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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768110007202/zb5012sup1.cif
Contains datablocks 1, 2, 3, 4, 5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50121sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50122sup3.hkl
Contains datablock 2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50123sup4.hkl
Contains datablock 3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50124sup5.hkl
Contains datablock 4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768110007202/zb50125sup6.hkl
Contains datablock 5

pdf

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
Mr = 613.43F(000) = 652
Triclinic, P1Dx = 1.506 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.8642 (1) ÅCell parameters from 6124 reflections
b = 11.7922 (1) Åθ = 1.0–27.5°
c = 12.8064 (2) ŵ = 0.18 mm1
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 tube3888 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.066
Detector resolution: 9.1 pixels mm-1θmax = 27.5°, θmin = 1.8°
ω scans at fixed χ = 55°h = 1212
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 1997)
k = 1515
Tmin = 0.957, Tmax = 0.988l = 1616
33872 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.117H atoms treated by a mixture of independent and constrained refinement
S = 0.99 w = 1/[σ2(Fo2) + (0.0583P)2]
where P = (Fo2 + 2Fc2)/3
6187 reflections(Δ/σ)max = 0.001
407 parametersΔρmax = 0.35 e Å3
31 restraintsΔρmin = 0.36 e Å3
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
xyzUiso*/Ueq
O10.17527 (15)0.00050 (12)0.66940 (11)0.0168 (3)
O20.11149 (16)0.02046 (12)0.67384 (12)0.0191 (3)
O30.24836 (16)0.19908 (11)0.86487 (12)0.0182 (3)
O40.02771 (15)0.34547 (12)0.84214 (12)0.0189 (3)
O50.22521 (16)0.19844 (12)0.80435 (12)0.0198 (4)
C10.1352 (2)0.06440 (18)0.58300 (18)0.0192 (5)
H1A0.14550.01980.52160.023*
H1B0.20060.13790.54810.023*
C20.0215 (2)0.08841 (17)0.63870 (18)0.0195 (5)
H2A0.03480.12470.70610.023*
H2B0.04890.14150.58370.023*
C30.2589 (2)0.01896 (18)0.75369 (18)0.0185 (5)
H3A0.31640.02340.71460.022*
H3B0.25850.02010.81650.022*
C40.3263 (2)0.14204 (17)0.80111 (18)0.0191 (5)
H4A0.43150.14420.85190.023*
H4B0.32060.18210.73750.023*
C50.2805 (2)0.32237 (17)0.88772 (19)0.0196 (5)
H5A0.27370.34910.81660.024*
H5B0.38200.34550.94610.024*
C60.1718 (2)0.37645 (18)0.93087 (18)0.0194 (5)
H6A0.17640.34821.00080.023*
H6B0.19510.46150.95040.023*
C70.0892 (2)0.38365 (18)0.87374 (19)0.0196 (5)
H7A0.09380.46730.87360.024*
H7B0.07260.37040.95190.024*
C80.2300 (2)0.31642 (17)0.78811 (19)0.0207 (5)
H8A0.31540.34820.80020.025*
H8B0.23990.32090.70900.025*
C90.3422 (2)0.11846 (18)0.71714 (18)0.0206 (5)
H9A0.42920.16000.68420.025*
H9B0.37060.05790.75280.025*
C100.2996 (2)0.06232 (19)0.62257 (18)0.0207 (5)
H10A0.38340.00840.56450.025*
H10B0.27440.12180.58440.025*
Al10.00000.00001.00000.0139 (2)
O610.02191 (16)0.12200 (12)0.92630 (12)0.0153 (3)
H61A0.0545 (19)0.1486 (18)0.8875 (18)0.023*
H61B0.088 (2)0.1402 (18)0.9081 (19)0.023*
O710.11305 (16)0.09346 (12)0.85699 (12)0.0169 (3)
H71A0.137 (2)0.0698 (17)0.7953 (16)0.025*
H71B0.149 (2)0.1648 (14)0.8420 (18)0.025*
O810.17318 (16)0.05180 (12)0.99374 (13)0.0171 (3)
H81A0.254 (2)0.0111 (17)1.0310 (18)0.026*
H81B0.181 (2)0.1191 (14)0.9674 (19)0.026*
Al20.00000.50000.50000.0150 (2)
O620.10598 (16)0.38342 (12)0.56327 (13)0.0198 (4)
H62A0.1976 (18)0.3746 (19)0.579 (2)0.030*
H62B0.068 (2)0.3281 (16)0.5800 (18)0.030*
O720.16957 (16)0.43412 (13)0.51022 (13)0.0184 (3)
H72A0.231 (2)0.3773 (16)0.4629 (16)0.028*
H72B0.208 (2)0.4594 (18)0.5567 (17)0.028*
O820.05372 (17)0.40838 (13)0.35424 (13)0.0206 (4)
H82A0.003 (2)0.3645 (18)0.339 (2)0.031*
H82B0.121 (2)0.4145 (19)0.2924 (16)0.031*
N10.4460 (2)0.76420 (15)0.60672 (16)0.0206 (4)
O150.44398 (18)0.70625 (14)0.51615 (14)0.0307 (4)
O160.35097 (17)0.73630 (13)0.64517 (13)0.0291 (4)
O170.53917 (17)0.84923 (13)0.66013 (14)0.0299 (4)
N20.2291 (2)0.35826 (15)1.28691 (15)0.0185 (4)
O180.25512 (17)0.31196 (12)1.20124 (12)0.0232 (4)
O190.26789 (18)0.46327 (12)1.32689 (13)0.0257 (4)
O200.16373 (16)0.29718 (12)1.32940 (12)0.0206 (4)
N30.2821 (2)0.70400 (15)0.89426 (15)0.0192 (4)
O210.15789 (17)0.73523 (13)0.88319 (14)0.0283 (4)
O220.39610 (17)0.76826 (13)0.95566 (13)0.0267 (4)
O230.28779 (16)0.60498 (12)0.84212 (12)0.0228 (4)
O110.00990 (18)0.22321 (13)0.62993 (13)0.0205 (4)
H11A0.012 (3)0.2551 (16)0.6923 (16)0.031*
H11B0.025 (3)0.1638 (15)0.641 (2)0.031*
O120.42297 (18)0.07725 (14)1.11018 (14)0.0276 (4)
H12A0.437 (3)0.111 (2)1.1777 (16)0.041*
H12B0.464 (3)0.1254 (19)1.0850 (19)0.041*
O130.53118 (18)0.51297 (13)0.80910 (15)0.0264 (4)
H13A0.468 (2)0.5505 (19)0.821 (2)0.040*
H13B0.590 (2)0.5619 (18)0.799 (2)0.040*
O140.37982 (17)0.34707 (14)0.61563 (14)0.0258 (4)
H14A0.437 (3)0.4020 (18)0.6647 (18)0.039*
H14B0.416 (3)0.335 (2)0.5664 (18)0.039*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0166 (8)0.0190 (8)0.0137 (8)0.0035 (6)0.0046 (6)0.0035 (6)
O20.0169 (8)0.0167 (8)0.0212 (8)0.0018 (6)0.0047 (7)0.0036 (6)
O30.0202 (8)0.0153 (8)0.0221 (8)0.0025 (6)0.0125 (7)0.0012 (6)
O40.0179 (8)0.0199 (8)0.0166 (8)0.0019 (6)0.0054 (7)0.0001 (6)
O50.0187 (8)0.0139 (8)0.0225 (8)0.0004 (6)0.0031 (7)0.0042 (6)
C10.0236 (13)0.0181 (11)0.0146 (11)0.0026 (9)0.0080 (10)0.0004 (9)
C20.0270 (13)0.0134 (11)0.0179 (11)0.0011 (9)0.0100 (10)0.0002 (9)
C30.0202 (12)0.0214 (12)0.0161 (11)0.0073 (9)0.0080 (10)0.0061 (9)
C40.0174 (12)0.0222 (12)0.0179 (12)0.0036 (9)0.0082 (10)0.0009 (9)
C50.0204 (12)0.0164 (11)0.0204 (12)0.0011 (9)0.0069 (10)0.0025 (9)
C60.0207 (12)0.0176 (11)0.0159 (11)0.0024 (9)0.0040 (10)0.0012 (9)
C70.0219 (12)0.0149 (11)0.0222 (12)0.0058 (9)0.0092 (10)0.0019 (9)
C80.0209 (12)0.0153 (11)0.0236 (12)0.0070 (9)0.0044 (10)0.0065 (9)
C90.0173 (12)0.0191 (12)0.0227 (12)0.0001 (9)0.0043 (10)0.0057 (10)
C100.0159 (12)0.0243 (12)0.0188 (12)0.0023 (9)0.0022 (9)0.0069 (10)
Al10.0156 (5)0.0125 (5)0.0125 (5)0.0021 (4)0.0047 (4)0.0015 (4)
O610.0127 (8)0.0167 (8)0.0173 (8)0.0030 (6)0.0057 (7)0.0056 (6)
O710.0227 (9)0.0146 (8)0.0115 (8)0.0005 (7)0.0047 (7)0.0026 (6)
O810.0171 (8)0.0119 (8)0.0187 (8)0.0000 (6)0.0048 (7)0.0009 (6)
Al20.0152 (5)0.0140 (5)0.0150 (5)0.0004 (4)0.0057 (4)0.0015 (4)
O620.0167 (8)0.0184 (8)0.0258 (9)0.0019 (7)0.0093 (7)0.0063 (7)
O720.0182 (9)0.0164 (8)0.0198 (9)0.0019 (6)0.0093 (7)0.0026 (6)
O820.0189 (9)0.0219 (9)0.0180 (8)0.0040 (7)0.0057 (7)0.0012 (7)
N10.0191 (10)0.0183 (10)0.0226 (11)0.0015 (8)0.0063 (9)0.0035 (8)
O150.0287 (10)0.0374 (10)0.0263 (9)0.0014 (8)0.0159 (8)0.0048 (8)
O160.0287 (10)0.0315 (10)0.0289 (10)0.0085 (7)0.0185 (8)0.0044 (7)
O170.0248 (9)0.0251 (9)0.0320 (10)0.0112 (7)0.0057 (8)0.0006 (7)
N20.0196 (10)0.0182 (10)0.0170 (10)0.0038 (8)0.0063 (8)0.0034 (8)
O180.0318 (9)0.0202 (8)0.0198 (8)0.0003 (7)0.0151 (7)0.0023 (7)
O190.0375 (10)0.0117 (8)0.0307 (9)0.0020 (7)0.0194 (8)0.0028 (7)
O200.0240 (9)0.0178 (8)0.0243 (9)0.0014 (7)0.0138 (7)0.0051 (7)
N30.0212 (11)0.0179 (10)0.0175 (10)0.0028 (8)0.0067 (8)0.0023 (8)
O210.0175 (9)0.0263 (9)0.0333 (10)0.0080 (7)0.0057 (7)0.0070 (7)
O220.0194 (9)0.0288 (9)0.0230 (9)0.0058 (7)0.0023 (7)0.0028 (7)
O230.0234 (9)0.0199 (9)0.0219 (8)0.0060 (7)0.0078 (7)0.0029 (7)
O110.0273 (9)0.0177 (8)0.0174 (8)0.0023 (7)0.0096 (7)0.0034 (7)
O120.0247 (10)0.0289 (10)0.0252 (10)0.0058 (7)0.0075 (8)0.0020 (8)
O130.0233 (10)0.0229 (9)0.0372 (10)0.0034 (7)0.0172 (8)0.0037 (8)
O140.0198 (9)0.0337 (10)0.0242 (10)0.0038 (7)0.0104 (8)0.0015 (8)
Geometric parameters (Å, º) top
O1—C101.432 (2)Al1—O71i1.8770 (14)
O1—C11.433 (2)Al1—O611.8883 (14)
O2—C31.429 (2)Al1—O61i1.8884 (14)
O2—C21.435 (2)O61—H61A0.836 (15)
O3—C41.434 (2)O61—H61B0.807 (15)
O3—C51.434 (2)O71—H71A0.831 (16)
O4—C71.427 (2)O71—H71B0.861 (15)
O4—C61.430 (2)O81—H81A0.841 (16)
O5—C91.438 (2)O81—H81B0.832 (15)
O5—C81.439 (2)Al2—O621.8626 (14)
C1—C21.498 (3)Al2—O62ii1.8626 (14)
C1—H1A0.9900Al2—O821.8699 (14)
C1—H1B0.9900Al2—O82ii1.8699 (14)
C2—H2A0.9900Al2—O72ii1.8731 (14)
C2—H2B0.9900Al2—O721.8731 (14)
C3—C41.501 (3)O62—H62A0.863 (16)
C3—H3A0.9900O62—H62B0.834 (14)
C3—H3B0.9900O72—H72A0.863 (15)
C4—H4A0.9900O72—H72B0.842 (16)
C4—H4B0.9900O82—H82A0.838 (16)
C5—C61.503 (3)O82—H82B0.833 (16)
C5—H5A0.9900N1—O151.242 (2)
C5—H5B0.9900N1—O171.244 (2)
C6—H6A0.9900N1—O161.267 (2)
C6—H6B0.9900N2—O191.246 (2)
C7—C81.497 (3)N2—O201.258 (2)
C7—H7A0.9900N2—O181.266 (2)
C7—H7B0.9900N3—O221.236 (2)
C8—H8A0.9900N3—O211.257 (2)
C8—H8B0.9900N3—O231.265 (2)
C9—C101.495 (3)O11—H11A0.836 (15)
C9—H9A0.9900O11—H11B0.801 (15)
C9—H9B0.9900O12—H12A0.849 (16)
C10—H10A0.9900O12—H12B0.855 (16)
C10—H10B0.9900O13—H13A0.824 (16)
Al1—O81i1.8635 (15)O13—H13B0.855 (16)
Al1—O811.8635 (15)O14—H14A0.838 (16)
Al1—O711.8770 (14)O14—H14B0.832 (16)
C10—O1—C1112.92 (15)C9—C10—H10B109.8
C3—O2—C2114.58 (15)H10A—C10—H10B108.3
C4—O3—C5112.24 (15)O81i—Al1—O81179.999 (1)
C7—O4—C6114.59 (15)O81i—Al1—O7188.78 (6)
C9—O5—C8114.45 (16)O81—Al1—O7191.22 (6)
O1—C1—C2108.19 (16)O81i—Al1—O71i91.22 (6)
O1—C1—H1A110.1O81—Al1—O71i88.78 (6)
C2—C1—H1A110.1O71—Al1—O71i180.0
O1—C1—H1B110.1O81i—Al1—O6190.23 (6)
C2—C1—H1B110.1O81—Al1—O6189.77 (6)
H1A—C1—H1B108.4O71—Al1—O6190.29 (6)
O2—C2—C1107.02 (16)O71i—Al1—O6189.71 (6)
O2—C2—H2A110.3O81i—Al1—O61i89.77 (6)
C1—C2—H2A110.3O81—Al1—O61i90.23 (6)
O2—C2—H2B110.3O71—Al1—O61i89.71 (6)
C1—C2—H2B110.3O71i—Al1—O61i90.29 (6)
H2A—C2—H2B108.6O61—Al1—O61i180.0
O2—C3—C4107.64 (17)Al1—O61—H61A117.6 (15)
O2—C3—H3A110.2Al1—O61—H61B129.5 (16)
C4—C3—H3A110.2H61A—O61—H61B110 (2)
O2—C3—H3B110.2Al1—O71—H71A123.1 (15)
C4—C3—H3B110.2Al1—O71—H71B128.8 (14)
H3A—C3—H3B108.5H71A—O71—H71B108.1 (19)
O3—C4—C3109.18 (17)Al1—O81—H81A120.4 (15)
O3—C4—H4A109.8Al1—O81—H81B124.9 (16)
C3—C4—H4A109.8H81A—O81—H81B114 (2)
O3—C4—H4B109.8O62—Al2—O62ii180.0
C3—C4—H4B109.8O62—Al2—O8288.85 (7)
H4A—C4—H4B108.3O62ii—Al2—O8291.15 (7)
O3—C5—C6108.97 (17)O62—Al2—O82ii91.15 (7)
O3—C5—H5A109.9O62ii—Al2—O82ii88.84 (7)
C6—C5—H5A109.9O82—Al2—O82ii179.999 (1)
O3—C5—H5B109.9O62—Al2—O72ii89.24 (7)
C6—C5—H5B109.9O62ii—Al2—O72ii90.76 (7)
H5A—C5—H5B108.3O82—Al2—O72ii90.41 (7)
O4—C6—C5108.09 (16)O82ii—Al2—O72ii89.59 (7)
O4—C6—H6A110.1O62—Al2—O7290.76 (7)
C5—C6—H6A110.1O62ii—Al2—O7289.24 (7)
O4—C6—H6B110.1O82—Al2—O7289.59 (7)
C5—C6—H6B110.1O82ii—Al2—O7290.41 (7)
H6A—C6—H6B108.4O72ii—Al2—O72180.0
O4—C7—C8107.78 (17)Al2—O62—H62A128.8 (15)
O4—C7—H7A110.2Al2—O62—H62B123.1 (16)
C8—C7—H7A110.2H62A—O62—H62B108 (2)
O4—C7—H7B110.2Al2—O72—H72A127.3 (15)
C8—C7—H7B110.2Al2—O72—H72B127.0 (15)
H7A—C7—H7B108.5H72A—O72—H72B105.2 (19)
O5—C8—C7107.40 (17)Al2—O82—H82A121.5 (16)
O5—C8—H8A110.2Al2—O82—H82B129.1 (16)
C7—C8—H8A110.2H82A—O82—H82B107 (2)
O5—C8—H8B110.2O15—N1—O17121.30 (19)
C7—C8—H8B110.2O15—N1—O16119.29 (17)
H8A—C8—H8B108.5O17—N1—O16119.41 (18)
O5—C9—C10112.64 (17)O19—N2—O20121.41 (17)
O5—C9—H9A109.1O19—N2—O18119.46 (17)
C10—C9—H9A109.1O20—N2—O18119.13 (17)
O5—C9—H9B109.1O22—N3—O21120.67 (17)
C10—C9—H9B109.1O22—N3—O23120.82 (18)
H9A—C9—H9B107.8O21—N3—O23118.51 (17)
O1—C10—C9109.32 (17)H11A—O11—H11B106 (2)
O1—C10—H10A109.8H12A—O12—H12B105 (2)
C9—C10—H10A109.8H13A—O13—H13B105 (2)
O1—C10—H10B109.8H14A—O14—H14B104 (2)
C10—O1—C1—C2159.42 (16)O3—C5—C6—O462.3 (2)
C3—O2—C2—C1164.80 (16)C6—O4—C7—C8163.31 (17)
O1—C1—C2—O267.1 (2)C9—O5—C8—C7170.80 (17)
C2—O2—C3—C4167.57 (16)O4—C7—C8—O568.2 (2)
C5—O3—C4—C3165.08 (17)C8—O5—C9—C1093.7 (2)
O2—C3—C4—O364.3 (2)C1—O1—C10—C9174.85 (16)
C4—O3—C5—C6167.68 (17)O5—C9—C10—O159.7 (2)
C7—O4—C6—C5175.57 (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
Mr = 613.43Dx = 1.502 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 6560 reflections
a = 18.6039 (3) Åθ = 1.0–27.5°
b = 9.3611 (1) ŵ = 0.18 mm1
c = 31.5795 (5) ÅT = 90 K
β = 99.3468 (7)°Block, colourless
V = 5426.65 (14) Å30.25 × 0.22 × 0.17 mm
Z = 8
Data collection top
Nonius KappaCCD
diffractometer
6212 independent reflections
Radiation source: fine-focus sealed tube4125 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
Detector resolution: 9.1 pixels mm-1θmax = 27.5°, θmin = 1.3°
ω scans at fixed χ = 55°h = 2324
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 1997)
k = 1212
Tmin = 0.957, Tmax = 0.970l = 4040
40687 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.114H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.0561P)2 + 1.7455P]
where P = (Fo2 + 2Fc2)/3
6212 reflections(Δ/σ)max < 0.001
440 parametersΔρmax = 0.79 e Å3
41 restraintsΔρmin = 0.47 e Å3
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.

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
xyzUiso*/UeqOcc. (<1)
O10.16129 (7)0.03541 (14)0.11965 (4)0.0216 (3)
O20.28192 (7)0.21150 (14)0.13652 (4)0.0199 (3)
O30.20544 (7)0.46676 (14)0.12655 (4)0.0235 (3)
O40.09378 (7)0.43426 (14)0.05462 (4)0.0226 (3)
O50.07704 (7)0.13060 (14)0.04249 (4)0.0212 (3)
C10.23193 (11)0.0252 (2)0.13278 (6)0.0225 (4)
H1A0.25480.04790.10740.027*
H1B0.22810.11440.14910.027*
C20.27675 (11)0.0832 (2)0.16048 (6)0.0238 (5)
H2A0.25390.10430.18600.029*
H2B0.32610.04450.17050.029*
C30.30244 (11)0.3318 (2)0.16403 (6)0.0224 (4)
H3A0.35550.32950.17460.027*
H3B0.27680.32780.18910.027*
C40.28273 (10)0.4669 (2)0.13928 (6)0.0222 (4)
H4A0.29810.55120.15750.027*
H4B0.30730.47040.11370.027*
C50.17903 (11)0.5826 (2)0.09960 (7)0.0244 (5)
H5A0.20670.59010.07540.029*
H5B0.18480.67310.11600.029*
C60.10010 (11)0.5557 (2)0.08295 (7)0.0245 (5)
H6A0.07370.53700.10720.029*
H6B0.07820.64080.06730.029*
C70.02354 (11)0.3667 (2)0.04979 (7)0.0238 (5)
H7A0.01450.43290.03570.029*
H7B0.01180.34050.07830.029*
C80.02597 (11)0.2353 (2)0.02283 (6)0.0224 (4)
H8A0.02320.19200.01730.027*
H8B0.03910.26320.00520.027*
C90.04892 (11)0.0368 (2)0.07202 (6)0.0223 (4)
H9A0.00950.02370.05650.027*
H9B0.02890.09310.09400.027*
C100.11083 (11)0.0544 (2)0.09285 (6)0.0216 (4)
H10A0.09260.13020.11020.026*
H10B0.13500.10050.07070.026*
Al10.00000.23840 (9)0.25000.0198 (2)
O610.00086 (8)0.23376 (16)0.19074 (4)0.0249 (3)
H61A0.0360 (10)0.264 (2)0.1729 (7)0.037*
H61B0.0382 (10)0.252 (2)0.1806 (7)0.037*
O710.10281 (7)0.24265 (15)0.25935 (5)0.0221 (3)
H71A0.1263 (12)0.3149 (19)0.2524 (7)0.033*
H71B0.1255 (12)0.1683 (18)0.2528 (7)0.033*
O810.00000.4402 (2)0.25000.0301 (5)
H810.0293 (12)0.492 (2)0.2384 (7)0.045*
O910.00000.0388 (2)0.25000.0223 (4)
H910.0103 (12)0.010 (2)0.2283 (6)0.034*
Al20.25000.25000.00000.01640 (19)
O620.21992 (7)0.18953 (15)0.05123 (4)0.0198 (3)
H62A0.2410 (11)0.209 (2)0.0769 (5)0.030*
H62B0.1753 (9)0.167 (2)0.0512 (6)0.030*
O720.19430 (7)0.41750 (15)0.00134 (4)0.0202 (3)
H72A0.1634 (11)0.427 (2)0.0182 (6)0.030*
H72B0.1902 (12)0.4934 (19)0.0144 (6)0.030*
O820.33117 (7)0.34266 (15)0.03054 (4)0.0196 (3)
H82A0.3366 (12)0.4312 (17)0.0368 (7)0.029*
H82B0.3619 (11)0.293 (2)0.0469 (6)0.029*
N10.06148 (13)0.2906 (4)0.11278 (7)0.0233 (5)0.873 (3)
O150.08802 (9)0.3463 (2)0.07714 (5)0.0269 (5)0.873 (3)
O160.05444 (9)0.1565 (2)0.11524 (6)0.0257 (4)0.873 (3)
O170.0419 (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)
N20.15749 (9)0.58808 (18)0.22196 (5)0.0230 (4)
O180.08912 (8)0.60215 (16)0.21283 (5)0.0380 (4)
O190.19791 (8)0.68393 (16)0.21336 (5)0.0321 (4)
O200.18285 (7)0.47372 (14)0.23965 (4)0.0229 (3)
N30.16419 (10)0.2319 (2)0.02974 (7)0.0197 (5)0.873 (3)
O210.17195 (10)0.2256 (2)0.00955 (5)0.0292 (5)0.873 (3)
O220.16597 (9)0.35206 (16)0.04861 (5)0.0250 (5)0.873 (3)
O230.15249 (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)
O110.11479 (8)0.27185 (16)0.15730 (5)0.0279 (4)
H11A0.1268 (13)0.1957 (19)0.1464 (7)0.042*
H11B0.1390 (13)0.339 (2)0.1506 (8)0.042*
O120.04285 (9)0.12000 (16)0.19051 (5)0.0295 (4)
H12A0.0092 (12)0.127 (2)0.1688 (6)0.044*
H12B0.0494 (13)0.2082 (19)0.1958 (7)0.044*
O130.16558 (8)0.00854 (16)0.25708 (5)0.0300 (4)
H13A0.2099 (9)0.000 (3)0.2546 (8)0.045*
H13B0.1453 (12)0.048 (2)0.2759 (7)0.045*
O140.09889 (10)0.3499 (2)0.36557 (6)0.0427 (4)
H14A0.1154 (16)0.292 (2)0.3881 (7)0.064*
H14B0.0893 (16)0.431 (2)0.3739 (9)0.064*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0201 (7)0.0192 (7)0.0264 (7)0.0008 (6)0.0060 (6)0.0023 (6)
O20.0236 (8)0.0188 (7)0.0178 (7)0.0006 (6)0.0048 (6)0.0021 (5)
O30.0191 (7)0.0201 (7)0.0315 (8)0.0010 (6)0.0051 (6)0.0054 (6)
O40.0188 (7)0.0210 (7)0.0291 (8)0.0014 (6)0.0077 (6)0.0025 (6)
O50.0183 (7)0.0201 (7)0.0263 (7)0.0010 (6)0.0068 (6)0.0046 (6)
C10.0246 (11)0.0189 (10)0.0252 (11)0.0042 (9)0.0078 (9)0.0058 (9)
C20.0264 (11)0.0232 (11)0.0225 (10)0.0024 (9)0.0064 (9)0.0078 (9)
C30.0219 (11)0.0267 (11)0.0188 (10)0.0018 (9)0.0037 (8)0.0045 (8)
C40.0190 (10)0.0233 (11)0.0252 (11)0.0034 (8)0.0063 (8)0.0025 (9)
C50.0272 (12)0.0169 (10)0.0290 (11)0.0019 (9)0.0039 (9)0.0009 (9)
C60.0264 (11)0.0189 (10)0.0292 (11)0.0040 (9)0.0070 (9)0.0019 (9)
C70.0164 (10)0.0237 (11)0.0323 (11)0.0005 (8)0.0065 (9)0.0045 (9)
C80.0164 (10)0.0251 (11)0.0250 (11)0.0007 (8)0.0008 (8)0.0039 (9)
C90.0224 (11)0.0210 (10)0.0253 (10)0.0054 (9)0.0096 (8)0.0002 (9)
C100.0254 (11)0.0166 (10)0.0248 (11)0.0043 (8)0.0102 (8)0.0022 (8)
Al10.0163 (4)0.0177 (4)0.0275 (5)0.0000.0097 (3)0.000
O610.0170 (8)0.0317 (9)0.0278 (8)0.0028 (7)0.0086 (6)0.0038 (7)
O710.0176 (7)0.0172 (7)0.0337 (8)0.0015 (6)0.0105 (6)0.0013 (6)
O810.0254 (12)0.0175 (11)0.0528 (15)0.0000.0224 (10)0.000
O910.0224 (11)0.0172 (11)0.0304 (12)0.0000.0130 (9)0.000
Al20.0145 (4)0.0193 (4)0.0154 (4)0.0002 (3)0.0025 (3)0.0033 (3)
O620.0159 (7)0.0278 (8)0.0161 (7)0.0024 (6)0.0034 (6)0.0039 (6)
O720.0201 (8)0.0210 (8)0.0207 (7)0.0029 (6)0.0069 (6)0.0051 (6)
O820.0181 (7)0.0197 (7)0.0202 (7)0.0000 (6)0.0003 (6)0.0031 (6)
N10.0118 (12)0.0384 (17)0.0197 (13)0.0015 (13)0.0024 (8)0.0016 (13)
O150.0276 (10)0.0322 (12)0.0188 (9)0.0049 (8)0.0025 (7)0.0043 (8)
O160.0252 (10)0.0237 (10)0.0273 (10)0.0032 (8)0.0019 (8)0.0042 (9)
O170.028 (2)0.0295 (18)0.0221 (17)0.0019 (16)0.0044 (10)0.0080 (9)
N20.0212 (9)0.0222 (9)0.0257 (9)0.0035 (8)0.0046 (7)0.0011 (7)
O180.0159 (8)0.0330 (9)0.0643 (11)0.0008 (7)0.0036 (7)0.0179 (8)
O190.0244 (8)0.0256 (8)0.0471 (10)0.0073 (7)0.0079 (7)0.0067 (7)
O200.0206 (7)0.0195 (7)0.0283 (8)0.0009 (6)0.0030 (6)0.0010 (6)
N30.0127 (10)0.0235 (11)0.0227 (11)0.0016 (8)0.0025 (8)0.0042 (10)
O210.0340 (11)0.0377 (11)0.0163 (9)0.0086 (9)0.0048 (8)0.0011 (9)
O220.0331 (10)0.0157 (9)0.0243 (9)0.0006 (7)0.0007 (7)0.0002 (7)
O230.0339 (14)0.0185 (12)0.0231 (12)0.0014 (10)0.0021 (12)0.0043 (12)
O110.0294 (9)0.0217 (8)0.0374 (9)0.0033 (7)0.0196 (7)0.0052 (7)
O120.0338 (9)0.0223 (8)0.0340 (9)0.0015 (7)0.0102 (7)0.0014 (7)
O130.0155 (7)0.0274 (9)0.0464 (10)0.0030 (7)0.0029 (7)0.0061 (7)
O140.0384 (10)0.0476 (11)0.0421 (10)0.0083 (9)0.0070 (8)0.0144 (9)
Geometric parameters (Å, º) top
O1—C11.430 (2)O61—H61A0.842 (16)
O1—C101.430 (2)O61—H61B0.856 (16)
O2—C21.431 (2)O71—H71A0.853 (16)
O2—C31.435 (2)O71—H71B0.857 (16)
O3—C51.416 (2)O81—H810.858 (16)
O3—C41.429 (2)O91—H910.869 (15)
O4—C71.437 (2)Al2—O821.8680 (13)
O4—C61.439 (2)Al2—O82ii1.8681 (13)
O5—C81.434 (2)Al2—O621.8828 (13)
O5—C91.440 (2)Al2—O62ii1.8829 (13)
C1—C21.501 (3)Al2—O721.8837 (14)
C1—H1A0.9900Al2—O72ii1.8837 (14)
C1—H1B0.9900O62—H62A0.861 (15)
C2—H2A0.9900O62—H62B0.857 (15)
C2—H2B0.9900O72—H72A0.849 (15)
C3—C41.501 (3)O72—H72B0.863 (15)
C3—H3A0.9900O82—H82A0.854 (15)
C3—H3B0.9900O82—H82B0.844 (16)
C4—H4A0.9900N1—O171.255 (4)
C4—H4B0.9900N1—O161.263 (4)
C5—C61.498 (3)N1—O151.266 (3)
C5—H5A0.9900N1'—O15'1.245 (16)
C5—H5B0.9900N1'—O16'1.270 (16)
C6—H6A0.9900N1'—O17'1.274 (17)
C6—H6B0.9900N2—O191.229 (2)
C7—C81.501 (3)N2—O201.263 (2)
C7—H7A0.9900N2—O181.265 (2)
C7—H7B0.9900N3—O211.227 (3)
C8—H8A0.9900N3—O231.262 (3)
C8—H8B0.9900N3—O221.276 (3)
C9—C101.497 (3)N3'—O21'1.184 (14)
C9—H9A0.9900N3'—O22'1.267 (15)
C9—H9B0.9900N3'—O23'1.302 (16)
C10—H10A0.9900O11—H11A0.837 (16)
C10—H10B0.9900O11—H11B0.823 (16)
Al1—O911.868 (2)O12—H12A0.852 (17)
Al1—O611.8695 (14)O12—H12B0.847 (17)
Al1—O61i1.8695 (14)O13—H13A0.819 (16)
Al1—O71i1.8877 (14)O13—H13B0.839 (16)
Al1—O711.8877 (14)O14—H14A0.906 (17)
Al1—O811.889 (2)O14—H14B0.830 (17)
C1—O1—C10114.99 (14)O91—Al1—O61i88.67 (5)
C2—O2—C3111.87 (14)O61—Al1—O61i177.34 (10)
C5—O3—C4113.79 (15)O91—Al1—O71i91.21 (5)
C7—O4—C6113.24 (14)O61—Al1—O71i90.01 (6)
C8—O5—C9114.35 (15)O61i—Al1—O71i90.04 (6)
O1—C1—C2107.36 (16)O91—Al1—O7191.21 (5)
O1—C1—H1A110.2O61—Al1—O7190.04 (6)
C2—C1—H1A110.2O61i—Al1—O7190.01 (6)
O1—C1—H1B110.2O71i—Al1—O71177.59 (10)
C2—C1—H1B110.2O91—Al1—O81180.000 (1)
H1A—C1—H1B108.5O61—Al1—O8191.33 (5)
O2—C2—C1109.76 (15)O61i—Al1—O8191.33 (5)
O2—C2—H2A109.7O71i—Al1—O8188.79 (5)
C1—C2—H2A109.7O71—Al1—O8188.79 (5)
O2—C2—H2B109.7Al1—O61—H61A122.9 (16)
C1—C2—H2B109.7Al1—O61—H61B119.9 (15)
H2A—C2—H2B108.2H61A—O61—H61B107 (2)
O2—C3—C4109.12 (15)Al1—O71—H71A121.6 (15)
O2—C3—H3A109.9Al1—O71—H71B118.2 (15)
C4—C3—H3A109.9H71A—O71—H71B106.8 (19)
O2—C3—H3B109.9Al1—O81—H81124.7 (16)
C4—C3—H3B109.9Al1—O91—H91121.4 (15)
H3A—C3—H3B108.3O82—Al2—O82ii180.00 (6)
O3—C4—C3107.17 (15)O82—Al2—O6291.39 (6)
O3—C4—H4A110.3O82ii—Al2—O6288.62 (6)
C3—C4—H4A110.3O82—Al2—O62ii88.62 (6)
O3—C4—H4B110.3O82ii—Al2—O62ii91.38 (6)
C3—C4—H4B110.3O62—Al2—O62ii180.0
H4A—C4—H4B108.5O82—Al2—O7290.19 (6)
O3—C5—C6107.88 (16)O82ii—Al2—O7289.81 (6)
O3—C5—H5A110.1O62—Al2—O7289.40 (6)
C6—C5—H5A110.1O62ii—Al2—O7290.60 (6)
O3—C5—H5B110.1O82—Al2—O72ii89.81 (6)
C6—C5—H5B110.1O82ii—Al2—O72ii90.19 (6)
H5A—C5—H5B108.4O62—Al2—O72ii90.60 (6)
O4—C6—C5109.10 (16)O62ii—Al2—O72ii89.40 (6)
O4—C6—H6A109.9O72—Al2—O72ii180.0
C5—C6—H6A109.9Al2—O62—H62A126.5 (14)
O4—C6—H6B109.9Al2—O62—H62B119.8 (14)
C5—C6—H6B109.9H62A—O62—H62B110.2 (18)
H6A—C6—H6B108.3Al2—O72—H72A121.9 (15)
O4—C7—C8108.08 (16)Al2—O72—H72B132.1 (14)
O4—C7—H7A110.1H72A—O72—H72B105.8 (19)
C8—C7—H7A110.1Al2—O82—H82A128.7 (15)
O4—C7—H7B110.1Al2—O82—H82B118.1 (15)
C8—C7—H7B110.1H82A—O82—H82B110.4 (19)
H7A—C7—H7B108.4O17—N1—O16121.0 (3)
O5—C8—C7113.17 (16)O17—N1—O15120.0 (4)
O5—C8—H8A108.9O16—N1—O15119.0 (2)
C7—C8—H8A108.9O15'—N1'—O16'125.6 (19)
O5—C8—H8B108.9O15'—N1'—O17'117 (2)
C7—C8—H8B108.9O16'—N1'—O17'117 (2)
H8A—C8—H8B107.8O19—N2—O20121.24 (16)
O5—C9—C10107.32 (16)O19—N2—O18120.16 (17)
O5—C9—H9A110.3O20—N2—O18118.60 (16)
C10—C9—H9A110.3O21—N3—O23122.6 (3)
O5—C9—H9B110.3O21—N3—O22120.46 (19)
C10—C9—H9B110.3O23—N3—O22116.9 (2)
H9A—C9—H9B108.5O21'—N3'—O22'125.1 (15)
O1—C10—C9107.99 (15)O21'—N3'—O23'120.5 (16)
O1—C10—H10A110.1O22'—N3'—O23'114.4 (17)
C9—C10—H10A110.1H11A—O11—H11B111 (2)
O1—C10—H10B110.1H12A—O12—H12B98 (2)
C9—C10—H10B110.1H13A—O13—H13B110 (2)
H10A—C10—H10B108.4H14A—O14—H14B111 (2)
O91—Al1—O6188.67 (5)
C10—O1—C1—C2179.84 (15)O3—C5—C6—O467.4 (2)
C3—O2—C2—C1160.82 (16)C6—O4—C7—C8175.15 (16)
O1—C1—C2—O260.0 (2)C9—O5—C8—C784.70 (19)
C2—O2—C3—C4161.00 (16)O4—C7—C8—O563.2 (2)
C5—O3—C4—C3174.91 (15)C8—O5—C9—C10174.16 (15)
O2—C3—C4—O361.96 (19)C1—O1—C10—C9163.96 (15)
C4—O3—C5—C6170.62 (16)O5—C9—C10—O168.02 (18)
C7—O4—C6—C5157.85 (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
Mr = 1351.48Dx = 1.533 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7085 reflections
a = 18.0939 (2) Åθ = 1.0–27.5°
b = 9.4487 (1) ŵ = 0.49 mm1
c = 19.0682 (3) ÅT = 90 K
β = 116.0858 (6)°Block, blue
V = 2927.90 (6) Å30.30 × 0.20 × 0.15 mm
Z = 2
Data collection top
Nonius KappaCCD
diffractometer
6683 independent reflections
Radiation source: fine-focus sealed tube5576 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Detector resolution: 9.1 pixels mm-1θmax = 27.5°, θmin = 2.2°
ω scans at fixed χ = 55°h = 2323
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 1997)
k = 1212
Tmin = 0.879, Tmax = 0.937l = 2424
49028 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.073Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.215H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.119P)2 + 4.6627P]
where P = (Fo2 + 2Fc2)/3
6683 reflections(Δ/σ)max = 0.001
660 parametersΔρmax = 1.38 e Å3
974 restraintsΔρmin = 0.38 e Å3
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.

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 Fo > 4sig(Fo) 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
xyzUiso*/UeqOcc. (<1)
Cr0.21221 (7)0.04104 (13)0.18835 (7)0.0259 (2)0.842 (3)
O1W0.15958 (17)0.0726 (4)0.25907 (17)0.0431 (7)0.842 (3)
H1W10.114 (2)0.111 (6)0.244 (3)0.065*0.842 (3)
H1W20.177 (3)0.061 (6)0.3061 (13)0.065*0.842 (3)
O2W0.1010 (2)0.0278 (4)0.0997 (2)0.0363 (8)0.842 (3)
H2W10.065 (2)0.090 (4)0.090 (3)0.055*0.842 (3)
H2W20.073 (3)0.046 (3)0.091 (3)0.055*0.842 (3)
O3W0.20681 (17)0.2421 (3)0.16525 (19)0.0396 (6)0.842 (3)
H3W10.179 (3)0.280 (5)0.184 (3)0.059*0.842 (3)
H3W20.242 (2)0.299 (4)0.167 (3)0.059*0.842 (3)
O4W0.3189 (3)0.0546 (6)0.2776 (3)0.0409 (10)0.842 (3)
O5W0.21461 (17)0.1615 (3)0.2117 (2)0.0433 (7)0.842 (3)
H5W10.181 (3)0.210 (5)0.220 (3)0.065*0.842 (3)
H5W20.239 (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)
O6W0.12198 (16)0.6872 (3)0.25425 (17)0.0486 (6)
H6W10.079 (2)0.710 (5)0.258 (3)0.073*
H6W20.109 (3)0.610 (3)0.229 (3)0.073*
N10.3155 (2)0.0358 (3)0.10498 (18)0.0378 (7)0.842 (3)
O110.25564 (17)0.0210 (3)0.11578 (17)0.0415 (7)0.842 (3)
O120.34353 (18)0.1494 (3)0.13527 (17)0.0456 (7)0.842 (3)
O130.3396 (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)
O11W0.2414 (14)0.183 (3)0.1272 (13)0.074 (6)*0.158 (3)
N20.2777 (7)0.5472 (13)0.1788 (6)0.0457 (17)0.50
O210.2989 (15)0.4457 (19)0.1463 (13)0.057 (3)0.50
O220.3172 (5)0.6571 (9)0.2028 (5)0.061 (2)0.50
O230.2168 (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
N30.0280 (2)0.3594 (3)0.2056 (2)0.0559 (9)
O310.02816 (16)0.2356 (3)0.23070 (15)0.0479 (6)
O320.0299 (2)0.4357 (3)0.1903 (2)0.0725 (10)
O330.0902 (2)0.3991 (3)0.1979 (3)0.0846 (13)
O1A0.3348 (4)0.0007 (8)0.4502 (4)0.0748 (17)0.50
C1A0.3363 (8)0.1416 (12)0.4438 (9)0.091 (3)0.50
H1A10.28650.17300.39740.110*0.50
H1A20.33550.18600.49050.110*0.50
C2A0.4140 (8)0.1904 (11)0.4361 (7)0.073 (3)0.50
H2A10.46420.16010.48230.088*0.50
H2A20.41470.29490.43230.088*0.50
O2A0.4116 (5)0.1302 (10)0.3702 (5)0.078 (2)0.50
C3A0.4936 (9)0.1271 (19)0.3757 (10)0.091 (4)0.50
H3A10.50530.21740.35620.110*0.50
H3A20.53420.11560.43090.110*0.50
C4A0.5012 (6)0.0034 (15)0.3269 (7)0.084 (3)0.50
H4A10.55600.00500.32710.101*0.50
H4A20.45870.01170.27220.101*0.50
O3A0.4903 (5)0.1299 (12)0.3614 (5)0.092 (2)0.50
C5A0.4894 (10)0.2408 (16)0.3156 (8)0.085 (3)0.50
H5A10.45360.22040.25980.102*0.50
H5A20.54560.26230.32200.102*0.50
C6A0.4560 (6)0.3606 (12)0.3436 (6)0.072 (2)0.50
H6A10.49300.37800.39930.086*0.50
H6A20.45600.44690.31410.086*0.50
O4A0.3748 (6)0.3378 (10)0.3354 (6)0.083 (2)0.50
C7A0.3625 (8)0.4182 (14)0.3885 (7)0.079 (3)0.50
H7A10.37190.51970.38240.094*0.50
H7A20.39920.38840.44250.094*0.50
C8A0.2747 (7)0.3903 (10)0.3692 (6)0.070 (2)0.50
H8A10.25800.45770.39940.084*0.50
H8A20.24130.41210.31320.084*0.50
O5A0.2543 (4)0.2566 (7)0.3828 (4)0.0613 (14)0.50
C9A0.2787 (11)0.2182 (14)0.4595 (8)0.071 (3)0.50
H9A10.24600.26920.48160.085*0.50
H9A20.33770.24030.49130.085*0.50
C10A0.2640 (10)0.0589 (14)0.4585 (9)0.072 (3)0.50
H10A0.26340.02710.50770.087*0.50
H10B0.21150.03170.41390.087*0.50
O1B0.2601 (4)0.0384 (8)0.4046 (3)0.0703 (17)0.50
C1B0.2854 (8)0.1743 (12)0.4237 (6)0.098 (3)0.50
H1B10.25270.23470.37810.118*0.50
H1B20.27190.20340.46660.118*0.50
C2B0.3736 (8)0.2055 (15)0.4482 (7)0.094 (4)0.50
H2B10.40890.14720.49390.113*0.50
H2B20.38550.30670.46200.113*0.50
O2B0.3868 (6)0.1731 (11)0.3862 (6)0.097 (3)0.50
C3B0.4730 (7)0.1950 (12)0.4088 (7)0.090 (3)0.50
H3B10.48370.29740.40710.108*0.50
H3B20.50530.16170.46310.108*0.50
C4B0.5003 (11)0.1158 (18)0.3548 (10)0.097 (4)0.50
H4B10.55580.14670.36320.117*0.50
H4B20.46140.13250.29940.117*0.50
O3B0.5008 (4)0.0270 (11)0.3740 (4)0.0747 (19)0.50
C5B0.5085 (6)0.1196 (15)0.3193 (6)0.078 (3)0.50
H5B10.47080.09100.26530.094*0.50
H5B20.56560.11920.32510.094*0.50
C6B0.4857 (9)0.2654 (18)0.3375 (9)0.095 (4)0.50
H6B10.52360.29030.39200.114*0.50
H6B20.49360.33570.30290.114*0.50
O4B0.4066 (6)0.2741 (9)0.3282 (5)0.087 (2)0.50
C7B0.3962 (8)0.3902 (11)0.3682 (7)0.077 (3)0.50
H7B10.38690.47710.33640.093*0.50
H7B20.44590.40410.41810.093*0.50
C8B0.3208 (10)0.3594 (13)0.3837 (9)0.102 (4)0.50
H8B10.31200.44010.41220.122*0.50
H8B20.27130.35020.33310.122*0.50
O5B0.3308 (5)0.2337 (8)0.4278 (4)0.083 (2)0.50
C9B0.2684 (13)0.1997 (16)0.4461 (11)0.087 (4)0.50
H9B10.21470.21150.39980.104*0.50
H9B20.26940.26270.48810.104*0.50
C10B0.2794 (9)0.0473 (14)0.4733 (8)0.072 (3)0.50
H10C0.33670.03030.51260.086*0.50
H10D0.24190.02440.49700.086*0.50
O1C0.0064 (8)0.1939 (14)0.0617 (8)0.036 (4)*0.25
C1C0.0247 (9)0.3044 (12)0.0223 (8)0.030 (3)*0.25
H1C10.02700.34500.01800.036*0.25
H1C20.05490.38040.05970.036*0.25
C2C0.0770 (8)0.2479 (14)0.0161 (8)0.029 (2)*0.25
H2C10.13330.22840.02470.035*0.25
H2C20.08100.32120.05140.035*0.25
O2C0.0452 (5)0.1282 (11)0.0574 (5)0.0272 (17)*0.25
C3C0.1039 (6)0.0574 (13)0.0782 (7)0.025 (2)*0.25
H3C10.10620.10570.12330.030*0.25
H3C20.15940.06050.03380.030*0.25
C4C0.0766 (9)0.0971 (14)0.0994 (7)0.029 (3)*0.25
H4C10.10870.14200.12420.035*0.25
H4C20.01760.10090.13670.035*0.25
O3C0.0903 (5)0.1702 (10)0.0291 (5)0.0330 (17)*0.25
C5C0.0661 (7)0.3116 (13)0.0406 (8)0.039 (3)*0.25
H5C10.07340.34980.08550.046*0.25
H5C20.10140.36710.00630.046*0.25
C6C0.0234 (8)0.3268 (14)0.0561 (8)0.038 (3)*0.25
H6C10.04030.42720.06700.045*0.25
H6C20.05870.27040.10260.045*0.25
O4C0.0346 (8)0.2808 (11)0.0084 (6)0.037 (2)*0.25
C7C0.1155 (8)0.2741 (13)0.0053 (7)0.035 (2)*0.25
H7C10.14920.24280.05980.042*0.25
H7C20.13430.36970.00060.042*0.25
C8C0.1279 (8)0.1749 (13)0.0490 (8)0.033 (3)*0.25
H8C10.09050.20130.10350.039*0.25
H8C20.18510.18380.04240.039*0.25
O5C0.1128 (6)0.0309 (9)0.0358 (6)0.035 (2)*0.25
C9C0.0823 (9)0.0599 (15)0.1006 (8)0.021 (3)*0.25
H9C10.12250.06800.12270.025*0.25
H9C20.03010.02220.14150.025*0.25
C10C0.0678 (12)0.2049 (17)0.0734 (13)0.032 (4)*0.25
H10E0.06060.27770.11320.039*0.25
H10F0.11540.23190.02400.039*0.25
O1D0.0071 (8)0.1848 (13)0.0591 (8)0.031 (3)*0.25
C1D0.0030 (9)0.3134 (13)0.0264 (9)0.029 (3)*0.25
H1D10.04800.33840.02050.034*0.25
H1D20.01680.39140.06480.034*0.25
C2D0.0750 (11)0.286 (2)0.0042 (13)0.036 (4)*0.25
H2D10.12480.25610.05090.043*0.25
H2D20.08820.37450.01610.043*0.25
O2D0.0519 (6)0.1851 (12)0.0505 (5)0.0329 (19)*0.25
C3D0.1180 (8)0.1349 (17)0.0661 (8)0.034 (3)*0.25
H3D10.12680.20000.10240.041*0.25
H3D20.16950.13020.01700.041*0.25
C4D0.0952 (11)0.0111 (16)0.1021 (10)0.043 (4)*0.25
H4D10.13550.04140.12120.051*0.25
H4D20.04020.00730.14740.051*0.25
O3D0.0940 (6)0.1104 (12)0.0475 (6)0.044 (2)*0.25
C5D0.0499 (11)0.2330 (16)0.0836 (9)0.045 (4)*0.25
H5D10.00650.20700.12210.055*0.25
H5D20.07730.28170.11170.055*0.25
C6D0.0457 (12)0.3293 (18)0.0239 (10)0.062 (4)*0.25
H6D10.10190.36510.00890.075*0.25
H6D20.01140.41180.05140.075*0.25
O4D0.0152 (10)0.2743 (16)0.0246 (8)0.078 (4)*0.25
C7D0.0686 (13)0.290 (3)0.007 (2)0.063 (7)*0.25
H7D10.09330.26110.06260.076*0.25
H7D20.08240.39030.00440.076*0.25
C8D0.1042 (11)0.2001 (14)0.0363 (10)0.049 (3)*0.25
H8D10.07860.22760.09210.059*0.25
H8D20.16410.21840.01490.059*0.25
O5D0.0910 (8)0.0528 (11)0.0301 (7)0.047 (3)*0.25
C9D0.0969 (14)0.0313 (18)0.0862 (12)0.046 (5)*0.25
H9D10.15280.02370.08310.056*0.25
H9D20.05670.00020.13870.056*0.25
C10D0.0795 (10)0.1837 (16)0.0728 (13)0.036 (4)*0.25
H10G0.07010.24200.11910.043*0.25
H10H0.12700.22350.02710.043*0.25
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr0.0228 (5)0.0243 (3)0.0281 (4)0.0040 (3)0.0088 (3)0.0031 (2)
O1W0.0303 (13)0.0621 (19)0.0384 (14)0.0053 (12)0.0165 (11)0.0004 (13)
O2W0.0285 (17)0.0413 (18)0.0319 (17)0.0057 (12)0.0065 (15)0.0020 (13)
O3W0.0396 (14)0.0206 (12)0.0627 (18)0.0048 (10)0.0263 (13)0.0038 (11)
O4W0.0318 (16)0.053 (3)0.0314 (17)0.0167 (19)0.0076 (11)0.0128 (19)
O5W0.0358 (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)
O6W0.0524 (15)0.0360 (13)0.0661 (17)0.0029 (11)0.0341 (13)0.0040 (11)
N10.0397 (17)0.0414 (18)0.0316 (15)0.0125 (13)0.0152 (13)0.0035 (13)
O110.0362 (14)0.0474 (16)0.0403 (15)0.0061 (12)0.0162 (12)0.0133 (12)
O120.0507 (17)0.0401 (15)0.0495 (16)0.0038 (13)0.0254 (14)0.0026 (13)
O130.075 (3)0.066 (3)0.044 (2)0.031 (2)0.035 (2)0.0024 (18)
N20.047 (3)0.0290 (15)0.077 (5)0.0067 (15)0.042 (3)0.012 (3)
O210.066 (5)0.028 (3)0.096 (8)0.017 (2)0.054 (6)0.021 (4)
O220.051 (4)0.032 (3)0.102 (6)0.000 (2)0.037 (5)0.012 (4)
O230.106 (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)
N30.084 (2)0.0365 (16)0.073 (2)0.0181 (16)0.058 (2)0.0217 (15)
O310.0590 (15)0.0430 (13)0.0533 (14)0.0160 (11)0.0352 (13)0.0082 (11)
O320.100 (3)0.0438 (16)0.106 (3)0.0012 (16)0.075 (2)0.0059 (16)
O330.114 (3)0.0328 (14)0.164 (4)0.0137 (16)0.113 (3)0.0107 (18)
O1A0.072 (4)0.079 (4)0.065 (4)0.005 (3)0.022 (3)0.006 (3)
C1A0.080 (6)0.073 (6)0.089 (6)0.015 (5)0.008 (5)0.008 (6)
C2A0.095 (7)0.040 (4)0.064 (5)0.013 (5)0.016 (5)0.005 (4)
O2A0.071 (5)0.072 (5)0.059 (4)0.032 (4)0.002 (3)0.016 (4)
C3A0.066 (6)0.123 (7)0.059 (7)0.047 (6)0.004 (5)0.018 (6)
C4A0.048 (4)0.143 (7)0.060 (5)0.014 (6)0.022 (4)0.024 (6)
O3A0.059 (4)0.142 (6)0.048 (4)0.039 (5)0.002 (3)0.005 (5)
C5A0.086 (6)0.123 (7)0.049 (6)0.053 (6)0.033 (5)0.002 (6)
C6A0.073 (5)0.081 (5)0.061 (4)0.051 (4)0.028 (4)0.008 (4)
O4A0.126 (6)0.053 (5)0.076 (5)0.017 (4)0.050 (4)0.014 (4)
C7A0.091 (7)0.069 (6)0.066 (6)0.022 (5)0.026 (5)0.021 (5)
C8A0.080 (6)0.057 (5)0.067 (5)0.017 (5)0.027 (5)0.025 (4)
O5A0.060 (3)0.067 (3)0.057 (3)0.011 (3)0.026 (3)0.010 (3)
C9A0.046 (5)0.097 (6)0.057 (5)0.012 (5)0.013 (4)0.029 (5)
C10A0.076 (7)0.114 (6)0.036 (5)0.011 (5)0.033 (5)0.008 (5)
O1B0.064 (3)0.105 (5)0.036 (3)0.036 (3)0.016 (3)0.008 (3)
C1B0.099 (7)0.099 (7)0.048 (5)0.041 (6)0.012 (5)0.027 (5)
C2B0.104 (8)0.063 (6)0.063 (5)0.014 (6)0.010 (6)0.025 (5)
O2B0.092 (6)0.070 (5)0.061 (5)0.015 (4)0.027 (4)0.010 (4)
C3B0.081 (6)0.064 (5)0.077 (6)0.028 (5)0.011 (5)0.008 (5)
C4B0.071 (6)0.138 (8)0.066 (8)0.052 (6)0.014 (5)0.019 (6)
O3B0.047 (3)0.128 (6)0.040 (3)0.007 (4)0.011 (3)0.016 (4)
C5B0.045 (4)0.146 (7)0.043 (4)0.027 (5)0.019 (3)0.002 (6)
C6B0.086 (6)0.132 (7)0.054 (7)0.052 (6)0.020 (5)0.007 (7)
O4B0.096 (5)0.056 (4)0.071 (4)0.040 (4)0.002 (4)0.001 (4)
C7B0.103 (7)0.042 (5)0.062 (5)0.013 (5)0.015 (5)0.031 (4)
C8B0.111 (7)0.064 (6)0.096 (6)0.006 (6)0.014 (6)0.017 (5)
O5B0.082 (4)0.067 (4)0.073 (4)0.006 (3)0.010 (3)0.021 (3)
C9B0.066 (7)0.113 (7)0.071 (7)0.024 (6)0.021 (6)0.018 (6)
C10B0.051 (5)0.127 (7)0.037 (6)0.025 (5)0.020 (4)0.009 (5)
Geometric parameters (Å, º) top
Cr—O4W1.936 (5)C5B—C6B1.521 (17)
Cr—O3W1.943 (3)C5B—H5B10.9900
Cr—O111.958 (3)C5B—H5B20.9900
Cr—O5W1.960 (3)C6B—O4B1.366 (15)
Cr—O2W1.983 (4)C6B—H6B10.9900
Cr—O1W1.986 (3)C6B—H6B20.9900
O1W—H1W10.832 (19)O4B—C7B1.395 (12)
O1W—H1W20.817 (19)C7B—C8B1.545 (16)
O2W—H2W10.834 (19)C7B—H7B10.9900
O2W—H2W20.832 (19)C7B—H7B20.9900
O3W—H3W10.817 (19)C8B—O5B1.420 (12)
O3W—H3W20.818 (19)C8B—H8B10.9900
O5W—H5W10.819 (19)C8B—H8B20.9900
O5W—H5W20.819 (19)O5B—C9B1.361 (15)
Cr'—O1W'1.72 (2)C9B—C10B1.513 (14)
Cr'—O5W'1.93 (3)C9B—H9B10.9900
Cr'—O2W'1.94 (2)C9B—H9B20.9900
Cr'—O3W'1.98 (2)C10B—H10C0.9900
Cr'—O4W'2.16 (3)C10B—H10D0.9900
Cr'—O11W2.20 (2)O1C—C1C1.407 (12)
O2W'—H2W10.76 (4)O1C—C10C1.459 (14)
O2W'—H2W20.77 (4)C1C—C2C1.526 (16)
O6W—H6W10.847 (19)C1C—H1C10.9900
O6W—H6W20.849 (19)C1C—H1C20.9900
N1—O121.218 (4)C2C—O2C1.353 (14)
N1—O131.230 (4)C2C—H2C10.9900
N1—O111.304 (4)C2C—H2C20.9900
N1'—O13'1.210 (18)O2C—C3C1.451 (11)
N1'—O12'1.240 (17)C3C—C4C1.537 (16)
N1'—O11'1.268 (17)C3C—H3C10.9900
N2—O231.181 (10)C3C—H3C20.9900
N2—O221.229 (10)C4C—O3C1.429 (14)
N2—O211.289 (11)C4C—H4C10.9900
N2'—O23'1.186 (10)C4C—H4C20.9900
N2'—O22'1.224 (10)O3C—C5C1.393 (13)
N2'—O21'1.280 (11)C5C—C6C1.521 (15)
N3—O321.197 (5)C5C—H5C10.9900
N3—O331.254 (4)C5C—H5C20.9900
N3—O311.263 (4)C6C—O4C1.399 (13)
O1A—C1A1.351 (12)C6C—H6C10.9900
O1A—C10A1.466 (13)C6C—H6C20.9900
C1A—C2A1.548 (15)O4C—C7C1.370 (13)
C1A—H1A10.9900C7C—C8C1.487 (15)
C1A—H1A20.9900C7C—H7C10.9900
C2A—O2A1.362 (13)C7C—H7C20.9900
C2A—H2A10.9900C8C—O5C1.432 (12)
C2A—H2A20.9900C8C—H8C10.9900
O2A—C3A1.441 (15)C8C—H8C20.9900
C3A—C4A1.537 (18)O5C—C9C1.403 (14)
C3A—H3A10.9900C9C—C10C1.528 (15)
C3A—H3A20.9900C9C—H9C10.9900
C4A—O3A1.474 (14)C9C—H9C20.9900
C4A—H4A10.9900C10C—H10E0.9900
C4A—H4A20.9900C10C—H10F0.9900
O3A—C5A1.360 (14)O1D—C1D1.414 (12)
C5A—C6A1.488 (16)O1D—C10D1.443 (13)
C5A—H5A10.9900C1D—C2D1.558 (17)
C5A—H5A20.9900C1D—H1D10.9900
C6A—O4A1.424 (12)C1D—H1D20.9900
C6A—H6A10.9900C2D—O2D1.341 (16)
C6A—H6A20.9900C2D—H2D10.9900
O4A—C7A1.359 (12)C2D—H2D20.9900
C7A—C8A1.489 (14)O2D—C3D1.434 (12)
C7A—H7A10.9900C3D—C4D1.515 (17)
C7A—H7A20.9900C3D—H3D10.9900
C8A—O5A1.372 (10)C3D—H3D20.9900
C8A—H8A10.9900C4D—O3D1.409 (15)
C8A—H8A20.9900C4D—H4D10.9900
O5A—C9A1.378 (13)C4D—H4D20.9900
C9A—C10A1.527 (13)O3D—C5D1.404 (15)
C9A—H9A10.9900C5D—C6D1.485 (16)
C9A—H9A20.9900C5D—H5D10.9900
C10A—H10A0.9900C5D—H5D20.9900
C10A—H10B0.9900C6D—O4D1.372 (15)
O1B—C1B1.359 (11)C6D—H6D10.9900
O1B—C10B1.447 (13)C6D—H6D20.9900
C1B—C2B1.482 (15)O4D—C7D1.371 (17)
C1B—H1B10.9900C7D—C8D1.510 (18)
C1B—H1B20.9900C7D—H7D10.9900
C2B—O2B1.340 (14)C7D—H7D20.9900
C2B—H2B10.9900C8D—O5D1.426 (13)
C2B—H2B20.9900C8D—H8D10.9900
O2B—C3B1.439 (13)C8D—H8D20.9900
C3B—C4B1.521 (18)O5D—C9D1.374 (15)
C3B—H3B10.9900C9D—C10D1.520 (15)
C3B—H3B20.9900C9D—H9D10.9900
C4B—O3B1.397 (16)C9D—H9D20.9900
C4B—H4B10.9900C10D—H10G0.9900
C4B—H4B20.9900C10D—H10H0.9900
O3B—C5B1.414 (12)
O4W—Cr—O3W93.78 (19)H5B1—C5B—H5B2108.8
O4W—Cr—O1194.97 (17)O4B—C6B—C5B113.5 (12)
O3W—Cr—O1197.38 (13)O4B—C6B—H6B1108.9
O4W—Cr—O5W87.20 (19)C5B—C6B—H6B1108.9
O3W—Cr—O5W178.39 (13)O4B—C6B—H6B2108.9
O11—Cr—O5W83.80 (14)C5B—C6B—H6B2108.9
O4W—Cr—O2W177.8 (2)H6B1—C6B—H6B2107.7
O3W—Cr—O2W86.40 (15)C6B—O4B—C7B111.2 (9)
O11—Cr—O2W87.20 (17)O4B—C7B—C8B107.3 (9)
O5W—Cr—O2W92.57 (15)O4B—C7B—H7B1110.2
O4W—Cr—O1W89.04 (17)C8B—C7B—H7B1110.2
O3W—Cr—O1W90.91 (14)O4B—C7B—H7B2110.2
O11—Cr—O1W170.51 (14)C8B—C7B—H7B2110.2
O5W—Cr—O1W87.82 (14)H7B1—C7B—H7B2108.5
O2W—Cr—O1W88.74 (16)O5B—C8B—C7B112.2 (11)
Cr—O1W—H1W1122 (3)O5B—C8B—H8B1109.2
Cr—O1W—H1W2131 (4)C7B—C8B—H8B1109.2
H1W1—O1W—H1W2107 (4)O5B—C8B—H8B2109.2
Cr—O2W—H2W1123 (3)C7B—C8B—H8B2109.2
Cr—O2W—H2W2121 (3)H8B1—C8B—H8B2107.9
H2W1—O2W—H2W2101 (3)C9B—O5B—C8B116.4 (10)
Cr—O3W—H3W1108 (4)O5B—C9B—C10B108.2 (14)
Cr—O3W—H3W2132 (4)O5B—C9B—H9B1110.1
H3W1—O3W—H3W2108 (4)C10B—C9B—H9B1110.1
Cr—O5W—H5W1130 (4)O5B—C9B—H9B2110.1
Cr—O5W—H5W2117 (4)C10B—C9B—H9B2110.1
H5W1—O5W—H5W2108 (4)H9B1—C9B—H9B2108.4
O1W'—Cr'—O5W'94.8 (11)O1B—C10B—C9B106.2 (12)
O1W'—Cr'—O2W'89.3 (10)O1B—C10B—H10C110.5
O5W'—Cr'—O2W'91.7 (11)C9B—C10B—H10C110.5
O1W'—Cr'—O3W'97.6 (11)O1B—C10B—H10D110.5
O5W'—Cr'—O3W'167.5 (11)C9B—C10B—H10D110.5
O2W'—Cr'—O3W'90.2 (9)H10C—C10B—H10D108.7
O1W'—Cr'—O4W'95.4 (11)C1C—O1C—C10C118.5 (12)
O5W'—Cr'—O4W'85.0 (11)O1C—C1C—C2C109.7 (10)
O2W'—Cr'—O4W'174.4 (11)O1C—C1C—H1C1109.7
O3W'—Cr'—O4W'92.1 (10)C2C—C1C—H1C1109.7
O1W'—Cr'—O11W174.0 (10)O1C—C1C—H1C2109.7
O5W'—Cr'—O11W88.3 (11)C2C—C1C—H1C2109.7
O2W'—Cr'—O11W95.8 (9)H1C1—C1C—H1C2108.2
O3W'—Cr'—O11W79.2 (10)O2C—C2C—C1C112.1 (10)
O4W'—Cr'—O11W79.7 (10)O2C—C2C—H2C1109.2
Cr'—O2W'—H2W1118 (4)C1C—C2C—H2C1109.2
Cr'—O2W'—H2W2121 (4)O2C—C2C—H2C2109.2
H2W1—O2W'—H2W2115 (5)C1C—C2C—H2C2109.2
Cr'—O3W'—H5W296.4 (15)H2C1—C2C—H2C2107.9
Cr'—O5W'—H1W179 (2)C2C—O2C—C3C111.7 (9)
Cr'—O5W'—H3W187 (2)O2C—C3C—C4C108.7 (9)
H1W1—O5W'—H3W1143 (4)O2C—C3C—H3C1109.9
H6W1—O6W—H6W2104 (3)C4C—C3C—H3C1109.9
O12—N1—O13123.4 (4)O2C—C3C—H3C2109.9
O12—N1—O11119.3 (3)C4C—C3C—H3C2109.9
O13—N1—O11117.3 (4)H3C1—C3C—H3C2108.3
N1—O11—Cr127.4 (2)O3C—C4C—C3C108.0 (10)
O13'—N1'—O12'124 (2)O3C—C4C—H4C1110.1
O13'—N1'—O11'119 (2)C3C—C4C—H4C1110.1
O12'—N1'—O11'116.3 (18)O3C—C4C—H4C2110.1
Cr'—O11W—H3W293.3 (19)C3C—C4C—H4C2110.1
O23—N2—O22116.3 (12)H4C1—C4C—H4C2108.4
O23—N2—O21119.7 (15)C5C—O3C—C4C113.8 (10)
O22—N2—O21124.0 (15)O3C—C5C—C6C110.9 (10)
O23'—N2'—O22'116.5 (12)O3C—C5C—H5C1109.5
O23'—N2'—O21'121.2 (15)C6C—C5C—H5C1109.5
O22'—N2'—O21'122.4 (15)O3C—C5C—H5C2109.5
O32—N3—O33121.6 (4)C6C—C5C—H5C2109.5
O32—N3—O31120.4 (3)H5C1—C5C—H5C2108.1
O33—N3—O31118.0 (4)O4C—C6C—C5C110.7 (12)
C1A—O1A—C10A115.8 (9)O4C—C6C—H6C1109.5
O1A—C1A—C2A111.1 (9)C5C—C6C—H6C1109.5
O1A—C1A—H1A1109.4O4C—C6C—H6C2109.5
C2A—C1A—H1A1109.4C5C—C6C—H6C2109.5
O1A—C1A—H1A2109.4H6C1—C6C—H6C2108.1
C2A—C1A—H1A2109.4C7C—O4C—C6C113.6 (11)
H1A1—C1A—H1A2108.0O4C—C7C—C8C111.9 (11)
O2A—C2A—C1A107.6 (9)O4C—C7C—H7C1109.2
O2A—C2A—H2A1110.2C8C—C7C—H7C1109.2
C1A—C2A—H2A1110.2O4C—C7C—H7C2109.2
O2A—C2A—H2A2110.2C8C—C7C—H7C2109.2
C1A—C2A—H2A2110.2H7C1—C7C—H7C2107.9
H2A1—C2A—H2A2108.5O5C—C8C—C7C112.1 (11)
C2A—O2A—C3A109.2 (9)O5C—C8C—H8C1109.2
O2A—C3A—C4A109.6 (11)C7C—C8C—H8C1109.2
O2A—C3A—H3A1109.8O5C—C8C—H8C2109.2
C4A—C3A—H3A1109.8C7C—C8C—H8C2109.2
O2A—C3A—H3A2109.8H8C1—C8C—H8C2107.9
C4A—C3A—H3A2109.8C9C—O5C—C8C117.2 (11)
H3A1—C3A—H3A2108.2O5C—C9C—C10C108.0 (12)
O3A—C4A—C3A108.3 (10)O5C—C9C—H9C1110.1
O3A—C4A—H4A1110.0C10C—C9C—H9C1110.1
C3A—C4A—H4A1110.0O5C—C9C—H9C2110.1
O3A—C4A—H4A2110.0C10C—C9C—H9C2110.1
C3A—C4A—H4A2110.0H9C1—C9C—H9C2108.4
H4A1—C4A—H4A2108.4O1C—C10C—C9C107.2 (11)
C5A—O3A—C4A109.8 (10)O1C—C10C—H10E110.3
O3A—C5A—C6A104.4 (10)C9C—C10C—H10E110.3
O3A—C5A—H5A1110.9O1C—C10C—H10F110.3
C6A—C5A—H5A1110.9C9C—C10C—H10F110.3
O3A—C5A—H5A2110.9H10E—C10C—H10F108.5
C6A—C5A—H5A2110.9C1D—O1D—C10D113.0 (11)
H5A1—C5A—H5A2108.9O1D—C1D—C2D105.4 (12)
O4A—C6A—C5A114.1 (9)O1D—C1D—H1D1110.7
O4A—C6A—H6A1108.7C2D—C1D—H1D1110.7
C5A—C6A—H6A1108.7O1D—C1D—H1D2110.7
O4A—C6A—H6A2108.7C2D—C1D—H1D2110.7
C5A—C6A—H6A2108.7H1D1—C1D—H1D2108.8
H6A1—C6A—H6A2107.6O2D—C2D—C1D108.4 (12)
C7A—O4A—C6A109.4 (9)O2D—C2D—H2D1110.0
O4A—C7A—C8A102.9 (8)C1D—C2D—H2D1110.0
O4A—C7A—H7A1111.2O2D—C2D—H2D2110.0
C8A—C7A—H7A1111.2C1D—C2D—H2D2110.0
O4A—C7A—H7A2111.2H2D1—C2D—H2D2108.4
C8A—C7A—H7A2111.2C2D—O2D—C3D113.2 (12)
H7A1—C7A—H7A2109.1O2D—C3D—C4D108.0 (12)
O5A—C8A—C7A117.5 (10)O2D—C3D—H3D1110.1
O5A—C8A—H8A1107.9C4D—C3D—H3D1110.1
C7A—C8A—H8A1107.9O2D—C3D—H3D2110.1
O5A—C8A—H8A2107.9C4D—C3D—H3D2110.1
C7A—C8A—H8A2107.9H3D1—C3D—H3D2108.4
H8A1—C8A—H8A2107.2O3D—C4D—C3D111.2 (12)
C8A—O5A—C9A117.1 (8)O3D—C4D—H4D1109.4
O5A—C9A—C10A105.9 (11)C3D—C4D—H4D1109.4
O5A—C9A—H9A1110.6O3D—C4D—H4D2109.4
C10A—C9A—H9A1110.6C3D—C4D—H4D2109.4
O5A—C9A—H9A2110.6H4D1—C4D—H4D2108.0
C10A—C9A—H9A2110.6C5D—O3D—C4D112.2 (11)
H9A1—C9A—H9A2108.7O3D—C5D—C6D109.9 (13)
O1A—C10A—C9A102.4 (12)O3D—C5D—H5D1109.7
O1A—C10A—H10A111.3C6D—C5D—H5D1109.7
C9A—C10A—H10A111.3O3D—C5D—H5D2109.7
O1A—C10A—H10B111.3C6D—C5D—H5D2109.7
C9A—C10A—H10B111.3H5D1—C5D—H5D2108.2
H10A—C10A—H10B109.2O4D—C6D—C5D117.1 (14)
C1B—O1B—C10B111.5 (8)O4D—C6D—H6D1108.0
O1B—C1B—C2B117.5 (10)C5D—C6D—H6D1108.0
O1B—C1B—H1B1107.9O4D—C6D—H6D2108.0
C2B—C1B—H1B1107.9C5D—C6D—H6D2108.0
O1B—C1B—H1B2107.9H6D1—C6D—H6D2107.3
C2B—C1B—H1B2107.9C7D—O4D—C6D111.0 (15)
H1B1—C1B—H1B2107.2O4D—C7D—C8D110.8 (16)
O2B—C2B—C1B105.1 (9)O4D—C7D—H7D1109.5
O2B—C2B—H2B1110.7C8D—C7D—H7D1109.5
C1B—C2B—H2B1110.7O4D—C7D—H7D2109.5
O2B—C2B—H2B2110.7C8D—C7D—H7D2109.5
C1B—C2B—H2B2110.7H7D1—C7D—H7D2108.1
H2B1—C2B—H2B2108.8O5D—C8D—C7D111.9 (17)
C2B—O2B—C3B107.0 (10)O5D—C8D—H8D1109.2
O2B—C3B—C4B111.0 (11)C7D—C8D—H8D1109.2
O2B—C3B—H3B1109.4O5D—C8D—H8D2109.2
C4B—C3B—H3B1109.4C7D—C8D—H8D2109.2
O2B—C3B—H3B2109.4H8D1—C8D—H8D2107.9
C4B—C3B—H3B2109.4C9D—O5D—C8D115.2 (12)
H3B1—C3B—H3B2108.0O5D—C9D—C10D108.9 (13)
O3B—C4B—C3B105.3 (11)O5D—C9D—H9D1109.9
O3B—C4B—H4B1110.7C10D—C9D—H9D1109.9
C3B—C4B—H4B1110.7O5D—C9D—H9D2109.9
O3B—C4B—H4B2110.7C10D—C9D—H9D2109.9
C3B—C4B—H4B2110.7H9D1—C9D—H9D2108.3
H4B1—C4B—H4B2108.8O1D—C10D—C9D108.0 (12)
C4B—O3B—C5B113.3 (10)O1D—C10D—H10G110.1
O3B—C5B—C6B105.6 (10)C9D—C10D—H10G110.1
O3B—C5B—H5B1110.6O1D—C10D—H10H110.1
C6B—C5B—H5B1110.6C9D—C10D—H10H110.1
O3B—C5B—H5B2110.6H10G—C10D—H10H108.4
C6B—C5B—H5B2110.6
O12—N1—O11—Cr9.2 (5)C8B—O5B—C9B—C10B165.2 (12)
O13—N1—O11—Cr172.2 (3)C1B—O1B—C10B—C9B166.1 (12)
O4W—Cr—O11—N149.2 (3)O5B—C9B—C10B—O1B71.3 (17)
O3W—Cr—O11—N145.3 (3)C10C—O1C—C1C—C2C154.2 (15)
O5W—Cr—O11—N1135.8 (3)O1C—C1C—C2C—O2C48.6 (16)
O2W—Cr—O11—N1131.3 (3)C1C—C2C—O2C—C3C166.6 (10)
O1W—Cr—O11—N1163.9 (7)C2C—O2C—C3C—C4C161.2 (10)
C10A—O1A—C1A—C2A179.5 (11)O2C—C3C—C4C—O3C71.4 (12)
O1A—C1A—C2A—O2A60.7 (14)C3C—C4C—O3C—C5C178.5 (9)
C1A—C2A—O2A—C3A158.5 (11)C4C—O3C—C5C—C6C89.3 (13)
C2A—O2A—C3A—C4A152.7 (11)O3C—C5C—C6C—O4C62.4 (14)
O2A—C3A—C4A—O3A64.0 (14)C5C—C6C—O4C—C7C171.9 (10)
C3A—C4A—O3A—C5A174.6 (11)C6C—O4C—C7C—C8C157.2 (11)
C4A—O3A—C5A—C6A165.2 (9)O4C—C7C—C8C—O5C67.2 (14)
O3A—C5A—C6A—O4A61.1 (13)C7C—C8C—O5C—C9C149.0 (12)
C5A—C6A—O4A—C7A155.1 (11)C8C—O5C—C9C—C10C177.8 (11)
C6A—O4A—C7A—C8A176.4 (9)C1C—O1C—C10C—C9C167.8 (14)
O4A—C7A—C8A—O5A67.4 (13)O5C—C9C—C10C—O1C74.8 (17)
C7A—C8A—O5A—C9A72.7 (13)C10D—O1D—C1D—C2D171.5 (14)
C8A—O5A—C9A—C10A169.0 (10)O1D—C1D—C2D—O2D63 (2)
C1A—O1A—C10A—C9A177.0 (11)C1D—C2D—O2D—C3D170.2 (13)
O5A—C9A—C10A—O1A78.5 (14)C2D—O2D—C3D—C4D158.1 (16)
C10B—O1B—C1B—C2B80.2 (13)O2D—C3D—C4D—O3D68.2 (15)
O1B—C1B—C2B—O2B61.8 (14)C3D—C4D—O3D—C5D161.8 (13)
C1B—C2B—O2B—C3B177.1 (10)C4D—O3D—C5D—C6D176.1 (14)
C2B—O2B—C3B—C4B160.6 (12)O3D—C5D—C6D—O4D54 (2)
O2B—C3B—C4B—O3B72.3 (14)C5D—C6D—O4D—C7D89 (3)
C3B—C4B—O3B—C5B167.9 (10)C6D—O4D—C7D—C8D167 (2)
C4B—O3B—C5B—C6B165.7 (11)O4D—C7D—C8D—O5D63 (3)
O3B—C5B—C6B—O4B62.2 (13)C7D—C8D—O5D—C9D160.0 (19)
C5B—C6B—O4B—C7B160.9 (11)C8D—O5D—C9D—C10D178.8 (15)
C6B—O4B—C7B—C8B157.0 (11)C1D—O1D—C10D—C9D164.7 (15)
O4B—C7B—C8B—O5B58.6 (14)O5D—C9D—C10D—O1D46 (2)
C7B—C8B—O5B—C9B178.3 (12)
(4) top
Crystal data top
C10H20O5·H4N2O8PdZ = 2
Mr = 486.71F(000) = 496
Triclinic, P1Dx = 1.839 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.4649 (1) ÅCell parameters from 3994 reflections
b = 9.5487 (1) Åθ = 1.0–27.5°
c = 13.3944 (2) ŵ = 1.13 mm1
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 tube3440 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Detector resolution: 9.1 pixels mm-1θmax = 27.5°, θmin = 1.6°
ω scans at fixed χ = 55°h = 99
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 1997)
k = 1212
Tmin = 0.849, Tmax = 0.972l = 1717
21461 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.052H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.015P)2 + 0.7189P]
where P = (Fo2 + 2Fc2)/3
4016 reflections(Δ/σ)max < 0.001
251 parametersΔρmax = 0.83 e Å3
6 restraintsΔρmin = 0.80 e Å3
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O10.44978 (18)0.84124 (14)0.21893 (10)0.0138 (3)
O20.10662 (17)0.94188 (14)0.29899 (9)0.0132 (3)
O30.00280 (17)0.68012 (14)0.37128 (10)0.0137 (3)
O40.03914 (19)0.55976 (15)0.19211 (10)0.0174 (3)
O50.36269 (17)0.63634 (14)0.11768 (10)0.0153 (3)
C10.3756 (3)0.9976 (2)0.21703 (15)0.0154 (4)
H1A0.29991.05550.15170.018*
H1B0.47861.04270.22080.018*
C20.2561 (3)1.0043 (2)0.30908 (15)0.0145 (4)
H2A0.33150.94520.37440.017*
H2B0.20531.11100.31120.017*
C30.0034 (3)0.9215 (2)0.38901 (14)0.0156 (4)
H3A0.08291.02120.39410.019*
H3B0.07920.87230.45280.019*
C40.1233 (3)0.8230 (2)0.37831 (15)0.0166 (4)
H4A0.20130.80690.43940.020*
H4B0.20700.87280.31500.020*
C50.0982 (3)0.5780 (2)0.35249 (15)0.0175 (4)
H5A0.21440.63700.30950.021*
H5B0.13280.51820.41950.021*
C60.0246 (3)0.4727 (2)0.29743 (15)0.0179 (4)
H6A0.15000.42750.33320.021*
H6B0.02990.38950.29740.021*
C70.1660 (3)0.4764 (2)0.13249 (16)0.0179 (4)
H7A0.12500.51930.05800.021*
H7B0.16230.36930.15410.021*
C80.3648 (3)0.4807 (2)0.14576 (15)0.0157 (4)
H8A0.41190.43040.21890.019*
H8B0.44720.42710.10040.019*
C90.5438 (3)0.6568 (2)0.12320 (15)0.0167 (4)
H9A0.61530.63420.06320.020*
H9B0.61320.58700.18800.020*
C100.5201 (3)0.8192 (2)0.12174 (14)0.0143 (4)
H10A0.64180.84230.11100.017*
H10B0.43180.88870.06380.017*
Pd10.50000.50000.50000.00905 (6)
O610.36808 (19)0.61191 (15)0.35964 (10)0.0152 (3)
H61A0.397 (3)0.680 (2)0.3221 (17)0.023*
H61B0.262 (3)0.633 (3)0.3622 (18)0.023*
O710.44716 (18)0.31460 (15)0.48166 (10)0.0164 (3)
N10.5632 (2)0.24692 (17)0.42048 (12)0.0145 (3)
O810.7008 (2)0.29036 (16)0.39221 (11)0.0211 (3)
O910.5235 (2)0.14365 (17)0.39839 (12)0.0275 (3)
Pd20.00001.00000.00000.00852 (6)
O620.0070 (2)0.86094 (15)0.14265 (10)0.0157 (3)
H62A0.042 (3)0.882 (3)0.1853 (17)0.024*
H62B0.040 (3)0.776 (2)0.1489 (18)0.024*
O720.01441 (17)1.17356 (14)0.05803 (10)0.0133 (3)
N20.1691 (2)1.21875 (17)0.10712 (12)0.0133 (3)
O820.29127 (19)1.15441 (15)0.11248 (11)0.0189 (3)
O920.1755 (2)1.32423 (16)0.14308 (12)0.0241 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0175 (7)0.0121 (6)0.0118 (6)0.0048 (5)0.0029 (5)0.0029 (5)
O20.0150 (6)0.0177 (6)0.0107 (6)0.0094 (5)0.0027 (5)0.0053 (5)
O30.0132 (6)0.0135 (6)0.0166 (6)0.0061 (5)0.0000 (5)0.0053 (5)
O40.0202 (7)0.0153 (7)0.0163 (7)0.0054 (5)0.0027 (5)0.0035 (5)
O50.0123 (6)0.0130 (6)0.0204 (7)0.0051 (5)0.0009 (5)0.0025 (5)
C10.0139 (9)0.0112 (9)0.0199 (10)0.0053 (7)0.0001 (7)0.0007 (7)
C20.0157 (9)0.0140 (9)0.0171 (9)0.0073 (7)0.0010 (7)0.0063 (7)
C30.0185 (9)0.0172 (9)0.0132 (9)0.0061 (8)0.0056 (7)0.0073 (7)
C40.0156 (9)0.0168 (9)0.0180 (9)0.0041 (7)0.0051 (7)0.0068 (8)
C50.0153 (9)0.0196 (10)0.0216 (10)0.0106 (8)0.0028 (8)0.0065 (8)
C60.0188 (10)0.0156 (9)0.0207 (10)0.0081 (8)0.0007 (8)0.0040 (8)
C70.0188 (10)0.0159 (9)0.0215 (10)0.0061 (8)0.0032 (8)0.0084 (8)
C80.0173 (9)0.0126 (9)0.0173 (9)0.0026 (7)0.0001 (7)0.0058 (7)
C90.0132 (9)0.0231 (10)0.0168 (9)0.0071 (8)0.0019 (7)0.0084 (8)
C100.0146 (9)0.0189 (9)0.0103 (8)0.0076 (7)0.0022 (7)0.0029 (7)
Pd10.00936 (10)0.00826 (9)0.00945 (10)0.00348 (7)0.00105 (7)0.00143 (7)
O610.0151 (7)0.0147 (7)0.0139 (6)0.0066 (6)0.0009 (6)0.0013 (5)
O710.0176 (7)0.0146 (6)0.0193 (7)0.0070 (5)0.0046 (5)0.0065 (5)
N10.0182 (8)0.0116 (7)0.0128 (7)0.0035 (6)0.0026 (6)0.0023 (6)
O810.0200 (7)0.0217 (7)0.0252 (8)0.0090 (6)0.0081 (6)0.0098 (6)
O910.0374 (9)0.0226 (8)0.0321 (8)0.0153 (7)0.0019 (7)0.0163 (7)
Pd20.00976 (10)0.00788 (9)0.00733 (9)0.00189 (7)0.00048 (7)0.00168 (7)
O620.0259 (8)0.0100 (6)0.0113 (6)0.0059 (6)0.0015 (5)0.0018 (5)
O720.0123 (6)0.0137 (6)0.0149 (6)0.0030 (5)0.0016 (5)0.0063 (5)
N20.0149 (8)0.0123 (7)0.0116 (7)0.0021 (6)0.0009 (6)0.0035 (6)
O820.0167 (7)0.0204 (7)0.0234 (7)0.0100 (6)0.0062 (6)0.0083 (6)
O920.0234 (8)0.0246 (8)0.0319 (8)0.0077 (6)0.0049 (6)0.0195 (7)
Geometric parameters (Å, º) top
O1—C11.432 (2)C7—H7B0.9900
O1—C101.435 (2)C8—H8A0.9900
O2—C21.431 (2)C8—H8B0.9900
O2—C31.435 (2)C9—C101.506 (3)
O3—C41.434 (2)C9—H9A0.9900
O3—C51.435 (2)C9—H9B0.9900
O4—C71.431 (2)C10—H10A0.9900
O4—C61.442 (2)C10—H10B0.9900
O5—C81.424 (2)Pd1—O711.9977 (13)
O5—C91.426 (2)Pd1—O71i1.9977 (13)
C1—C21.502 (3)Pd1—O61i2.0155 (13)
C1—H1A0.9900Pd1—O612.0155 (13)
C1—H1B0.9900O61—H61A0.784 (18)
C2—H2A0.9900O61—H61B0.765 (18)
C2—H2B0.9900O71—N11.331 (2)
C3—C41.504 (3)N1—O911.216 (2)
C3—H3A0.9900N1—O811.224 (2)
C3—H3B0.9900Pd2—O721.9934 (12)
C4—H4A0.9900Pd2—O72ii1.9935 (12)
C4—H4B0.9900Pd2—O622.0091 (13)
C5—C61.498 (3)Pd2—O62ii2.0091 (13)
C5—H5A0.9900O62—H62A0.784 (18)
C5—H5B0.9900O62—H62B0.770 (18)
C6—H6A0.9900O72—N21.3335 (19)
C6—H6B0.9900N2—O921.221 (2)
C7—C81.513 (3)N2—O821.225 (2)
C7—H7A0.9900
C1—O1—C10113.95 (14)H7A—C7—H7B107.8
C2—O2—C3113.95 (14)O5—C8—C7107.28 (15)
C4—O3—C5114.57 (14)O5—C8—H8A110.3
C7—O4—C6114.13 (14)C7—C8—H8A110.3
C8—O5—C9113.12 (14)O5—C8—H8B110.3
O1—C1—C2107.99 (14)C7—C8—H8B110.3
O1—C1—H1A110.1H8A—C8—H8B108.5
C2—C1—H1A110.1O5—C9—C10108.22 (15)
O1—C1—H1B110.1O5—C9—H9A110.1
C2—C1—H1B110.1C10—C9—H9A110.1
H1A—C1—H1B108.4O5—C9—H9B110.1
O2—C2—C1108.15 (15)C10—C9—H9B110.1
O2—C2—H2A110.1H9A—C9—H9B108.4
C1—C2—H2A110.1O1—C10—C9109.12 (14)
O2—C2—H2B110.1O1—C10—H10A109.9
C1—C2—H2B110.1C9—C10—H10A109.9
H2A—C2—H2B108.4O1—C10—H10B109.9
O2—C3—C4108.11 (15)C9—C10—H10B109.9
O2—C3—H3A110.1H10A—C10—H10B108.3
C4—C3—H3A110.1O71—Pd1—O71i180.0
O2—C3—H3B110.1O71—Pd1—O61i93.08 (5)
C4—C3—H3B110.1O71i—Pd1—O61i86.92 (5)
H3A—C3—H3B108.4O71—Pd1—O6186.92 (5)
O3—C4—C3108.23 (15)O71i—Pd1—O6193.08 (5)
O3—C4—H4A110.1O61i—Pd1—O61179.999 (1)
C3—C4—H4A110.1Pd1—O61—H61A121.4 (17)
O3—C4—H4B110.1Pd1—O61—H61B112.6 (18)
C3—C4—H4B110.1H61A—O61—H61B110 (2)
H4A—C4—H4B108.4N1—O71—Pd1114.36 (10)
O3—C5—C6110.22 (15)O91—N1—O81125.14 (16)
O3—C5—H5A109.6O91—N1—O71116.21 (15)
C6—C5—H5A109.6O81—N1—O71118.63 (15)
O3—C5—H5B109.6O72—Pd2—O72ii180.00 (7)
C6—C5—H5B109.6O72—Pd2—O6291.55 (5)
H5A—C5—H5B108.1O72ii—Pd2—O6288.45 (5)
O4—C6—C5107.93 (15)O72—Pd2—O62ii88.45 (5)
O4—C6—H6A110.1O72ii—Pd2—O62ii91.55 (5)
C5—C6—H6A110.1O62—Pd2—O62ii179.999 (1)
O4—C6—H6B110.1Pd2—O62—H62A111.9 (18)
C5—C6—H6B110.1Pd2—O62—H62B115.3 (18)
H6A—C6—H6B108.4H62A—O62—H62B106 (2)
O4—C7—C8112.45 (16)N2—O72—Pd2115.97 (10)
O4—C7—H7A109.1O92—N2—O82125.46 (16)
C8—C7—H7A109.1O92—N2—O72115.34 (15)
O4—C7—H7B109.1O82—N2—O72119.20 (15)
C8—C7—H7B109.1
C10—O1—C1—C2162.68 (14)C8—O5—C9—C10164.40 (15)
C3—O2—C2—C1171.64 (14)C1—O1—C10—C9164.36 (15)
O1—C1—C2—O261.31 (18)O5—C9—C10—O171.00 (18)
C2—O2—C3—C4166.83 (15)O61i—Pd1—O71—N1100.46 (12)
C5—O3—C4—C3175.34 (15)O61—Pd1—O71—N179.54 (12)
O2—C3—C4—O359.79 (19)Pd1—O71—N1—O91172.34 (12)
C4—O3—C5—C6152.96 (15)Pd1—O71—N1—O818.7 (2)
C7—O4—C6—C5174.84 (15)O62—Pd2—O72—N262.55 (12)
O3—C5—C6—O471.36 (19)O62ii—Pd2—O72—N2117.45 (12)
C6—O4—C7—C887.05 (19)Pd2—O72—N2—O92179.39 (12)
C9—O5—C8—C7177.92 (15)Pd2—O72—N2—O821.0 (2)
O4—C7—C8—O556.6 (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
Mr = 869.04F(000) = 452
Triclinic, P1Dx = 1.623 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.0048 (1) ÅCell parameters from 7640 reflections
b = 9.8871 (2) Åθ = 1.0–27.5°
c = 13.8440 (3) ŵ = 0.62 mm1
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 tube3946 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
Detector resolution: 9.1 pixels mm-1θmax = 27.5°, θmin = 2.5°
ω scans at fixed χ = 55°h = 99
Absorption correction: multi-scan
SADABS (Sheldrick, 1996)
k = 1212
Tmin = 0.596, Tmax = 0.940l = 1717
24163 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.063H atoms treated by a mixture of independent and constrained refinement
S = 1.09 w = 1/[σ2(Fo2) + (0.0166P)2 + 0.5279P]
where P = (Fo2 + 2Fc2)/3
4040 reflections(Δ/σ)max = 0.001
248 parametersΔρmax = 0.61 e Å3
6 restraintsΔρmin = 0.78 e Å3
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O10.44859 (18)0.76046 (12)0.26456 (8)0.0179 (2)
O20.50643 (16)0.47734 (11)0.37780 (8)0.0157 (2)
O30.32545 (16)0.36081 (11)0.25227 (8)0.0146 (2)
O40.00778 (16)0.60402 (11)0.17921 (8)0.0151 (2)
O50.18429 (17)0.82662 (11)0.10688 (8)0.0170 (2)
C10.5224 (2)0.71708 (17)0.36298 (11)0.0175 (3)
H1A0.40810.73480.40880.021*
H1B0.60910.77340.37590.021*
C20.6438 (2)0.55676 (17)0.37717 (12)0.0174 (3)
H2A0.74050.53660.32320.021*
H2B0.72160.52670.44000.021*
C30.5995 (2)0.33242 (16)0.35770 (11)0.0159 (3)
H3A0.68660.26960.41410.019*
H3B0.68470.33390.29900.019*
C40.4330 (2)0.27459 (16)0.34020 (11)0.0164 (3)
H4A0.49080.17100.33270.020*
H4B0.34020.28170.39630.020*
C50.1311 (2)0.34818 (16)0.23942 (12)0.0167 (3)
H5A0.05330.35960.30050.020*
H5B0.14690.25100.22400.020*
C60.0208 (2)0.46584 (16)0.15624 (12)0.0162 (3)
H6A0.09480.45100.09450.019*
H6B0.11680.46220.14730.019*
C70.0763 (2)0.72315 (17)0.10046 (12)0.0189 (3)
H7A0.22480.74620.09580.023*
H7B0.01720.69680.03750.023*
C80.0287 (2)0.85312 (17)0.12069 (12)0.0183 (3)
H8A0.10830.94180.07530.022*
H8B0.06440.86810.18880.022*
C90.2528 (3)0.93496 (16)0.13642 (12)0.0194 (3)
H9A0.14611.03150.12020.023*
H9B0.37480.93920.09920.023*
C100.3027 (3)0.90252 (16)0.24537 (11)0.0179 (3)
H10A0.35850.97470.26320.022*
H10B0.17950.90610.28390.022*
Pd0.50000.50000.00000.01145 (6)
O610.46157 (17)0.55162 (12)0.13540 (8)0.0148 (2)
H61A0.412 (3)0.497 (2)0.1710 (14)0.022*
H61B0.385 (3)0.6339 (18)0.1310 (15)0.022*
N10.4049 (2)0.78769 (14)0.10510 (10)0.0167 (3)
O710.54243 (17)0.69096 (12)0.04279 (8)0.0174 (2)
O810.25517 (18)0.76050 (12)0.12672 (9)0.0211 (2)
O910.4395 (2)0.90026 (13)0.13799 (10)0.0275 (3)
O110.09790 (18)0.61520 (13)0.36789 (8)0.0172 (2)
H11B0.055 (3)0.624 (2)0.3153 (13)0.026*
H11A0.218 (3)0.582 (2)0.3672 (15)0.026*
N20.1473 (2)0.90971 (14)0.46176 (10)0.0177 (3)
O140.1678 (2)0.94905 (13)0.37352 (9)0.0252 (3)
O150.2131 (2)0.98334 (14)0.52467 (10)0.0292 (3)
O160.04218 (19)0.76821 (12)0.49542 (8)0.0201 (2)
H160.004 (3)0.729 (2)0.4462 (17)0.030*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0256 (6)0.0148 (5)0.0118 (5)0.0037 (5)0.0027 (4)0.0038 (4)
O20.0141 (5)0.0150 (5)0.0180 (5)0.0038 (4)0.0007 (4)0.0048 (4)
O30.0133 (5)0.0168 (5)0.0131 (5)0.0049 (4)0.0009 (4)0.0008 (4)
O40.0176 (5)0.0141 (5)0.0128 (5)0.0036 (4)0.0037 (4)0.0031 (4)
O50.0203 (6)0.0147 (5)0.0165 (5)0.0046 (4)0.0009 (4)0.0058 (4)
C10.0226 (8)0.0198 (7)0.0130 (7)0.0098 (6)0.0028 (6)0.0046 (6)
C20.0152 (7)0.0214 (7)0.0164 (8)0.0070 (6)0.0024 (6)0.0030 (6)
C30.0160 (7)0.0153 (7)0.0138 (7)0.0016 (6)0.0012 (6)0.0024 (5)
C40.0190 (7)0.0132 (6)0.0144 (7)0.0034 (6)0.0011 (6)0.0007 (5)
C50.0142 (7)0.0159 (7)0.0225 (8)0.0069 (6)0.0012 (6)0.0062 (6)
C60.0148 (7)0.0181 (7)0.0184 (7)0.0061 (6)0.0007 (6)0.0085 (6)
C70.0186 (8)0.0210 (7)0.0149 (7)0.0041 (6)0.0068 (6)0.0008 (6)
C80.0193 (8)0.0153 (7)0.0165 (7)0.0007 (6)0.0028 (6)0.0020 (6)
C90.0292 (9)0.0134 (7)0.0167 (8)0.0087 (6)0.0023 (6)0.0020 (6)
C100.0258 (8)0.0127 (7)0.0157 (7)0.0057 (6)0.0004 (6)0.0048 (5)
Pd0.01332 (9)0.01180 (8)0.01011 (9)0.00443 (6)0.00176 (6)0.00400 (6)
O610.0181 (5)0.0149 (5)0.0123 (5)0.0054 (4)0.0033 (4)0.0053 (4)
N10.0190 (7)0.0133 (6)0.0168 (6)0.0032 (5)0.0033 (5)0.0050 (5)
O710.0192 (6)0.0162 (5)0.0168 (5)0.0058 (4)0.0008 (4)0.0032 (4)
O810.0201 (6)0.0199 (5)0.0226 (6)0.0049 (5)0.0029 (5)0.0045 (4)
O910.0318 (7)0.0143 (5)0.0348 (7)0.0082 (5)0.0058 (6)0.0001 (5)
O110.0145 (5)0.0213 (5)0.0143 (5)0.0016 (4)0.0007 (4)0.0075 (4)
N20.0175 (7)0.0168 (6)0.0206 (7)0.0069 (5)0.0031 (5)0.0063 (5)
O140.0301 (7)0.0213 (6)0.0185 (6)0.0023 (5)0.0005 (5)0.0006 (5)
O150.0376 (7)0.0252 (6)0.0289 (7)0.0107 (6)0.0114 (6)0.0173 (5)
O160.0265 (6)0.0169 (5)0.0139 (6)0.0021 (5)0.0003 (5)0.0044 (4)
Geometric parameters (Å, º) top
O1—C11.4173 (18)C7—C81.504 (2)
O1—C101.4203 (18)C7—H7A0.9900
O2—C21.4298 (18)C7—H7B0.9900
O2—C31.4342 (17)C8—H8A0.9900
O3—C51.4284 (17)C8—H8B0.9900
O3—C41.4325 (17)C9—C101.515 (2)
O4—C61.4296 (17)C9—H9A0.9900
O4—C71.4339 (18)C9—H9B0.9900
O5—C91.4346 (17)C10—H10A0.9900
O5—C81.4373 (19)C10—H10B0.9900
C1—C21.508 (2)Pd—O71i1.9928 (11)
C1—H1A0.9900Pd—O711.9928 (11)
C1—H1B0.9900Pd—O612.0131 (10)
C2—H2A0.9900Pd—O61i2.0132 (10)
C2—H2B0.9900O61—H61A0.824 (16)
C3—C41.505 (2)O61—H61B0.803 (16)
C3—H3A0.9900N1—O911.2238 (17)
C3—H3B0.9900N1—O811.2260 (17)
C4—H4A0.9900N1—O711.3210 (17)
C4—H4B0.9900O11—H11B0.778 (17)
C5—C61.508 (2)O11—H11A0.795 (17)
C5—H5A0.9900N2—O151.2118 (18)
C5—H5B0.9900N2—O141.2137 (18)
C6—H6A0.9900N2—O161.3506 (17)
C6—H6B0.9900O16—H160.84 (2)
C1—O1—C10113.60 (11)O4—C7—H7A110.0
C2—O2—C3113.94 (12)C8—C7—H7A110.0
C5—O3—C4114.50 (12)O4—C7—H7B110.0
C6—O4—C7113.31 (11)C8—C7—H7B110.0
C9—O5—C8113.28 (12)H7A—C7—H7B108.4
O1—C1—C2107.55 (12)O5—C8—C7108.25 (12)
O1—C1—H1A110.2O5—C8—H8A110.0
C2—C1—H1A110.2C7—C8—H8A110.0
O1—C1—H1B110.2O5—C8—H8B110.0
C2—C1—H1B110.2C7—C8—H8B110.0
H1A—C1—H1B108.5H8A—C8—H8B108.4
O2—C2—C1108.35 (12)O5—C9—C10111.89 (12)
O2—C2—H2A110.0O5—C9—H9A109.2
C1—C2—H2A110.0C10—C9—H9A109.2
O2—C2—H2B110.0O5—C9—H9B109.2
C1—C2—H2B110.0C10—C9—H9B109.2
H2A—C2—H2B108.4H9A—C9—H9B107.9
O2—C3—C4107.70 (12)O1—C10—C9106.47 (12)
O2—C3—H3A110.2O1—C10—H10A110.4
C4—C3—H3A110.2C9—C10—H10A110.4
O2—C3—H3B110.2O1—C10—H10B110.4
C4—C3—H3B110.2C9—C10—H10B110.4
H3A—C3—H3B108.5H10A—C10—H10B108.6
O3—C4—C3107.45 (12)O71i—Pd—O71180.0
O3—C4—H4A110.2O71i—Pd—O6193.61 (4)
C3—C4—H4A110.2O71—Pd—O6186.39 (4)
O3—C4—H4B110.2O71i—Pd—O61i86.39 (4)
C3—C4—H4B110.2O71—Pd—O61i93.61 (4)
H4A—C4—H4B108.5O61—Pd—O61i180.000 (1)
O3—C5—C6108.12 (12)Pd—O61—H61A109.9 (14)
O3—C5—H5A110.1Pd—O61—H61B108.2 (14)
C6—C5—H5A110.1H61A—O61—H61B109.2 (19)
O3—C5—H5B110.1O91—N1—O81124.53 (14)
C6—C5—H5B110.1O91—N1—O71115.88 (13)
H5A—C5—H5B108.4O81—N1—O71119.59 (12)
O4—C6—C5108.60 (12)N1—O71—Pd115.71 (9)
O4—C6—H6A110.0H11B—O11—H11A109 (2)
C5—C6—H6A110.0O15—N2—O14127.20 (14)
O4—C6—H6B110.0O15—N2—O16115.15 (14)
C5—C6—H6B110.0O14—N2—O16117.65 (12)
H6A—C6—H6B108.4N2—O16—H16106.8 (16)
O4—C7—C8108.40 (12)
C10—O1—C1—C2169.59 (13)C9—O5—C8—C7172.38 (12)
C3—O2—C2—C1160.14 (12)O4—C7—C8—O571.41 (16)
O1—C1—C2—O271.58 (15)C8—O5—C9—C1084.82 (16)
C2—O2—C3—C4168.49 (12)C1—O1—C10—C9175.87 (12)
C5—O3—C4—C3163.46 (12)O5—C9—C10—O156.16 (17)
O2—C3—C4—O365.60 (15)O91—N1—O71—Pd174.00 (10)
C4—O3—C5—C6168.73 (12)O81—N1—O71—Pd5.52 (16)
C7—O4—C6—C5173.98 (12)O61—Pd—O71—N1115.14 (10)
O3—C5—C6—O457.44 (15)O61i—Pd—O71—N164.86 (10)
C6—O4—C7—C8164.09 (13)
Symmetry code: (i) x+1, y+1, z.
 

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