.16479 (7)	0.0221 (3)
H4	0.7119	−0.0960	0.1605	0.026*
C5	0.73743 (9)	−0.24877 (14)	0.11854 (8)	0.0270 (4)
H5	0.7650	−0.2172	0.0835	0.032*
C6	0.62990 (7)	−0.14455 (11)	0.26945 (7)	0.0160 (3)
C7	0.66619 (7)	−0.04790 (11)	0.29570 (7)	0.0151 (3)
H7	0.7132	−0.0309	0.2819	0.018*
C8	0.63064 (7)	0.02161 (11)	0.34253 (7)	0.0143 (3)
C9	0.55917 (7)	−0.00362 (11)	0.36188 (7)	0.0154 (3)
C10	0.52343 (7)	−0.09932 (12)	0.33659 (7)	0.0171 (3)
H10	0.4762	−0.1157	0.3499	0.021*
C11	0.55950 (8)	−0.16984 (12)	0.29113 (7)	0.0177 (3)
H11	0.5365	−0.2353	0.2747	0.021*
C12	0.53493 (7)	0.08223 (11)	0.41092 (7)	0.0154 (3)
C13	0.46785 (7)	0.09609 (12)	0.44180 (7)	0.0184 (3)
H13	0.4299	0.0460	0.4322	0.022*
C14	0.45856 (7)	0.18578 (12)	0.48705 (7)	0.0181 (3)
H14	0.4136	0.1968	0.5074	0.022*
C15	0.51574 (7)	0.26061 (12)	0.50282 (7)	0.0156 (3)
C16	0.58333 (7)	0.24591 (11)	0.47135 (7)	0.0153 (3)
H16	0.6217	0.2948	0.4816	0.018*
C17	0.59229 (7)	0.15742 (11)	0.42466 (6)	0.0143 (3)
C18	0.65824 (7)	0.12760 (11)	0.38081 (7)	0.0139 (3)
C19	0.72616 (7)	0.10035 (12)	0.42370 (7)	0.0160 (3)
H19A	0.7656	0.0811	0.3930	0.019*
H19B	0.7401	0.1690	0.4485	0.019*
C20	0.71675 (8)	0.00344 (13)	0.47407 (8)	0.0236 (3)
H20A	0.6790	0.0226	0.5066	0.028*
H20B	0.7026	−0.0660	0.4503	0.028*
C21	0.67701 (7)	0.22850 (11)	0.33251 (7)	0.0161 (3)
H21A	0.6865	0.2963	0.3598	0.019*
H21B	0.7212	0.2099	0.3080	0.019*
C22	0.61797 (8)	0.25646 (12)	0.28110 (7)	0.0215 (3)
H22A	0.6194	0.2007	0.2443	0.026*
H22B	0.5710	0.2506	0.3031	0.026*
C23	0.50192 (7)	0.35247 (11)	0.55343 (7)	0.0156 (3)
C24	0.55159 (8)	0.38098 (12)	0.60438 (7)	0.0196 (3)
H24	0.5974	0.3478	0.6048	0.023*
C25	0.53198 (8)	0.45901 (12)	0.65426 (7)	0.0219 (3)
H25	0.5656	0.4764	0.6881	0.026*
C26	0.42142 (8)	0.48729 (12)	0.60573 (7)	0.0194 (3)
H26	0.3770	0.5251	0.6051	0.023*
C27	0.43578 (7)	0.41040 (12)	0.55415 (7)	0.0177 (3)
H27	0.4017	0.3972	0.5201	0.021*
N1	0.73088 (7)	−0.36304 (11)	0.12099 (6)	0.0257 (3)
N2	0.46717 (7)	0.51112 (10)	0.65671 (6)	0.0210 (3)
O1	0.78318 (5)	−0.01461 (10)	0.50879 (5)	0.0263 (3)
H1	0.7756	−0.0501	0.5442	0.039*
O2	0.62634 (6)	0.36894 (8)	0.25347 (5)	0.0222 (2)
H2	0.5970	0.4124	0.2714	0.033*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0243 (7)	0.0182 (7)	0.0248 (8)	0.0016 (6)	−0.0041 (6)	−0.0037 (6)
C2	0.0208 (7)	0.0188 (7)	0.0187 (7)	0.0008 (6)	−0.0011 (6)	0.0005 (6)
C3	0.0157 (6)	0.0193 (7)	0.0158 (7)	0.0013 (5)	−0.0046 (5)	−0.0023 (5)
C4	0.0253 (8)	0.0187 (7)	0.0222 (7)	−0.0025 (6)	0.0022 (6)	−0.0032 (6)
C5	0.0290 (8)	0.0299 (9)	0.0219 (8)	−0.0027 (7)	0.0063 (7)	−0.0037 (6)
C6	0.0192 (7)	0.0143 (7)	0.0144 (7)	0.0022 (5)	−0.0023 (5)	0.0010 (5)
C7	0.0151 (6)	0.0155 (7)	0.0146 (7)	0.0013 (5)	−0.0002 (5)	0.0017 (5)
C8	0.0157 (6)	0.0141 (6)	0.0130 (6)	0.0007 (5)	−0.0017 (5)	0.0016 (5)
C9	0.0161 (7)	0.0170 (7)	0.0132 (6)	0.0007 (5)	−0.0006 (5)	0.0024 (5)
C10	0.0153 (6)	0.0186 (7)	0.0175 (7)	−0.0028 (5)	0.0006 (5)	0.0001 (6)
C11	0.0198 (7)	0.0154 (7)	0.0180 (7)	−0.0023 (6)	−0.0030 (6)	−0.0008 (5)
C12	0.0163 (6)	0.0163 (7)	0.0135 (6)	−0.0001 (5)	−0.0013 (5)	0.0011 (5)
C13	0.0150 (7)	0.0202 (7)	0.0199 (7)	−0.0031 (5)	0.0006 (6)	−0.0009 (6)
C14	0.0132 (6)	0.0228 (7)	0.0183 (7)	0.0012 (5)	0.0035 (5)	0.0000 (6)
C15	0.0171 (7)	0.0170 (7)	0.0127 (6)	0.0014 (5)	−0.0002 (5)	0.0015 (5)
C16	0.0148 (6)	0.0161 (7)	0.0151 (7)	−0.0008 (5)	−0.0010 (5)	0.0008 (5)
C17	0.0139 (6)	0.0161 (7)	0.0128 (6)	0.0012 (5)	−0.0007 (5)	0.0022 (5)
C18	0.0136 (6)	0.0140 (6)	0.0142 (6)	0.0004 (5)	0.0010 (5)	−0.0010 (5)
C19	0.0126 (6)	0.0184 (7)	0.0169 (7)	−0.0010 (5)	0.0007 (5)	−0.0005 (5)
C20	0.0165 (7)	0.0289 (8)	0.0254 (8)	−0.0035 (6)	−0.0037 (6)	0.0085 (6)
C21	0.0165 (6)	0.0151 (7)	0.0166 (7)	0.0000 (5)	0.0029 (5)	−0.0009 (5)
C22	0.0267 (8)	0.0174 (7)	0.0204 (7)	−0.0006 (6)	−0.0028 (6)	0.0024 (6)
C23	0.0168 (7)	0.0157 (7)	0.0143 (6)	−0.0017 (5)	0.0034 (5)	0.0025 (5)
C24	0.0168 (7)	0.0202 (7)	0.0217 (7)	0.0023 (6)	−0.0002 (6)	−0.0014 (6)
C25	0.0232 (7)	0.0218 (7)	0.0207 (7)	0.0009 (6)	−0.0036 (6)	−0.0044 (6)
C26	0.0178 (7)	0.0165 (7)	0.0240 (8)	0.0020 (6)	0.0022 (6)	0.0006 (6)
C27	0.0169 (7)	0.0180 (7)	0.0182 (7)	−0.0005 (5)	−0.0005 (5)	0.0012 (5)
N1	0.0270 (7)	0.0258 (7)	0.0244 (7)	0.0014 (6)	0.0005 (5)	−0.0089 (5)
N2	0.0230 (6)	0.0179 (6)	0.0220 (6)	0.0013 (5)	0.0012 (5)	−0.0026 (5)
O1	0.0173 (5)	0.0385 (6)	0.0232 (6)	−0.0010 (5)	−0.0017 (4)	0.0153 (5)
O2	0.0268 (6)	0.0181 (5)	0.0217 (5)	0.0064 (4)	0.0035 (4)	0.0044 (4)

Geometric parameters (Å, º)

C1—N1	1.340 (2)	C16—C17	1.3878 (19)
C1—C2	1.380 (2)	C16—H16	0.9300
C1—H1A	0.9300	C17—C18	1.5293 (18)
C2—C3	1.394 (2)	C18—C19	1.5417 (18)
C2—H2A	0.9300	C18—C21	1.5480 (18)
C3—C4	1.390 (2)	C19—C20	1.5092 (19)
C3—C6	1.4797 (19)	C19—H19A	0.9700
C4—C5	1.379 (2)	C19—H19B	0.9700
C4—H4	0.9300	C20—O1	1.4174 (17)
C5—N1	1.337 (2)	C20—H20A	0.9700
C5—H5	0.9300	C20—H20B	0.9700
C6—C11	1.3979 (19)	C21—C22	1.5190 (19)
C6—C7	1.4069 (19)	C21—H21A	0.9700
C7—C8	1.3881 (19)	C21—H21B	0.9700
C7—H7	0.9300	C22—O2	1.4258 (17)
C8—C9	1.4032 (19)	C22—H22A	0.9700
C8—C18	1.5314 (18)	C22—H22B	0.9700
C9—C10	1.3864 (19)	C23—C27	1.3943 (19)
C9—C12	1.4570 (19)	C23—C24	1.3951 (19)
C10—C11	1.3823 (19)	C24—C25	1.383 (2)
C10—H10	0.9300	C24—H24	0.9300
C11—H11	0.9300	C25—N2	1.3417 (19)
C12—C13	1.3869 (19)	C25—H25	0.9300
C12—C17	1.3997 (19)	C26—N2	1.3367 (19)
C13—C14	1.3806 (19)	C26—C27	1.376 (2)
C13—H13	0.9300	C26—H26	0.9300
C14—C15	1.403 (2)	C27—H27	0.9300
C14—H14	0.9300	O1—H1	0.8200
C15—C16	1.4017 (19)	O2—H2	0.8200
C15—C23	1.4808 (19)
N1—C1—C2	123.59 (14)	C12—C17—C18	110.57 (11)
N1—C1—H1A	118.2	C17—C18—C8	101.18 (10)
C2—C1—H1A	118.2	C17—C18—C19	112.77 (11)
C1—C2—C3	119.57 (14)	C8—C18—C19	111.80 (11)
C1—C2—H2A	120.2	C17—C18—C21	110.43 (11)
C3—C2—H2A	120.2	C8—C18—C21	112.75 (11)
C4—C3—C2	116.94 (13)	C19—C18—C21	107.91 (10)
C4—C3—C6	121.77 (13)	C20—C19—C18	114.64 (11)
C2—C3—C6	121.28 (13)	C20—C19—H19A	108.6
C5—C4—C3	119.43 (14)	C18—C19—H19A	108.6
C5—C4—H4	120.3	C20—C19—H19B	108.6
C3—C4—H4	120.3	C18—C19—H19B	108.6
N1—C5—C4	123.94 (14)	H19A—C19—H19B	107.6
N1—C5—H5	118.0	O1—C20—C19	108.98 (11)
C4—C5—H5	118.0	O1—C20—H20A	109.9
C11—C6—C7	119.98 (12)	C19—C20—H20A	109.9
C11—C6—C3	118.92 (12)	O1—C20—H20B	109.9
C7—C6—C3	121.10 (12)	C19—C20—H20B	109.9
C8—C7—C6	118.90 (12)	H20A—C20—H20B	108.3
C8—C7—H7	120.5	C22—C21—C18	114.06 (11)
C6—C7—H7	120.5	C22—C21—H21A	108.7
C7—C8—C9	120.03 (12)	C18—C21—H21A	108.7
C7—C8—C18	129.55 (12)	C22—C21—H21B	108.7
C9—C8—C18	110.41 (11)	C18—C21—H21B	108.7
C10—C9—C8	121.25 (13)	H21A—C21—H21B	107.6
C10—C9—C12	129.89 (13)	O2—C22—C21	111.78 (12)
C8—C9—C12	108.84 (12)	O2—C22—H22A	109.3
C11—C10—C9	118.61 (13)	C21—C22—H22A	109.3
C11—C10—H10	120.7	O2—C22—H22B	109.3
C9—C10—H10	120.7	C21—C22—H22B	109.3
C10—C11—C6	121.19 (13)	H22A—C22—H22B	107.9
C10—C11—H11	119.4	C27—C23—C24	116.90 (12)
C6—C11—H11	119.4	C27—C23—C15	120.46 (12)
C13—C12—C17	121.19 (12)	C24—C23—C15	122.54 (12)
C13—C12—C9	129.90 (13)	C25—C24—C23	119.36 (13)
C17—C12—C9	108.91 (12)	C25—C24—H24	120.3
C14—C13—C12	118.62 (13)	C23—C24—H24	120.3
C14—C13—H13	120.7	N2—C25—C24	123.75 (13)
C12—C13—H13	120.7	N2—C25—H25	118.1
C13—C14—C15	121.20 (13)	C24—C25—H25	118.1
C13—C14—H14	119.4	N2—C26—C27	124.22 (13)
C15—C14—H14	119.4	N2—C26—H26	117.9
C16—C15—C14	119.76 (12)	C27—C26—H26	117.9
C16—C15—C23	122.41 (12)	C26—C27—C23	119.39 (13)
C14—C15—C23	117.83 (12)	C26—C27—H27	120.3
C17—C16—C15	119.12 (12)	C23—C27—H27	120.3
C17—C16—H16	120.4	C5—N1—C1	116.49 (13)
C15—C16—H16	120.4	C26—N2—C25	116.24 (12)
C16—C17—C12	120.08 (12)	C20—O1—H1	109.5
C16—C17—C18	129.32 (12)	C22—O2—H2	109.5
N1—C1—C2—C3	0.0 (2)	C9—C12—C17—C16	−178.53 (12)
C1—C2—C3—C4	2.0 (2)	C13—C12—C17—C18	−176.44 (12)
C1—C2—C3—C6	−179.46 (13)	C9—C12—C17—C18	3.20 (15)
C2—C3—C4—C5	−2.1 (2)	C16—C17—C18—C8	179.72 (13)
C6—C3—C4—C5	179.31 (13)	C12—C17—C18—C8	−2.21 (14)
C3—C4—C5—N1	0.4 (2)	C16—C17—C18—C19	60.16 (18)
C4—C3—C6—C11	138.82 (14)	C12—C17—C18—C19	−121.78 (12)
C2—C3—C6—C11	−39.70 (19)	C16—C17—C18—C21	−60.66 (17)
C4—C3—C6—C7	−40.04 (19)	C12—C17—C18—C21	117.41 (12)
C2—C3—C6—C7	141.44 (14)	C7—C8—C18—C17	−178.19 (13)
C11—C6—C7—C8	−0.65 (19)	C9—C8—C18—C17	0.41 (14)
C3—C6—C7—C8	178.20 (12)	C7—C8—C18—C19	−57.93 (18)
C6—C7—C8—C9	−1.31 (19)	C9—C8—C18—C19	120.67 (12)
C6—C7—C8—C18	177.17 (12)	C7—C8—C18—C21	63.86 (18)
C7—C8—C9—C10	1.9 (2)	C9—C8—C18—C21	−117.54 (12)
C18—C8—C9—C10	−176.85 (12)	C17—C18—C19—C20	57.50 (16)
C7—C8—C9—C12	−179.81 (12)	C8—C18—C19—C20	−55.72 (15)
C18—C8—C9—C12	1.44 (15)	C21—C18—C19—C20	179.74 (11)
C8—C9—C10—C11	−0.5 (2)	C18—C19—C20—O1	178.59 (11)
C12—C9—C10—C11	−178.35 (13)	C17—C18—C21—C22	−62.97 (14)
C9—C10—C11—C6	−1.5 (2)	C8—C18—C21—C22	49.39 (15)
C7—C6—C11—C10	2.1 (2)	C19—C18—C21—C22	173.35 (11)
C3—C6—C11—C10	−176.76 (12)	C18—C21—C22—O2	161.16 (11)
C10—C9—C12—C13	−5.2 (2)	C16—C15—C23—C27	141.61 (14)
C8—C9—C12—C13	176.70 (14)	C14—C15—C23—C27	−39.04 (18)
C10—C9—C12—C17	175.20 (14)	C16—C15—C23—C24	−42.00 (19)
C8—C9—C12—C17	−2.89 (15)	C14—C15—C23—C24	137.35 (14)
C17—C12—C13—C14	−0.3 (2)	C27—C23—C24—C25	3.4 (2)
C9—C12—C13—C14	−179.89 (13)	C15—C23—C24—C25	−173.12 (13)
C12—C13—C14—C15	−1.2 (2)	C23—C24—C25—N2	−0.6 (2)
C13—C14—C15—C16	1.2 (2)	N2—C26—C27—C23	−0.2 (2)
C13—C14—C15—C23	−178.18 (13)	C24—C23—C27—C26	−3.00 (19)
C14—C15—C16—C17	0.3 (2)	C15—C23—C27—C26	173.59 (13)
C23—C15—C16—C17	179.66 (12)	C4—C5—N1—C1	1.5 (2)
C15—C16—C17—C12	−1.79 (19)	C2—C1—N1—C5	−1.7 (2)
C15—C16—C17—C18	176.12 (13)	C27—C26—N2—C25	3.0 (2)
C13—C12—C17—C16	1.8 (2)	C24—C25—N2—C26	−2.6 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···N1^i	0.82	1.99	2.7918 (16)	165
O2—H2···N2^ii	0.82	2.04	2.8327 (16)	161

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

Poly[[[µ₃-9,9-bis(2-hydroxyethyl)-2,7-bis(pyridin-4-yl)fluorene-κ³N:N':O]bis(methanol-κO)(µ-sulfato-κ²O:O')nickel(II)] methanol disolvate] (I)

Crystal data

[Ni(SO4)(C27H24N2O2)(CH4O)]·2CH4O	F(000) = 1384
Mr = 659.38	Dx = 1.474 Mg m^−3
Monoclinic, P21/c	Cu Kα radiation, λ = 1.54184 Å
a = 10.2810 (2) Å	Cell parameters from 5220 reflections
b = 23.5073 (5) Å	θ = 4.1–70.8°
c = 12.3557 (2) Å	µ = 2.09 mm^−1
β = 95.674 (2)°	T = 100 K
V = 2971.47 (11) Å^3	Block, clear pale blue
Z = 4	0.10 × 0.08 × 0.01 mm

Data collection

Rigaku Oxford Diffraction SuperNova Dual Source diffractometer with an Eos detector	5310 independent reflections
Radiation source: micro-focus sealed X-ray tube	4551 reflections with I > 2σ(I)
Detector resolution: 16.0793 pixels mm^-1	Rint = 0.027
ω scans	θmax = 67.1°, θmin = 3.8°
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015)	h = −11→12
Tmin = 0.777, Tmax = 1.000	k = −28→26
11187 measured reflections	l = −14→14

Refinement

Refinement on F^2	26 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.037	H-atom parameters constrained
wR(F^2) = 0.101	w = 1/[σ^2(Fo^2) + (0.0483P)^2 + 2.7762P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.067
5310 reflections	Δρmax = 0.51 e Å^−3
423 parameters	Δρmin = −0.63 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.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
C1	0.4692 (2)	0.20471 (12)	0.35664 (19)	0.0238 (5)
H1	0.5027	0.2022	0.4292	0.029*
C2	0.3510 (2)	0.17916 (12)	0.32597 (19)	0.0239 (5)
H2	0.3068	0.1605	0.3777	0.029*
C3	0.2968 (2)	0.18089 (10)	0.21819 (18)	0.0176 (5)
C4	0.3628 (2)	0.21536 (11)	0.1499 (2)	0.0223 (5)
H4	0.3269	0.2220	0.0790	0.027*
C5	0.4814 (2)	0.23979 (10)	0.18668 (19)	0.0202 (5)
H5	0.5234	0.2621	0.1386	0.024*
C6	0.1799 (2)	0.14712 (9)	0.17857 (18)	0.0153 (4)
C7	0.1044 (2)	0.11951 (10)	0.25195 (18)	0.0168 (5)
H7	0.1239	0.1243	0.3265	0.020*
C8	0.0015 (2)	0.08530 (9)	0.21254 (17)	0.0149 (4)
C9	−0.0309 (2)	0.07832 (9)	0.10036 (17)	0.0146 (4)
C10	0.0429 (2)	0.10554 (9)	0.02689 (18)	0.0158 (5)
H10	0.0219	0.1013	−0.0476	0.019*
C11	0.1474 (2)	0.13887 (10)	0.06659 (18)	0.0170 (5)
H11	0.1979	0.1564	0.0177	0.020*
C12	−0.0872 (2)	0.04926 (9)	0.27703 (17)	0.0155 (5)
C13	−0.0088 (2)	0.00542 (10)	0.35055 (18)	0.0174 (5)
H13A	0.0500	0.0259	0.4031	0.021*
H13B	−0.0695	−0.0156	0.3908	0.021*
C14	0.0710 (3)	−0.03699 (11)	0.2917 (2)	0.0277 (6)
H14A	0.0127	−0.0637	0.2517	0.033*
H14B	0.1194	−0.0170	0.2399	0.033*
C15	−0.1679 (2)	0.08531 (10)	0.35113 (18)	0.0175 (5)
H15A	−0.2221	0.0597	0.3888	0.021*
H15B	−0.1076	0.1035	0.4058	0.021*
C16	−0.2553 (2)	0.13086 (10)	0.2962 (2)	0.0192 (5)
H16A	−0.2896	0.1175	0.2247	0.023*
H16B	−0.3288	0.1371	0.3383	0.023*
C17	−0.1751 (2)	0.02164 (9)	0.18539 (18)	0.0148 (4)
C18	−0.1425 (2)	0.04007 (9)	0.08320 (18)	0.0144 (4)
C19	−0.2152 (2)	0.02163 (10)	−0.01157 (18)	0.0163 (5)
H19	−0.1953	0.0345	−0.0792	0.020*
C20	−0.3173 (2)	−0.01609 (10)	−0.00387 (18)	0.0169 (5)
H20	−0.3652	−0.0288	−0.0671	0.020*
C21	−0.3499 (2)	−0.03555 (9)	0.09732 (18)	0.0162 (5)
C22	−0.2778 (2)	−0.01565 (9)	0.19269 (18)	0.0165 (5)
H22	−0.2992	−0.0276	0.2605	0.020*
C23	−0.4568 (2)	−0.07725 (9)	0.10493 (18)	0.0157 (5)
C24	−0.5247 (2)	−0.08084 (10)	0.19721 (19)	0.0182 (5)
H24	−0.5071	−0.0549	0.2536	0.022*
C25	−0.6174 (2)	−0.12239 (10)	0.20528 (18)	0.0174 (5)
H25	−0.6611	−0.1235	0.2677	0.021*
C26	−0.5875 (2)	−0.15632 (10)	0.03599 (18)	0.0183 (5)
H26	−0.6097	−0.1817	−0.0206	0.022*
C27	−0.4946 (2)	−0.11562 (10)	0.02178 (18)	0.0200 (5)
H27	−0.4570	−0.1137	−0.0435	0.024*
C30	1.0356 (2)	0.27073 (12)	0.3438 (2)	0.0243 (5)
H30A	1.0228	0.2623	0.2675	0.036*
H30B	1.0596	0.2366	0.3836	0.036*
H30C	1.1040	0.2984	0.3569	0.036*
N1	0.53889 (18)	0.23304 (8)	0.28799 (15)	0.0150 (4)
N2	−0.64818 (18)	−0.16156 (8)	0.12745 (15)	0.0156 (4)
Ni1	0.73221 (3)	0.26092 (2)	0.33202 (3)	0.01156 (11)
O1	−0.18821 (15)	0.18421 (6)	0.28478 (12)	0.0164 (3)
H1A	−0.1081	0.1844	0.2558	0.020*
O2	0.16005 (19)	−0.06725 (8)	0.36675 (15)	0.0318 (4)
H2A	0.1266	−0.0973	0.3832	0.048*
O3	0.72141 (14)	0.22520 (7)	0.48372 (11)	0.0146 (3)
O4	0.74612 (15)	0.21042 (6)	0.67592 (12)	0.0152 (3)
O5	0.91173 (16)	0.17564 (7)	0.56826 (13)	0.0214 (4)
O6	0.88783 (16)	0.27725 (7)	0.59425 (12)	0.0178 (3)
O7	0.91715 (15)	0.29293 (7)	0.37878 (12)	0.0157 (3)
H7A	0.9274	0.2977	0.4466	0.024*
S1	0.81885 (5)	0.22197 (2)	0.58076 (4)	0.01186 (13)
O8	0.5056 (5)	0.4624 (3)	0.8614 (5)	0.0554 (18)	0.438 (5)
H8	0.5469	0.4741	0.9171	0.083*	0.438 (5)
C29	0.3701 (8)	0.4678 (4)	0.8708 (9)	0.045 (2)	0.438 (5)
H29A	0.3538	0.4621	0.9452	0.068*	0.438 (5)
H29B	0.3232	0.4398	0.8258	0.068*	0.438 (5)
H29C	0.3415	0.5051	0.8478	0.068*	0.438 (5)
O8'	0.3952 (5)	0.5231 (2)	0.9260 (4)	0.0602 (15)	0.562 (5)
H8'	0.4400	0.5298	0.9832	0.090*	0.562 (5)
C29'	0.3853 (13)	0.4621 (4)	0.9099 (10)	0.099 (5)	0.562 (5)
H29D	0.4667	0.4445	0.9358	0.149*	0.562 (5)
H29E	0.3657	0.4541	0.8339	0.149*	0.562 (5)
H29F	0.3169	0.4474	0.9495	0.149*	0.562 (5)
O9	0.1546 (7)	0.1396 (5)	0.5265 (5)	0.044 (2)	0.417 (13)
H9	0.0944	0.1625	0.5270	0.066*	0.417 (13)
C28	0.2307 (3)	0.14239 (14)	0.6223 (3)	0.0409 (7)	0.417 (13)
H28A	0.2235	0.1795	0.6535	0.061*	0.417 (13)
H28B	0.3201	0.1353	0.6101	0.061*	0.417 (13)
H28C	0.2026	0.1143	0.6713	0.061*	0.417 (13)
O9'	0.1727 (4)	0.1712 (3)	0.5312 (3)	0.0327 (14)	0.583 (13)
H9'	0.0948	0.1759	0.5374	0.049*	0.583 (13)
C28'	0.2307 (3)	0.14239 (14)	0.6223 (3)	0.0409 (7)	0.583 (13)
H28D	0.3091	0.1619	0.6501	0.061*	0.583 (13)
H28E	0.2519	0.1043	0.6022	0.061*	0.583 (13)
H28F	0.1711	0.1412	0.6773	0.061*	0.583 (13)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0207 (12)	0.0380 (15)	0.0128 (11)	−0.0053 (11)	0.0028 (9)	−0.0014 (10)
C2	0.0193 (12)	0.0379 (15)	0.0152 (11)	−0.0077 (11)	0.0054 (9)	0.0013 (10)
C3	0.0167 (11)	0.0183 (11)	0.0181 (11)	0.0023 (9)	0.0027 (9)	−0.0014 (9)
C4	0.0233 (12)	0.0252 (13)	0.0175 (12)	−0.0058 (10)	−0.0026 (9)	0.0052 (10)
C5	0.0207 (12)	0.0211 (12)	0.0186 (12)	−0.0055 (10)	0.0006 (9)	0.0053 (9)
C6	0.0146 (11)	0.0158 (11)	0.0155 (11)	0.0018 (9)	0.0008 (8)	0.0012 (9)
C7	0.0181 (11)	0.0190 (11)	0.0135 (11)	0.0008 (9)	0.0019 (9)	0.0007 (9)
C8	0.0169 (11)	0.0137 (11)	0.0146 (11)	0.0020 (9)	0.0049 (9)	0.0010 (8)
C9	0.0154 (11)	0.0140 (10)	0.0145 (11)	0.0038 (9)	0.0029 (8)	0.0012 (8)
C10	0.0189 (11)	0.0165 (11)	0.0119 (10)	0.0004 (9)	0.0015 (8)	0.0015 (8)
C11	0.0166 (11)	0.0170 (11)	0.0178 (11)	0.0000 (9)	0.0045 (9)	0.0031 (9)
C12	0.0184 (11)	0.0159 (11)	0.0127 (10)	−0.0024 (9)	0.0038 (9)	0.0000 (9)
C13	0.0228 (12)	0.0162 (11)	0.0134 (10)	−0.0003 (9)	0.0034 (9)	0.0014 (9)
C14	0.0418 (16)	0.0226 (13)	0.0194 (12)	0.0093 (12)	0.0068 (11)	0.0046 (10)
C15	0.0223 (12)	0.0158 (11)	0.0150 (11)	−0.0025 (9)	0.0055 (9)	0.0001 (9)
C16	0.0182 (11)	0.0155 (11)	0.0248 (12)	−0.0029 (9)	0.0062 (9)	−0.0033 (9)
C17	0.0165 (11)	0.0151 (11)	0.0131 (11)	0.0014 (9)	0.0027 (8)	0.0002 (8)
C18	0.0147 (10)	0.0136 (10)	0.0155 (11)	0.0012 (9)	0.0047 (8)	0.0001 (8)
C19	0.0187 (11)	0.0164 (11)	0.0141 (11)	0.0009 (9)	0.0040 (9)	0.0018 (8)
C20	0.0173 (11)	0.0185 (11)	0.0148 (11)	−0.0011 (9)	0.0004 (9)	−0.0016 (9)
C21	0.0164 (11)	0.0146 (11)	0.0183 (11)	0.0008 (9)	0.0050 (9)	0.0000 (9)
C22	0.0207 (11)	0.0158 (11)	0.0138 (11)	−0.0007 (9)	0.0054 (9)	0.0019 (9)
C23	0.0152 (11)	0.0149 (11)	0.0171 (11)	0.0011 (9)	0.0010 (9)	0.0030 (9)
C24	0.0208 (11)	0.0169 (11)	0.0171 (11)	−0.0028 (9)	0.0029 (9)	−0.0008 (9)
C25	0.0200 (11)	0.0178 (11)	0.0150 (11)	0.0014 (9)	0.0051 (9)	−0.0003 (9)
C26	0.0216 (12)	0.0193 (11)	0.0143 (11)	−0.0036 (10)	0.0035 (9)	−0.0015 (9)
C27	0.0227 (12)	0.0230 (12)	0.0152 (11)	−0.0034 (10)	0.0058 (9)	0.0016 (9)
C30	0.0164 (12)	0.0366 (15)	0.0203 (12)	0.0012 (10)	0.0039 (9)	−0.0073 (11)
N1	0.0148 (9)	0.0174 (9)	0.0131 (9)	−0.0008 (8)	0.0030 (7)	−0.0015 (7)
N2	0.0163 (9)	0.0161 (9)	0.0150 (9)	0.0007 (8)	0.0042 (7)	0.0012 (7)
Ni1	0.01259 (19)	0.0133 (2)	0.00914 (19)	0.00018 (14)	0.00260 (14)	0.00016 (14)
O1	0.0178 (8)	0.0142 (8)	0.0181 (8)	0.0002 (6)	0.0069 (6)	0.0003 (6)
O2	0.0370 (11)	0.0247 (10)	0.0341 (10)	0.0095 (8)	0.0055 (8)	0.0088 (8)
O3	0.0150 (8)	0.0190 (8)	0.0095 (7)	−0.0008 (6)	0.0006 (6)	0.0022 (6)
O4	0.0207 (8)	0.0158 (8)	0.0100 (7)	−0.0039 (6)	0.0053 (6)	0.0000 (6)
O5	0.0194 (8)	0.0237 (9)	0.0211 (8)	0.0064 (7)	0.0030 (7)	−0.0013 (7)
O6	0.0224 (8)	0.0202 (8)	0.0113 (7)	−0.0067 (7)	0.0045 (6)	−0.0008 (6)
O7	0.0159 (8)	0.0208 (8)	0.0107 (7)	−0.0022 (6)	0.0026 (6)	−0.0016 (6)
S1	0.0128 (2)	0.0146 (3)	0.0086 (2)	0.0005 (2)	0.00273 (19)	0.00013 (19)
O8	0.043 (3)	0.073 (4)	0.050 (3)	0.009 (3)	0.007 (2)	0.003 (3)
C29	0.037 (3)	0.039 (3)	0.059 (4)	−0.007 (3)	0.004 (3)	0.004 (3)
O8'	0.064 (3)	0.056 (3)	0.061 (3)	−0.011 (2)	0.003 (2)	0.003 (2)
C29'	0.099 (6)	0.095 (5)	0.102 (6)	0.002 (4)	0.004 (4)	0.000 (4)
O9	0.034 (3)	0.064 (4)	0.033 (3)	0.010 (3)	0.006 (2)	−0.006 (3)
C28	0.0334 (16)	0.0428 (18)	0.0459 (18)	0.0013 (14)	0.0001 (13)	0.0091 (14)
O9'	0.0215 (18)	0.049 (3)	0.0290 (18)	0.0058 (18)	0.0095 (13)	0.0089 (18)
C28'	0.0334 (16)	0.0428 (18)	0.0459 (18)	0.0013 (14)	0.0001 (13)	0.0091 (14)

Geometric parameters (Å, º)

C1—N1	1.340 (3)	C23—C27	1.393 (3)
C1—C2	1.375 (3)	C23—C24	1.397 (3)
C1—H1	0.9300	C24—C25	1.375 (3)
C2—C3	1.392 (3)	C24—H24	0.9300
C2—H2	0.9300	C25—N2	1.346 (3)
C3—C4	1.394 (3)	C25—H25	0.9300
C3—C6	1.483 (3)	C26—N2	1.350 (3)
C4—C5	1.383 (3)	C26—C27	1.375 (3)
C4—H4	0.9300	C26—H26	0.9300
C5—N1	1.340 (3)	C27—H27	0.9300
C5—H5	0.9300	C30—O7	1.431 (3)
C6—C11	1.404 (3)	C30—H30A	0.9600
C6—C7	1.409 (3)	C30—H30B	0.9600
C7—C8	1.379 (3)	C30—H30C	0.9600
C7—H7	0.9300	N1—Ni1	2.1123 (19)
C8—C9	1.403 (3)	N2—Ni1^i	2.0984 (19)
C8—C12	1.526 (3)	Ni1—O4^ii	2.0612 (15)
C9—C10	1.394 (3)	Ni1—O3	2.0669 (15)
C9—C18	1.457 (3)	Ni1—O7	2.0732 (15)
C10—C11	1.381 (3)	Ni1—O1^iii	2.0869 (16)
C10—H10	0.9300	Ni1—N2^iv	2.0984 (19)
C11—H11	0.9300	O1—Ni1^v	2.0871 (16)
C12—C17	1.522 (3)	O1—H1A	0.9300
C12—C13	1.547 (3)	O2—H2A	0.8200
C12—C15	1.547 (3)	O3—S1	1.4864 (15)
C13—C14	1.521 (3)	O4—S1	1.4795 (15)
C13—H13A	0.9700	O4—Ni1^vi	2.0612 (15)
C13—H13B	0.9700	O5—S1	1.4666 (17)
C14—O2	1.427 (3)	O6—S1	1.4820 (16)
C14—H14A	0.9700	O7—H7A	0.8417
C14—H14B	0.9700	O8—C29	1.414 (8)
C15—C16	1.514 (3)	O8—H8	0.8200
C15—H15A	0.9700	C29—H29A	0.9600
C15—H15B	0.9700	C29—H29B	0.9600
C16—O1	1.445 (3)	C29—H29C	0.9600
C16—H16A	0.9700	O8'—C29'	1.449 (8)
C16—H16B	0.9700	O8'—H8'	0.8200
C17—C22	1.382 (3)	C29'—H29D	0.9600
C17—C18	1.406 (3)	C29'—H29E	0.9600
C18—C19	1.394 (3)	C29'—H29F	0.9600
C19—C20	1.385 (3)	O9—C28	1.354 (7)
C19—H19	0.9300	O9—H9	0.8200
C20—C21	1.403 (3)	C28—H28A	0.9600
C20—H20	0.9300	C28—H28B	0.9600
C21—C22	1.409 (3)	C28—H28C	0.9600
C21—C23	1.482 (3)	O9'—H9'	0.8200
C22—H22	0.9300
N1—C1—C2	123.8 (2)	C21—C22—H22	120.1
N1—C1—H1	118.1	C27—C23—C24	115.9 (2)
C2—C1—H1	118.1	C27—C23—C21	122.4 (2)
C1—C2—C3	120.7 (2)	C24—C23—C21	121.7 (2)
C1—C2—H2	119.7	C25—C24—C23	120.5 (2)
C3—C2—H2	119.7	C25—C24—H24	119.7
C2—C3—C4	115.0 (2)	C23—C24—H24	119.7
C2—C3—C6	122.3 (2)	N2—C25—C24	123.3 (2)
C4—C3—C6	122.6 (2)	N2—C25—H25	118.3
C5—C4—C3	120.5 (2)	C24—C25—H25	118.3
C5—C4—H4	119.7	N2—C26—C27	123.7 (2)
C3—C4—H4	119.7	N2—C26—H26	118.2
N1—C5—C4	123.5 (2)	C27—C26—H26	118.2
N1—C5—H5	118.3	C26—C27—C23	120.2 (2)
C4—C5—H5	118.3	C26—C27—H27	119.9
C11—C6—C7	118.6 (2)	C23—C27—H27	119.9
C11—C6—C3	120.4 (2)	O7—C30—H30A	109.5
C7—C6—C3	121.0 (2)	O7—C30—H30B	109.5
C8—C7—C6	119.6 (2)	H30A—C30—H30B	109.5
C8—C7—H7	120.2	O7—C30—H30C	109.5
C6—C7—H7	120.2	H30A—C30—H30C	109.5
C7—C8—C9	121.0 (2)	H30B—C30—H30C	109.5
C7—C8—C12	128.1 (2)	C5—N1—C1	115.8 (2)
C9—C8—C12	110.84 (19)	C5—N1—Ni1	121.40 (15)
C10—C9—C8	119.9 (2)	C1—N1—Ni1	122.65 (15)
C10—C9—C18	131.3 (2)	C25—N2—C26	116.1 (2)
C8—C9—C18	108.79 (19)	C25—N2—Ni1^i	119.78 (15)
C11—C10—C9	118.9 (2)	C26—N2—Ni1^i	120.97 (15)
C11—C10—H10	120.5	O4^ii—Ni1—O3	175.05 (6)
C9—C10—H10	120.5	O4^ii—Ni1—O7	89.74 (6)
C10—C11—C6	122.0 (2)	O3—Ni1—O7	91.42 (6)
C10—C11—H11	119.0	O4^ii—Ni1—O1^iii	87.44 (6)
C6—C11—H11	119.0	O3—Ni1—O1^iii	87.73 (6)
C17—C12—C8	100.94 (17)	O7—Ni1—O1^iii	91.00 (6)
C17—C12—C13	112.91 (18)	O4^ii—Ni1—N2^iv	90.44 (7)
C8—C12—C13	111.89 (18)	O3—Ni1—N2^iv	94.36 (7)
C17—C12—C15	111.11 (18)	O7—Ni1—N2^iv	90.35 (7)
C8—C12—C15	112.82 (18)	O1^iii—Ni1—N2^iv	177.49 (7)
C13—C12—C15	107.23 (17)	O4^ii—Ni1—N1	90.63 (7)
C14—C13—C12	115.50 (19)	O3—Ni1—N1	88.51 (7)
C14—C13—H13A	108.4	O7—Ni1—N1	176.42 (7)
C12—C13—H13A	108.4	O1^iii—Ni1—N1	92.57 (7)
C14—C13—H13B	108.4	N2^iv—Ni1—N1	86.09 (7)
C12—C13—H13B	108.4	C16—O1—Ni1^v	121.23 (13)
H13A—C13—H13B	107.5	C16—O1—H1A	119.4
O2—C14—C13	111.0 (2)	Ni1^v—O1—H1A	119.4
O2—C14—H14A	109.4	C14—O2—H2A	109.5
C13—C14—H14A	109.4	S1—O3—Ni1	131.30 (9)
O2—C14—H14B	109.4	S1—O4—Ni1^vi	140.44 (10)
C13—C14—H14B	109.4	C30—O7—Ni1	124.62 (14)
H14A—C14—H14B	108.0	C30—O7—H7A	108.8
C16—C15—C12	116.81 (19)	Ni1—O7—H7A	110.3
C16—C15—H15A	108.1	O5—S1—O4	109.45 (9)
C12—C15—H15A	108.1	O5—S1—O6	110.71 (10)
C16—C15—H15B	108.1	O4—S1—O6	110.20 (9)
C12—C15—H15B	108.1	O5—S1—O3	110.30 (9)
H15A—C15—H15B	107.3	O4—S1—O3	107.29 (9)
O1—C16—C15	112.93 (19)	O6—S1—O3	108.83 (9)
O1—C16—H16A	109.0	C29—O8—H8	109.5
C15—C16—H16A	109.0	O8—C29—H29A	109.5
O1—C16—H16B	109.0	O8—C29—H29B	109.5
C15—C16—H16B	109.0	H29A—C29—H29B	109.5
H16A—C16—H16B	107.8	O8—C29—H29C	109.5
C22—C17—C18	120.4 (2)	H29A—C29—H29C	109.5
C22—C17—C12	128.5 (2)	H29B—C29—H29C	109.5
C18—C17—C12	111.09 (19)	C29'—O8'—H8'	109.5
C19—C18—C17	120.2 (2)	O8'—C29'—H29D	109.5
C19—C18—C9	131.5 (2)	O8'—C29'—H29E	109.5
C17—C18—C9	108.29 (19)	H29D—C29'—H29E	109.5
C20—C19—C18	119.2 (2)	O8'—C29'—H29F	109.5
C20—C19—H19	120.4	H29D—C29'—H29F	109.5
C18—C19—H19	120.4	H29E—C29'—H29F	109.5
C19—C20—C21	121.3 (2)	C28—O9—H9	109.5
C19—C20—H20	119.3	O9—C28—H28A	109.5
C21—C20—H20	119.3	O9—C28—H28B	109.5
C20—C21—C22	119.0 (2)	H28A—C28—H28B	109.5
C20—C21—C23	121.1 (2)	O9—C28—H28C	109.5
C22—C21—C23	119.9 (2)	H28A—C28—H28C	109.5
C17—C22—C21	119.9 (2)	H28B—C28—H28C	109.5
C17—C22—H22	120.1
N1—C1—C2—C3	0.8 (4)	C22—C17—C18—C19	1.2 (3)
C1—C2—C3—C4	−7.2 (4)	C12—C17—C18—C19	−177.3 (2)
C1—C2—C3—C6	171.0 (2)	C22—C17—C18—C9	−179.5 (2)
C2—C3—C4—C5	7.3 (4)	C12—C17—C18—C9	2.1 (3)
C6—C3—C4—C5	−170.9 (2)	C10—C9—C18—C19	−4.6 (4)
C3—C4—C5—N1	−1.0 (4)	C8—C9—C18—C19	176.7 (2)
C2—C3—C6—C11	−164.2 (2)	C10—C9—C18—C17	176.2 (2)
C4—C3—C6—C11	13.8 (3)	C8—C9—C18—C17	−2.5 (3)
C2—C3—C6—C7	11.4 (3)	C17—C18—C19—C20	−1.7 (3)
C4—C3—C6—C7	−170.5 (2)	C9—C18—C19—C20	179.2 (2)
C11—C6—C7—C8	0.1 (3)	C18—C19—C20—C21	0.8 (3)
C3—C6—C7—C8	−175.7 (2)	C19—C20—C21—C22	0.7 (3)
C6—C7—C8—C9	−1.1 (3)	C19—C20—C21—C23	−178.2 (2)
C6—C7—C8—C12	176.3 (2)	C18—C17—C22—C21	0.3 (3)
C7—C8—C9—C10	1.0 (3)	C12—C17—C22—C21	178.4 (2)
C12—C8—C9—C10	−176.92 (19)	C20—C21—C22—C17	−1.2 (3)
C7—C8—C9—C18	179.9 (2)	C23—C21—C22—C17	177.7 (2)
C12—C8—C9—C18	2.0 (2)	C20—C21—C23—C27	26.2 (3)
C8—C9—C10—C11	0.3 (3)	C22—C21—C23—C27	−152.7 (2)
C18—C9—C10—C11	−178.3 (2)	C20—C21—C23—C24	−154.7 (2)
C9—C10—C11—C6	−1.4 (3)	C22—C21—C23—C24	26.5 (3)
C7—C6—C11—C10	1.2 (3)	C27—C23—C24—C25	3.6 (3)
C3—C6—C11—C10	177.0 (2)	C21—C23—C24—C25	−175.6 (2)
C7—C8—C12—C17	−178.4 (2)	C23—C24—C25—N2	0.3 (4)
C9—C8—C12—C17	−0.7 (2)	N2—C26—C27—C23	1.0 (4)
C7—C8—C12—C13	−58.1 (3)	C24—C23—C27—C26	−4.2 (3)
C9—C8—C12—C13	119.6 (2)	C21—C23—C27—C26	175.1 (2)
C7—C8—C12—C15	63.0 (3)	C4—C5—N1—C1	−5.6 (4)
C9—C8—C12—C15	−119.3 (2)	C4—C5—N1—Ni1	170.6 (2)
C17—C12—C13—C14	53.5 (3)	C2—C1—N1—C5	5.7 (4)
C8—C12—C13—C14	−59.5 (3)	C2—C1—N1—Ni1	−170.4 (2)
C15—C12—C13—C14	176.3 (2)	C24—C25—N2—C26	−3.6 (3)
C12—C13—C14—O2	167.7 (2)	C24—C25—N2—Ni1^i	156.65 (18)
C17—C12—C15—C16	−55.1 (3)	C27—C26—N2—C25	3.0 (3)
C8—C12—C15—C16	57.4 (3)	C27—C26—N2—Ni1^i	−157.00 (19)
C13—C12—C15—C16	−178.91 (19)	C15—C16—O1—Ni1^v	−130.85 (16)
C12—C15—C16—O1	−86.7 (2)	Ni1^vi—O4—S1—O5	108.51 (16)
C8—C12—C17—C22	−179.1 (2)	Ni1^vi—O4—S1—O6	−13.46 (19)
C13—C12—C17—C22	61.3 (3)	Ni1^vi—O4—S1—O3	−131.80 (15)
C15—C12—C17—C22	−59.3 (3)	Ni1—O3—S1—O5	−80.46 (14)
C8—C12—C17—C18	−0.9 (2)	Ni1—O3—S1—O4	160.40 (11)
C13—C12—C17—C18	−120.5 (2)	Ni1—O3—S1—O6	41.17 (15)
C15—C12—C17—C18	119.0 (2)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O9′—H9′···O5^v	0.82	1.96	2.768 (4)	170
O9—H9···O5^v	0.82	2.02	2.733 (6)	146
O2—H2A···O5^vii	0.82	1.99	2.793 (3)	167
O1—H1A···O6^viii	0.93	2.19	2.709 (2)	115
O7—H7A···O6	0.84	1.97	2.734 (2)	151

Symmetry codes: (v) x−1, y, z; (vii) −x+1, −y, −z+1; (viii) x−1, −y+1/2, z−1/2.