Two-dimensionally stacked heterometallic layers hosting a discrete chair dodecameric ring of water clusters: synthesis and structural study

The stacked two-dimensional supramolecular compound catena-{Co(amp)₃Cr(ox)₃·6H₂O} (amp = 2-picolylamine, ox = oxalate) has been synthesized from the bimolecular approach using hydrogen bonds. It is built from layers in which both Co(amp)³⁺ (D) and Cr(ox)^3- (A) ions are bonded in a repeating DADADA... pattern along the a and c axes by multiple hydrogen bonds. These layers host a well resolved R12 dodecameric discrete ring of water clusters built by six independent molecules located around the 2c centrosymmetric Wyckoff positions of the P2₁/n space group in which the compound crystallizes. These clusters are ranged along the [001] direction, occupy 733.5 Å³ (22.0%) of the unit cell and have a chair conformation via 12 hydrogen bonds. The water molecules of the cluster are linked with stronger hydrogen bonds than those between the cluster and its host, which explains the single continuous step of the dehydration process of the compound.

Computing details

Data collection: APEX2 v2013.4-1 (Bruker AXS, 2013); cell refinement: APEX2 v2013.4-1 (Bruker AXS, 2013); data reduction: APEX2 v2013.4-1 (Bruker AXS, 2013); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND for Windows (Klaus, 2004); software used to prepare material for publication: enCIFer 1.3 (Allen et al., 2004)).

Figures

Catena-{Co(amp)3Cr(ox)3.6H2O}

Crystal data

Co(C6H8N2)3Cr(C2O4)3.6H2O	F(000) = 1668
Mr = 807.52	Dx = 1.612 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 13.1923 (8) Å	θ = 2.3–31.6°
b = 18.0299 (10) Å	µ = 0.91 mm^−1
c = 14.1801 (9) Å	T = 100 K
β = 99.357 (2)°	Prismatic, brown
V = 3327.9 (3) Å^3	0.18 × 0.12 × 0.10 mm
Z = 4

Data collection

D8 Venture Photon, Bruker AXS diffractometer	10353 independent reflections
Radiation source: fine-focus sealed tube	8042 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.054
ω–scans	θmax = 31.6°, θmin = 2.3°
Absorption correction: multi-scan APEX2 v2013.4-1 (Bruker AXS, 2013) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −18→19
Tmin = 0.693, Tmax = 0.746	k = −26→26
100946 measured reflections	l = −19→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.094	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0376P)^2 + 3.4133P] where P = (Fo^2 + 2Fc^2)/3
10353 reflections	(Δ/σ)max = 0.005
505 parameters	Δρmax = 0.70 e Å^−3
18 restraints	Δρmin = −0.56 e Å^−3

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	Uiso*/Ueq
Co	0.221891 (17)	0.211154 (13)	0.417512 (16)	0.01164 (6)
Cr	0.20036 (2)	0.148639 (15)	0.896164 (19)	0.01152 (6)
O3	0.15148 (10)	0.09276 (7)	0.99868 (9)	0.0174 (3)
O11	0.49965 (10)	0.11928 (8)	0.89630 (10)	0.0205 (3)
O6	0.26803 (9)	0.20883 (7)	0.80730 (9)	0.0153 (2)
O12	0.42345 (10)	0.22937 (8)	0.76808 (10)	0.0207 (3)
O2	0.15075 (10)	0.07367 (7)	0.79948 (9)	0.0183 (3)
O4	0.22995 (10)	0.22388 (7)	0.99741 (9)	0.0201 (3)
O1	0.06500 (10)	0.19200 (7)	0.85587 (9)	0.0177 (3)
O5	0.33972 (9)	0.10337 (7)	0.92644 (9)	0.0172 (3)
N4	0.15445 (12)	0.27904 (8)	0.32060 (11)	0.0141 (3)
N5	0.28725 (11)	0.29973 (8)	0.47583 (10)	0.0140 (3)
O10	0.21405 (14)	0.24494 (10)	1.14837 (12)	0.0427 (5)
O7	−0.08746 (10)	0.16494 (8)	0.77116 (10)	0.0235 (3)
O8	0.00560 (13)	0.04289 (9)	0.70042 (12)	0.0358 (4)
N1	0.29683 (11)	0.14262 (8)	0.51120 (10)	0.0144 (3)
N6	0.34045 (12)	0.19734 (9)	0.35248 (11)	0.0161 (3)
N3	0.14964 (12)	0.12764 (9)	0.35107 (11)	0.0157 (3)
N2	0.10514 (11)	0.21718 (8)	0.48382 (10)	0.0149 (3)
O9	0.13700 (11)	0.10025 (9)	1.15293 (10)	0.0285 (3)
C12	0.20497 (13)	0.35287 (10)	0.32656 (12)	0.0148 (3)
H12A	0.1521	0.3923	0.3200	0.018*
H12B	0.2451	0.3583	0.2737	0.018*
C1	0.36526 (13)	0.19708 (9)	0.81295 (12)	0.0139 (3)
C11	0.27467 (13)	0.36086 (10)	0.42036 (12)	0.0148 (3)
C14	0.31662 (15)	0.05566 (10)	0.64058 (14)	0.0210 (4)
H14A	0.2878	0.0301	0.6885	0.025*
C7	0.34713 (14)	0.30352 (10)	0.56295 (13)	0.0187 (4)
H7A	0.3537	0.2610	0.6031	0.022*
C2	0.40790 (13)	0.13491 (10)	0.88434 (12)	0.0147 (3)
C17	0.39554 (14)	0.13095 (10)	0.50074 (13)	0.0166 (3)
C19	0.09717 (15)	0.26067 (11)	0.55960 (13)	0.0200 (4)
H19A	0.1506	0.2948	0.5817	0.024*
C10	0.32543 (15)	0.42658 (10)	0.44855 (14)	0.0199 (4)
H10A	0.3165	0.4689	0.4082	0.024*
C22	−0.05850 (15)	0.16395 (12)	0.49476 (15)	0.0256 (4)
H22A	−0.1120	0.1304	0.4708	0.031*
C3	0.20480 (14)	0.20502 (11)	1.07769 (14)	0.0216 (4)
C6	0.00405 (14)	0.15158 (10)	0.79811 (12)	0.0172 (3)
C24	0.03988 (14)	0.12762 (11)	0.36308 (15)	0.0226 (4)
H24A	0.0159	0.0760	0.3685	0.027*
H24B	−0.0024	0.1507	0.3066	0.027*
C9	0.38924 (16)	0.42961 (11)	0.53621 (14)	0.0231 (4)
H9A	0.4261	0.4737	0.5561	0.028*
C16	0.45803 (14)	0.08212 (11)	0.55956 (14)	0.0209 (4)
H16A	0.5275	0.0750	0.5516	0.025*
C18	0.43160 (14)	0.17573 (11)	0.42348 (13)	0.0184 (4)
H18A	0.4681	0.2206	0.4512	0.022*
H18B	0.4797	0.1461	0.3919	0.022*
C13	0.25810 (14)	0.10527 (10)	0.57998 (13)	0.0171 (3)
H13A	0.1885	0.1133	0.5870	0.021*
C15	0.41839 (16)	0.04396 (11)	0.62985 (14)	0.0228 (4)
H15A	0.4601	0.0101	0.6704	0.027*
C8	0.39850 (15)	0.36745 (11)	0.59453 (14)	0.0225 (4)
H8A	0.4400	0.3690	0.6559	0.027*
C4	0.16032 (13)	0.12603 (11)	1.07948 (13)	0.0188 (4)
C21	−0.06553 (15)	0.20721 (13)	0.57318 (14)	0.0270 (4)
H21A	−0.1236	0.2033	0.6047	0.032*
C23	0.02786 (14)	0.16998 (10)	0.45100 (13)	0.0179 (3)
C5	0.05497 (15)	0.08235 (11)	0.76112 (13)	0.0200 (4)
C20	0.01265 (16)	0.25652 (12)	0.60590 (14)	0.0253 (4)
H20A	0.0084	0.2872	0.6596	0.030*
O1W	0.34866 (14)	−0.06415 (9)	0.85997 (13)	0.0372 (4)
O2W	0.43457 (12)	0.02806 (8)	1.09685 (10)	0.0255 (3)
O5W	0.18874 (12)	0.38509 (8)	0.99724 (12)	0.0299 (3)
O6W	0.2190 (3)	0.36554 (11)	0.81306 (15)	0.0793 (9)
O4W	0.28792 (11)	0.47485 (8)	1.14099 (11)	0.0263 (3)
O3W	0.36046 (11)	0.05199 (8)	0.27300 (11)	0.0267 (3)
H4A	0.158 (2)	0.2611 (14)	0.2656 (19)	0.032*
H4B	0.089 (2)	0.2844 (14)	0.3257 (19)	0.032*
H6B	0.358 (2)	0.2389 (15)	0.3224 (19)	0.032*
H6A	0.332 (2)	0.1599 (15)	0.3138 (19)	0.032*
H3B	0.179 (2)	0.0863 (15)	0.3736 (19)	0.032*
H3A	0.152 (2)	0.1308 (14)	0.289 (2)	0.032*
H1W	0.4196 (8)	−0.0532 (13)	0.8783 (19)	0.040*
H2W	0.3110 (16)	−0.0219 (10)	0.8719 (19)	0.040*
H3W	0.3973 (18)	0.0499 (12)	1.0412 (12)	0.040*
H4W	0.448 (2)	−0.0221 (7)	1.0836 (17)	0.040*
H9W	0.201 (2)	0.3356 (7)	1.0183 (16)	0.040*
H10W	0.195 (2)	0.3862 (14)	0.9315 (8)	0.040*
H11W	0.197 (2)	0.3872 (12)	0.7522 (10)	0.040*
H12W	0.234 (2)	0.3153 (7)	0.8007 (17)	0.040*
H7W	0.3542 (11)	0.4559 (13)	1.1651 (17)	0.040*
H8W	0.2610 (17)	0.4439 (12)	1.0883 (13)	0.040*
H5W	0.3099 (16)	0.0206 (12)	0.2906 (17)	0.040*
H6W	0.369 (2)	0.0428 (14)	0.2099 (9)	0.040*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co	0.01124 (11)	0.01325 (11)	0.01088 (11)	0.00200 (8)	0.00311 (8)	0.00023 (8)
Cr	0.01049 (12)	0.01193 (12)	0.01229 (13)	0.00021 (9)	0.00230 (9)	−0.00001 (10)
O3	0.0188 (6)	0.0188 (6)	0.0159 (6)	−0.0011 (5)	0.0064 (5)	0.0012 (5)
O11	0.0132 (6)	0.0232 (7)	0.0255 (7)	0.0029 (5)	0.0044 (5)	0.0056 (5)
O6	0.0143 (6)	0.0151 (6)	0.0167 (6)	0.0002 (5)	0.0026 (5)	0.0036 (5)
O12	0.0182 (6)	0.0230 (7)	0.0213 (7)	−0.0024 (5)	0.0045 (5)	0.0068 (5)
O2	0.0209 (6)	0.0158 (6)	0.0194 (6)	−0.0020 (5)	0.0070 (5)	−0.0041 (5)
O4	0.0217 (7)	0.0195 (6)	0.0192 (6)	−0.0040 (5)	0.0037 (5)	−0.0049 (5)
O1	0.0129 (6)	0.0196 (6)	0.0200 (6)	0.0022 (5)	0.0011 (5)	−0.0003 (5)
O5	0.0130 (6)	0.0204 (6)	0.0188 (6)	0.0023 (5)	0.0040 (5)	0.0069 (5)
N4	0.0124 (7)	0.0172 (7)	0.0129 (7)	0.0012 (5)	0.0029 (5)	−0.0001 (6)
N5	0.0137 (7)	0.0158 (7)	0.0127 (7)	0.0024 (5)	0.0028 (5)	0.0004 (5)
O10	0.0421 (10)	0.0567 (11)	0.0348 (9)	−0.0245 (9)	0.0231 (8)	−0.0292 (8)
O7	0.0134 (6)	0.0357 (8)	0.0214 (7)	−0.0010 (6)	0.0025 (5)	0.0051 (6)
O8	0.0337 (9)	0.0313 (8)	0.0389 (9)	−0.0052 (7)	−0.0049 (7)	−0.0154 (7)
N1	0.0149 (7)	0.0146 (7)	0.0139 (7)	0.0017 (5)	0.0026 (5)	0.0000 (5)
N6	0.0149 (7)	0.0187 (7)	0.0154 (7)	0.0030 (6)	0.0044 (6)	0.0011 (6)
N3	0.0169 (7)	0.0152 (7)	0.0149 (7)	0.0015 (6)	0.0021 (6)	−0.0013 (6)
N2	0.0148 (7)	0.0172 (7)	0.0134 (7)	0.0042 (6)	0.0043 (5)	0.0026 (6)
O9	0.0270 (8)	0.0431 (9)	0.0168 (7)	0.0012 (7)	0.0079 (6)	0.0050 (6)
C12	0.0141 (8)	0.0161 (8)	0.0143 (8)	0.0022 (6)	0.0032 (6)	0.0026 (6)
C1	0.0151 (8)	0.0121 (7)	0.0140 (8)	−0.0021 (6)	0.0012 (6)	−0.0004 (6)
C11	0.0140 (8)	0.0166 (8)	0.0148 (8)	0.0040 (6)	0.0050 (6)	0.0001 (6)
C14	0.0255 (10)	0.0183 (9)	0.0193 (9)	0.0030 (7)	0.0040 (7)	0.0038 (7)
C7	0.0201 (9)	0.0196 (9)	0.0158 (8)	0.0021 (7)	0.0014 (7)	0.0009 (7)
C2	0.0144 (8)	0.0160 (8)	0.0137 (8)	−0.0007 (6)	0.0026 (6)	0.0002 (6)
C17	0.0157 (8)	0.0155 (8)	0.0184 (8)	0.0009 (6)	0.0027 (7)	−0.0020 (7)
C19	0.0224 (9)	0.0218 (9)	0.0168 (8)	0.0048 (7)	0.0063 (7)	0.0005 (7)
C10	0.0214 (9)	0.0169 (8)	0.0215 (9)	0.0003 (7)	0.0040 (7)	−0.0010 (7)
C22	0.0147 (9)	0.0360 (11)	0.0261 (10)	0.0000 (8)	0.0035 (7)	0.0096 (8)
C3	0.0137 (8)	0.0305 (10)	0.0214 (9)	−0.0026 (7)	0.0049 (7)	−0.0085 (8)
C6	0.0159 (8)	0.0218 (9)	0.0146 (8)	−0.0030 (7)	0.0046 (6)	0.0046 (7)
C24	0.0161 (9)	0.0236 (9)	0.0276 (10)	−0.0008 (7)	0.0018 (7)	−0.0055 (8)
C9	0.0249 (10)	0.0193 (9)	0.0244 (10)	−0.0022 (7)	0.0017 (8)	−0.0052 (7)
C16	0.0157 (8)	0.0215 (9)	0.0252 (9)	0.0054 (7)	0.0023 (7)	0.0003 (7)
C18	0.0133 (8)	0.0220 (9)	0.0202 (9)	0.0033 (7)	0.0033 (7)	0.0033 (7)
C13	0.0178 (8)	0.0169 (8)	0.0172 (8)	0.0019 (7)	0.0043 (7)	0.0013 (7)
C15	0.0259 (10)	0.0191 (9)	0.0220 (9)	0.0077 (7)	−0.0005 (8)	0.0040 (7)
C8	0.0218 (9)	0.0260 (10)	0.0181 (9)	−0.0006 (8)	−0.0015 (7)	−0.0027 (7)
C4	0.0111 (8)	0.0275 (9)	0.0179 (8)	0.0028 (7)	0.0028 (6)	0.0010 (7)
C21	0.0163 (9)	0.0451 (13)	0.0210 (9)	0.0092 (9)	0.0069 (7)	0.0142 (9)
C23	0.0141 (8)	0.0205 (9)	0.0188 (8)	0.0025 (7)	0.0017 (7)	0.0060 (7)
C5	0.0223 (9)	0.0200 (9)	0.0176 (8)	−0.0062 (7)	0.0027 (7)	0.0002 (7)
C20	0.0276 (10)	0.0347 (11)	0.0157 (9)	0.0120 (9)	0.0096 (8)	0.0051 (8)
O1W	0.0396 (10)	0.0257 (8)	0.0451 (10)	−0.0026 (7)	0.0035 (8)	−0.0066 (7)
O2W	0.0350 (8)	0.0221 (7)	0.0194 (7)	0.0036 (6)	0.0040 (6)	0.0037 (5)
O5W	0.0242 (7)	0.0249 (7)	0.0407 (9)	0.0018 (6)	0.0052 (7)	0.0007 (7)
O6W	0.172 (3)	0.0289 (10)	0.0341 (11)	0.0403 (14)	0.0080 (14)	−0.0004 (8)
O4W	0.0221 (7)	0.0228 (7)	0.0328 (8)	0.0012 (6)	0.0005 (6)	0.0012 (6)
O3W	0.0241 (7)	0.0281 (8)	0.0282 (8)	0.0010 (6)	0.0054 (6)	−0.0067 (6)

Geometric parameters (Å, º)

Co—N2	1.9336 (14)	N1—C17	1.351 (2)
Co—N5	1.9355 (15)	N1—C13	1.352 (2)
Co—N3	1.9420 (15)	N6—C18	1.489 (2)
Co—N4	1.9444 (15)	N3—C24	1.485 (2)
Co—N6	1.9564 (15)	N2—C19	1.348 (2)
Co—N1	1.9601 (15)	N2—C23	1.351 (2)
Cr—O1	1.9480 (13)	O9—C4	1.225 (2)
Cr—O2	1.9604 (13)	C12—C11	1.496 (2)
Cr—O3	1.9619 (13)	C1—C2	1.553 (2)
Cr—O4	1.9677 (13)	C11—C10	1.388 (3)
Cr—O6	1.9819 (12)	C14—C13	1.385 (3)
Cr—O5	1.9933 (13)	C14—C15	1.392 (3)
O3—C4	1.282 (2)	C7—C8	1.375 (3)
O11—C2	1.227 (2)	C17—C16	1.388 (3)
O6—C1	1.290 (2)	C17—C18	1.499 (3)
O12—C1	1.221 (2)	C19—C20	1.385 (3)
O2—C5	1.301 (2)	C10—C9	1.384 (3)
O4—C3	1.282 (2)	C22—C21	1.374 (3)
O1—C6	1.278 (2)	C22—C23	1.387 (3)
O5—C2	1.290 (2)	C3—C4	1.542 (3)
N4—C12	1.485 (2)	C6—C5	1.549 (3)
N5—C11	1.348 (2)	C24—C23	1.492 (3)
N5—C7	1.356 (2)	C9—C8	1.386 (3)
O10—C3	1.224 (2)	C16—C15	1.382 (3)
O7—C6	1.229 (2)	C21—C20	1.383 (3)
O8—C5	1.220 (2)
N2—Co—N5	94.62 (6)	C19—N2—C23	119.25 (16)
N2—Co—N3	84.99 (6)	C19—N2—Co	126.29 (13)
N5—Co—N3	175.19 (7)	C23—N2—Co	114.40 (12)
N2—Co—N4	89.95 (6)	N4—C12—C11	110.01 (14)
N5—Co—N4	84.46 (6)	O12—C1—O6	126.32 (16)
N3—Co—N4	90.75 (7)	O12—C1—C2	119.46 (15)
N2—Co—N6	175.84 (7)	O6—C1—C2	114.22 (14)
N5—Co—N6	88.38 (7)	N5—C11—C10	121.47 (17)
N3—Co—N6	92.27 (7)	N5—C11—C12	116.07 (15)
N4—Co—N6	93.21 (6)	C10—C11—C12	122.45 (16)
N2—Co—N1	93.42 (6)	C13—C14—C15	118.71 (18)
N5—Co—N1	95.17 (6)	N5—C7—C8	121.49 (17)
N3—Co—N1	89.64 (7)	O11—C2—O5	125.53 (16)
N4—Co—N1	176.62 (6)	O11—C2—C1	120.02 (15)
N6—Co—N1	83.42 (6)	O5—C2—C1	114.45 (15)
O1—Cr—O2	83.44 (6)	N1—C17—C16	121.44 (17)
O1—Cr—O3	91.56 (6)	N1—C17—C18	114.99 (15)
O2—Cr—O3	92.95 (5)	C16—C17—C18	123.55 (16)
O1—Cr—O4	90.05 (6)	N2—C19—C20	121.31 (19)
O2—Cr—O4	171.77 (6)	C9—C10—C11	119.14 (18)
O3—Cr—O4	82.16 (6)	C21—C22—C23	119.1 (2)
O1—Cr—O6	94.58 (5)	O10—C3—O4	124.4 (2)
O2—Cr—O6	93.82 (5)	O10—C3—C4	121.14 (18)
O3—Cr—O6	171.33 (6)	O4—C3—C4	114.43 (16)
O4—Cr—O6	91.72 (5)	O7—C6—O1	124.82 (18)
O1—Cr—O5	175.45 (5)	O7—C6—C5	120.71 (17)
O2—Cr—O5	93.42 (6)	O1—C6—C5	114.46 (15)
O3—Cr—O5	91.89 (5)	N3—C24—C23	109.49 (15)
O4—Cr—O5	93.36 (6)	C10—C9—C8	119.04 (18)
O6—Cr—O5	82.31 (5)	C15—C16—C17	119.46 (17)
C4—O3—Cr	115.40 (12)	N6—C18—C17	108.52 (15)
C1—O6—Cr	114.63 (11)	N1—C13—C14	122.09 (17)
C5—O2—Cr	113.61 (12)	C16—C15—C14	119.23 (17)
C3—O4—Cr	114.56 (12)	C7—C8—C9	119.51 (18)
C6—O1—Cr	114.22 (12)	O9—C4—O3	125.72 (19)
C2—O5—Cr	114.08 (11)	O9—C4—C3	120.89 (18)
C12—N4—Co	112.00 (11)	O3—C4—C3	113.39 (16)
C11—N5—C7	119.25 (16)	C22—C21—C20	119.44 (18)
C11—N5—Co	114.91 (12)	N2—C23—C22	121.58 (18)
C7—N5—Co	125.73 (12)	N2—C23—C24	115.68 (16)
C17—N1—C13	119.07 (15)	C22—C23—C24	122.69 (18)
C17—N1—Co	114.37 (12)	O8—C5—O2	126.54 (19)
C13—N1—Co	126.50 (12)	O8—C5—C6	119.84 (18)
C18—N6—Co	109.53 (11)	O2—C5—C6	113.61 (15)
C24—N3—Co	110.81 (11)	C21—C20—C19	119.32 (19)
O1—Cr—O3—C4	−90.54 (13)	N3—Co—N2—C23	−5.77 (13)
O2—Cr—O3—C4	−174.04 (13)	N4—Co—N2—C23	84.99 (13)
O4—Cr—O3—C4	−0.70 (12)	N6—Co—N2—C23	−54.5 (9)
O6—Cr—O3—C4	44.7 (4)	N1—Co—N2—C23	−95.10 (13)
O5—Cr—O3—C4	92.43 (13)	Co—N4—C12—C11	−15.27 (17)
O1—Cr—O6—C1	178.82 (12)	Cr—O6—C1—O12	−177.16 (15)
O2—Cr—O6—C1	−97.47 (12)	Cr—O6—C1—C2	3.25 (18)
O3—Cr—O6—C1	43.8 (4)	C7—N5—C11—C10	3.0 (3)
O4—Cr—O6—C1	88.63 (12)	Co—N5—C11—C10	−173.43 (13)
O5—Cr—O6—C1	−4.53 (12)	C7—N5—C11—C12	−178.20 (15)
O1—Cr—O2—C5	−5.18 (12)	Co—N5—C11—C12	5.32 (19)
O3—Cr—O2—C5	86.05 (13)	N4—C12—C11—N5	6.6 (2)
O4—Cr—O2—C5	32.8 (5)	N4—C12—C11—C10	−174.63 (16)
O6—Cr—O2—C5	−99.37 (12)	C11—N5—C7—C8	−2.5 (3)
O5—Cr—O2—C5	178.12 (12)	Co—N5—C7—C8	173.52 (14)
O1—Cr—O4—C3	90.58 (13)	Cr—O5—C2—O11	175.71 (15)
O2—Cr—O4—C3	52.9 (5)	Cr—O5—C2—C1	−4.70 (18)
O3—Cr—O4—C3	−0.99 (13)	O12—C1—C2—O11	1.0 (3)
O6—Cr—O4—C3	−174.83 (13)	O6—C1—C2—O11	−179.38 (16)
O5—Cr—O4—C3	−92.43 (13)	O12—C1—C2—O5	−178.61 (16)
O2—Cr—O1—C6	7.67 (12)	O6—C1—C2—O5	1.0 (2)
O3—Cr—O1—C6	−85.12 (12)	C13—N1—C17—C16	−0.6 (3)
O4—Cr—O1—C6	−167.28 (12)	Co—N1—C17—C16	−177.97 (14)
O6—Cr—O1—C6	101.00 (12)	C13—N1—C17—C18	−179.19 (16)
O5—Cr—O1—C6	54.2 (7)	Co—N1—C17—C18	3.5 (2)
O1—Cr—O5—C2	52.3 (7)	C23—N2—C19—C20	1.7 (3)
O2—Cr—O5—C2	98.50 (12)	Co—N2—C19—C20	−175.22 (14)
O3—Cr—O5—C2	−168.43 (12)	N5—C11—C10—C9	−0.9 (3)
O4—Cr—O5—C2	−86.18 (12)	C12—C11—C10—C9	−179.60 (17)
O6—Cr—O5—C2	5.10 (12)	Cr—O4—C3—O10	−177.64 (18)
N2—Co—N4—C12	109.39 (12)	Cr—O4—C3—C4	2.2 (2)
N5—Co—N4—C12	14.74 (11)	Cr—O1—C6—O7	172.68 (14)
N3—Co—N4—C12	−165.62 (12)	Cr—O1—C6—C5	−8.33 (18)
N6—Co—N4—C12	−73.31 (12)	Co—N3—C24—C23	−23.15 (19)
N1—Co—N4—C12	−69.0 (11)	C11—C10—C9—C8	−1.7 (3)
N2—Co—N5—C11	−100.94 (12)	N1—C17—C16—C15	0.6 (3)
N3—Co—N5—C11	−15.8 (8)	C18—C17—C16—C15	179.07 (18)
N4—Co—N5—C11	−11.44 (12)	Co—N6—C18—C17	32.35 (17)
N6—Co—N5—C11	81.95 (13)	N1—C17—C18—N6	−23.6 (2)
N1—Co—N5—C11	165.19 (12)	C16—C17—C18—N6	157.86 (17)
N2—Co—N5—C7	82.84 (15)	C17—N1—C13—C14	0.4 (3)
N3—Co—N5—C7	168.0 (7)	Co—N1—C13—C14	177.39 (14)
N4—Co—N5—C7	172.35 (15)	C15—C14—C13—N1	−0.2 (3)
N6—Co—N5—C7	−94.27 (15)	C17—C16—C15—C14	−0.4 (3)
N1—Co—N5—C7	−11.03 (15)	C13—C14—C15—C16	0.2 (3)
N2—Co—N1—C17	−170.13 (13)	N5—C7—C8—C9	−0.1 (3)
N5—Co—N1—C17	−75.17 (13)	C10—C9—C8—C7	2.2 (3)
N3—Co—N1—C17	104.91 (13)	Cr—O3—C4—O9	−178.01 (15)
N4—Co—N1—C17	8.3 (11)	Cr—O3—C4—C3	1.96 (19)
N6—Co—N1—C17	12.59 (13)	O10—C3—C4—O9	−3.0 (3)
N2—Co—N1—C13	12.75 (15)	O4—C3—C4—O9	177.17 (17)
N5—Co—N1—C13	107.71 (15)	O10—C3—C4—O3	177.06 (19)
N3—Co—N1—C13	−72.21 (15)	O4—C3—C4—O3	−2.8 (2)
N4—Co—N1—C13	−168.9 (10)	C23—C22—C21—C20	1.0 (3)
N6—Co—N1—C13	−164.53 (16)	C19—N2—C23—C22	−1.5 (3)
N2—Co—N6—C18	−65.9 (9)	Co—N2—C23—C22	175.77 (14)
N5—Co—N6—C18	70.27 (13)	C19—N2—C23—C24	176.11 (16)
N3—Co—N6—C18	−114.50 (13)	Co—N2—C23—C24	−6.6 (2)
N4—Co—N6—C18	154.62 (12)	C21—C22—C23—N2	0.2 (3)
N1—Co—N6—C18	−25.12 (12)	C21—C22—C23—C24	−177.27 (18)
N2—Co—N3—C24	16.43 (13)	N3—C24—C23—N2	19.6 (2)
N5—Co—N3—C24	−69.1 (8)	N3—C24—C23—C22	−162.81 (17)
N4—Co—N3—C24	−73.46 (13)	Cr—O2—C5—O8	−179.02 (17)
N6—Co—N3—C24	−166.70 (13)	Cr—O2—C5—C6	2.22 (19)
N1—Co—N3—C24	109.89 (13)	O7—C6—C5—O8	4.3 (3)
N5—Co—N2—C19	−13.53 (16)	O1—C6—C5—O8	−174.76 (18)
N3—Co—N2—C19	171.28 (16)	O7—C6—C5—O2	−176.86 (16)
N4—Co—N2—C19	−97.96 (15)	O1—C6—C5—O2	4.1 (2)
N6—Co—N2—C19	122.5 (9)	C22—C21—C20—C19	−0.8 (3)
N1—Co—N2—C19	81.94 (15)	N2—C19—C20—C21	−0.6 (3)
N5—Co—N2—C23	169.43 (12)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N4—H4A···O10^i	0.85 (3)	1.95 (3)	2.754 (2)	158 (2)
N4—H4B···O12^ii	0.89 (3)	2.21 (3)	3.021 (2)	151 (2)
N4—H4B···O11^ii	0.89 (3)	2.40 (3)	3.065 (2)	132 (2)
N6—H6B···O7^iii	0.91 (3)	2.06 (3)	2.959 (2)	172 (2)
N3—H3A···O9^i	0.89 (3)	1.98 (3)	2.831 (2)	158 (2)
N3—H3B···O4W^iv	0.88 (3)	2.07 (3)	2.872 (2)	151 (2)
O1W—H1W···O2W^v	0.95 (1)	1.95 (1)	2.899 (2)	174 (3)
N6—H6A···O3W	0.87 (3)	2.08 (3)	2.882 (2)	153 (2)
O1W—H2W···O5	0.94 (1)	2.40 (2)	3.172 (2)	140 (2)
O2W—H3W···O5	0.95 (1)	1.94 (1)	2.8751 (19)	171 (2)
O2W—H4W···O11^v	0.94 (1)	1.89 (1)	2.791 (2)	159 (2)
O5W—H9W···O4	0.95 (1)	2.08 (2)	2.957 (2)	153 (2)
O5W—H9W···O10	0.95 (1)	2.45 (1)	3.295 (3)	149 (2)
O5W—H10W···O6W	0.95 (1)	1.80 (1)	2.728 (3)	166 (2)
O6W—H11W···O1W^vi	0.95 (1)	1.83 (1)	2.777 (3)	175 (2)
O6W—H12W···O6	0.95 (1)	1.97 (1)	2.903 (2)	167 (2)
O4W—H7W···O8^vii	0.95 (1)	1.98 (1)	2.876 (2)	157 (2)
O4W—H8W···O5W	0.95 (1)	1.82 (1)	2.760 (2)	170 (2)
O3W—H5W···O4W^iv	0.94 (1)	1.92 (1)	2.834 (2)	163 (2)
O3W—H6W···O2W^i	0.94 (1)	1.96 (1)	2.859 (2)	161 (2)
C7—H7A···O12	0.95	2.44	3.211 (2)	138
C9—H9A···O3^vi	0.95	2.45	3.017 (2)	118
C10—H10A···O3^vi	0.95	2.59	3.091 (2)	113
C16—H16A···O5W^iii	0.95	2.48	3.357 (2)	153
C21—H21A···O10^ii	0.95	2.50	3.368 (3)	151
C21—H21A···O7	0.95	2.43	2.968 (2)	116

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