More examples of the 15-crown-5⋯H2O—M—OH2⋯15-crown-5 motif, M = Al3+, Cr3+ and Pd2+

Siegler, M.A.; Prewitt, J.H.; Kelley, S.P.; Parkin, S.; Selegue, J.P.; Brock, C.P.

doi:10.1107/S0108768110007202

More examples of the 15-crown-5H₂O—M—OH₂15-crown-5 motif, M = Al³⁺, Cr³⁺ and Pd²⁺

M. A. Siegler, J. H. Prewitt, S. P. Kelley, S. Parkin, J. P. Selegue and C. P. Brock

Five structures of co-crystals grown from aqueous solutions equimolar in 15-crown-5 (or 15C5) and [M(H₂O)₆](NO₃)_n, M = Al³⁺, Cr³⁺ and Pd²⁺, are reported. The hydrogen-bonding patterns in all are similar: metal complexes including the fragment trans-H₂O—M—OH₂ alternate with 15C5 molecules, to which they are hydrogen bonded, to form stacks. A literature survey shows that this hydrogen-bonding pattern is very common. In each of the two polymorphs of the compound [Al(H₂O)₆](NO₃)₃·15C5·4H₂O there are two independent cations; one forms hydrogen bonds directly to the 15C5 molecules adjacent in the stack, while the other cation is hydrogen-bonded to two water molecules that act as spacers in the stack. These stacks are then crosslinked by hydrogen bonds formed by the three nitrate counterions and the three lattice water molecules. The hydrogen-bonded stacks in [Cr(H₂O)₅(NO₃)](NO₃)₂·1.5(15C5)·H₂O are discrete rather than infinite; each unit contains two Cr³⁺ complex cations and three 15C5 molecules. These units are again crosslinked by the uncoordinated nitrate ions and a lattice water molecule. In [Pd(H₂O)₂(NO₃)₂]·15C5 the infinite stacks are electrically neutral and are not crosslinked. In [Pd(H₂O)₂(NO₃)₂]·2(15C5)·2H₂O·2HNO₃ a discrete, uncharged unit containing one Pd complex and two 15C5 molecules is `capped off' at either end by a lattice water molecule and an included nitric acid molecule. In all five structures the infinite stacks or discrete units form an array that is at least approximately hexagonal.

Keywords: co-crystals; hydrogen bonding; polymorphism.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768110007202/zb5012sup1.cif Contains datablocks 1, 2, 3, 4, 5
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50121sup2.hkl Contains datablock 1
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50122sup3.hkl Contains datablock 2
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50123sup4.hkl Contains datablock 3
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50124sup5.hkl Contains datablock 4
	Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50125sup6.hkl Contains datablock 5
	Portable Document Format (PDF) file https://doi.org/10.1107/S0108768110007202/zb5012sup7.pdf List of CSD structures, reciprocal lattice slices and details of disorder

CCDC references: 775207; 775208; 775209; 775210; 775211

Computing details top

For all structures, data collection: COLLECT (Nonius, 1998); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO-SMN (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELX97 (Sheldrick, 2008) and local procedures.

(1) top

Crystal data top

C₁₀H₂₀O₅·AlH₁₂O₆·3(NO₃)·4(H₂O)	Z = 2
M_r = 613.43	F(000) = 652
Triclinic, P1	D_x = 1.506 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.8642 (1) Å	Cell parameters from 6124 reflections
b = 11.7922 (1) Å	θ = 1.0–27.5°
c = 12.8064 (2) Å	µ = 0.18 mm⁻¹
α = 99.1087 (5)°	T = 90 K
β = 112.2703 (5)°	Block, colourless
γ = 92.3805 (5)°	0.25 × 0.15 × 0.07 mm
V = 1352.72 (3) Å³

Data collection top

Nonius KappaCCD diffractometer	6187 independent reflections
Radiation source: fine-focus sealed tube	3888 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.066
Detector resolution: 9.1 pixels mm^-1	θ_max = 27.5°, θ_min = 1.8°
ω scans at fixed χ = 55°	h = −12→12
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 1997)	k = −15→15
T_min = 0.957, T_max = 0.988	l = −16→16
33872 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.117	H atoms treated by a mixture of independent and constrained refinement
S = 0.99	w = 1/[σ²(F_o²) + (0.0583P)²] where P = (F_o² + 2F_c²)/3
6187 reflections	(Δ/σ)_max = 0.001
407 parameters	Δρ_max = 0.35 e Å⁻³
31 restraints	Δρ_min = −0.36 e Å⁻³

Special details top

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 > 2σ(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.

Water hydrogen atoms were subject to distance restraints (DFIX) applied to 1,2 and 1,3 distances thereby restraining both OH distances and HOH angles. An 'anti-bumping' restraint (negative DFIX) was used to prevent a short contact between H11A and H62B. This restraint increased the distance between these H atoms by 0.07 Å over the unrestrained distance.

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

	x	y	z	U_iso*/U_eq
O1	−0.17527 (15)	0.00050 (12)	0.66940 (11)	0.0168 (3)
O2	0.11149 (16)	0.02046 (12)	0.67384 (12)	0.0191 (3)
O3	0.24836 (16)	0.19908 (11)	0.86487 (12)	0.0182 (3)
O4	0.02771 (15)	0.34547 (12)	0.84214 (12)	0.0189 (3)
O5	−0.22521 (16)	0.19844 (12)	0.80435 (12)	0.0198 (4)
C1	−0.1352 (2)	−0.06440 (18)	0.58300 (18)	0.0192 (5)
H1A	−0.1455	−0.0198	0.5216	0.023*
H1B	−0.2006	−0.1379	0.5481	0.023*
C2	0.0215 (2)	−0.08841 (17)	0.63870 (18)	0.0195 (5)
H2A	0.0348	−0.1247	0.7061	0.023*
H2B	0.0489	−0.1415	0.5837	0.023*
C3	0.2589 (2)	0.01896 (18)	0.75369 (18)	0.0185 (5)
H3A	0.3164	−0.0234	0.7146	0.022*
H3B	0.2585	−0.0201	0.8165	0.022*
C4	0.3263 (2)	0.14204 (17)	0.80111 (18)	0.0191 (5)
H4A	0.4315	0.1442	0.8519	0.023*
H4B	0.3206	0.1821	0.7375	0.023*
C5	0.2805 (2)	0.32237 (17)	0.88772 (19)	0.0196 (5)
H5A	0.2737	0.3491	0.8166	0.024*
H5B	0.3820	0.3455	0.9461	0.024*
C6	0.1718 (2)	0.37645 (18)	0.93087 (18)	0.0194 (5)
H6A	0.1764	0.3482	1.0008	0.023*
H6B	0.1951	0.4615	0.9504	0.023*
C7	−0.0892 (2)	0.38365 (18)	0.87374 (19)	0.0196 (5)
H7A	−0.0938	0.4673	0.8736	0.024*
H7B	−0.0726	0.3704	0.9519	0.024*
C8	−0.2300 (2)	0.31642 (17)	0.78811 (19)	0.0207 (5)
H8A	−0.3154	0.3482	0.8002	0.025*
H8B	−0.2399	0.3209	0.7090	0.025*
C9	−0.3422 (2)	0.11846 (18)	0.71714 (18)	0.0206 (5)
H9A	−0.4292	0.1600	0.6842	0.025*
H9B	−0.3706	0.0579	0.7528	0.025*
C10	−0.2996 (2)	0.06232 (19)	0.62257 (18)	0.0207 (5)
H10A	−0.3834	0.0084	0.5645	0.025*
H10B	−0.2744	0.1218	0.5844	0.025*
Al1	0.0000	0.0000	1.0000	0.0139 (2)
O61	0.02191 (16)	0.12200 (12)	0.92630 (12)	0.0153 (3)
H61A	−0.0545 (19)	0.1486 (18)	0.8875 (18)	0.023*
H61B	0.088 (2)	0.1402 (18)	0.9081 (19)	0.023*
O71	−0.11305 (16)	−0.09346 (12)	0.85699 (12)	0.0169 (3)
H71A	−0.137 (2)	−0.0698 (17)	0.7953 (16)	0.025*
H71B	−0.149 (2)	−0.1648 (14)	0.8420 (18)	0.025*
O81	0.17318 (16)	−0.05180 (12)	0.99374 (13)	0.0171 (3)
H81A	0.254 (2)	−0.0111 (17)	1.0310 (18)	0.026*
H81B	0.181 (2)	−0.1191 (14)	0.9674 (19)	0.026*
Al2	0.0000	0.5000	0.5000	0.0150 (2)
O62	0.10598 (16)	0.38342 (12)	0.56327 (13)	0.0198 (4)
H62A	0.1976 (18)	0.3746 (19)	0.579 (2)	0.030*
H62B	0.068 (2)	0.3281 (16)	0.5800 (18)	0.030*
O72	−0.16957 (16)	0.43412 (13)	0.51022 (13)	0.0184 (3)
H72A	−0.231 (2)	0.3773 (16)	0.4629 (16)	0.028*
H72B	−0.208 (2)	0.4594 (18)	0.5567 (17)	0.028*
O82	−0.05372 (17)	0.40838 (13)	0.35424 (13)	0.0206 (4)
H82A	0.003 (2)	0.3645 (18)	0.339 (2)	0.031*
H82B	−0.121 (2)	0.4145 (19)	0.2924 (16)	0.031*
N1	0.4460 (2)	0.76420 (15)	0.60672 (16)	0.0206 (4)
O15	0.44398 (18)	0.70625 (14)	0.51615 (14)	0.0307 (4)
O16	0.35097 (17)	0.73630 (13)	0.64517 (13)	0.0291 (4)
O17	0.53917 (17)	0.84923 (13)	0.66013 (14)	0.0299 (4)
N2	0.2291 (2)	0.35826 (15)	1.28691 (15)	0.0185 (4)
O18	0.25512 (17)	0.31196 (12)	1.20124 (12)	0.0232 (4)
O19	0.26789 (18)	0.46327 (12)	1.32689 (13)	0.0257 (4)
O20	0.16373 (16)	0.29718 (12)	1.32940 (12)	0.0206 (4)
N3	0.2821 (2)	0.70400 (15)	0.89426 (15)	0.0192 (4)
O21	0.15789 (17)	0.73523 (13)	0.88319 (14)	0.0283 (4)
O22	0.39610 (17)	0.76826 (13)	0.95566 (13)	0.0267 (4)
O23	0.28779 (16)	0.60498 (12)	0.84212 (12)	0.0228 (4)
O11	−0.00990 (18)	0.22321 (13)	0.62993 (13)	0.0205 (4)
H11A	−0.012 (3)	0.2551 (16)	0.6923 (16)	0.031*
H11B	0.025 (3)	0.1638 (15)	0.641 (2)	0.031*
O12	0.42297 (18)	0.07725 (14)	1.11018 (14)	0.0276 (4)
H12A	0.437 (3)	0.111 (2)	1.1777 (16)	0.041*
H12B	0.464 (3)	0.1254 (19)	1.0850 (19)	0.041*
O13	0.53118 (18)	0.51297 (13)	0.80910 (15)	0.0264 (4)
H13A	0.468 (2)	0.5505 (19)	0.821 (2)	0.040*
H13B	0.590 (2)	0.5619 (18)	0.799 (2)	0.040*
O14	0.37982 (17)	0.34707 (14)	0.61563 (14)	0.0258 (4)
H14A	0.437 (3)	0.4020 (18)	0.6647 (18)	0.039*
H14B	0.416 (3)	0.335 (2)	0.5664 (18)	0.039*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O1	0.0166 (8)	0.0190 (8)	0.0137 (8)	0.0035 (6)	0.0046 (6)	0.0035 (6)
O2	0.0169 (8)	0.0167 (8)	0.0212 (8)	0.0018 (6)	0.0047 (7)	0.0036 (6)
O3	0.0202 (8)	0.0153 (8)	0.0221 (8)	0.0025 (6)	0.0125 (7)	0.0012 (6)
O4	0.0179 (8)	0.0199 (8)	0.0166 (8)	0.0019 (6)	0.0054 (7)	−0.0001 (6)
O5	0.0187 (8)	0.0139 (8)	0.0225 (8)	0.0004 (6)	0.0031 (7)	0.0042 (6)
C1	0.0236 (13)	0.0181 (11)	0.0146 (11)	−0.0026 (9)	0.0080 (10)	−0.0004 (9)
C2	0.0270 (13)	0.0134 (11)	0.0179 (11)	−0.0011 (9)	0.0100 (10)	0.0002 (9)
C3	0.0202 (12)	0.0214 (12)	0.0161 (11)	0.0073 (9)	0.0080 (10)	0.0061 (9)
C4	0.0174 (12)	0.0222 (12)	0.0179 (12)	0.0036 (9)	0.0082 (10)	0.0009 (9)
C5	0.0204 (12)	0.0164 (11)	0.0204 (12)	−0.0011 (9)	0.0069 (10)	0.0025 (9)
C6	0.0207 (12)	0.0176 (11)	0.0159 (11)	−0.0024 (9)	0.0040 (10)	0.0012 (9)
C7	0.0219 (12)	0.0149 (11)	0.0222 (12)	0.0058 (9)	0.0092 (10)	0.0019 (9)
C8	0.0209 (12)	0.0153 (11)	0.0236 (12)	0.0070 (9)	0.0044 (10)	0.0065 (9)
C9	0.0173 (12)	0.0191 (12)	0.0227 (12)	0.0001 (9)	0.0043 (10)	0.0057 (10)
C10	0.0159 (12)	0.0243 (12)	0.0188 (12)	0.0023 (9)	0.0022 (9)	0.0069 (10)
Al1	0.0156 (5)	0.0125 (5)	0.0125 (5)	0.0021 (4)	0.0047 (4)	0.0015 (4)
O61	0.0127 (8)	0.0167 (8)	0.0173 (8)	0.0030 (6)	0.0057 (7)	0.0056 (6)
O71	0.0227 (9)	0.0146 (8)	0.0115 (8)	−0.0005 (7)	0.0047 (7)	0.0026 (6)
O81	0.0171 (8)	0.0119 (8)	0.0187 (8)	0.0000 (6)	0.0048 (7)	−0.0009 (6)
Al2	0.0152 (5)	0.0140 (5)	0.0150 (5)	0.0004 (4)	0.0057 (4)	0.0015 (4)
O62	0.0167 (8)	0.0184 (8)	0.0258 (9)	0.0019 (7)	0.0093 (7)	0.0063 (7)
O72	0.0182 (9)	0.0164 (8)	0.0198 (9)	−0.0019 (6)	0.0093 (7)	−0.0026 (6)
O82	0.0189 (9)	0.0219 (9)	0.0180 (8)	0.0040 (7)	0.0057 (7)	−0.0012 (7)
N1	0.0191 (10)	0.0183 (10)	0.0226 (11)	0.0015 (8)	0.0063 (9)	0.0035 (8)
O15	0.0287 (10)	0.0374 (10)	0.0263 (9)	−0.0014 (8)	0.0159 (8)	−0.0048 (8)
O16	0.0287 (10)	0.0315 (10)	0.0289 (10)	−0.0085 (7)	0.0185 (8)	−0.0044 (7)
O17	0.0248 (9)	0.0251 (9)	0.0320 (10)	−0.0112 (7)	0.0057 (8)	0.0006 (7)
N2	0.0196 (10)	0.0182 (10)	0.0170 (10)	0.0038 (8)	0.0063 (8)	0.0034 (8)
O18	0.0318 (9)	0.0202 (8)	0.0198 (8)	−0.0003 (7)	0.0151 (7)	−0.0023 (7)
O19	0.0375 (10)	0.0117 (8)	0.0307 (9)	−0.0020 (7)	0.0194 (8)	−0.0028 (7)
O20	0.0240 (9)	0.0178 (8)	0.0243 (9)	0.0014 (7)	0.0138 (7)	0.0051 (7)
N3	0.0212 (11)	0.0179 (10)	0.0175 (10)	0.0028 (8)	0.0067 (8)	0.0023 (8)
O21	0.0175 (9)	0.0263 (9)	0.0333 (10)	0.0080 (7)	0.0057 (7)	−0.0070 (7)
O22	0.0194 (9)	0.0288 (9)	0.0230 (9)	−0.0058 (7)	0.0023 (7)	−0.0028 (7)
O23	0.0234 (9)	0.0199 (9)	0.0219 (8)	0.0060 (7)	0.0078 (7)	−0.0029 (7)
O11	0.0273 (9)	0.0177 (8)	0.0174 (8)	0.0023 (7)	0.0096 (7)	0.0034 (7)
O12	0.0247 (10)	0.0289 (10)	0.0252 (10)	−0.0058 (7)	0.0075 (8)	0.0020 (8)
O13	0.0233 (10)	0.0229 (9)	0.0372 (10)	0.0034 (7)	0.0172 (8)	0.0037 (8)
O14	0.0198 (9)	0.0337 (10)	0.0242 (10)	0.0038 (7)	0.0104 (8)	0.0015 (8)

Geometric parameters (Å, º) top

O1—C10	1.432 (2)	Al1—O71ⁱ	1.8770 (14)
O1—C1	1.433 (2)	Al1—O61	1.8883 (14)
O2—C3	1.429 (2)	Al1—O61ⁱ	1.8884 (14)
O2—C2	1.435 (2)	O61—H61A	0.836 (15)
O3—C4	1.434 (2)	O61—H61B	0.807 (15)
O3—C5	1.434 (2)	O71—H71A	0.831 (16)
O4—C7	1.427 (2)	O71—H71B	0.861 (15)
O4—C6	1.430 (2)	O81—H81A	0.841 (16)
O5—C9	1.438 (2)	O81—H81B	0.832 (15)
O5—C8	1.439 (2)	Al2—O62	1.8626 (14)
C1—C2	1.498 (3)	Al2—O62ⁱⁱ	1.8626 (14)
C1—H1A	0.9900	Al2—O82	1.8699 (14)
C1—H1B	0.9900	Al2—O82ⁱⁱ	1.8699 (14)
C2—H2A	0.9900	Al2—O72ⁱⁱ	1.8731 (14)
C2—H2B	0.9900	Al2—O72	1.8731 (14)
C3—C4	1.501 (3)	O62—H62A	0.863 (16)
C3—H3A	0.9900	O62—H62B	0.834 (14)
C3—H3B	0.9900	O72—H72A	0.863 (15)
C4—H4A	0.9900	O72—H72B	0.842 (16)
C4—H4B	0.9900	O82—H82A	0.838 (16)
C5—C6	1.503 (3)	O82—H82B	0.833 (16)
C5—H5A	0.9900	N1—O15	1.242 (2)
C5—H5B	0.9900	N1—O17	1.244 (2)
C6—H6A	0.9900	N1—O16	1.267 (2)
C6—H6B	0.9900	N2—O19	1.246 (2)
C7—C8	1.497 (3)	N2—O20	1.258 (2)
C7—H7A	0.9900	N2—O18	1.266 (2)
C7—H7B	0.9900	N3—O22	1.236 (2)
C8—H8A	0.9900	N3—O21	1.257 (2)
C8—H8B	0.9900	N3—O23	1.265 (2)
C9—C10	1.495 (3)	O11—H11A	0.836 (15)
C9—H9A	0.9900	O11—H11B	0.801 (15)
C9—H9B	0.9900	O12—H12A	0.849 (16)
C10—H10A	0.9900	O12—H12B	0.855 (16)
C10—H10B	0.9900	O13—H13A	0.824 (16)
Al1—O81ⁱ	1.8635 (15)	O13—H13B	0.855 (16)
Al1—O81	1.8635 (15)	O14—H14A	0.838 (16)
Al1—O71	1.8770 (14)	O14—H14B	0.832 (16)

C10—O1—C1	112.92 (15)	C9—C10—H10B	109.8
C3—O2—C2	114.58 (15)	H10A—C10—H10B	108.3
C4—O3—C5	112.24 (15)	O81ⁱ—Al1—O81	179.999 (1)
C7—O4—C6	114.59 (15)	O81ⁱ—Al1—O71	88.78 (6)
C9—O5—C8	114.45 (16)	O81—Al1—O71	91.22 (6)
O1—C1—C2	108.19 (16)	O81ⁱ—Al1—O71ⁱ	91.22 (6)
O1—C1—H1A	110.1	O81—Al1—O71ⁱ	88.78 (6)
C2—C1—H1A	110.1	O71—Al1—O71ⁱ	180.0
O1—C1—H1B	110.1	O81ⁱ—Al1—O61	90.23 (6)
C2—C1—H1B	110.1	O81—Al1—O61	89.77 (6)
H1A—C1—H1B	108.4	O71—Al1—O61	90.29 (6)
O2—C2—C1	107.02 (16)	O71ⁱ—Al1—O61	89.71 (6)
O2—C2—H2A	110.3	O81ⁱ—Al1—O61ⁱ	89.77 (6)
C1—C2—H2A	110.3	O81—Al1—O61ⁱ	90.23 (6)
O2—C2—H2B	110.3	O71—Al1—O61ⁱ	89.71 (6)
C1—C2—H2B	110.3	O71ⁱ—Al1—O61ⁱ	90.29 (6)
H2A—C2—H2B	108.6	O61—Al1—O61ⁱ	180.0
O2—C3—C4	107.64 (17)	Al1—O61—H61A	117.6 (15)
O2—C3—H3A	110.2	Al1—O61—H61B	129.5 (16)
C4—C3—H3A	110.2	H61A—O61—H61B	110 (2)
O2—C3—H3B	110.2	Al1—O71—H71A	123.1 (15)
C4—C3—H3B	110.2	Al1—O71—H71B	128.8 (14)
H3A—C3—H3B	108.5	H71A—O71—H71B	108.1 (19)
O3—C4—C3	109.18 (17)	Al1—O81—H81A	120.4 (15)
O3—C4—H4A	109.8	Al1—O81—H81B	124.9 (16)
C3—C4—H4A	109.8	H81A—O81—H81B	114 (2)
O3—C4—H4B	109.8	O62—Al2—O62ⁱⁱ	180.0
C3—C4—H4B	109.8	O62—Al2—O82	88.85 (7)
H4A—C4—H4B	108.3	O62ⁱⁱ—Al2—O82	91.15 (7)
O3—C5—C6	108.97 (17)	O62—Al2—O82ⁱⁱ	91.15 (7)
O3—C5—H5A	109.9	O62ⁱⁱ—Al2—O82ⁱⁱ	88.84 (7)
C6—C5—H5A	109.9	O82—Al2—O82ⁱⁱ	179.999 (1)
O3—C5—H5B	109.9	O62—Al2—O72ⁱⁱ	89.24 (7)
C6—C5—H5B	109.9	O62ⁱⁱ—Al2—O72ⁱⁱ	90.76 (7)
H5A—C5—H5B	108.3	O82—Al2—O72ⁱⁱ	90.41 (7)
O4—C6—C5	108.09 (16)	O82ⁱⁱ—Al2—O72ⁱⁱ	89.59 (7)
O4—C6—H6A	110.1	O62—Al2—O72	90.76 (7)
C5—C6—H6A	110.1	O62ⁱⁱ—Al2—O72	89.24 (7)
O4—C6—H6B	110.1	O82—Al2—O72	89.59 (7)
C5—C6—H6B	110.1	O82ⁱⁱ—Al2—O72	90.41 (7)
H6A—C6—H6B	108.4	O72ⁱⁱ—Al2—O72	180.0
O4—C7—C8	107.78 (17)	Al2—O62—H62A	128.8 (15)
O4—C7—H7A	110.2	Al2—O62—H62B	123.1 (16)
C8—C7—H7A	110.2	H62A—O62—H62B	108 (2)
O4—C7—H7B	110.2	Al2—O72—H72A	127.3 (15)
C8—C7—H7B	110.2	Al2—O72—H72B	127.0 (15)
H7A—C7—H7B	108.5	H72A—O72—H72B	105.2 (19)
O5—C8—C7	107.40 (17)	Al2—O82—H82A	121.5 (16)
O5—C8—H8A	110.2	Al2—O82—H82B	129.1 (16)
C7—C8—H8A	110.2	H82A—O82—H82B	107 (2)
O5—C8—H8B	110.2	O15—N1—O17	121.30 (19)
C7—C8—H8B	110.2	O15—N1—O16	119.29 (17)
H8A—C8—H8B	108.5	O17—N1—O16	119.41 (18)
O5—C9—C10	112.64 (17)	O19—N2—O20	121.41 (17)
O5—C9—H9A	109.1	O19—N2—O18	119.46 (17)
C10—C9—H9A	109.1	O20—N2—O18	119.13 (17)
O5—C9—H9B	109.1	O22—N3—O21	120.67 (17)
C10—C9—H9B	109.1	O22—N3—O23	120.82 (18)
H9A—C9—H9B	107.8	O21—N3—O23	118.51 (17)
O1—C10—C9	109.32 (17)	H11A—O11—H11B	106 (2)
O1—C10—H10A	109.8	H12A—O12—H12B	105 (2)
C9—C10—H10A	109.8	H13A—O13—H13B	105 (2)
O1—C10—H10B	109.8	H14A—O14—H14B	104 (2)

C10—O1—C1—C2	159.42 (16)	O3—C5—C6—O4	−62.3 (2)
C3—O2—C2—C1	164.80 (16)	C6—O4—C7—C8	−163.31 (17)
O1—C1—C2—O2	−67.1 (2)	C9—O5—C8—C7	−170.80 (17)
C2—O2—C3—C4	−167.57 (16)	O4—C7—C8—O5	68.2 (2)
C5—O3—C4—C3	−165.08 (17)	C8—O5—C9—C10	93.7 (2)
O2—C3—C4—O3	64.3 (2)	C1—O1—C10—C9	174.85 (16)
C4—O3—C5—C6	167.68 (17)	O5—C9—C10—O1	59.7 (2)
C7—O4—C6—C5	175.57 (17)

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

(2) top

Crystal data top

C₁₀H₂₀O₅·AlH₁₂O₆·3(NO₃)·4(H₂O)	F(000) = 2608
M_r = 613.43	D_x = 1.502 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 6560 reflections
a = 18.6039 (3) Å	θ = 1.0–27.5°
b = 9.3611 (1) Å	µ = 0.18 mm⁻¹
c = 31.5795 (5) Å	T = 90 K
β = 99.3468 (7)°	Block, colourless
V = 5426.65 (14) Å³	0.25 × 0.22 × 0.17 mm
Z = 8

Data collection top

Nonius KappaCCD diffractometer	6212 independent reflections
Radiation source: fine-focus sealed tube	4125 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.061
Detector resolution: 9.1 pixels mm^-1	θ_max = 27.5°, θ_min = 1.3°
ω scans at fixed χ = 55°	h = −23→24
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 1997)	k = −12→12
T_min = 0.957, T_max = 0.970	l = −40→40
40687 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.114	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.0561P)² + 1.7455P] where P = (F_o² + 2F_c²)/3
6212 reflections	(Δ/σ)_max < 0.001
440 parameters	Δρ_max = 0.79 e Å⁻³
41 restraints	Δρ_min = −0.47 e Å⁻³

Special details top

Restraints on geometry (SAME in SHELXL) were used to ensure that the minor components of disordered nitrate anions retained sensible geometry during refinement. Water hydrogen atoms were subject to distance restraints (DFIX) applied to 1,2 and 1,3 distances thereby restraining both OH distances and HOH angles.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
O1	0.16129 (7)	0.03541 (14)	0.11965 (4)	0.0216 (3)
O2	0.28192 (7)	0.21150 (14)	0.13652 (4)	0.0199 (3)
O3	0.20544 (7)	0.46676 (14)	0.12655 (4)	0.0235 (3)
O4	0.09378 (7)	0.43426 (14)	0.05462 (4)	0.0226 (3)
O5	0.07704 (7)	0.13060 (14)	0.04249 (4)	0.0212 (3)
C1	0.23193 (11)	−0.0252 (2)	0.13278 (6)	0.0225 (4)
H1A	0.2548	−0.0479	0.1074	0.027*
H1B	0.2281	−0.1144	0.1491	0.027*
C2	0.27675 (11)	0.0832 (2)	0.16048 (6)	0.0238 (5)
H2A	0.2539	0.1043	0.1860	0.029*
H2B	0.3261	0.0445	0.1705	0.029*
C3	0.30244 (11)	0.3318 (2)	0.16403 (6)	0.0224 (4)
H3A	0.3555	0.3295	0.1746	0.027*
H3B	0.2768	0.3278	0.1891	0.027*
C4	0.28273 (10)	0.4669 (2)	0.13928 (6)	0.0222 (4)
H4A	0.2981	0.5512	0.1575	0.027*
H4B	0.3073	0.4704	0.1137	0.027*
C5	0.17903 (11)	0.5826 (2)	0.09960 (7)	0.0244 (5)
H5A	0.2067	0.5901	0.0754	0.029*
H5B	0.1848	0.6731	0.1160	0.029*
C6	0.10010 (11)	0.5557 (2)	0.08295 (7)	0.0245 (5)
H6A	0.0737	0.5370	0.1072	0.029*
H6B	0.0782	0.6408	0.0673	0.029*
C7	0.02354 (11)	0.3667 (2)	0.04979 (7)	0.0238 (5)
H7A	−0.0145	0.4329	0.0357	0.029*
H7B	0.0118	0.3405	0.0783	0.029*
C8	0.02597 (11)	0.2353 (2)	0.02283 (6)	0.0224 (4)
H8A	−0.0232	0.1920	0.0173	0.027*
H8B	0.0391	0.2632	−0.0052	0.027*
C9	0.04892 (11)	0.0368 (2)	0.07202 (6)	0.0223 (4)
H9A	0.0095	−0.0237	0.0565	0.027*
H9B	0.0289	0.0931	0.0940	0.027*
C10	0.11083 (11)	−0.0544 (2)	0.09285 (6)	0.0216 (4)
H10A	0.0926	−0.1302	0.1102	0.026*
H10B	0.1350	−0.1005	0.0707	0.026*
Al1	0.0000	0.23840 (9)	0.2500	0.0198 (2)
O61	−0.00086 (8)	0.23376 (16)	0.19074 (4)	0.0249 (3)
H61A	−0.0360 (10)	0.264 (2)	0.1729 (7)	0.037*
H61B	0.0382 (10)	0.252 (2)	0.1806 (7)	0.037*
O71	0.10281 (7)	0.24265 (15)	0.25935 (5)	0.0221 (3)
H71A	0.1263 (12)	0.3149 (19)	0.2524 (7)	0.033*
H71B	0.1255 (12)	0.1683 (18)	0.2528 (7)	0.033*
O81	0.0000	0.4402 (2)	0.2500	0.0301 (5)
H81	0.0293 (12)	0.492 (2)	0.2384 (7)	0.045*
O91	0.0000	0.0388 (2)	0.2500	0.0223 (4)
H91	0.0103 (12)	−0.010 (2)	0.2283 (6)	0.034*
Al2	0.2500	0.2500	0.0000	0.01640 (19)
O62	0.21992 (7)	0.18953 (15)	0.05123 (4)	0.0198 (3)
H62A	0.2410 (11)	0.209 (2)	0.0769 (5)	0.030*
H62B	0.1753 (9)	0.167 (2)	0.0512 (6)	0.030*
O72	0.19430 (7)	0.41750 (15)	0.00134 (4)	0.0202 (3)
H72A	0.1634 (11)	0.427 (2)	0.0182 (6)	0.030*
H72B	0.1902 (12)	0.4934 (19)	−0.0144 (6)	0.030*
O82	0.33117 (7)	0.34266 (15)	0.03054 (4)	0.0196 (3)
H82A	0.3366 (12)	0.4312 (17)	0.0368 (7)	0.029*
H82B	0.3619 (11)	0.293 (2)	0.0469 (6)	0.029*
N1	0.06148 (13)	0.2906 (4)	−0.11278 (7)	0.0233 (5)	0.873 (3)
O15	0.08802 (9)	0.3463 (2)	−0.07714 (5)	0.0269 (5)	0.873 (3)
O16	0.05444 (9)	0.1565 (2)	−0.11524 (6)	0.0257 (4)	0.873 (3)
O17	0.0419 (5)	0.3686 (6)	−0.14492 (12)	0.0276 (11)	0.873 (3)
N1'	0.0744 (13)	0.3412 (19)	−0.1077 (7)	0.041 (8)*	0.127 (3)
O15'	0.1016 (7)	0.4327 (15)	−0.0812 (4)	0.029 (3)*	0.127 (3)
O16'	0.0680 (9)	0.2091 (18)	−0.1000 (5)	0.035 (4)*	0.127 (3)
O17'	0.050 (3)	0.384 (4)	−0.1456 (9)	0.040 (14)*	0.127 (3)
N2	0.15749 (9)	0.58808 (18)	0.22196 (5)	0.0230 (4)
O18	0.08912 (8)	0.60215 (16)	0.21283 (5)	0.0380 (4)
O19	0.19791 (8)	0.68393 (16)	0.21336 (5)	0.0321 (4)
O20	0.18285 (7)	0.47372 (14)	0.23965 (4)	0.0229 (3)
N3	0.16419 (10)	−0.2319 (2)	−0.02974 (7)	0.0197 (5)	0.873 (3)
O21	0.17195 (10)	−0.2256 (2)	0.00955 (5)	0.0292 (5)	0.873 (3)
O22	0.16597 (9)	−0.35206 (16)	−0.04861 (5)	0.0250 (5)	0.873 (3)
O23	0.15249 (19)	−0.1228 (3)	−0.05334 (10)	0.0254 (7)	0.873 (3)
N3'	0.1680 (8)	−0.1740 (16)	−0.0092 (5)	0.025 (4)*	0.127 (3)
O21'	0.2113 (6)	−0.1265 (12)	0.0189 (3)	0.024 (3)*	0.127 (3)
O22'	0.1386 (6)	−0.2961 (11)	−0.0089 (4)	0.027 (3)*	0.127 (3)
O23'	0.1486 (15)	−0.102 (2)	−0.0445 (6)	0.024 (6)*	0.127 (3)
O11	0.11479 (8)	0.27185 (16)	0.15730 (5)	0.0279 (4)
H11A	0.1268 (13)	0.1957 (19)	0.1464 (7)	0.042*
H11B	0.1390 (13)	0.339 (2)	0.1506 (8)	0.042*
O12	0.04285 (9)	−0.12000 (16)	0.19051 (5)	0.0295 (4)
H12A	0.0092 (12)	−0.127 (2)	0.1688 (6)	0.044*
H12B	0.0494 (13)	−0.2082 (19)	0.1958 (7)	0.044*
O13	−0.16558 (8)	0.00854 (16)	0.25708 (5)	0.0300 (4)
H13A	−0.2099 (9)	0.000 (3)	0.2546 (8)	0.045*
H13B	−0.1453 (12)	−0.048 (2)	0.2759 (7)	0.045*
O14	0.09889 (10)	0.3499 (2)	0.36557 (6)	0.0427 (4)
H14A	0.1154 (16)	0.292 (2)	0.3881 (7)	0.064*
H14B	0.0893 (16)	0.431 (2)	0.3739 (9)	0.064*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O1	0.0201 (7)	0.0192 (7)	0.0264 (7)	0.0008 (6)	0.0060 (6)	−0.0023 (6)
O2	0.0236 (8)	0.0188 (7)	0.0178 (7)	−0.0006 (6)	0.0048 (6)	0.0021 (5)
O3	0.0191 (7)	0.0201 (7)	0.0315 (8)	0.0010 (6)	0.0051 (6)	0.0054 (6)
O4	0.0188 (7)	0.0210 (7)	0.0291 (8)	−0.0014 (6)	0.0077 (6)	−0.0025 (6)
O5	0.0183 (7)	0.0201 (7)	0.0263 (7)	−0.0010 (6)	0.0068 (6)	0.0046 (6)
C1	0.0246 (11)	0.0189 (10)	0.0252 (11)	0.0042 (9)	0.0078 (9)	0.0058 (9)
C2	0.0264 (11)	0.0232 (11)	0.0225 (10)	0.0024 (9)	0.0064 (9)	0.0078 (9)
C3	0.0219 (11)	0.0267 (11)	0.0188 (10)	−0.0018 (9)	0.0037 (8)	−0.0045 (8)
C4	0.0190 (10)	0.0233 (11)	0.0252 (11)	−0.0034 (8)	0.0063 (8)	−0.0025 (9)
C5	0.0272 (12)	0.0169 (10)	0.0290 (11)	0.0019 (9)	0.0039 (9)	0.0009 (9)
C6	0.0264 (11)	0.0189 (10)	0.0292 (11)	0.0040 (9)	0.0070 (9)	−0.0019 (9)
C7	0.0164 (10)	0.0237 (11)	0.0323 (11)	0.0005 (8)	0.0065 (9)	0.0045 (9)
C8	0.0164 (10)	0.0251 (11)	0.0250 (11)	−0.0007 (8)	0.0008 (8)	0.0039 (9)
C9	0.0224 (11)	0.0210 (10)	0.0253 (10)	−0.0054 (9)	0.0096 (8)	−0.0002 (9)
C10	0.0254 (11)	0.0166 (10)	0.0248 (11)	−0.0043 (8)	0.0102 (8)	−0.0022 (8)
Al1	0.0163 (4)	0.0177 (4)	0.0275 (5)	0.000	0.0097 (3)	0.000
O61	0.0170 (8)	0.0317 (9)	0.0278 (8)	0.0028 (7)	0.0086 (6)	0.0038 (7)
O71	0.0176 (7)	0.0172 (7)	0.0337 (8)	−0.0015 (6)	0.0105 (6)	−0.0013 (6)
O81	0.0254 (12)	0.0175 (11)	0.0528 (15)	0.000	0.0224 (10)	0.000
O91	0.0224 (11)	0.0172 (11)	0.0304 (12)	0.000	0.0130 (9)	0.000
Al2	0.0145 (4)	0.0193 (4)	0.0154 (4)	0.0002 (3)	0.0025 (3)	0.0033 (3)
O62	0.0159 (7)	0.0278 (8)	0.0161 (7)	−0.0024 (6)	0.0034 (6)	0.0039 (6)
O72	0.0201 (8)	0.0210 (8)	0.0207 (7)	0.0029 (6)	0.0069 (6)	0.0051 (6)
O82	0.0181 (7)	0.0197 (7)	0.0202 (7)	0.0000 (6)	0.0003 (6)	0.0031 (6)
N1	0.0118 (12)	0.0384 (17)	0.0197 (13)	0.0015 (13)	0.0024 (8)	−0.0016 (13)
O15	0.0276 (10)	0.0322 (12)	0.0188 (9)	0.0049 (8)	−0.0025 (7)	−0.0043 (8)
O16	0.0252 (10)	0.0237 (10)	0.0273 (10)	−0.0032 (8)	0.0019 (8)	0.0042 (9)
O17	0.028 (2)	0.0295 (18)	0.0221 (17)	0.0019 (16)	−0.0044 (10)	0.0080 (9)
N2	0.0212 (9)	0.0222 (9)	0.0257 (9)	−0.0035 (8)	0.0046 (7)	−0.0011 (7)
O18	0.0159 (8)	0.0330 (9)	0.0643 (11)	−0.0008 (7)	0.0036 (7)	0.0179 (8)
O19	0.0244 (8)	0.0256 (8)	0.0471 (10)	−0.0073 (7)	0.0079 (7)	0.0067 (7)
O20	0.0206 (7)	0.0195 (7)	0.0283 (8)	−0.0009 (6)	0.0030 (6)	0.0010 (6)
N3	0.0127 (10)	0.0235 (11)	0.0227 (11)	0.0016 (8)	0.0025 (8)	0.0042 (10)
O21	0.0340 (11)	0.0377 (11)	0.0163 (9)	0.0086 (9)	0.0048 (8)	0.0011 (9)
O22	0.0331 (10)	0.0157 (9)	0.0243 (9)	0.0006 (7)	−0.0007 (7)	−0.0002 (7)
O23	0.0339 (14)	0.0185 (12)	0.0231 (12)	−0.0014 (10)	0.0021 (12)	0.0043 (12)
O11	0.0294 (9)	0.0217 (8)	0.0374 (9)	−0.0033 (7)	0.0196 (7)	−0.0052 (7)
O12	0.0338 (9)	0.0223 (8)	0.0340 (9)	0.0015 (7)	0.0102 (7)	−0.0014 (7)
O13	0.0155 (7)	0.0274 (9)	0.0464 (10)	−0.0030 (7)	0.0029 (7)	0.0061 (7)
O14	0.0384 (10)	0.0476 (11)	0.0421 (10)	−0.0083 (9)	0.0070 (8)	−0.0144 (9)

Geometric parameters (Å, º) top

O1—C1	1.430 (2)	O61—H61A	0.842 (16)
O1—C10	1.430 (2)	O61—H61B	0.856 (16)
O2—C2	1.431 (2)	O71—H71A	0.853 (16)
O2—C3	1.435 (2)	O71—H71B	0.857 (16)
O3—C5	1.416 (2)	O81—H81	0.858 (16)
O3—C4	1.429 (2)	O91—H91	0.869 (15)
O4—C7	1.437 (2)	Al2—O82	1.8680 (13)
O4—C6	1.439 (2)	Al2—O82ⁱⁱ	1.8681 (13)
O5—C8	1.434 (2)	Al2—O62	1.8828 (13)
O5—C9	1.440 (2)	Al2—O62ⁱⁱ	1.8829 (13)
C1—C2	1.501 (3)	Al2—O72	1.8837 (14)
C1—H1A	0.9900	Al2—O72ⁱⁱ	1.8837 (14)
C1—H1B	0.9900	O62—H62A	0.861 (15)
C2—H2A	0.9900	O62—H62B	0.857 (15)
C2—H2B	0.9900	O72—H72A	0.849 (15)
C3—C4	1.501 (3)	O72—H72B	0.863 (15)
C3—H3A	0.9900	O82—H82A	0.854 (15)
C3—H3B	0.9900	O82—H82B	0.844 (16)
C4—H4A	0.9900	N1—O17	1.255 (4)
C4—H4B	0.9900	N1—O16	1.263 (4)
C5—C6	1.498 (3)	N1—O15	1.266 (3)
C5—H5A	0.9900	N1'—O15'	1.245 (16)
C5—H5B	0.9900	N1'—O16'	1.270 (16)
C6—H6A	0.9900	N1'—O17'	1.274 (17)
C6—H6B	0.9900	N2—O19	1.229 (2)
C7—C8	1.501 (3)	N2—O20	1.263 (2)
C7—H7A	0.9900	N2—O18	1.265 (2)
C7—H7B	0.9900	N3—O21	1.227 (3)
C8—H8A	0.9900	N3—O23	1.262 (3)
C8—H8B	0.9900	N3—O22	1.276 (3)
C9—C10	1.497 (3)	N3'—O21'	1.184 (14)
C9—H9A	0.9900	N3'—O22'	1.267 (15)
C9—H9B	0.9900	N3'—O23'	1.302 (16)
C10—H10A	0.9900	O11—H11A	0.837 (16)
C10—H10B	0.9900	O11—H11B	0.823 (16)
Al1—O91	1.868 (2)	O12—H12A	0.852 (17)
Al1—O61	1.8695 (14)	O12—H12B	0.847 (17)
Al1—O61ⁱ	1.8695 (14)	O13—H13A	0.819 (16)
Al1—O71ⁱ	1.8877 (14)	O13—H13B	0.839 (16)
Al1—O71	1.8877 (14)	O14—H14A	0.906 (17)
Al1—O81	1.889 (2)	O14—H14B	0.830 (17)

C1—O1—C10	114.99 (14)	O91—Al1—O61ⁱ	88.67 (5)
C2—O2—C3	111.87 (14)	O61—Al1—O61ⁱ	177.34 (10)
C5—O3—C4	113.79 (15)	O91—Al1—O71ⁱ	91.21 (5)
C7—O4—C6	113.24 (14)	O61—Al1—O71ⁱ	90.01 (6)
C8—O5—C9	114.35 (15)	O61ⁱ—Al1—O71ⁱ	90.04 (6)
O1—C1—C2	107.36 (16)	O91—Al1—O71	91.21 (5)
O1—C1—H1A	110.2	O61—Al1—O71	90.04 (6)
C2—C1—H1A	110.2	O61ⁱ—Al1—O71	90.01 (6)
O1—C1—H1B	110.2	O71ⁱ—Al1—O71	177.59 (10)
C2—C1—H1B	110.2	O91—Al1—O81	180.000 (1)
H1A—C1—H1B	108.5	O61—Al1—O81	91.33 (5)
O2—C2—C1	109.76 (15)	O61ⁱ—Al1—O81	91.33 (5)
O2—C2—H2A	109.7	O71ⁱ—Al1—O81	88.79 (5)
C1—C2—H2A	109.7	O71—Al1—O81	88.79 (5)
O2—C2—H2B	109.7	Al1—O61—H61A	122.9 (16)
C1—C2—H2B	109.7	Al1—O61—H61B	119.9 (15)
H2A—C2—H2B	108.2	H61A—O61—H61B	107 (2)
O2—C3—C4	109.12 (15)	Al1—O71—H71A	121.6 (15)
O2—C3—H3A	109.9	Al1—O71—H71B	118.2 (15)
C4—C3—H3A	109.9	H71A—O71—H71B	106.8 (19)
O2—C3—H3B	109.9	Al1—O81—H81	124.7 (16)
C4—C3—H3B	109.9	Al1—O91—H91	121.4 (15)
H3A—C3—H3B	108.3	O82—Al2—O82ⁱⁱ	180.00 (6)
O3—C4—C3	107.17 (15)	O82—Al2—O62	91.39 (6)
O3—C4—H4A	110.3	O82ⁱⁱ—Al2—O62	88.62 (6)
C3—C4—H4A	110.3	O82—Al2—O62ⁱⁱ	88.62 (6)
O3—C4—H4B	110.3	O82ⁱⁱ—Al2—O62ⁱⁱ	91.38 (6)
C3—C4—H4B	110.3	O62—Al2—O62ⁱⁱ	180.0
H4A—C4—H4B	108.5	O82—Al2—O72	90.19 (6)
O3—C5—C6	107.88 (16)	O82ⁱⁱ—Al2—O72	89.81 (6)
O3—C5—H5A	110.1	O62—Al2—O72	89.40 (6)
C6—C5—H5A	110.1	O62ⁱⁱ—Al2—O72	90.60 (6)
O3—C5—H5B	110.1	O82—Al2—O72ⁱⁱ	89.81 (6)
C6—C5—H5B	110.1	O82ⁱⁱ—Al2—O72ⁱⁱ	90.19 (6)
H5A—C5—H5B	108.4	O62—Al2—O72ⁱⁱ	90.60 (6)
O4—C6—C5	109.10 (16)	O62ⁱⁱ—Al2—O72ⁱⁱ	89.40 (6)
O4—C6—H6A	109.9	O72—Al2—O72ⁱⁱ	180.0
C5—C6—H6A	109.9	Al2—O62—H62A	126.5 (14)
O4—C6—H6B	109.9	Al2—O62—H62B	119.8 (14)
C5—C6—H6B	109.9	H62A—O62—H62B	110.2 (18)
H6A—C6—H6B	108.3	Al2—O72—H72A	121.9 (15)
O4—C7—C8	108.08 (16)	Al2—O72—H72B	132.1 (14)
O4—C7—H7A	110.1	H72A—O72—H72B	105.8 (19)
C8—C7—H7A	110.1	Al2—O82—H82A	128.7 (15)
O4—C7—H7B	110.1	Al2—O82—H82B	118.1 (15)
C8—C7—H7B	110.1	H82A—O82—H82B	110.4 (19)
H7A—C7—H7B	108.4	O17—N1—O16	121.0 (3)
O5—C8—C7	113.17 (16)	O17—N1—O15	120.0 (4)
O5—C8—H8A	108.9	O16—N1—O15	119.0 (2)
C7—C8—H8A	108.9	O15'—N1'—O16'	125.6 (19)
O5—C8—H8B	108.9	O15'—N1'—O17'	117 (2)
C7—C8—H8B	108.9	O16'—N1'—O17'	117 (2)
H8A—C8—H8B	107.8	O19—N2—O20	121.24 (16)
O5—C9—C10	107.32 (16)	O19—N2—O18	120.16 (17)
O5—C9—H9A	110.3	O20—N2—O18	118.60 (16)
C10—C9—H9A	110.3	O21—N3—O23	122.6 (3)
O5—C9—H9B	110.3	O21—N3—O22	120.46 (19)
C10—C9—H9B	110.3	O23—N3—O22	116.9 (2)
H9A—C9—H9B	108.5	O21'—N3'—O22'	125.1 (15)
O1—C10—C9	107.99 (15)	O21'—N3'—O23'	120.5 (16)
O1—C10—H10A	110.1	O22'—N3'—O23'	114.4 (17)
C9—C10—H10A	110.1	H11A—O11—H11B	111 (2)
O1—C10—H10B	110.1	H12A—O12—H12B	98 (2)
C9—C10—H10B	110.1	H13A—O13—H13B	110 (2)
H10A—C10—H10B	108.4	H14A—O14—H14B	111 (2)
O91—Al1—O61	88.67 (5)

C10—O1—C1—C2	−179.84 (15)	O3—C5—C6—O4	−67.4 (2)
C3—O2—C2—C1	160.82 (16)	C6—O4—C7—C8	−175.15 (16)
O1—C1—C2—O2	−60.0 (2)	C9—O5—C8—C7	84.70 (19)
C2—O2—C3—C4	−161.00 (16)	O4—C7—C8—O5	63.2 (2)
C5—O3—C4—C3	−174.91 (15)	C8—O5—C9—C10	−174.16 (15)
O2—C3—C4—O3	61.96 (19)	C1—O1—C10—C9	−163.96 (15)
C4—O3—C5—C6	170.62 (16)	O5—C9—C10—O1	68.02 (18)
C7—O4—C6—C5	157.85 (16)

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

(3) top

Crystal data top

3(C₁₀H₂₀O₅)·1.68(CrH₈NO₈)·0.32(CrO₆)·4.32(NO₃)·2(H₂O)	F(000) = 1420
M_r = 1351.48	D_x = 1.533 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 7085 reflections
a = 18.0939 (2) Å	θ = 1.0–27.5°
b = 9.4487 (1) Å	µ = 0.49 mm⁻¹
c = 19.0682 (3) Å	T = 90 K
β = 116.0858 (6)°	Block, blue
V = 2927.90 (6) Å³	0.30 × 0.20 × 0.15 mm
Z = 2

Data collection top

Nonius KappaCCD diffractometer	6683 independent reflections
Radiation source: fine-focus sealed tube	5576 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.035
Detector resolution: 9.1 pixels mm^-1	θ_max = 27.5°, θ_min = 2.2°
ω scans at fixed χ = 55°	h = −23→23
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 1997)	k = −12→12
T_min = 0.879, T_max = 0.937	l = −24→24
49028 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.073	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.215	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.119P)² + 4.6627P] where P = (F_o² + 2F_c²)/3
6683 reflections	(Δ/σ)_max = 0.001
660 parameters	Δρ_max = 1.38 e Å⁻³
974 restraints	Δρ_min = −0.38 e Å⁻³

Special details top

Due the very extensive and complicated nature of disorder in this crystal structure, a large number (974) restraints were required during refinement. To ensure that chemically sensible geometry was retained, the SHELXL97 commands DFIX, SAME and FLAT were used, while the SIMU and DELU commands were used for displacement parameters. In addition to these restraints, some constraints (EADP) were used.

Final SHELXL97. res file follows:

TITL k08127 - P21/c CELL 0.71073 18.0939 9.4487 19.0682 90.0000 116.0858 90.0000 ZERR 2 0.0002 0.0001 0.0003 0.0000 0.0006 0.0000 L A T T 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O N Cr UNIT 60 154.93 90.63 12 4 SIZE 0.30 0.20 0.15 TEMP -183

REM Slow cooled from RT to 90 K

LIST 4 ACTA BOND $H CONF HTAB

ACTA

FMAP 2 PLAN 20 L·S. 8 OMIT -2.0000 55

REM EXTI 0.000000 tries to go negative

DFIX 0.840 0.020 O6w H6w1 O6w H6w2 O3w H3w1 O3w H3w2 O5w H5w1 O5w H5w2 DFIX 0.840 0.020 O1W H1W1 O1W H1W2 O2w H2W1 O2w H2W2 DFIX 1.328 0.030 H6w1 H6w2 H3W1 H3W2 H5W1 H5W2 H1W1 H1W2 H2W1 H2W2

REM EXYZ Cr Cr' EADP Cr Cr' SAME 0.020 Cr > O5w' SIMU 0.020 Cr > O5w' WGHT 0.119000 4.662700 FVAR 0.59937 0.84171 PART 1 CR 5 0.212210 0.041044 0.188352 21.00000 0.02279 0.02433 = 0.02809 - 0.00310 0.00881 - 0.00401 O1W 3 0.159581 0.072587 0.259068 21.00000 0.03033 0.06211 = 0.03839 - 0.00037 0.01649 - 0.00532 H1W1 2 0.113868 0.111462 0.243692 21.00000 - 1.50000 H1W2 2 0.177023 0.060675 0.306078 21.00000 - 1.50000

O2W 3 0.100955 0.027841 0.099711 21.00000 0.02848 0.04126 = 0.03193 0.00198 0.00654 - 0.00575 H2W1 2 0.064835 0.089658 0.089857 21.00000 - 1.50000 H2W2 2 0.073086 - 0.045765 0.091292 21.00000 - 1.50000 O3W 3 0.206815 0.242105 0.165248 21.00000 0.03958 0.02060 = 0.06274 - 0.00378 0.02630 - 0.00482 H3W1 2 0.178832 0.279966 0.183852 21.00000 - 1.50000 H3W2 2 0.241668 0.299044 0.166990 21.00000 - 1.50000 O4W 3 0.318861 0.054598 0.277625 21.00000 0.03176 0.05264 = 0.03141 - 0.01279 0.00759 - 0.01672 O5W 3 0.214609 - 0.161453 0.211652 21.00000 0.03582 0.02265 = 0.06936 0.00629 0.02119 - 0.00040 H5W1 2 0.181447 - 0.209639 0.219613 21.00000 - 1.50000 H5W2 2 0.239247 - 0.213113 0.194600 21.00000 - 1.50000 PART 2 CR' 5 0.197891 0.047410 0.195195 - 21.00000 0.02279 0.02433 = 0.02809 - 0.00310 0.00881 - 0.00401 O1W' 3 0.174231 - 0.065065 0.253007 - 21.00000 0.06614 O2W' 3 0.086893 0.024675 0.113067 - 21.00000 0.02891 O3W' 3 0.238044 - 0.097012 0.145035 - 21.00000 0.06820 O4W' 3 0.320862 0.093161 0.282215 - 21.00000 0.03159 O5W' 3 0.167651 0.217053 0.232805 - 21.00000 0.08724 PART 0

O6W 3 0.121979 0.687215 0.254248 11.00000 0.05239 0.03605 = 0.06612 0.00399 0.03411 0.00293 H6W1 2 0.078833 0.709867 0.258480 11.00000 - 1.50000 H6W2 2 0.109297 0.609859 0.229088 11.00000 - 1.50000 SAME 0.02 N1' > O13' SIMU 0.02 N1 > O11w PART 1 N1 4 0.315466 0.035820 0.104975 21.00000 0.03973 0.04140 = 0.03157 0.00350 0.01517 0.01254 O11 3 0.255636 - 0.021049 0.115778 21.00000 0.03617 0.04743 = 0.04026 - 0.01327 0.01616 - 0.00613 O12 3 0.343530 0.149357 0.135273 21.00000 0.05074 0.04011 = 0.04950 - 0.00263 0.02536 - 0.00381 O13 3 0.339571 - 0.028232 0.062801 21.00000 0.07547 0.06619 = 0.04411 0.00241 0.03463 0.03083 PART 2 N1' 4 0.368038 0.003603 0.063958 - 21.00000 0.05582 O11' 3 0.423678 0.003899 0.040573 - 21.00000 0.05658 O12' 3 0.381335 0.076719 0.122312 - 21.00000 0.04025 O13' 3 0.303239 - 0.054041 0.024220 - 21.00000 0.08000

O11W 3 0.241402 0.182599 0.127218 - 21.00000 0.07394 PART 0

EADP N2 N2' EADP O21 O21' FLAT 0.02 N2 > O23 FLAT 0.02 N2' > O23' SAME 0.02 N2' > O23' SIMU 0.02 N2 > O23' DELU 0.02 N2 > O23' PART 1 N2 4 0.277653 0.547232 0.178823 10.50000 0.04712 0.02895 = 0.07659 0.01187 0.04159 0.00666 O21 3 0.298854 0.445724 0.146305 10.50000 0.06610 0.02813 = 0.09592 0.02091 0.05406 0.01737 O22 3 0.317201 0.657114 0.202807 10.50000 0.05142 0.03223 = 0.10183 0.01216 0.03720 0.00032 O23 3 0.216809 0.537219 0.186902 10.50000 0.10631 0.04099 = 0.16776 - 0.00825 0.11511 - 0.00505 PART 2 N2' 4 0.268723 0.543416 0.156288 10.50000 0.04712 0.02895 = 0.07659 0.01187 0.04159 0.00666 O21' 3 0.309779 0.429851 0.162797 10.50000 0.06610 0.02813 = 0.09592 0.02091 0.05406 0.01737 O22' 3 0.297570 0.661068 0.157504 10.50000 0.07580 0.03041 = 0.14894 0.01790 0.07811 0.00300 O23' 3 0.199749 0.539423 0.147728 10.50000 0.04778 0.05778 = 0.11366 - 0.00580 0.03576 - 0.00033 PART 0 N3 4 0.028021 0.359352 0.205634 11.00000 0.08382 0.03648 = 0.07349 - 0.02172 0.05843 - 0.01806 O31 3 0.028162 0.235563 0.230704 11.00000 0.05896 0.04298 = 0.05330 - 0.00821 0.03516 - 0.01596 O32 3 - 0.029862 0.435666 0.190314 11.00000 0.10029 0.04377 = 0.10570 - 0.00593 0.07476 0.00118 O33 3 0.090160 0.399083 0.197908 11.00000 0.11369 0.03278 = 0.16372 - 0.01071 0.11268 - 0.01370 SIMU 0.020 o1a > C10b SAME 0.020 O1b > C10b SAME 0.020 O1c > C10C DELU 0.020 o1a > C10b PART 1 O1A 3 0.334824 0.000652 0.450167 10.50000 0.07199 0.07882 = 0.06519 - 0.00646 0.02241 0.00523 C1A 1 0.336264 - 0.141622 0.443804 10.50000 0.07961 0.07342 = 0.08909 0.00771 0.00769 - 0.01468 AFIX 23 H1A1 2 0.286541 - 0.173020 0.397410 10.50000 - 1.20000 H1A2 2 0.335458 - 0.186041 0.490484 10.50000 - 1.20000 AFIX 0 C2A 1 0.414019 - 0.190433 0.436081 10.50000 0.09535 0.03986 = 0.06369 0.00499 0.01649 0.01337 AFIX 23 H2A1 2 0.464213 - 0.160145 0.482331 10.50000 - 1.20000 H2A2 2 0.414714 - 0.294878 0.432284 10.50000 - 1.20000 AFIX 0 O2A 3 0.411639 - 0.130234 0.370245 10.50000 0.07090 0.07157 = 0.05889 - 0.01638 - 0.00179 0.03155 C3A 1 0.493625 - 0.127084 0.375679 10.50000 0.06637 0.12327 = 0.05878 - 0.01827 0.00381 0.04687 AFIX 23 H3A1 2 0.505304 - 0.217422 0.356208 10.50000 - 1.20000 H3A2 2 0.534239 - 0.115563 0.430899 10.50000 - 1.20000 AFIX 0 C4A 1 0.501227 - 0.003407 0.326902 10.50000 0.04809 0.14279 = 0.05957 - 0.02353 0.02229 0.01351 AFIX 23 H4A1 2 0.556009 - 0.005001 0.327061 10.50000 - 1.20000 H4A2 2 0.458700 - 0.011683 0.272209 10.50000 - 1.20000 AFIX 0 O3A 3 0.490265 0.129872 0.361353 10.50000 0.05859 0.14192 = 0.04829 0.00507 - 0.00159 - 0.03878 C5A 1 0.489374 0.240793 0.315561 10.50000 0.08569 0.12318 = 0.04891 - 0.00187 0.03259 - 0.05258 AFIX 23 H5A1 2 0.453621 0.220356 0.259844 10.50000 - 1.20000 H5A2 2 0.545572 0.262253 0.322023 10.50000 - 1.20000 AFIX 0 C6A 1 0.455971 0.360585 0.343555 10.50000 0.07315 0.08058 = 0.06056 - 0.00814 0.02808 - 0.05066 AFIX 23 H6A1 2 0.493039 0.377970 0.399313 10.50000 - 1.20000 H6A2 2 0.456031 0.446869 0.314126 10.50000 - 1.20000 AFIX 0 O4A 3 0.374800 0.337775 0.335437 10.50000 0.12581 0.05271 = 0.07580 - 0.01423 0.05023 - 0.01709 C7A 1 0.362515 0.418168 0.388506 10.50000 0.09139 0.06873 = 0.06632 - 0.02055 0.02604 - 0.02248 AFIX 23 H7A1 2 0.371851 0.519709 0.382373 10.50000 - 1.20000 H7A2 2 0.399211 0.388360 0.442538 10.50000 - 1.20000 AFIX 0 C8A 1 0.274666 0.390292 0.369220 10.50000 0.07968 0.05687 = 0.06748 - 0.02546 0.02661 - 0.01696 AFIX 23 H8A1 2 0.257985 0.457711 0.399373 10.50000 - 1.20000 H8A2 2 0.241321 0.412080 0.313219 10.50000 - 1.20000 AFIX 0 O5A 3 0.254313 0.256606 0.382751 10.50000 0.06027 0.06684 = 0.05714 - 0.01008 0.02626 0.01069 C9A 1 0.278746 0.218196 0.459457 10.50000 0.04637 0.09723 = 0.05720 - 0.02852 0.01291 0.01190 AFIX 23 H9A1 2 0.246037 0.269222 0.481575 10.50000 - 1.20000 H9A2 2 0.337685 0.240333 0.491267 10.50000 - 1.20000 AFIX 0 C10A 1 0.263992 0.058933 0.458471 10.50000 0.07590 0.11381 = 0.03560 0.00825 0.03277 0.01138 AFIX 23 H10A 2 0.263353 0.027055 0.507659 10.50000 - 1.20000 H10B 2 0.211544 0.031711 0.413879 10.50000 - 1.20000 AFIX 0 PART 2 O1B 3 0.260142 - 0.038361 0.404578 10.50000 0.06377 0.10475 = 0.03635 - 0.00799 0.01647 - 0.03584 C1B 1 0.285448 - 0.174328 0.423728 10.50000 0.09881 0.09902 = 0.04799 0.02682 - 0.01181 - 0.04115 AFIX 23 H1B1 2 0.252684 - 0.234703 0.378106 10.50000 - 1.20000 H1B2 2 0.271918 - 0.203405 0.466611 10.50000 - 1.20000 AFIX 0 C2B 1 0.373625 - 0.205530 0.448194 10.50000 0.10440 0.06348 = 0.06283 0.02533 - 0.01044 - 0.01417 AFIX 23 H2B1 2 0.408850 - 0.147239 0.493876 10.50000 - 1.20000 H2B2 2 0.385515 - 0.306721 0.462022 10.50000 - 1.20000 AFIX 0 O2B 3 0.386761 - 0.173089 0.386174 10.50000 0.09222 0.07009 = 0.06139 0.01024 - 0.02731 - 0.01471 C3B 1 0.472954 - 0.194996 0.408796 10.50000 0.08115 0.06352 = 0.07671 - 0.00835 - 0.01051 0.02832 AFIX 23 H3B1 2 0.483674 - 0.297394 0.407144 10.50000 - 1.20000 H3B2 2 0.505327 - 0.161709 0.463076 10.50000 - 1.20000 AFIX 0 C4B 1 0.500257 - 0.115775 0.354752 10.50000 0.07132 0.13794 = 0.06598 - 0.01858 0.01437 0.05205 AFIX 23 H4B1 2 0.555847 - 0.146701 0.363243 10.50000 - 1.20000 H4B2 2 0.461372 - 0.132463 0.299426 10.50000 - 1.20000 AFIX 0 O3B 3 0.500764 0.026965 0.373992 10.50000 0.04729 0.12798 = 0.03963 - 0.01641 0.01065 - 0.00698 C5B 1 0.508466 0.119591 0.319311 10.50000 0.04510 0.14627 = 0.04328 0.00214 0.01915 - 0.02674 AFIX 23 H5B1 2 0.470818 0.091040 0.265315 10.50000 - 1.20000 H5B2 2 0.565575 0.119180 0.325064 10.50000 - 1.20000 AFIX 0 C6B 1 0.485709 0.265371 0.337472 10.50000 0.08649 0.13209 = 0.05384 - 0.00725 0.02032 - 0.05164 AFIX 23 H6B1 2 0.523572 0.290331 0.392018 10.50000 - 1.20000 H6B2 2 0.493596 0.335703 0.302872 10.50000 - 1.20000 AFIX 0 O4B 3 0.406590 0.274063 0.328200 10.50000 0.09575 0.05559 = 0.07131 - 0.00122 0.00155 - 0.03996 C7B 1 0.396215 0.390225 0.368152 10.50000 0.10344 0.04228 = 0.06234 - 0.03074 0.01509 - 0.01255 AFIX 23 H7B1 2 0.386867 0.477129 0.336365 10.50000 - 1.20000 H7B2 2 0.445931 0.404096 0.418104 10.50000 - 1.20000 AFIX 0 C8B 1 0.320814 0.359378 0.383658 10.50000 0.11077 0.06409 = 0.09631 - 0.01675 0.01436 - 0.00565 AFIX 23 H8B1 2 0.312046 0.440134 0.412225 10.50000 - 1.20000 H8B2 2 0.271251 0.350218 0.333133 10.50000 - 1.20000 AFIX 0 O5B 3 0.330848 0.233656 0.427774 10.50000 0.08231 0.06695 = 0.07255 - 0.02113 0.01022 0.00571 C9B 1 0.268364 0.199684 0.446143 10.50000 0.06620 0.11285 = 0.07113 - 0.01818 0.02099 0.02358 AFIX 23 H9B1 2 0.214748 0.211513 0.399828 10.50000 - 1.20000 H9B2 2 0.269406 0.262680 0.488055 10.50000 - 1.20000 AFIX 0 C10B 1 0.279401 0.047319 0.473311 10.50000 0.05141 0.12657 = 0.03732 - 0.00910 0.01973 - 0.02521 AFIX 23 H10C 2 0.336742 0.030338 0.512622 10.50000 - 1.20000 H10D 2 0.241877 0.024429 0.496950 10.50000 - 1.20000 AFIX 0 PART 0

SIMU 0.020 O1c > C10D SAME 0.020 O1D > C10D PART -1 O1C 3 0.006423 - 0.193950 0.061672 10.25000 0.03567 C1C 1 0.024689 - 0.304435 0.022298 10.25000 0.02964 AFIX 23 H1C1 2 - 0.027018 - 0.345032 - 0.017958 10.25000 - 1.20000 H1C2 2 0.054906 - 0.380360 0.059745 10.25000 - 1.20000 AFIX 0 C2C 1 0.077001 - 0.247944 - 0.016137 10.25000 0.02929 AFIX 23 H2C1 2 0.133292 - 0.228411 0.024683 10.25000 - 1.20000 H2C2 2 0.081015 - 0.321170 - 0.051439 10.25000 - 1.20000 AFIX 0 O2C 3 0.045205 - 0.128222 - 0.057383 10.25000 0.02716 C3C 1 0.103900 - 0.057380 - 0.078250 10.25000 0.02538 AFIX 23 H3C1 2 0.106239 - 0.105662 - 0.123308 10.25000 - 1.20000 H3C2 2 0.159438 - 0.060519 - 0.033798 10.25000 - 1.20000 AFIX 0 C4C 1 0.076619 0.097130 - 0.099416 10.25000 0.02894 AFIX 23 H4C1 2 0.108715 0.141972 - 0.124151 10.25000 - 1.20000 H4C2 2 0.017576 0.100941 - 0.136702 10.25000 - 1.20000 AFIX 0 O3C 3 0.090343 0.170175 - 0.029144 10.25000 0.03301 C5C 1 0.066107 0.311572 - 0.040606 10.25000 0.03853 AFIX 23 H5C1 2 0.073380 0.349801 - 0.085512 10.25000 - 1.20000 H5C2 2 0.101364 0.367104 0.006285 10.25000 - 1.20000 AFIX 0 C6C 1 - 0.023448 0.326846 - 0.056064 10.25000 0.03771 AFIX 23 H6C1 2 - 0.040260 0.427237 - 0.067035 10.25000 - 1.20000 H6C2 2 - 0.058680 0.270353 - 0.102550 10.25000 - 1.20000 AFIX 0 O4C 3 - 0.034570 0.280799 0.008381 10.25000 0.03664 C7C 1 - 0.115455 0.274085 - 0.005333 10.25000 0.03511 AFIX 23 H7C1 2 - 0.149249 0.242793 - 0.059752 10.25000 - 1.20000 H7C2 2 - 0.134338 0.369703 0.000631 10.25000 - 1.20000 AFIX 0 C8C 1 - 0.127931 0.174866 0.049042 10.25000 0.03257 AFIX 23 H8C1 2 - 0.090487 0.201251 0.103476 10.25000 - 1.20000 H8C2 2 - 0.185148 0.183784 0.042439 10.25000 - 1.20000 AFIX 0 O5C 3 - 0.112825 0.030917 0.035788 10.25000 0.03468 C9C 1 - 0.082334 - 0.059933 0.100553 10.25000 0.02085 AFIX 23 H9C1 2 - 0.122476 - 0.067953 0.122656 10.25000 - 1.20000 H9C2 2 - 0.030132 - 0.022221 0.141494 10.25000 - 1.20000 AFIX 0 C10C 1 - 0.067821 - 0.204916 0.073371 10.25000 0.03226 AFIX 23 H10E 2 - 0.060562 - 0.277670 0.113246 10.25000 - 1.20000 H10F 2 - 0.115390 - 0.231918 0.023977 10.25000 - 1.20000 AFIX 0 PART -2 O1D 3 - 0.007141 - 0.184822 0.059085 10.25000 0.03070 C1D 1 0.003013 - 0.313413 0.026387 10.25000 0.02872 AFIX 23 H1D1 2 - 0.047966 - 0.338427 - 0.020464 10.25000 - 1.20000 H1D2 2 0.016842 - 0.391374 0.064781 10.25000 - 1.20000 AFIX 0 C2D 1 0.075042 - 0.286436 0.004214 10.25000 0.03615 AFIX 23 H2D1 2 0.124801 - 0.256079 0.050879 10.25000 - 1.20000 H2D2 2 0.088184 - 0.374508 - 0.016099 10.25000 - 1.20000 AFIX 0 O2D 3 0.051895 - 0.185101 - 0.050533 10.25000 0.03294 C3D 1 0.118021 - 0.134905 - 0.066060 10.25000 0.03402 AFIX 23 H3D1 2 0.126758 - 0.199995 - 0.102412 10.25000 - 1.20000 H3D2 2 0.169543 - 0.130209 - 0.016955 10.25000 - 1.20000 AFIX 0 C4D 1 0.095176 0.011061 - 0.102087 10.25000 0.04273 AFIX 23 H4D1 2 0.135482 0.041403 - 0.121180 10.25000 - 1.20000 H4D2 2 0.040233 0.007330 - 0.147364 10.25000 - 1.20000 AFIX 0 O3D 3 0.093965 0.110357 - 0.047505 10.25000 0.04374 C5D 1 0.049869 0.233005 - 0.083602 10.25000 0.04546 AFIX 23 H5D1 2 - 0.006481 0.207047 - 0.122073 10.25000 - 1.20000 H5D2 2 0.077308 0.281685 - 0.111737 10.25000 - 1.20000 AFIX 0 C6D 1 0.045701 0.329343 - 0.023942 10.25000 0.06214 AFIX 23 H6D1 2 0.101901 0.365103 0.008862 10.25000 - 1.20000 H6D2 2 0.011381 0.411781 - 0.051354 10.25000 - 1.20000 AFIX 0 O4D 3 0.015192 0.274346 0.024606 10.25000 0.07778 C7D 1 - 0.068620 0.289611 - 0.007027 10.25000 0.06341 AFIX 23 H7D1 2 - 0.093306 0.261101 - 0.062641 10.25000 - 1.20000 H7D2 2 - 0.082411 0.390269 - 0.004436 10.25000 - 1.20000 AFIX 0 C8D 1 - 0.104216 0.200079 0.036289 10.25000 0.04944 AFIX 23 H8D1 2 - 0.078569 0.227592 0.092068 10.25000 - 1.20000 H8D2 2 - 0.164053 0.218360 0.014915 10.25000 - 1.20000 AFIX 0 O5D 3 - 0.090980 0.052787 0.030050 10.25000 0.04738 C9D 1 - 0.096917 - 0.031278 0.086180 10.25000 0.04645 AFIX 23 H9D1 2 - 0.152823 - 0.023733 0.083140 10.25000 - 1.20000 H9D2 2 - 0.056747 0.000194 0.138723 10.25000 - 1.20000 AFIX 0 C10D 1 - 0.079493 - 0.183722 0.072784 10.25000 0.03614 AFIX 23 H10G 2 - 0.070078 - 0.241956 0.119122 10.25000 - 1.20000 H10H 2 - 0.126990 - 0.223511 0.027114 10.25000 - 1.20000 PART 0 HKLF 4

REM k08127 - P21/c REM R1 = 0.0727 for 5576 F_o > 4sig(F_o) and 0.0843 for all 6683 data REM 660 parameters refined using 974 restraints

END

WGHT 0.1161 4.8549 REM Highest difference peak 1.382, deepest hole -0.378, 1-σ level 0.084 Q1 1 0.2484 0.1273 0.3991 11.00000 0.05 1.38 Q2 1 0.3214 0.3285 0.3313 11.00000 0.05 1.07 Q3 1 0.4399 - 0.0984 0.3259 11.00000 0.05 1.03 Q4 1 0.2886 0.3214 0.4229 11.00000 0.05 0.82 Q5 1 0.2401 0.0599 0.1163 11.00000 0.05 0.74 Q6 1 0.0443 - 0.2251 0.0384 11.00000 0.05 0.70 Q7 1 0.0432 0.4604 0.1741 11.00000 0.05 0.69 Q8 1 0.2843 - 0.0519 0.0478 11.00000 0.05 0.65 Q9 1 0.3021 - 0.0635 0.4733 11.00000 0.05 0.64 Q10 1 0.3457 - 0.1002 0.4100 11.00000 0.05 0.60 Q11 1 0.4704 0.2026 0.3664 11.00000 0.05 0.58 Q12 1 0.3917 0.0011 0.0477 11.00000 0.05 0.58 Q13 1 - 0.0067 0.2938 0.2283 11.00000 0.05 0.52 Q14 1 - 0.0814 0.4474 0.1528 11.00000 0.05 0.50 Q15 1 0.3693 0.3116 0.4082 11.00000 0.05 0.47 Q16 1 0.3196 0.4557 0.2103 11.00000 0.05 0.42 Q17 1 0.5223 - 0.0405 0.3632 11.00000 0.05 0.41 Q18 1 0.4284 - 0.2430 0.3559 11.00000 0.05 0.40 Q19 1 0.3408 - 0.0197 0.3171 11.00000 0.05 0.40 Q20 1 0.4367 0.2345 0.3074 11.00000 0.05 0.34

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Cr	0.21221 (7)	0.04104 (13)	0.18835 (7)	0.0259 (2)	0.842 (3)
O1W	0.15958 (17)	0.0726 (4)	0.25907 (17)	0.0431 (7)	0.842 (3)
H1W1	0.114 (2)	0.111 (6)	0.244 (3)	0.065*	0.842 (3)
H1W2	0.177 (3)	0.061 (6)	0.3061 (13)	0.065*	0.842 (3)
O2W	0.1010 (2)	0.0278 (4)	0.0997 (2)	0.0363 (8)	0.842 (3)
H2W1	0.065 (2)	0.090 (4)	0.090 (3)	0.055*	0.842 (3)
H2W2	0.073 (3)	−0.046 (3)	0.091 (3)	0.055*	0.842 (3)
O3W	0.20681 (17)	0.2421 (3)	0.16525 (19)	0.0396 (6)	0.842 (3)
H3W1	0.179 (3)	0.280 (5)	0.184 (3)	0.059*	0.842 (3)
H3W2	0.242 (2)	0.299 (4)	0.167 (3)	0.059*	0.842 (3)
O4W	0.3189 (3)	0.0546 (6)	0.2776 (3)	0.0409 (10)	0.842 (3)
O5W	0.21461 (17)	−0.1615 (3)	0.2117 (2)	0.0433 (7)	0.842 (3)
H5W1	0.181 (3)	−0.210 (5)	0.220 (3)	0.065*	0.842 (3)
H5W2	0.239 (3)	−0.213 (5)	0.195 (3)	0.065*	0.842 (3)
Cr'	0.1979 (4)	0.0474 (8)	0.1952 (5)	0.0259 (2)	0.158 (3)
O1W'	0.1742 (13)	−0.065 (2)	0.2530 (13)	0.066 (5)*	0.158 (3)
O2W'	0.0869 (14)	0.025 (3)	0.1131 (13)	0.029 (5)*	0.158 (3)
O3W'	0.2380 (13)	−0.097 (2)	0.1450 (13)	0.068 (5)*	0.158 (3)
O4W'	0.3209 (18)	0.093 (2)	0.2822 (17)	0.032 (6)*	0.158 (3)
O5W'	0.1677 (16)	0.217 (3)	0.2328 (15)	0.087 (7)*	0.158 (3)
O6W	0.12198 (16)	0.6872 (3)	0.25425 (17)	0.0486 (6)
H6W1	0.079 (2)	0.710 (5)	0.258 (3)	0.073*
H6W2	0.109 (3)	0.610 (3)	0.229 (3)	0.073*
N1	0.3155 (2)	0.0358 (3)	0.10498 (18)	0.0378 (7)	0.842 (3)
O11	0.25564 (17)	−0.0210 (3)	0.11578 (17)	0.0415 (7)	0.842 (3)
O12	0.34353 (18)	0.1494 (3)	0.13527 (17)	0.0456 (7)	0.842 (3)
O13	0.3396 (3)	−0.0282 (5)	0.0628 (2)	0.0589 (10)	0.842 (3)
N1'	0.3680 (14)	0.004 (3)	0.0640 (15)	0.056 (7)*	0.158 (3)
O11'	0.4237 (11)	0.004 (2)	0.0406 (11)	0.057 (4)*	0.158 (3)
O12'	0.3813 (9)	0.0767 (16)	0.1223 (8)	0.040 (3)*	0.158 (3)
O13'	0.3032 (13)	−0.054 (3)	0.0242 (16)	0.080 (7)*	0.158 (3)
O11W	0.2414 (14)	0.183 (3)	0.1272 (13)	0.074 (6)*	0.158 (3)
N2	0.2777 (7)	0.5472 (13)	0.1788 (6)	0.0457 (17)	0.50
O21	0.2989 (15)	0.4457 (19)	0.1463 (13)	0.057 (3)	0.50
O22	0.3172 (5)	0.6571 (9)	0.2028 (5)	0.061 (2)	0.50
O23	0.2168 (8)	0.5372 (14)	0.1869 (8)	0.085 (4)	0.50
N2'	0.2687 (7)	0.5434 (13)	0.1563 (5)	0.0457 (17)	0.50
O21'	0.3098 (15)	0.4299 (19)	0.1628 (14)	0.057 (3)	0.50
O22'	0.2976 (6)	0.6611 (9)	0.1575 (6)	0.075 (3)	0.50
O23'	0.1997 (7)	0.5394 (16)	0.1477 (6)	0.073 (3)	0.50
N3	0.0280 (2)	0.3594 (3)	0.2056 (2)	0.0559 (9)
O31	0.02816 (16)	0.2356 (3)	0.23070 (15)	0.0479 (6)
O32	−0.0299 (2)	0.4357 (3)	0.1903 (2)	0.0725 (10)
O33	0.0902 (2)	0.3991 (3)	0.1979 (3)	0.0846 (13)
O1A	0.3348 (4)	0.0007 (8)	0.4502 (4)	0.0748 (17)	0.50
C1A	0.3363 (8)	−0.1416 (12)	0.4438 (9)	0.091 (3)	0.50
H1A1	0.2865	−0.1730	0.3974	0.110*	0.50
H1A2	0.3355	−0.1860	0.4905	0.110*	0.50
C2A	0.4140 (8)	−0.1904 (11)	0.4361 (7)	0.073 (3)	0.50
H2A1	0.4642	−0.1601	0.4823	0.088*	0.50
H2A2	0.4147	−0.2949	0.4323	0.088*	0.50
O2A	0.4116 (5)	−0.1302 (10)	0.3702 (5)	0.078 (2)	0.50
C3A	0.4936 (9)	−0.1271 (19)	0.3757 (10)	0.091 (4)	0.50
H3A1	0.5053	−0.2174	0.3562	0.110*	0.50
H3A2	0.5342	−0.1156	0.4309	0.110*	0.50
C4A	0.5012 (6)	−0.0034 (15)	0.3269 (7)	0.084 (3)	0.50
H4A1	0.5560	−0.0050	0.3271	0.101*	0.50
H4A2	0.4587	−0.0117	0.2722	0.101*	0.50
O3A	0.4903 (5)	0.1299 (12)	0.3614 (5)	0.092 (2)	0.50
C5A	0.4894 (10)	0.2408 (16)	0.3156 (8)	0.085 (3)	0.50
H5A1	0.4536	0.2204	0.2598	0.102*	0.50
H5A2	0.5456	0.2623	0.3220	0.102*	0.50
C6A	0.4560 (6)	0.3606 (12)	0.3436 (6)	0.072 (2)	0.50
H6A1	0.4930	0.3780	0.3993	0.086*	0.50
H6A2	0.4560	0.4469	0.3141	0.086*	0.50
O4A	0.3748 (6)	0.3378 (10)	0.3354 (6)	0.083 (2)	0.50
C7A	0.3625 (8)	0.4182 (14)	0.3885 (7)	0.079 (3)	0.50
H7A1	0.3719	0.5197	0.3824	0.094*	0.50
H7A2	0.3992	0.3884	0.4425	0.094*	0.50
C8A	0.2747 (7)	0.3903 (10)	0.3692 (6)	0.070 (2)	0.50
H8A1	0.2580	0.4577	0.3994	0.084*	0.50
H8A2	0.2413	0.4121	0.3132	0.084*	0.50
O5A	0.2543 (4)	0.2566 (7)	0.3828 (4)	0.0613 (14)	0.50
C9A	0.2787 (11)	0.2182 (14)	0.4595 (8)	0.071 (3)	0.50
H9A1	0.2460	0.2692	0.4816	0.085*	0.50
H9A2	0.3377	0.2403	0.4913	0.085*	0.50
C10A	0.2640 (10)	0.0589 (14)	0.4585 (9)	0.072 (3)	0.50
H10A	0.2634	0.0271	0.5077	0.087*	0.50
H10B	0.2115	0.0317	0.4139	0.087*	0.50
O1B	0.2601 (4)	−0.0384 (8)	0.4046 (3)	0.0703 (17)	0.50
C1B	0.2854 (8)	−0.1743 (12)	0.4237 (6)	0.098 (3)	0.50
H1B1	0.2527	−0.2347	0.3781	0.118*	0.50
H1B2	0.2719	−0.2034	0.4666	0.118*	0.50
C2B	0.3736 (8)	−0.2055 (15)	0.4482 (7)	0.094 (4)	0.50
H2B1	0.4089	−0.1472	0.4939	0.113*	0.50
H2B2	0.3855	−0.3067	0.4620	0.113*	0.50
O2B	0.3868 (6)	−0.1731 (11)	0.3862 (6)	0.097 (3)	0.50
C3B	0.4730 (7)	−0.1950 (12)	0.4088 (7)	0.090 (3)	0.50
H3B1	0.4837	−0.2974	0.4071	0.108*	0.50
H3B2	0.5053	−0.1617	0.4631	0.108*	0.50
C4B	0.5003 (11)	−0.1158 (18)	0.3548 (10)	0.097 (4)	0.50
H4B1	0.5558	−0.1467	0.3632	0.117*	0.50
H4B2	0.4614	−0.1325	0.2994	0.117*	0.50
O3B	0.5008 (4)	0.0270 (11)	0.3740 (4)	0.0747 (19)	0.50
C5B	0.5085 (6)	0.1196 (15)	0.3193 (6)	0.078 (3)	0.50
H5B1	0.4708	0.0910	0.2653	0.094*	0.50
H5B2	0.5656	0.1192	0.3251	0.094*	0.50
C6B	0.4857 (9)	0.2654 (18)	0.3375 (9)	0.095 (4)	0.50
H6B1	0.5236	0.2903	0.3920	0.114*	0.50
H6B2	0.4936	0.3357	0.3029	0.114*	0.50
O4B	0.4066 (6)	0.2741 (9)	0.3282 (5)	0.087 (2)	0.50
C7B	0.3962 (8)	0.3902 (11)	0.3682 (7)	0.077 (3)	0.50
H7B1	0.3869	0.4771	0.3364	0.093*	0.50
H7B2	0.4459	0.4041	0.4181	0.093*	0.50
C8B	0.3208 (10)	0.3594 (13)	0.3837 (9)	0.102 (4)	0.50
H8B1	0.3120	0.4401	0.4122	0.122*	0.50
H8B2	0.2713	0.3502	0.3331	0.122*	0.50
O5B	0.3308 (5)	0.2337 (8)	0.4278 (4)	0.083 (2)	0.50
C9B	0.2684 (13)	0.1997 (16)	0.4461 (11)	0.087 (4)	0.50
H9B1	0.2147	0.2115	0.3998	0.104*	0.50
H9B2	0.2694	0.2627	0.4881	0.104*	0.50
C10B	0.2794 (9)	0.0473 (14)	0.4733 (8)	0.072 (3)	0.50
H10C	0.3367	0.0303	0.5126	0.086*	0.50
H10D	0.2419	0.0244	0.4970	0.086*	0.50
O1C	0.0064 (8)	−0.1939 (14)	0.0617 (8)	0.036 (4)*	0.25
C1C	0.0247 (9)	−0.3044 (12)	0.0223 (8)	0.030 (3)*	0.25
H1C1	−0.0270	−0.3450	−0.0180	0.036*	0.25
H1C2	0.0549	−0.3804	0.0597	0.036*	0.25
C2C	0.0770 (8)	−0.2479 (14)	−0.0161 (8)	0.029 (2)*	0.25
H2C1	0.1333	−0.2284	0.0247	0.035*	0.25
H2C2	0.0810	−0.3212	−0.0514	0.035*	0.25
O2C	0.0452 (5)	−0.1282 (11)	−0.0574 (5)	0.0272 (17)*	0.25
C3C	0.1039 (6)	−0.0574 (13)	−0.0782 (7)	0.025 (2)*	0.25
H3C1	0.1062	−0.1057	−0.1233	0.030*	0.25
H3C2	0.1594	−0.0605	−0.0338	0.030*	0.25
C4C	0.0766 (9)	0.0971 (14)	−0.0994 (7)	0.029 (3)*	0.25
H4C1	0.1087	0.1420	−0.1242	0.035*	0.25
H4C2	0.0176	0.1009	−0.1367	0.035*	0.25
O3C	0.0903 (5)	0.1702 (10)	−0.0291 (5)	0.0330 (17)*	0.25
C5C	0.0661 (7)	0.3116 (13)	−0.0406 (8)	0.039 (3)*	0.25
H5C1	0.0734	0.3498	−0.0855	0.046*	0.25
H5C2	0.1014	0.3671	0.0063	0.046*	0.25
C6C	−0.0234 (8)	0.3268 (14)	−0.0561 (8)	0.038 (3)*	0.25
H6C1	−0.0403	0.4272	−0.0670	0.045*	0.25
H6C2	−0.0587	0.2704	−0.1026	0.045*	0.25
O4C	−0.0346 (8)	0.2808 (11)	0.0084 (6)	0.037 (2)*	0.25
C7C	−0.1155 (8)	0.2741 (13)	−0.0053 (7)	0.035 (2)*	0.25
H7C1	−0.1492	0.2428	−0.0598	0.042*	0.25
H7C2	−0.1343	0.3697	0.0006	0.042*	0.25
C8C	−0.1279 (8)	0.1749 (13)	0.0490 (8)	0.033 (3)*	0.25
H8C1	−0.0905	0.2013	0.1035	0.039*	0.25
H8C2	−0.1851	0.1838	0.0424	0.039*	0.25
O5C	−0.1128 (6)	0.0309 (9)	0.0358 (6)	0.035 (2)*	0.25
C9C	−0.0823 (9)	−0.0599 (15)	0.1006 (8)	0.021 (3)*	0.25
H9C1	−0.1225	−0.0680	0.1227	0.025*	0.25
H9C2	−0.0301	−0.0222	0.1415	0.025*	0.25
C10C	−0.0678 (12)	−0.2049 (17)	0.0734 (13)	0.032 (4)*	0.25
H10E	−0.0606	−0.2777	0.1132	0.039*	0.25
H10F	−0.1154	−0.2319	0.0240	0.039*	0.25
O1D	−0.0071 (8)	−0.1848 (13)	0.0591 (8)	0.031 (3)*	0.25
C1D	0.0030 (9)	−0.3134 (13)	0.0264 (9)	0.029 (3)*	0.25
H1D1	−0.0480	−0.3384	−0.0205	0.034*	0.25
H1D2	0.0168	−0.3914	0.0648	0.034*	0.25
C2D	0.0750 (11)	−0.286 (2)	0.0042 (13)	0.036 (4)*	0.25
H2D1	0.1248	−0.2561	0.0509	0.043*	0.25
H2D2	0.0882	−0.3745	−0.0161	0.043*	0.25
O2D	0.0519 (6)	−0.1851 (12)	−0.0505 (5)	0.0329 (19)*	0.25
C3D	0.1180 (8)	−0.1349 (17)	−0.0661 (8)	0.034 (3)*	0.25
H3D1	0.1268	−0.2000	−0.1024	0.041*	0.25
H3D2	0.1695	−0.1302	−0.0170	0.041*	0.25
C4D	0.0952 (11)	0.0111 (16)	−0.1021 (10)	0.043 (4)*	0.25
H4D1	0.1355	0.0414	−0.1212	0.051*	0.25
H4D2	0.0402	0.0073	−0.1474	0.051*	0.25
O3D	0.0940 (6)	0.1104 (12)	−0.0475 (6)	0.044 (2)*	0.25
C5D	0.0499 (11)	0.2330 (16)	−0.0836 (9)	0.045 (4)*	0.25
H5D1	−0.0065	0.2070	−0.1221	0.055*	0.25
H5D2	0.0773	0.2817	−0.1117	0.055*	0.25
C6D	0.0457 (12)	0.3293 (18)	−0.0239 (10)	0.062 (4)*	0.25
H6D1	0.1019	0.3651	0.0089	0.075*	0.25
H6D2	0.0114	0.4118	−0.0514	0.075*	0.25
O4D	0.0152 (10)	0.2743 (16)	0.0246 (8)	0.078 (4)*	0.25
C7D	−0.0686 (13)	0.290 (3)	−0.007 (2)	0.063 (7)*	0.25
H7D1	−0.0933	0.2611	−0.0626	0.076*	0.25
H7D2	−0.0824	0.3903	−0.0044	0.076*	0.25
C8D	−0.1042 (11)	0.2001 (14)	0.0363 (10)	0.049 (3)*	0.25
H8D1	−0.0786	0.2276	0.0921	0.059*	0.25
H8D2	−0.1641	0.2184	0.0149	0.059*	0.25
O5D	−0.0910 (8)	0.0528 (11)	0.0301 (7)	0.047 (3)*	0.25
C9D	−0.0969 (14)	−0.0313 (18)	0.0862 (12)	0.046 (5)*	0.25
H9D1	−0.1528	−0.0237	0.0831	0.056*	0.25
H9D2	−0.0567	0.0002	0.1387	0.056*	0.25
C10D	−0.0795 (10)	−0.1837 (16)	0.0728 (13)	0.036 (4)*	0.25
H10G	−0.0701	−0.2420	0.1191	0.043*	0.25
H10H	−0.1270	−0.2235	0.0271	0.043*	0.25

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr	0.0228 (5)	0.0243 (3)	0.0281 (4)	−0.0040 (3)	0.0088 (3)	−0.0031 (2)
O1W	0.0303 (13)	0.0621 (19)	0.0384 (14)	−0.0053 (12)	0.0165 (11)	−0.0004 (13)
O2W	0.0285 (17)	0.0413 (18)	0.0319 (17)	−0.0057 (12)	0.0065 (15)	0.0020 (13)
O3W	0.0396 (14)	0.0206 (12)	0.0627 (18)	−0.0048 (10)	0.0263 (13)	−0.0038 (11)
O4W	0.0318 (16)	0.053 (3)	0.0314 (17)	−0.0167 (19)	0.0076 (11)	−0.0128 (19)
O5W	0.0358 (14)	0.0226 (12)	0.0694 (19)	−0.0004 (10)	0.0212 (13)	0.0063 (12)
Cr'	0.0228 (5)	0.0243 (3)	0.0281 (4)	−0.0040 (3)	0.0088 (3)	−0.0031 (2)
O6W	0.0524 (15)	0.0360 (13)	0.0661 (17)	0.0029 (11)	0.0341 (13)	0.0040 (11)
N1	0.0397 (17)	0.0414 (18)	0.0316 (15)	0.0125 (13)	0.0152 (13)	0.0035 (13)
O11	0.0362 (14)	0.0474 (16)	0.0403 (15)	−0.0061 (12)	0.0162 (12)	−0.0133 (12)
O12	0.0507 (17)	0.0401 (15)	0.0495 (16)	−0.0038 (13)	0.0254 (14)	−0.0026 (13)
O13	0.075 (3)	0.066 (3)	0.044 (2)	0.031 (2)	0.035 (2)	0.0024 (18)
N2	0.047 (3)	0.0290 (15)	0.077 (5)	0.0067 (15)	0.042 (3)	0.012 (3)
O21	0.066 (5)	0.028 (3)	0.096 (8)	0.017 (2)	0.054 (6)	0.021 (4)
O22	0.051 (4)	0.032 (3)	0.102 (6)	0.000 (2)	0.037 (5)	0.012 (4)
O23	0.106 (9)	0.041 (4)	0.168 (11)	−0.005 (5)	0.115 (9)	−0.008 (7)
N2'	0.047 (3)	0.0290 (15)	0.077 (5)	0.0067 (15)	0.042 (3)	0.012 (3)
O21'	0.066 (5)	0.028 (3)	0.096 (8)	0.017 (2)	0.054 (6)	0.021 (4)
O22'	0.076 (6)	0.030 (3)	0.149 (8)	0.003 (3)	0.078 (7)	0.018 (5)
O23'	0.048 (4)	0.058 (5)	0.114 (8)	0.000 (3)	0.036 (5)	−0.006 (6)
N3	0.084 (2)	0.0365 (16)	0.073 (2)	−0.0181 (16)	0.058 (2)	−0.0217 (15)
O31	0.0590 (15)	0.0430 (13)	0.0533 (14)	−0.0160 (11)	0.0352 (13)	−0.0082 (11)
O32	0.100 (3)	0.0438 (16)	0.106 (3)	0.0012 (16)	0.075 (2)	−0.0059 (16)
O33	0.114 (3)	0.0328 (14)	0.164 (4)	−0.0137 (16)	0.113 (3)	−0.0107 (18)
O1A	0.072 (4)	0.079 (4)	0.065 (4)	0.005 (3)	0.022 (3)	−0.006 (3)
C1A	0.080 (6)	0.073 (6)	0.089 (6)	−0.015 (5)	0.008 (5)	0.008 (6)
C2A	0.095 (7)	0.040 (4)	0.064 (5)	0.013 (5)	0.016 (5)	0.005 (4)
O2A	0.071 (5)	0.072 (5)	0.059 (4)	0.032 (4)	−0.002 (3)	−0.016 (4)
C3A	0.066 (6)	0.123 (7)	0.059 (7)	0.047 (6)	0.004 (5)	−0.018 (6)
C4A	0.048 (4)	0.143 (7)	0.060 (5)	0.014 (6)	0.022 (4)	−0.024 (6)
O3A	0.059 (4)	0.142 (6)	0.048 (4)	−0.039 (5)	−0.002 (3)	0.005 (5)
C5A	0.086 (6)	0.123 (7)	0.049 (6)	−0.053 (6)	0.033 (5)	−0.002 (6)
C6A	0.073 (5)	0.081 (5)	0.061 (4)	−0.051 (4)	0.028 (4)	−0.008 (4)
O4A	0.126 (6)	0.053 (5)	0.076 (5)	−0.017 (4)	0.050 (4)	−0.014 (4)
C7A	0.091 (7)	0.069 (6)	0.066 (6)	−0.022 (5)	0.026 (5)	−0.021 (5)
C8A	0.080 (6)	0.057 (5)	0.067 (5)	−0.017 (5)	0.027 (5)	−0.025 (4)
O5A	0.060 (3)	0.067 (3)	0.057 (3)	0.011 (3)	0.026 (3)	−0.010 (3)
C9A	0.046 (5)	0.097 (6)	0.057 (5)	0.012 (5)	0.013 (4)	−0.029 (5)
C10A	0.076 (7)	0.114 (6)	0.036 (5)	0.011 (5)	0.033 (5)	0.008 (5)
O1B	0.064 (3)	0.105 (5)	0.036 (3)	−0.036 (3)	0.016 (3)	−0.008 (3)
C1B	0.099 (7)	0.099 (7)	0.048 (5)	−0.041 (6)	−0.012 (5)	0.027 (5)
C2B	0.104 (8)	0.063 (6)	0.063 (5)	−0.014 (6)	−0.010 (6)	0.025 (5)
O2B	0.092 (6)	0.070 (5)	0.061 (5)	−0.015 (4)	−0.027 (4)	0.010 (4)
C3B	0.081 (6)	0.064 (5)	0.077 (6)	0.028 (5)	−0.011 (5)	−0.008 (5)
C4B	0.071 (6)	0.138 (8)	0.066 (8)	0.052 (6)	0.014 (5)	−0.019 (6)
O3B	0.047 (3)	0.128 (6)	0.040 (3)	−0.007 (4)	0.011 (3)	−0.016 (4)
C5B	0.045 (4)	0.146 (7)	0.043 (4)	−0.027 (5)	0.019 (3)	0.002 (6)
C6B	0.086 (6)	0.132 (7)	0.054 (7)	−0.052 (6)	0.020 (5)	−0.007 (7)
O4B	0.096 (5)	0.056 (4)	0.071 (4)	−0.040 (4)	0.002 (4)	−0.001 (4)
C7B	0.103 (7)	0.042 (5)	0.062 (5)	−0.013 (5)	0.015 (5)	−0.031 (4)
C8B	0.111 (7)	0.064 (6)	0.096 (6)	−0.006 (6)	0.014 (6)	−0.017 (5)
O5B	0.082 (4)	0.067 (4)	0.073 (4)	0.006 (3)	0.010 (3)	−0.021 (3)
C9B	0.066 (7)	0.113 (7)	0.071 (7)	0.024 (6)	0.021 (6)	−0.018 (6)
C10B	0.051 (5)	0.127 (7)	0.037 (6)	−0.025 (5)	0.020 (4)	−0.009 (5)

Geometric parameters (Å, º) top

Cr—O4W	1.936 (5)	C5B—C6B	1.521 (17)
Cr—O3W	1.943 (3)	C5B—H5B1	0.9900
Cr—O11	1.958 (3)	C5B—H5B2	0.9900
Cr—O5W	1.960 (3)	C6B—O4B	1.366 (15)
Cr—O2W	1.983 (4)	C6B—H6B1	0.9900
Cr—O1W	1.986 (3)	C6B—H6B2	0.9900
O1W—H1W1	0.832 (19)	O4B—C7B	1.395 (12)
O1W—H1W2	0.817 (19)	C7B—C8B	1.545 (16)
O2W—H2W1	0.834 (19)	C7B—H7B1	0.9900
O2W—H2W2	0.832 (19)	C7B—H7B2	0.9900
O3W—H3W1	0.817 (19)	C8B—O5B	1.420 (12)
O3W—H3W2	0.818 (19)	C8B—H8B1	0.9900
O5W—H5W1	0.819 (19)	C8B—H8B2	0.9900
O5W—H5W2	0.819 (19)	O5B—C9B	1.361 (15)
Cr'—O1W'	1.72 (2)	C9B—C10B	1.513 (14)
Cr'—O5W'	1.93 (3)	C9B—H9B1	0.9900
Cr'—O2W'	1.94 (2)	C9B—H9B2	0.9900
Cr'—O3W'	1.98 (2)	C10B—H10C	0.9900
Cr'—O4W'	2.16 (3)	C10B—H10D	0.9900
Cr'—O11W	2.20 (2)	O1C—C1C	1.407 (12)
O2W'—H2W1	0.76 (4)	O1C—C10C	1.459 (14)
O2W'—H2W2	0.77 (4)	C1C—C2C	1.526 (16)
O6W—H6W1	0.847 (19)	C1C—H1C1	0.9900
O6W—H6W2	0.849 (19)	C1C—H1C2	0.9900
N1—O12	1.218 (4)	C2C—O2C	1.353 (14)
N1—O13	1.230 (4)	C2C—H2C1	0.9900
N1—O11	1.304 (4)	C2C—H2C2	0.9900
N1'—O13'	1.210 (18)	O2C—C3C	1.451 (11)
N1'—O12'	1.240 (17)	C3C—C4C	1.537 (16)
N1'—O11'	1.268 (17)	C3C—H3C1	0.9900
N2—O23	1.181 (10)	C3C—H3C2	0.9900
N2—O22	1.229 (10)	C4C—O3C	1.429 (14)
N2—O21	1.289 (11)	C4C—H4C1	0.9900
N2'—O23'	1.186 (10)	C4C—H4C2	0.9900
N2'—O22'	1.224 (10)	O3C—C5C	1.393 (13)
N2'—O21'	1.280 (11)	C5C—C6C	1.521 (15)
N3—O32	1.197 (5)	C5C—H5C1	0.9900
N3—O33	1.254 (4)	C5C—H5C2	0.9900
N3—O31	1.263 (4)	C6C—O4C	1.399 (13)
O1A—C1A	1.351 (12)	C6C—H6C1	0.9900
O1A—C10A	1.466 (13)	C6C—H6C2	0.9900
C1A—C2A	1.548 (15)	O4C—C7C	1.370 (13)
C1A—H1A1	0.9900	C7C—C8C	1.487 (15)
C1A—H1A2	0.9900	C7C—H7C1	0.9900
C2A—O2A	1.362 (13)	C7C—H7C2	0.9900
C2A—H2A1	0.9900	C8C—O5C	1.432 (12)
C2A—H2A2	0.9900	C8C—H8C1	0.9900
O2A—C3A	1.441 (15)	C8C—H8C2	0.9900
C3A—C4A	1.537 (18)	O5C—C9C	1.403 (14)
C3A—H3A1	0.9900	C9C—C10C	1.528 (15)
C3A—H3A2	0.9900	C9C—H9C1	0.9900
C4A—O3A	1.474 (14)	C9C—H9C2	0.9900
C4A—H4A1	0.9900	C10C—H10E	0.9900
C4A—H4A2	0.9900	C10C—H10F	0.9900
O3A—C5A	1.360 (14)	O1D—C1D	1.414 (12)
C5A—C6A	1.488 (16)	O1D—C10D	1.443 (13)
C5A—H5A1	0.9900	C1D—C2D	1.558 (17)
C5A—H5A2	0.9900	C1D—H1D1	0.9900
C6A—O4A	1.424 (12)	C1D—H1D2	0.9900
C6A—H6A1	0.9900	C2D—O2D	1.341 (16)
C6A—H6A2	0.9900	C2D—H2D1	0.9900
O4A—C7A	1.359 (12)	C2D—H2D2	0.9900
C7A—C8A	1.489 (14)	O2D—C3D	1.434 (12)
C7A—H7A1	0.9900	C3D—C4D	1.515 (17)
C7A—H7A2	0.9900	C3D—H3D1	0.9900
C8A—O5A	1.372 (10)	C3D—H3D2	0.9900
C8A—H8A1	0.9900	C4D—O3D	1.409 (15)
C8A—H8A2	0.9900	C4D—H4D1	0.9900
O5A—C9A	1.378 (13)	C4D—H4D2	0.9900
C9A—C10A	1.527 (13)	O3D—C5D	1.404 (15)
C9A—H9A1	0.9900	C5D—C6D	1.485 (16)
C9A—H9A2	0.9900	C5D—H5D1	0.9900
C10A—H10A	0.9900	C5D—H5D2	0.9900
C10A—H10B	0.9900	C6D—O4D	1.372 (15)
O1B—C1B	1.359 (11)	C6D—H6D1	0.9900
O1B—C10B	1.447 (13)	C6D—H6D2	0.9900
C1B—C2B	1.482 (15)	O4D—C7D	1.371 (17)
C1B—H1B1	0.9900	C7D—C8D	1.510 (18)
C1B—H1B2	0.9900	C7D—H7D1	0.9900
C2B—O2B	1.340 (14)	C7D—H7D2	0.9900
C2B—H2B1	0.9900	C8D—O5D	1.426 (13)
C2B—H2B2	0.9900	C8D—H8D1	0.9900
O2B—C3B	1.439 (13)	C8D—H8D2	0.9900
C3B—C4B	1.521 (18)	O5D—C9D	1.374 (15)
C3B—H3B1	0.9900	C9D—C10D	1.520 (15)
C3B—H3B2	0.9900	C9D—H9D1	0.9900
C4B—O3B	1.397 (16)	C9D—H9D2	0.9900
C4B—H4B1	0.9900	C10D—H10G	0.9900
C4B—H4B2	0.9900	C10D—H10H	0.9900
O3B—C5B	1.414 (12)

O4W—Cr—O3W	93.78 (19)	H5B1—C5B—H5B2	108.8
O4W—Cr—O11	94.97 (17)	O4B—C6B—C5B	113.5 (12)
O3W—Cr—O11	97.38 (13)	O4B—C6B—H6B1	108.9
O4W—Cr—O5W	87.20 (19)	C5B—C6B—H6B1	108.9
O3W—Cr—O5W	178.39 (13)	O4B—C6B—H6B2	108.9
O11—Cr—O5W	83.80 (14)	C5B—C6B—H6B2	108.9
O4W—Cr—O2W	177.8 (2)	H6B1—C6B—H6B2	107.7
O3W—Cr—O2W	86.40 (15)	C6B—O4B—C7B	111.2 (9)
O11—Cr—O2W	87.20 (17)	O4B—C7B—C8B	107.3 (9)
O5W—Cr—O2W	92.57 (15)	O4B—C7B—H7B1	110.2
O4W—Cr—O1W	89.04 (17)	C8B—C7B—H7B1	110.2
O3W—Cr—O1W	90.91 (14)	O4B—C7B—H7B2	110.2
O11—Cr—O1W	170.51 (14)	C8B—C7B—H7B2	110.2
O5W—Cr—O1W	87.82 (14)	H7B1—C7B—H7B2	108.5
O2W—Cr—O1W	88.74 (16)	O5B—C8B—C7B	112.2 (11)
Cr—O1W—H1W1	122 (3)	O5B—C8B—H8B1	109.2
Cr—O1W—H1W2	131 (4)	C7B—C8B—H8B1	109.2
H1W1—O1W—H1W2	107 (4)	O5B—C8B—H8B2	109.2
Cr—O2W—H2W1	123 (3)	C7B—C8B—H8B2	109.2
Cr—O2W—H2W2	121 (3)	H8B1—C8B—H8B2	107.9
H2W1—O2W—H2W2	101 (3)	C9B—O5B—C8B	116.4 (10)
Cr—O3W—H3W1	108 (4)	O5B—C9B—C10B	108.2 (14)
Cr—O3W—H3W2	132 (4)	O5B—C9B—H9B1	110.1
H3W1—O3W—H3W2	108 (4)	C10B—C9B—H9B1	110.1
Cr—O5W—H5W1	130 (4)	O5B—C9B—H9B2	110.1
Cr—O5W—H5W2	117 (4)	C10B—C9B—H9B2	110.1
H5W1—O5W—H5W2	108 (4)	H9B1—C9B—H9B2	108.4
O1W'—Cr'—O5W'	94.8 (11)	O1B—C10B—C9B	106.2 (12)
O1W'—Cr'—O2W'	89.3 (10)	O1B—C10B—H10C	110.5
O5W'—Cr'—O2W'	91.7 (11)	C9B—C10B—H10C	110.5
O1W'—Cr'—O3W'	97.6 (11)	O1B—C10B—H10D	110.5
O5W'—Cr'—O3W'	167.5 (11)	C9B—C10B—H10D	110.5
O2W'—Cr'—O3W'	90.2 (9)	H10C—C10B—H10D	108.7
O1W'—Cr'—O4W'	95.4 (11)	C1C—O1C—C10C	118.5 (12)
O5W'—Cr'—O4W'	85.0 (11)	O1C—C1C—C2C	109.7 (10)
O2W'—Cr'—O4W'	174.4 (11)	O1C—C1C—H1C1	109.7
O3W'—Cr'—O4W'	92.1 (10)	C2C—C1C—H1C1	109.7
O1W'—Cr'—O11W	174.0 (10)	O1C—C1C—H1C2	109.7
O5W'—Cr'—O11W	88.3 (11)	C2C—C1C—H1C2	109.7
O2W'—Cr'—O11W	95.8 (9)	H1C1—C1C—H1C2	108.2
O3W'—Cr'—O11W	79.2 (10)	O2C—C2C—C1C	112.1 (10)
O4W'—Cr'—O11W	79.7 (10)	O2C—C2C—H2C1	109.2
Cr'—O2W'—H2W1	118 (4)	C1C—C2C—H2C1	109.2
Cr'—O2W'—H2W2	121 (4)	O2C—C2C—H2C2	109.2
H2W1—O2W'—H2W2	115 (5)	C1C—C2C—H2C2	109.2
Cr'—O3W'—H5W2	96.4 (15)	H2C1—C2C—H2C2	107.9
Cr'—O5W'—H1W1	79 (2)	C2C—O2C—C3C	111.7 (9)
Cr'—O5W'—H3W1	87 (2)	O2C—C3C—C4C	108.7 (9)
H1W1—O5W'—H3W1	143 (4)	O2C—C3C—H3C1	109.9
H6W1—O6W—H6W2	104 (3)	C4C—C3C—H3C1	109.9
O12—N1—O13	123.4 (4)	O2C—C3C—H3C2	109.9
O12—N1—O11	119.3 (3)	C4C—C3C—H3C2	109.9
O13—N1—O11	117.3 (4)	H3C1—C3C—H3C2	108.3
N1—O11—Cr	127.4 (2)	O3C—C4C—C3C	108.0 (10)
O13'—N1'—O12'	124 (2)	O3C—C4C—H4C1	110.1
O13'—N1'—O11'	119 (2)	C3C—C4C—H4C1	110.1
O12'—N1'—O11'	116.3 (18)	O3C—C4C—H4C2	110.1
Cr'—O11W—H3W2	93.3 (19)	C3C—C4C—H4C2	110.1
O23—N2—O22	116.3 (12)	H4C1—C4C—H4C2	108.4
O23—N2—O21	119.7 (15)	C5C—O3C—C4C	113.8 (10)
O22—N2—O21	124.0 (15)	O3C—C5C—C6C	110.9 (10)
O23'—N2'—O22'	116.5 (12)	O3C—C5C—H5C1	109.5
O23'—N2'—O21'	121.2 (15)	C6C—C5C—H5C1	109.5
O22'—N2'—O21'	122.4 (15)	O3C—C5C—H5C2	109.5
O32—N3—O33	121.6 (4)	C6C—C5C—H5C2	109.5
O32—N3—O31	120.4 (3)	H5C1—C5C—H5C2	108.1
O33—N3—O31	118.0 (4)	O4C—C6C—C5C	110.7 (12)
C1A—O1A—C10A	115.8 (9)	O4C—C6C—H6C1	109.5
O1A—C1A—C2A	111.1 (9)	C5C—C6C—H6C1	109.5
O1A—C1A—H1A1	109.4	O4C—C6C—H6C2	109.5
C2A—C1A—H1A1	109.4	C5C—C6C—H6C2	109.5
O1A—C1A—H1A2	109.4	H6C1—C6C—H6C2	108.1
C2A—C1A—H1A2	109.4	C7C—O4C—C6C	113.6 (11)
H1A1—C1A—H1A2	108.0	O4C—C7C—C8C	111.9 (11)
O2A—C2A—C1A	107.6 (9)	O4C—C7C—H7C1	109.2
O2A—C2A—H2A1	110.2	C8C—C7C—H7C1	109.2
C1A—C2A—H2A1	110.2	O4C—C7C—H7C2	109.2
O2A—C2A—H2A2	110.2	C8C—C7C—H7C2	109.2
C1A—C2A—H2A2	110.2	H7C1—C7C—H7C2	107.9
H2A1—C2A—H2A2	108.5	O5C—C8C—C7C	112.1 (11)
C2A—O2A—C3A	109.2 (9)	O5C—C8C—H8C1	109.2
O2A—C3A—C4A	109.6 (11)	C7C—C8C—H8C1	109.2
O2A—C3A—H3A1	109.8	O5C—C8C—H8C2	109.2
C4A—C3A—H3A1	109.8	C7C—C8C—H8C2	109.2
O2A—C3A—H3A2	109.8	H8C1—C8C—H8C2	107.9
C4A—C3A—H3A2	109.8	C9C—O5C—C8C	117.2 (11)
H3A1—C3A—H3A2	108.2	O5C—C9C—C10C	108.0 (12)
O3A—C4A—C3A	108.3 (10)	O5C—C9C—H9C1	110.1
O3A—C4A—H4A1	110.0	C10C—C9C—H9C1	110.1
C3A—C4A—H4A1	110.0	O5C—C9C—H9C2	110.1
O3A—C4A—H4A2	110.0	C10C—C9C—H9C2	110.1
C3A—C4A—H4A2	110.0	H9C1—C9C—H9C2	108.4
H4A1—C4A—H4A2	108.4	O1C—C10C—C9C	107.2 (11)
C5A—O3A—C4A	109.8 (10)	O1C—C10C—H10E	110.3
O3A—C5A—C6A	104.4 (10)	C9C—C10C—H10E	110.3
O3A—C5A—H5A1	110.9	O1C—C10C—H10F	110.3
C6A—C5A—H5A1	110.9	C9C—C10C—H10F	110.3
O3A—C5A—H5A2	110.9	H10E—C10C—H10F	108.5
C6A—C5A—H5A2	110.9	C1D—O1D—C10D	113.0 (11)
H5A1—C5A—H5A2	108.9	O1D—C1D—C2D	105.4 (12)
O4A—C6A—C5A	114.1 (9)	O1D—C1D—H1D1	110.7
O4A—C6A—H6A1	108.7	C2D—C1D—H1D1	110.7
C5A—C6A—H6A1	108.7	O1D—C1D—H1D2	110.7
O4A—C6A—H6A2	108.7	C2D—C1D—H1D2	110.7
C5A—C6A—H6A2	108.7	H1D1—C1D—H1D2	108.8
H6A1—C6A—H6A2	107.6	O2D—C2D—C1D	108.4 (12)
C7A—O4A—C6A	109.4 (9)	O2D—C2D—H2D1	110.0
O4A—C7A—C8A	102.9 (8)	C1D—C2D—H2D1	110.0
O4A—C7A—H7A1	111.2	O2D—C2D—H2D2	110.0
C8A—C7A—H7A1	111.2	C1D—C2D—H2D2	110.0
O4A—C7A—H7A2	111.2	H2D1—C2D—H2D2	108.4
C8A—C7A—H7A2	111.2	C2D—O2D—C3D	113.2 (12)
H7A1—C7A—H7A2	109.1	O2D—C3D—C4D	108.0 (12)
O5A—C8A—C7A	117.5 (10)	O2D—C3D—H3D1	110.1
O5A—C8A—H8A1	107.9	C4D—C3D—H3D1	110.1
C7A—C8A—H8A1	107.9	O2D—C3D—H3D2	110.1
O5A—C8A—H8A2	107.9	C4D—C3D—H3D2	110.1
C7A—C8A—H8A2	107.9	H3D1—C3D—H3D2	108.4
H8A1—C8A—H8A2	107.2	O3D—C4D—C3D	111.2 (12)
C8A—O5A—C9A	117.1 (8)	O3D—C4D—H4D1	109.4
O5A—C9A—C10A	105.9 (11)	C3D—C4D—H4D1	109.4
O5A—C9A—H9A1	110.6	O3D—C4D—H4D2	109.4
C10A—C9A—H9A1	110.6	C3D—C4D—H4D2	109.4
O5A—C9A—H9A2	110.6	H4D1—C4D—H4D2	108.0
C10A—C9A—H9A2	110.6	C5D—O3D—C4D	112.2 (11)
H9A1—C9A—H9A2	108.7	O3D—C5D—C6D	109.9 (13)
O1A—C10A—C9A	102.4 (12)	O3D—C5D—H5D1	109.7
O1A—C10A—H10A	111.3	C6D—C5D—H5D1	109.7
C9A—C10A—H10A	111.3	O3D—C5D—H5D2	109.7
O1A—C10A—H10B	111.3	C6D—C5D—H5D2	109.7
C9A—C10A—H10B	111.3	H5D1—C5D—H5D2	108.2
H10A—C10A—H10B	109.2	O4D—C6D—C5D	117.1 (14)
C1B—O1B—C10B	111.5 (8)	O4D—C6D—H6D1	108.0
O1B—C1B—C2B	117.5 (10)	C5D—C6D—H6D1	108.0
O1B—C1B—H1B1	107.9	O4D—C6D—H6D2	108.0
C2B—C1B—H1B1	107.9	C5D—C6D—H6D2	108.0
O1B—C1B—H1B2	107.9	H6D1—C6D—H6D2	107.3
C2B—C1B—H1B2	107.9	C7D—O4D—C6D	111.0 (15)
H1B1—C1B—H1B2	107.2	O4D—C7D—C8D	110.8 (16)
O2B—C2B—C1B	105.1 (9)	O4D—C7D—H7D1	109.5
O2B—C2B—H2B1	110.7	C8D—C7D—H7D1	109.5
C1B—C2B—H2B1	110.7	O4D—C7D—H7D2	109.5
O2B—C2B—H2B2	110.7	C8D—C7D—H7D2	109.5
C1B—C2B—H2B2	110.7	H7D1—C7D—H7D2	108.1
H2B1—C2B—H2B2	108.8	O5D—C8D—C7D	111.9 (17)
C2B—O2B—C3B	107.0 (10)	O5D—C8D—H8D1	109.2
O2B—C3B—C4B	111.0 (11)	C7D—C8D—H8D1	109.2
O2B—C3B—H3B1	109.4	O5D—C8D—H8D2	109.2
C4B—C3B—H3B1	109.4	C7D—C8D—H8D2	109.2
O2B—C3B—H3B2	109.4	H8D1—C8D—H8D2	107.9
C4B—C3B—H3B2	109.4	C9D—O5D—C8D	115.2 (12)
H3B1—C3B—H3B2	108.0	O5D—C9D—C10D	108.9 (13)
O3B—C4B—C3B	105.3 (11)	O5D—C9D—H9D1	109.9
O3B—C4B—H4B1	110.7	C10D—C9D—H9D1	109.9
C3B—C4B—H4B1	110.7	O5D—C9D—H9D2	109.9
O3B—C4B—H4B2	110.7	C10D—C9D—H9D2	109.9
C3B—C4B—H4B2	110.7	H9D1—C9D—H9D2	108.3
H4B1—C4B—H4B2	108.8	O1D—C10D—C9D	108.0 (12)
C4B—O3B—C5B	113.3 (10)	O1D—C10D—H10G	110.1
O3B—C5B—C6B	105.6 (10)	C9D—C10D—H10G	110.1
O3B—C5B—H5B1	110.6	O1D—C10D—H10H	110.1
C6B—C5B—H5B1	110.6	C9D—C10D—H10H	110.1
O3B—C5B—H5B2	110.6	H10G—C10D—H10H	108.4
C6B—C5B—H5B2	110.6

O12—N1—O11—Cr	−9.2 (5)	C8B—O5B—C9B—C10B	165.2 (12)
O13—N1—O11—Cr	172.2 (3)	C1B—O1B—C10B—C9B	166.1 (12)
O4W—Cr—O11—N1	−49.2 (3)	O5B—C9B—C10B—O1B	−71.3 (17)
O3W—Cr—O11—N1	45.3 (3)	C10C—O1C—C1C—C2C	154.2 (15)
O5W—Cr—O11—N1	−135.8 (3)	O1C—C1C—C2C—O2C	−48.6 (16)
O2W—Cr—O11—N1	131.3 (3)	C1C—C2C—O2C—C3C	166.6 (10)
O1W—Cr—O11—N1	−163.9 (7)	C2C—O2C—C3C—C4C	−161.2 (10)
C10A—O1A—C1A—C2A	−179.5 (11)	O2C—C3C—C4C—O3C	71.4 (12)
O1A—C1A—C2A—O2A	−60.7 (14)	C3C—C4C—O3C—C5C	−178.5 (9)
C1A—C2A—O2A—C3A	158.5 (11)	C4C—O3C—C5C—C6C	89.3 (13)
C2A—O2A—C3A—C4A	−152.7 (11)	O3C—C5C—C6C—O4C	62.4 (14)
O2A—C3A—C4A—O3A	64.0 (14)	C5C—C6C—O4C—C7C	−171.9 (10)
C3A—C4A—O3A—C5A	−174.6 (11)	C6C—O4C—C7C—C8C	157.2 (11)
C4A—O3A—C5A—C6A	165.2 (9)	O4C—C7C—C8C—O5C	−67.2 (14)
O3A—C5A—C6A—O4A	−61.1 (13)	C7C—C8C—O5C—C9C	149.0 (12)
C5A—C6A—O4A—C7A	155.1 (11)	C8C—O5C—C9C—C10C	−177.8 (11)
C6A—O4A—C7A—C8A	176.4 (9)	C1C—O1C—C10C—C9C	−167.8 (14)
O4A—C7A—C8A—O5A	67.4 (13)	O5C—C9C—C10C—O1C	74.8 (17)
C7A—C8A—O5A—C9A	72.7 (13)	C10D—O1D—C1D—C2D	171.5 (14)
C8A—O5A—C9A—C10A	−169.0 (10)	O1D—C1D—C2D—O2D	−63 (2)
C1A—O1A—C10A—C9A	−177.0 (11)	C1D—C2D—O2D—C3D	170.2 (13)
O5A—C9A—C10A—O1A	78.5 (14)	C2D—O2D—C3D—C4D	−158.1 (16)
C10B—O1B—C1B—C2B	−80.2 (13)	O2D—C3D—C4D—O3D	68.2 (15)
O1B—C1B—C2B—O2B	−61.8 (14)	C3D—C4D—O3D—C5D	−161.8 (13)
C1B—C2B—O2B—C3B	177.1 (10)	C4D—O3D—C5D—C6D	176.1 (14)
C2B—O2B—C3B—C4B	−160.6 (12)	O3D—C5D—C6D—O4D	−54 (2)
O2B—C3B—C4B—O3B	72.3 (14)	C5D—C6D—O4D—C7D	−89 (3)
C3B—C4B—O3B—C5B	−167.9 (10)	C6D—O4D—C7D—C8D	167 (2)
C4B—O3B—C5B—C6B	165.7 (11)	O4D—C7D—C8D—O5D	−63 (3)
O3B—C5B—C6B—O4B	−62.2 (13)	C7D—C8D—O5D—C9D	160.0 (19)
C5B—C6B—O4B—C7B	160.9 (11)	C8D—O5D—C9D—C10D	−178.8 (15)
C6B—O4B—C7B—C8B	−157.0 (11)	C1D—O1D—C10D—C9D	−164.7 (15)
O4B—C7B—C8B—O5B	58.6 (14)	O5D—C9D—C10D—O1D	46 (2)
C7B—C8B—O5B—C9B	178.3 (12)

(4) top

Crystal data top

C₁₀H₂₀O₅·H₄N₂O₈Pd	Z = 2
M_r = 486.71	F(000) = 496
Triclinic, P1	D_x = 1.839 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.4649 (1) Å	Cell parameters from 3994 reflections
b = 9.5487 (1) Å	θ = 1.0–27.5°
c = 13.3944 (2) Å	µ = 1.13 mm⁻¹
α = 73.8388 (7)°	T = 90 K
β = 88.0601 (7)°	Plate, colourless
γ = 73.6959 (7)°	0.15 × 0.07 × 0.03 mm
V = 879.13 (2) Å³

Data collection top

Nonius KappaCCD diffractometer	4016 independent reflections
Radiation source: fine-focus sealed tube	3440 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.035
Detector resolution: 9.1 pixels mm^-1	θ_max = 27.5°, θ_min = 1.6°
ω scans at fixed χ = 55°	h = −9→9
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 1997)	k = −12→12
T_min = 0.849, T_max = 0.972	l = −17→17
21461 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.052	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ²(F_o²) + (0.015P)² + 0.7189P] where P = (F_o² + 2F_c²)/3
4016 reflections	(Δ/σ)_max < 0.001
251 parameters	Δρ_max = 0.83 e Å⁻³
6 restraints	Δρ_min = −0.80 e Å⁻³

Special details top

Water hydrogen atoms were subject to distance restraints (DFIX) applied to 1,2 and 1,3 distances thereby restraining both OH distances and HOH angles.

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

	x	y	z	U_iso*/U_eq
O1	0.44978 (18)	0.84124 (14)	0.21893 (10)	0.0138 (3)
O2	0.10662 (17)	0.94188 (14)	0.29899 (9)	0.0132 (3)
O3	−0.00280 (17)	0.68012 (14)	0.37128 (10)	0.0137 (3)
O4	0.03914 (19)	0.55976 (15)	0.19211 (10)	0.0174 (3)
O5	0.36269 (17)	0.63634 (14)	0.11768 (10)	0.0153 (3)
C1	0.3756 (3)	0.9976 (2)	0.21703 (15)	0.0154 (4)
H1A	0.2999	1.0555	0.1517	0.018*
H1B	0.4786	1.0427	0.2208	0.018*
C2	0.2561 (3)	1.0043 (2)	0.30908 (15)	0.0145 (4)
H2A	0.3315	0.9452	0.3744	0.017*
H2B	0.2053	1.1110	0.3112	0.017*
C3	−0.0034 (3)	0.9215 (2)	0.38901 (14)	0.0156 (4)
H3A	−0.0829	1.0212	0.3941	0.019*
H3B	0.0792	0.8723	0.4528	0.019*
C4	−0.1233 (3)	0.8230 (2)	0.37831 (15)	0.0166 (4)
H4A	−0.2013	0.8069	0.4394	0.020*
H4B	−0.2070	0.8728	0.3150	0.020*
C5	−0.0982 (3)	0.5780 (2)	0.35249 (15)	0.0175 (4)
H5A	−0.2144	0.6370	0.3095	0.021*
H5B	−0.1328	0.5182	0.4195	0.021*
C6	0.0246 (3)	0.4727 (2)	0.29743 (15)	0.0179 (4)
H6A	0.1500	0.4275	0.3332	0.021*
H6B	−0.0299	0.3895	0.2974	0.021*
C7	0.1660 (3)	0.4764 (2)	0.13249 (16)	0.0179 (4)
H7A	0.1250	0.5193	0.0580	0.021*
H7B	0.1623	0.3693	0.1541	0.021*
C8	0.3648 (3)	0.4807 (2)	0.14576 (15)	0.0157 (4)
H8A	0.4119	0.4304	0.2189	0.019*
H8B	0.4472	0.4271	0.1004	0.019*
C9	0.5438 (3)	0.6568 (2)	0.12320 (15)	0.0167 (4)
H9A	0.6153	0.6342	0.0632	0.020*
H9B	0.6132	0.5870	0.1880	0.020*
C10	0.5201 (3)	0.8192 (2)	0.12174 (14)	0.0143 (4)
H10A	0.6418	0.8423	0.1110	0.017*
H10B	0.4318	0.8887	0.0638	0.017*
Pd1	0.5000	0.5000	0.5000	0.00905 (6)
O61	0.36808 (19)	0.61191 (15)	0.35964 (10)	0.0152 (3)
H61A	0.397 (3)	0.680 (2)	0.3221 (17)	0.023*
H61B	0.262 (3)	0.633 (3)	0.3622 (18)	0.023*
O71	0.44716 (18)	0.31460 (15)	0.48166 (10)	0.0164 (3)
N1	0.5632 (2)	0.24692 (17)	0.42048 (12)	0.0145 (3)
O81	0.7008 (2)	0.29036 (16)	0.39221 (11)	0.0211 (3)
O91	0.5235 (2)	0.14365 (17)	0.39839 (12)	0.0275 (3)
Pd2	0.0000	1.0000	0.0000	0.00852 (6)
O62	−0.0070 (2)	0.86094 (15)	0.14265 (10)	0.0157 (3)
H62A	0.042 (3)	0.882 (3)	0.1853 (17)	0.024*
H62B	0.040 (3)	0.776 (2)	0.1489 (18)	0.024*
O72	−0.01441 (17)	1.17356 (14)	0.05803 (10)	0.0133 (3)
N2	−0.1691 (2)	1.21875 (17)	0.10712 (12)	0.0133 (3)
O82	−0.29127 (19)	1.15441 (15)	0.11248 (11)	0.0189 (3)
O92	−0.1755 (2)	1.32423 (16)	0.14308 (12)	0.0241 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O1	0.0175 (7)	0.0121 (6)	0.0118 (6)	−0.0048 (5)	0.0029 (5)	−0.0029 (5)
O2	0.0150 (6)	0.0177 (6)	0.0107 (6)	−0.0094 (5)	0.0027 (5)	−0.0053 (5)
O3	0.0132 (6)	0.0135 (6)	0.0166 (6)	−0.0061 (5)	0.0000 (5)	−0.0053 (5)
O4	0.0202 (7)	0.0153 (7)	0.0163 (7)	−0.0054 (5)	0.0027 (5)	−0.0035 (5)
O5	0.0123 (6)	0.0130 (6)	0.0204 (7)	−0.0051 (5)	−0.0009 (5)	−0.0025 (5)
C1	0.0139 (9)	0.0112 (9)	0.0199 (10)	−0.0053 (7)	0.0001 (7)	−0.0007 (7)
C2	0.0157 (9)	0.0140 (9)	0.0171 (9)	−0.0073 (7)	−0.0010 (7)	−0.0063 (7)
C3	0.0185 (9)	0.0172 (9)	0.0132 (9)	−0.0061 (8)	0.0056 (7)	−0.0073 (7)
C4	0.0156 (9)	0.0168 (9)	0.0180 (9)	−0.0041 (7)	0.0051 (7)	−0.0068 (8)
C5	0.0153 (9)	0.0196 (10)	0.0216 (10)	−0.0106 (8)	0.0028 (8)	−0.0065 (8)
C6	0.0188 (10)	0.0156 (9)	0.0207 (10)	−0.0081 (8)	0.0007 (8)	−0.0040 (8)
C7	0.0188 (10)	0.0159 (9)	0.0215 (10)	−0.0061 (8)	0.0032 (8)	−0.0084 (8)
C8	0.0173 (9)	0.0126 (9)	0.0173 (9)	−0.0026 (7)	−0.0001 (7)	−0.0058 (7)
C9	0.0132 (9)	0.0231 (10)	0.0168 (9)	−0.0071 (8)	0.0019 (7)	−0.0084 (8)
C10	0.0146 (9)	0.0189 (9)	0.0103 (8)	−0.0076 (7)	0.0022 (7)	−0.0029 (7)
Pd1	0.00936 (10)	0.00826 (9)	0.00945 (10)	−0.00348 (7)	0.00105 (7)	−0.00143 (7)
O61	0.0151 (7)	0.0147 (7)	0.0139 (6)	−0.0066 (6)	−0.0009 (6)	0.0013 (5)
O71	0.0176 (7)	0.0146 (6)	0.0193 (7)	−0.0070 (5)	0.0046 (5)	−0.0065 (5)
N1	0.0182 (8)	0.0116 (7)	0.0128 (7)	−0.0035 (6)	−0.0026 (6)	−0.0023 (6)
O81	0.0200 (7)	0.0217 (7)	0.0252 (8)	−0.0090 (6)	0.0081 (6)	−0.0098 (6)
O91	0.0374 (9)	0.0226 (8)	0.0321 (8)	−0.0153 (7)	0.0019 (7)	−0.0163 (7)
Pd2	0.00976 (10)	0.00788 (9)	0.00733 (9)	−0.00189 (7)	−0.00048 (7)	−0.00168 (7)
O62	0.0259 (8)	0.0100 (6)	0.0113 (6)	−0.0059 (6)	−0.0015 (5)	−0.0018 (5)
O72	0.0123 (6)	0.0137 (6)	0.0149 (6)	−0.0030 (5)	0.0016 (5)	−0.0063 (5)
N2	0.0149 (8)	0.0123 (7)	0.0116 (7)	−0.0021 (6)	0.0009 (6)	−0.0035 (6)
O82	0.0167 (7)	0.0204 (7)	0.0234 (7)	−0.0100 (6)	0.0062 (6)	−0.0083 (6)
O92	0.0234 (8)	0.0246 (8)	0.0319 (8)	−0.0077 (6)	0.0049 (6)	−0.0195 (7)

Geometric parameters (Å, º) top

O1—C1	1.432 (2)	C7—H7B	0.9900
O1—C10	1.435 (2)	C8—H8A	0.9900
O2—C2	1.431 (2)	C8—H8B	0.9900
O2—C3	1.435 (2)	C9—C10	1.506 (3)
O3—C4	1.434 (2)	C9—H9A	0.9900
O3—C5	1.435 (2)	C9—H9B	0.9900
O4—C7	1.431 (2)	C10—H10A	0.9900
O4—C6	1.442 (2)	C10—H10B	0.9900
O5—C8	1.424 (2)	Pd1—O71	1.9977 (13)
O5—C9	1.426 (2)	Pd1—O71ⁱ	1.9977 (13)
C1—C2	1.502 (3)	Pd1—O61ⁱ	2.0155 (13)
C1—H1A	0.9900	Pd1—O61	2.0155 (13)
C1—H1B	0.9900	O61—H61A	0.784 (18)
C2—H2A	0.9900	O61—H61B	0.765 (18)
C2—H2B	0.9900	O71—N1	1.331 (2)
C3—C4	1.504 (3)	N1—O91	1.216 (2)
C3—H3A	0.9900	N1—O81	1.224 (2)
C3—H3B	0.9900	Pd2—O72	1.9934 (12)
C4—H4A	0.9900	Pd2—O72ⁱⁱ	1.9935 (12)
C4—H4B	0.9900	Pd2—O62	2.0091 (13)
C5—C6	1.498 (3)	Pd2—O62ⁱⁱ	2.0091 (13)
C5—H5A	0.9900	O62—H62A	0.784 (18)
C5—H5B	0.9900	O62—H62B	0.770 (18)
C6—H6A	0.9900	O72—N2	1.3335 (19)
C6—H6B	0.9900	N2—O92	1.221 (2)
C7—C8	1.513 (3)	N2—O82	1.225 (2)
C7—H7A	0.9900

C1—O1—C10	113.95 (14)	H7A—C7—H7B	107.8
C2—O2—C3	113.95 (14)	O5—C8—C7	107.28 (15)
C4—O3—C5	114.57 (14)	O5—C8—H8A	110.3
C7—O4—C6	114.13 (14)	C7—C8—H8A	110.3
C8—O5—C9	113.12 (14)	O5—C8—H8B	110.3
O1—C1—C2	107.99 (14)	C7—C8—H8B	110.3
O1—C1—H1A	110.1	H8A—C8—H8B	108.5
C2—C1—H1A	110.1	O5—C9—C10	108.22 (15)
O1—C1—H1B	110.1	O5—C9—H9A	110.1
C2—C1—H1B	110.1	C10—C9—H9A	110.1
H1A—C1—H1B	108.4	O5—C9—H9B	110.1
O2—C2—C1	108.15 (15)	C10—C9—H9B	110.1
O2—C2—H2A	110.1	H9A—C9—H9B	108.4
C1—C2—H2A	110.1	O1—C10—C9	109.12 (14)
O2—C2—H2B	110.1	O1—C10—H10A	109.9
C1—C2—H2B	110.1	C9—C10—H10A	109.9
H2A—C2—H2B	108.4	O1—C10—H10B	109.9
O2—C3—C4	108.11 (15)	C9—C10—H10B	109.9
O2—C3—H3A	110.1	H10A—C10—H10B	108.3
C4—C3—H3A	110.1	O71—Pd1—O71ⁱ	180.0
O2—C3—H3B	110.1	O71—Pd1—O61ⁱ	93.08 (5)
C4—C3—H3B	110.1	O71ⁱ—Pd1—O61ⁱ	86.92 (5)
H3A—C3—H3B	108.4	O71—Pd1—O61	86.92 (5)
O3—C4—C3	108.23 (15)	O71ⁱ—Pd1—O61	93.08 (5)
O3—C4—H4A	110.1	O61ⁱ—Pd1—O61	179.999 (1)
C3—C4—H4A	110.1	Pd1—O61—H61A	121.4 (17)
O3—C4—H4B	110.1	Pd1—O61—H61B	112.6 (18)
C3—C4—H4B	110.1	H61A—O61—H61B	110 (2)
H4A—C4—H4B	108.4	N1—O71—Pd1	114.36 (10)
O3—C5—C6	110.22 (15)	O91—N1—O81	125.14 (16)
O3—C5—H5A	109.6	O91—N1—O71	116.21 (15)
C6—C5—H5A	109.6	O81—N1—O71	118.63 (15)
O3—C5—H5B	109.6	O72—Pd2—O72ⁱⁱ	180.00 (7)
C6—C5—H5B	109.6	O72—Pd2—O62	91.55 (5)
H5A—C5—H5B	108.1	O72ⁱⁱ—Pd2—O62	88.45 (5)
O4—C6—C5	107.93 (15)	O72—Pd2—O62ⁱⁱ	88.45 (5)
O4—C6—H6A	110.1	O72ⁱⁱ—Pd2—O62ⁱⁱ	91.55 (5)
C5—C6—H6A	110.1	O62—Pd2—O62ⁱⁱ	179.999 (1)
O4—C6—H6B	110.1	Pd2—O62—H62A	111.9 (18)
C5—C6—H6B	110.1	Pd2—O62—H62B	115.3 (18)
H6A—C6—H6B	108.4	H62A—O62—H62B	106 (2)
O4—C7—C8	112.45 (16)	N2—O72—Pd2	115.97 (10)
O4—C7—H7A	109.1	O92—N2—O82	125.46 (16)
C8—C7—H7A	109.1	O92—N2—O72	115.34 (15)
O4—C7—H7B	109.1	O82—N2—O72	119.20 (15)
C8—C7—H7B	109.1

C10—O1—C1—C2	162.68 (14)	C8—O5—C9—C10	−164.40 (15)
C3—O2—C2—C1	171.64 (14)	C1—O1—C10—C9	−164.36 (15)
O1—C1—C2—O2	−61.31 (18)	O5—C9—C10—O1	71.00 (18)
C2—O2—C3—C4	−166.83 (15)	O61ⁱ—Pd1—O71—N1	−100.46 (12)
C5—O3—C4—C3	−175.34 (15)	O61—Pd1—O71—N1	79.54 (12)
O2—C3—C4—O3	59.79 (19)	Pd1—O71—N1—O91	−172.34 (12)
C4—O3—C5—C6	152.96 (15)	Pd1—O71—N1—O81	8.7 (2)
C7—O4—C6—C5	174.84 (15)	O62—Pd2—O72—N2	−62.55 (12)
O3—C5—C6—O4	−71.36 (19)	O62ⁱⁱ—Pd2—O72—N2	117.45 (12)
C6—O4—C7—C8	−87.05 (19)	Pd2—O72—N2—O92	179.39 (12)
C9—O5—C8—C7	−177.92 (15)	Pd2—O72—N2—O82	−1.0 (2)
O4—C7—C8—O5	−56.6 (2)

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

(5) top

Crystal data top

2(C₁₀H₂₀O₅)·H₄N₂O₈Pd·2(HNO₃)·2(H₂O)	Z = 1
M_r = 869.04	F(000) = 452
Triclinic, P1	D_x = 1.623 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.0048 (1) Å	Cell parameters from 7640 reflections
b = 9.8871 (2) Å	θ = 1.0–27.5°
c = 13.8440 (3) Å	µ = 0.62 mm⁻¹
α = 79.8454 (9)°	T = 90 K
β = 87.7567 (9)°	Rod, brown
γ = 70.4587 (11)°	0.50 × 0.10 × 0.10 mm
V = 889.21 (3) Å³

Data collection top

Nonius KappaCCD diffractometer	4040 independent reflections
Radiation source: fine-focus sealed tube	3946 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.052
Detector resolution: 9.1 pixels mm^-1	θ_max = 27.5°, θ_min = 2.5°
ω scans at fixed χ = 55°	h = −9→9
Absorption correction: multi-scan SADABS (Sheldrick, 1996)	k = −12→12
T_min = 0.596, T_max = 0.940	l = −17→17
24163 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.063	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ²(F_o²) + (0.0166P)² + 0.5279P] where P = (F_o² + 2F_c²)/3
4040 reflections	(Δ/σ)_max = 0.001
248 parameters	Δρ_max = 0.61 e Å⁻³
6 restraints	Δρ_min = −0.78 e Å⁻³

Special details top

Water hydrogen atoms were subject to distance restraints (DFIX) applied to 1,2 and 1,3 distances thereby restraining both OH distances and HOH angles.

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

	x	y	z	U_iso*/U_eq
O1	0.44859 (18)	0.76046 (12)	0.26456 (8)	0.0179 (2)
O2	0.50643 (16)	0.47734 (11)	0.37780 (8)	0.0157 (2)
O3	0.32545 (16)	0.36081 (11)	0.25227 (8)	0.0146 (2)
O4	0.00778 (16)	0.60402 (11)	0.17921 (8)	0.0151 (2)
O5	0.18429 (17)	0.82662 (11)	0.10688 (8)	0.0170 (2)
C1	0.5224 (2)	0.71708 (17)	0.36298 (11)	0.0175 (3)
H1A	0.4081	0.7348	0.4088	0.021*
H1B	0.6091	0.7734	0.3759	0.021*
C2	0.6438 (2)	0.55676 (17)	0.37717 (12)	0.0174 (3)
H2A	0.7405	0.5366	0.3232	0.021*
H2B	0.7216	0.5267	0.4400	0.021*
C3	0.5995 (2)	0.33242 (16)	0.35770 (11)	0.0159 (3)
H3A	0.6866	0.2696	0.4141	0.019*
H3B	0.6847	0.3339	0.2990	0.019*
C4	0.4330 (2)	0.27459 (16)	0.34020 (11)	0.0164 (3)
H4A	0.4908	0.1710	0.3327	0.020*
H4B	0.3402	0.2817	0.3963	0.020*
C5	0.1311 (2)	0.34818 (16)	0.23942 (12)	0.0167 (3)
H5A	0.0533	0.3596	0.3005	0.020*
H5B	0.1469	0.2510	0.2240	0.020*
C6	0.0208 (2)	0.46584 (16)	0.15624 (12)	0.0162 (3)
H6A	0.0948	0.4510	0.0945	0.019*
H6B	−0.1168	0.4622	0.1473	0.019*
C7	−0.0763 (2)	0.72315 (17)	0.10046 (12)	0.0189 (3)
H7A	−0.2248	0.7462	0.0958	0.023*
H7B	−0.0172	0.6968	0.0375	0.023*
C8	−0.0287 (2)	0.85312 (17)	0.12069 (12)	0.0183 (3)
H8A	−0.1083	0.9418	0.0753	0.022*
H8B	−0.0644	0.8681	0.1888	0.022*
C9	0.2528 (3)	0.93496 (16)	0.13642 (12)	0.0194 (3)
H9A	0.1461	1.0315	0.1202	0.023*
H9B	0.3748	0.9392	0.0992	0.023*
C10	0.3027 (3)	0.90252 (16)	0.24537 (11)	0.0179 (3)
H10A	0.3585	0.9747	0.2632	0.022*
H10B	0.1795	0.9061	0.2839	0.022*
Pd	0.5000	0.5000	0.0000	0.01145 (6)
O61	0.46157 (17)	0.55162 (12)	0.13540 (8)	0.0148 (2)
H61A	0.412 (3)	0.497 (2)	0.1710 (14)	0.022*
H61B	0.385 (3)	0.6339 (18)	0.1310 (15)	0.022*
N1	0.4049 (2)	0.78769 (14)	−0.10510 (10)	0.0167 (3)
O71	0.54243 (17)	0.69096 (12)	−0.04279 (8)	0.0174 (2)
O81	0.25517 (18)	0.76050 (12)	−0.12672 (9)	0.0211 (2)
O91	0.4395 (2)	0.90026 (13)	−0.13799 (10)	0.0275 (3)
O11	0.09790 (18)	0.61520 (13)	0.36789 (8)	0.0172 (2)
H11B	0.055 (3)	0.624 (2)	0.3153 (13)	0.026*
H11A	0.218 (3)	0.582 (2)	0.3672 (15)	0.026*
N2	−0.1473 (2)	0.90971 (14)	0.46176 (10)	0.0177 (3)
O14	−0.1678 (2)	0.94905 (13)	0.37352 (9)	0.0252 (3)
O15	−0.2131 (2)	0.98334 (14)	0.52467 (10)	0.0292 (3)
O16	−0.04218 (19)	0.76821 (12)	0.49542 (8)	0.0201 (2)
H16	−0.004 (3)	0.729 (2)	0.4462 (17)	0.030*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
O1	0.0256 (6)	0.0148 (5)	0.0118 (5)	−0.0037 (5)	−0.0027 (4)	−0.0038 (4)
O2	0.0141 (5)	0.0150 (5)	0.0180 (5)	−0.0038 (4)	0.0007 (4)	−0.0048 (4)
O3	0.0133 (5)	0.0168 (5)	0.0131 (5)	−0.0049 (4)	−0.0009 (4)	−0.0008 (4)
O4	0.0176 (5)	0.0141 (5)	0.0128 (5)	−0.0036 (4)	−0.0037 (4)	−0.0031 (4)
O5	0.0203 (6)	0.0147 (5)	0.0165 (5)	−0.0046 (4)	−0.0009 (4)	−0.0058 (4)
C1	0.0226 (8)	0.0198 (7)	0.0130 (7)	−0.0098 (6)	−0.0028 (6)	−0.0046 (6)
C2	0.0152 (7)	0.0214 (7)	0.0164 (8)	−0.0070 (6)	−0.0024 (6)	−0.0030 (6)
C3	0.0160 (7)	0.0153 (7)	0.0138 (7)	−0.0016 (6)	−0.0012 (6)	−0.0024 (5)
C4	0.0190 (7)	0.0132 (6)	0.0144 (7)	−0.0034 (6)	−0.0011 (6)	0.0007 (5)
C5	0.0142 (7)	0.0159 (7)	0.0225 (8)	−0.0069 (6)	0.0012 (6)	−0.0062 (6)
C6	0.0148 (7)	0.0181 (7)	0.0184 (7)	−0.0061 (6)	−0.0007 (6)	−0.0085 (6)
C7	0.0186 (8)	0.0210 (7)	0.0149 (7)	−0.0041 (6)	−0.0068 (6)	−0.0008 (6)
C8	0.0193 (8)	0.0153 (7)	0.0165 (7)	−0.0007 (6)	−0.0028 (6)	−0.0020 (6)
C9	0.0292 (9)	0.0134 (7)	0.0167 (8)	−0.0087 (6)	−0.0023 (6)	−0.0020 (6)
C10	0.0258 (8)	0.0127 (7)	0.0157 (7)	−0.0057 (6)	−0.0004 (6)	−0.0048 (5)
Pd	0.01332 (9)	0.01180 (8)	0.01011 (9)	−0.00443 (6)	0.00176 (6)	−0.00400 (6)
O61	0.0181 (5)	0.0149 (5)	0.0123 (5)	−0.0054 (4)	0.0033 (4)	−0.0053 (4)
N1	0.0190 (7)	0.0133 (6)	0.0168 (6)	−0.0032 (5)	0.0033 (5)	−0.0050 (5)
O71	0.0192 (6)	0.0162 (5)	0.0168 (5)	−0.0058 (4)	0.0008 (4)	−0.0032 (4)
O81	0.0201 (6)	0.0199 (5)	0.0226 (6)	−0.0049 (5)	−0.0029 (5)	−0.0045 (4)
O91	0.0318 (7)	0.0143 (5)	0.0348 (7)	−0.0082 (5)	0.0058 (6)	−0.0001 (5)
O11	0.0145 (5)	0.0213 (5)	0.0143 (5)	−0.0016 (4)	−0.0007 (4)	−0.0075 (4)
N2	0.0175 (7)	0.0168 (6)	0.0206 (7)	−0.0069 (5)	0.0031 (5)	−0.0063 (5)
O14	0.0301 (7)	0.0213 (6)	0.0185 (6)	−0.0023 (5)	−0.0005 (5)	−0.0006 (5)
O15	0.0376 (7)	0.0252 (6)	0.0289 (7)	−0.0107 (6)	0.0114 (6)	−0.0173 (5)
O16	0.0265 (6)	0.0169 (5)	0.0139 (6)	−0.0021 (5)	−0.0003 (5)	−0.0044 (4)

Geometric parameters (Å, º) top

O1—C1	1.4173 (18)	C7—C8	1.504 (2)
O1—C10	1.4203 (18)	C7—H7A	0.9900
O2—C2	1.4298 (18)	C7—H7B	0.9900
O2—C3	1.4342 (17)	C8—H8A	0.9900
O3—C5	1.4284 (17)	C8—H8B	0.9900
O3—C4	1.4325 (17)	C9—C10	1.515 (2)
O4—C6	1.4296 (17)	C9—H9A	0.9900
O4—C7	1.4339 (18)	C9—H9B	0.9900
O5—C9	1.4346 (17)	C10—H10A	0.9900
O5—C8	1.4373 (19)	C10—H10B	0.9900
C1—C2	1.508 (2)	Pd—O71ⁱ	1.9928 (11)
C1—H1A	0.9900	Pd—O71	1.9928 (11)
C1—H1B	0.9900	Pd—O61	2.0131 (10)
C2—H2A	0.9900	Pd—O61ⁱ	2.0132 (10)
C2—H2B	0.9900	O61—H61A	0.824 (16)
C3—C4	1.505 (2)	O61—H61B	0.803 (16)
C3—H3A	0.9900	N1—O91	1.2238 (17)
C3—H3B	0.9900	N1—O81	1.2260 (17)
C4—H4A	0.9900	N1—O71	1.3210 (17)
C4—H4B	0.9900	O11—H11B	0.778 (17)
C5—C6	1.508 (2)	O11—H11A	0.795 (17)
C5—H5A	0.9900	N2—O15	1.2118 (18)
C5—H5B	0.9900	N2—O14	1.2137 (18)
C6—H6A	0.9900	N2—O16	1.3506 (17)
C6—H6B	0.9900	O16—H16	0.84 (2)

C1—O1—C10	113.60 (11)	O4—C7—H7A	110.0
C2—O2—C3	113.94 (12)	C8—C7—H7A	110.0
C5—O3—C4	114.50 (12)	O4—C7—H7B	110.0
C6—O4—C7	113.31 (11)	C8—C7—H7B	110.0
C9—O5—C8	113.28 (12)	H7A—C7—H7B	108.4
O1—C1—C2	107.55 (12)	O5—C8—C7	108.25 (12)
O1—C1—H1A	110.2	O5—C8—H8A	110.0
C2—C1—H1A	110.2	C7—C8—H8A	110.0
O1—C1—H1B	110.2	O5—C8—H8B	110.0
C2—C1—H1B	110.2	C7—C8—H8B	110.0
H1A—C1—H1B	108.5	H8A—C8—H8B	108.4
O2—C2—C1	108.35 (12)	O5—C9—C10	111.89 (12)
O2—C2—H2A	110.0	O5—C9—H9A	109.2
C1—C2—H2A	110.0	C10—C9—H9A	109.2
O2—C2—H2B	110.0	O5—C9—H9B	109.2
C1—C2—H2B	110.0	C10—C9—H9B	109.2
H2A—C2—H2B	108.4	H9A—C9—H9B	107.9
O2—C3—C4	107.70 (12)	O1—C10—C9	106.47 (12)
O2—C3—H3A	110.2	O1—C10—H10A	110.4
C4—C3—H3A	110.2	C9—C10—H10A	110.4
O2—C3—H3B	110.2	O1—C10—H10B	110.4
C4—C3—H3B	110.2	C9—C10—H10B	110.4
H3A—C3—H3B	108.5	H10A—C10—H10B	108.6
O3—C4—C3	107.45 (12)	O71ⁱ—Pd—O71	180.0
O3—C4—H4A	110.2	O71ⁱ—Pd—O61	93.61 (4)
C3—C4—H4A	110.2	O71—Pd—O61	86.39 (4)
O3—C4—H4B	110.2	O71ⁱ—Pd—O61ⁱ	86.39 (4)
C3—C4—H4B	110.2	O71—Pd—O61ⁱ	93.61 (4)
H4A—C4—H4B	108.5	O61—Pd—O61ⁱ	180.000 (1)
O3—C5—C6	108.12 (12)	Pd—O61—H61A	109.9 (14)
O3—C5—H5A	110.1	Pd—O61—H61B	108.2 (14)
C6—C5—H5A	110.1	H61A—O61—H61B	109.2 (19)
O3—C5—H5B	110.1	O91—N1—O81	124.53 (14)
C6—C5—H5B	110.1	O91—N1—O71	115.88 (13)
H5A—C5—H5B	108.4	O81—N1—O71	119.59 (12)
O4—C6—C5	108.60 (12)	N1—O71—Pd	115.71 (9)
O4—C6—H6A	110.0	H11B—O11—H11A	109 (2)
C5—C6—H6A	110.0	O15—N2—O14	127.20 (14)
O4—C6—H6B	110.0	O15—N2—O16	115.15 (14)
C5—C6—H6B	110.0	O14—N2—O16	117.65 (12)
H6A—C6—H6B	108.4	N2—O16—H16	106.8 (16)
O4—C7—C8	108.40 (12)

C10—O1—C1—C2	169.59 (13)	C9—O5—C8—C7	−172.38 (12)
C3—O2—C2—C1	160.14 (12)	O4—C7—C8—O5	71.41 (16)
O1—C1—C2—O2	−71.58 (15)	C8—O5—C9—C10	84.82 (16)
C2—O2—C3—C4	−168.49 (12)	C1—O1—C10—C9	175.87 (12)
C5—O3—C4—C3	−163.46 (12)	O5—C9—C10—O1	56.16 (17)
O2—C3—C4—O3	65.60 (15)	O91—N1—O71—Pd	−174.00 (10)
C4—O3—C5—C6	168.73 (12)	O81—N1—O71—Pd	5.52 (16)
C7—O4—C6—C5	173.98 (12)	O61—Pd—O71—N1	−115.14 (10)
O3—C5—C6—O4	−57.44 (15)	O61ⁱ—Pd—O71—N1	64.86 (10)
C6—O4—C7—C8	−164.09 (13)

Symmetry code: (i) −x+1, −y+1, −z.

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More examples of the 15-crown-5H2O—M—OH215-crown-5 motif, M = Al3+, Cr3+ and Pd2+

Supporting information

More examples of the 15-crown-5H₂O—M—OH₂15-crown-5 motif, M = Al³⁺, Cr³⁺ and Pd²⁺