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The title compound, [Co(C5H11)(C62H88N13O14P)]·0.385C3H6O·12.650H2O, contains the isoamyl (3-methyl­butyl) anion bonded to the CoIII ion through a C atom. The compound is thus a structural analog of the two biologically important vitamin B12 coenzymes adenosyl­cobalamin and methyl­cobalamin. The lower axial Co—N bond length [2.277 (2) Å] is one of the longest ever reported for a cobalamin and reflects the strong σ-donor ability of the isoamyl group.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010400366X/gd1306sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S010827010400366X/gd1306Isup2.hkl
Contains datablock I

CCDC reference: 237911

Comment top

Cobalamins (derivatives of vitamin B12) contain a six coordinate cobalt(III) atom coordinated equatorially by four pyrrole N atoms of a corrin ligand. The lower (α) axial ligand is 5,6-dimethylbenzimidazole-α-D-ribofuranose-3'-phosphate (DMB), while the upper (β) ligand, R, is variable (R = CN in B12 itself). Adenosylcobalamin (AdoCbl; R = 5'-deoxyadenosyl) and methylcobalamin (MeCbl; R = CH3) function as coenzymes in a number of biologically important 1,2 rearrangement and transmethylation reactions, respectively (Ludwig et al., 1999). The first step in the AdoCbl-dependent enzymes is homolytic cleavage of the Co—C bond to produce a CoII ion and an Ado radical (Marsh, 1999). The means by which the enzyme activates the Co—C bond in AdoCbl for homolytic cleavage by a factor of 109–1012 (Hay & Finke, 1986; Brown & Li, 1998) remains unclear. The rate enhancement may be caused either by an upward conformational distortion of the corrin ring, induced by steric interactions with the large DMB base (Halpern, 1985; Hay et al., 1987; Pett et al., 1987), or by the enzyme directly lengthening the Co—C bond or distorting the Co—C—C angle (Williams, 1995). Electronic effects of the trans ligand may also play a role in activating the Co—C bond for homolysis (Pratt, 1999). The trans influence refers to the effect that the β ligand has on the length of the Co—DMB(N13) bond.

We have determined the X-ray crystal structure of isoamylcobalamin (isoamylCbl), (I) (Fig. 1), a structural analogue of AdoCbl and MeCbl, in order to compare the ground-state trans influence of the C5H11 ligand to the β ligands in other cobalamin derivatives.

Compound (I) crystallizes in the orthorhombic space group P212121 and is isomorphous with the other cobalamin derivatives belonging to packing type I (Gruber et al., 1998). Selected bond lengths and bond angles involving the coordination sphere of the metal ion are listed in Table 1. The β alkyl ligand is disordered over two slightly different positions; in the first position [0.615 (4) occupancy], atom C65A points directly towards the c side chain, whereas in the second position [0.385 (4) occupancy], atom C65B points towards atom C10 when viewed from above the corrin ring. The β Co—C bond length [2.044 (3) Å] is longer than the corresponding bond length for MeCbl (Randaccio et al., 2000; Rossi et al., 1985) [average for two MeCbl structures = 1.984 (7) Å], and is also slightly longer than the corresponding bond length in AdoCbl (Bouquiere et al., 1993; Savage et al., 1987) [average for four AdoCbl structures = 2.01 (3) Å]. The Co—N13 bond length [2.277 (2) Å] is substantially longer than that observed in MeCbl [mean for two structures = 2.18 (2) Å] and slightly longer than that in AdoCbl [average for four structures = 2.23 (2) Å], and is the second longest Co—N13 bond length ever reported for a cobalamin structure, the longest being for (S)-2,3-dihydroxypropyl-cobalamin (2.367 Å; Alcock et al., 1985). The isoamyl group clearly is a strong σ-donor (comparable to the Ado group of AdoCbl) and markedly lengthens the trans Co—N13 bond. The Co—C—C angle [119.0 (3) or 116.0 (4)°] is slightly smaller than that observed for AdoCbl [mean for four structures = 122 (2)°], where there is steric pressure exerted on the adenine moiety by the C34 methyl group (Alcock et al., 1985). The six amide side chains are extensively hydrogen bonded to either solvent water molecules, or the side chains of symmetry-related molecules. This hydrogen-bonding scheme is similar to that seen for other cobalamin molecules belonging to packing type I.

The corrin fold angle, defined as the angle between the normals of the two least-squares planes passing through atoms N1, C4, C5, C6, N2, C9 and C10 (plane 1), and C10, C11, N3, C14, C15, C16 and N4 (plane 2), is calculated to be 10.57°. This angle is less than the fold angles for both MeCbl (14.72°) and AdoCbl [mean for four structures = 13.4 (6)°], and reflects the long Co—N13 bond.

Experimental top

IsoamylCbl was prepared by a method similar to that used to prepare MeCbl (Brown et al., 1997). CNCbl (50 mg) was dissolved in a methanol solution (40 ml) containing a 10%(v/v) acetic acid solution (10 ml). After purging the solution with argon for 40 min, zinc wool was added in excess. The reduction process was accompanied by a change in colour from red to brown and was monitored by high-pressure liquid chromatography (HPLC). Once the reduction process had been completed, a 100-fold excess of redistilled 1-bromo-3-methyl butane dissolved in deaerated methanol was transferred by canula into the reduced cobalamin solution in a darkroom, working only under dim red light. Formation of the product was again monitored by HPLC, and on completion of the reaction, the solution was transferred by canula into an empty vessel and exposed to air. The solution was then desalted on a 6 ml ISOLUTE SPE C18(EC) column and rotary-evaporated (303 K) to dryness in the dark. The isoamylCbl solution was redissolved in a minimal amount of deionized water. Crystals were grown in H tubes in a refrigerator, by vapour diffusion of acetone into the aqueous solution. Crystals appeared after about two weeks.

Refinement top

H atoms were positioned geometrically and allowed to ride on their respective parent atoms, with C—H distances of 0.98–1.00 Å, N—H distances of 0.88 Å and O—H distances of 0.84–0.93 Å, and with Uiso(H) equal to 1.2Ueq(C) [1.5Ueq(C) for methyl groups]. The structure contains eleven ordered water molecules, one disordered water molecule and two water molecules that were assigned partial occupancy. In addition, there is a solvent acetone molecule that was assigned partial occupancy (site occupancy 0.385). No elemental analyses were performed, as these have been found to be unreliable with respect to the water content. The upper axial isoamyl group was found to be disordered and was refined over two positions, with the final occupancies over the two positions being 0.615 (4) and 0.385 (4), respectively.

Computing details top

Data collection: SMART (Bruker,1998); cell refinement: SMART; data reduction: SAINT (Bruker,1999); program(s) used to solve structure: SHELXTL (Bruker,1999); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 (Farrugia,1997); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of the cobalamin complex of (I). Displacement ellipsoids are drawn at the 50% probability level. H atoms, solvent atoms and disorder in the upper axial ligand have been omitted for clarity (for missing labels, see scheme).
(I) top
Crystal data top
[Co(C5H11)(C62H88N13O14P)]·0.385C3H6O·12.650H2OF(000) = 3539
Mr = 1650.69Dx = 1.354 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 1015 reflections
a = 15.959 (3) Åθ = 3.0–26.5°
b = 20.793 (4) ŵ = 0.32 mm1
c = 24.403 (5) ÅT = 123 K
V = 8098 (3) Å3Rectangular, dark red
Z = 40.48 × 0.26 × 0.26 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
14388 reflections with I > 2σ(I)
ϕ and ω scansRint = 0.031
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
θmax = 26.5°, θmin = 1.3°
Tmin = 0.863, Tmax = 0.922h = 2019
45443 measured reflectionsk = 1726
16502 independent reflectionsl = 3030
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.107 w = 1/[σ2(Fo2) + (0.052P)2 + 5.1666P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.002
16502 reflectionsΔρmax = 0.59 e Å3
1085 parametersΔρmin = 0.44 e Å3
45 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 7369 Friedel pairs.
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.010 (10)
Crystal data top
[Co(C5H11)(C62H88N13O14P)]·0.385C3H6O·12.650H2OV = 8098 (3) Å3
Mr = 1650.69Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 15.959 (3) ŵ = 0.32 mm1
b = 20.793 (4) ÅT = 123 K
c = 24.403 (5) Å0.48 × 0.26 × 0.26 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer
16502 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
14388 reflections with I > 2σ(I)
Tmin = 0.863, Tmax = 0.922Rint = 0.031
45443 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.043H-atom parameters constrained
wR(F2) = 0.107Δρmax = 0.59 e Å3
S = 1.05Δρmin = 0.44 e Å3
16502 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 7369 Friedel pairs.
1085 parametersAbsolute structure parameter: 0.010 (10)
45 restraints
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.63334 (17)0.21189 (13)0.76263 (11)0.0148 (6)
C20.53670 (17)0.22198 (13)0.75104 (11)0.0155 (6)
C30.50596 (17)0.15100 (13)0.74537 (11)0.0165 (6)
H30.46060.14950.71720.02*
C40.58364 (16)0.11845 (13)0.72198 (10)0.0147 (6)
C50.58131 (17)0.05684 (13)0.69391 (11)0.0162 (6)
C60.65307 (17)0.02419 (13)0.68262 (11)0.0153 (6)
C70.66304 (18)0.04396 (13)0.65751 (11)0.0174 (6)
C80.75190 (17)0.06203 (13)0.67907 (11)0.0176 (6)
H80.78210.08960.65190.021*
C90.79170 (17)0.00327 (13)0.68253 (11)0.0161 (6)
C100.87671 (18)0.01328 (14)0.67563 (12)0.0188 (6)
H100.910.02280.66560.023*
C110.91710 (17)0.07161 (13)0.68213 (11)0.0155 (6)
C121.00924 (17)0.08189 (13)0.66868 (12)0.0174 (6)
C131.02776 (16)0.14324 (13)0.70301 (11)0.0170 (6)
H131.06580.17280.68230.02*
C140.94025 (17)0.17313 (13)0.70849 (11)0.0168 (6)
C150.92664 (17)0.23561 (13)0.72407 (11)0.0163 (6)
C160.84297 (17)0.25880 (13)0.73539 (10)0.0140 (5)
C170.81865 (17)0.32917 (13)0.74750 (11)0.0157 (6)
C180.72669 (17)0.32029 (12)0.76782 (11)0.0158 (6)
H180.72840.31020.80790.019*
C190.69816 (16)0.25944 (13)0.73736 (11)0.0148 (5)
H190.67860.2720.69990.018*
C200.65419 (17)0.20274 (13)0.82355 (11)0.0153 (6)
H20A0.62770.16320.83690.023*
H20B0.63320.23960.84450.023*
H20C0.71510.19950.82810.023*
C210.49233 (17)0.26036 (13)0.79588 (12)0.0187 (6)
H21A0.52010.3020.80050.028*
H21B0.49470.23640.83040.028*
H21C0.43370.26720.78550.028*
C220.52404 (17)0.25487 (14)0.69420 (12)0.0192 (6)
H22A0.5430.30010.69680.023*
H22B0.56010.2330.6670.023*
C230.43386 (18)0.25410 (14)0.67337 (12)0.0224 (6)
C240.47476 (17)0.11536 (13)0.79772 (12)0.0178 (6)
H24A0.48550.06870.79350.021*
H24B0.50730.13070.82970.021*
C250.38098 (17)0.12589 (14)0.80884 (12)0.0211 (6)
H25A0.37150.17140.8190.025*
H25B0.34890.11710.77490.025*
C260.34909 (19)0.08288 (16)0.85427 (13)0.0251 (7)
C270.49416 (19)0.03306 (15)0.67825 (14)0.0258 (7)
H27A0.49910.00160.65130.039*
H27B0.46190.06860.66250.039*
H27C0.46550.01690.7110.039*
C280.59835 (19)0.09515 (14)0.67364 (13)0.0223 (6)
H28A0.58640.09180.71290.033*
H28B0.62070.1380.66550.033*
H28C0.54660.08830.65280.033*
C290.67263 (19)0.04022 (14)0.59381 (12)0.0201 (6)
H29A0.72980.02440.58560.024*
H29B0.66860.08450.57910.024*
C300.61064 (19)0.00153 (15)0.56262 (12)0.0220 (6)
C310.75121 (18)0.09449 (13)0.73680 (11)0.0205 (6)
H31A0.70960.07230.76020.025*
H31B0.73310.13980.73280.025*
C320.83668 (18)0.09298 (15)0.76536 (12)0.0223 (6)
H32A0.87730.11620.74190.027*
H32B0.85530.04760.76740.027*
C330.84156 (19)0.12103 (14)0.82183 (12)0.0229 (6)
C341.0166 (2)0.09901 (16)0.60772 (12)0.0248 (7)
H34A0.9920.06450.58560.037*
H34B1.07580.10420.5980.037*
H34C0.98660.13930.60060.037*
C351.06333 (19)0.02276 (14)0.68084 (13)0.0237 (7)
H35A1.05560.00990.71910.035*
H35B1.12240.03320.67440.035*
H35C1.04660.01270.65670.035*
C361.06093 (17)0.13290 (14)0.76199 (11)0.0186 (6)
H36A1.05220.17330.78270.022*
H36B1.0260.09940.77960.022*
C371.15354 (18)0.11320 (14)0.76844 (12)0.0206 (6)
H37A1.17130.12120.80670.025*
H37B1.15890.06650.76130.025*
C381.21096 (17)0.14916 (14)0.73033 (12)0.0212 (6)
C391.00126 (18)0.28058 (14)0.72844 (13)0.0222 (6)
H39A1.01250.28990.76710.033*
H39B0.98890.32070.7090.033*
H39C1.05050.26010.7120.033*
C400.82215 (18)0.36648 (14)0.69287 (11)0.0192 (6)
H40A0.87840.36270.67710.029*
H40B0.80930.41190.69950.029*
H40C0.7810.34850.66730.029*
C410.66849 (18)0.37875 (13)0.75955 (13)0.0214 (6)
H41A0.66890.39090.72030.026*
H41B0.61050.36620.76920.026*
C420.69335 (16)0.43663 (14)0.79349 (13)0.0209 (6)
C430.87346 (16)0.36465 (13)0.78985 (11)0.0166 (5)
H43A0.92840.3740.77280.02*
H43B0.84660.40640.79840.02*
C440.88901 (19)0.32876 (15)0.84395 (12)0.0227 (6)
H44A0.8390.33220.86780.027*
H44B0.89940.28270.83650.027*
C450.96465 (18)0.35811 (14)0.87270 (12)0.0224 (6)
C461.0202 (2)0.41661 (15)0.95112 (13)0.0246 (7)
H46A0.99820.45080.97540.03*
H46B1.05990.43670.92510.03*
C471.06647 (18)0.36664 (15)0.98558 (11)0.0207 (6)
H471.08580.33030.96190.025*
C481.1401 (2)0.39540 (17)1.01615 (14)0.0308 (8)
H48A1.12030.43041.03970.046*
H48B1.18090.41230.98980.046*
H48C1.16660.36211.03870.046*
C490.91939 (18)0.08993 (14)0.91683 (11)0.0182 (6)
H490.92560.05260.94240.022*
C500.89082 (18)0.14950 (13)0.94849 (11)0.0186 (6)
H500.85360.13820.980.022*
C510.97461 (18)0.17573 (13)0.96731 (12)0.0182 (6)
H510.99520.15130.99990.022*
C521.03166 (19)0.16393 (15)0.91805 (12)0.0223 (6)
H521.02640.20050.89170.027*
C531.1231 (2)0.15311 (17)0.93144 (13)0.0291 (7)
H53A1.15440.14610.89690.035*
H53B1.14580.19220.94910.035*
C540.85476 (18)0.10701 (13)0.82496 (11)0.0177 (6)
H540.89430.13810.81290.021*
C550.66598 (18)0.01899 (13)0.82503 (12)0.0203 (6)
H550.63250.02750.79360.024*
C560.63787 (19)0.02319 (14)0.86545 (13)0.0238 (7)
C570.6885 (2)0.03592 (14)0.91239 (13)0.0250 (7)
C580.7662 (2)0.00699 (14)0.91879 (12)0.0237 (6)
H580.80060.01570.94970.028*
C590.79185 (18)0.03584 (13)0.87740 (12)0.0184 (6)
C600.74397 (17)0.04863 (12)0.83123 (11)0.0167 (6)
C610.5540 (2)0.05519 (17)0.85920 (15)0.0350 (8)
H61A0.51610.03990.8880.053*
H61B0.56070.10190.86240.053*
H61C0.53050.04470.82320.053*
C620.6572 (3)0.08032 (17)0.95700 (15)0.0393 (9)
H62A0.69720.08050.98750.059*
H62B0.65150.1240.94230.059*
H62C0.60250.06520.97010.059*
C630.74226 (18)0.16013 (14)0.63267 (11)0.0200 (6)
H63A0.74320.12030.61050.024*
H63B0.68480.17790.63010.024*
N10.65111 (14)0.15070 (10)0.73191 (9)0.0134 (5)
N20.73390 (14)0.04848 (10)0.69223 (9)0.0153 (5)
N30.88029 (13)0.12598 (11)0.69988 (9)0.0152 (5)
N40.77725 (14)0.22186 (11)0.73194 (9)0.0143 (5)
N50.42035 (17)0.22324 (14)0.62626 (11)0.0311 (6)
H5A0.36950.22170.61230.037*
H5B0.46220.20440.60920.037*
N60.35252 (18)0.10684 (16)0.90431 (11)0.0371 (7)
H6A0.33370.08430.93220.044*
H6B0.37370.14540.90980.044*
N70.53576 (17)0.02341 (14)0.54999 (11)0.0289 (6)
H7A0.49970.00070.53080.035*
H7B0.52260.06250.56090.035*
N80.77766 (17)0.15596 (12)0.84060 (11)0.0269 (6)
H8A0.78010.17310.87350.032*
H8B0.7330.16190.82010.032*
N91.22518 (16)0.21052 (12)0.74193 (11)0.0251 (6)
H9A1.25790.23360.72060.03*
H9B1.20190.22810.7710.03*
N100.70352 (15)0.49194 (11)0.76769 (11)0.0220 (5)
H10A0.71760.52660.78620.026*
H10B0.69620.49410.7320.026*
N110.95123 (16)0.38823 (12)0.92076 (10)0.0236 (6)
H110.90.39070.93390.028*
N120.86414 (15)0.07301 (11)0.87206 (9)0.0183 (5)
N130.78637 (14)0.09329 (11)0.79744 (10)0.0168 (5)
O10.37668 (13)0.28110 (11)0.69856 (9)0.0291 (5)
O20.31973 (16)0.02849 (11)0.84433 (10)0.0373 (6)
O30.63201 (15)0.05629 (11)0.54817 (9)0.0324 (5)
O40.90527 (13)0.11217 (11)0.85040 (9)0.0284 (5)
O51.24248 (13)0.12188 (9)0.68965 (8)0.0255 (5)
O60.70306 (14)0.43141 (10)0.84391 (9)0.0276 (5)
O71.03526 (13)0.35586 (11)0.85197 (9)0.0277 (5)
O81.07770 (13)0.24025 (10)1.05514 (8)0.0236 (5)
O90.92504 (13)0.26532 (10)1.07792 (8)0.0254 (5)
O100.97022 (13)0.24291 (9)0.97934 (8)0.0219 (4)
O111.00484 (13)0.34389 (10)1.02491 (8)0.0213 (4)
O120.99877 (13)0.10570 (10)0.89316 (8)0.0233 (5)
O130.85129 (13)0.19134 (10)0.91126 (8)0.0211 (4)
H13A0.81650.21440.92810.032*
O141.13589 (14)0.10023 (11)0.96627 (9)0.0310 (5)
H141.13650.06620.94770.047*
P0.99602 (5)0.26981 (4)1.03867 (3)0.01786 (15)
Co0.76241 (2)0.134650 (17)0.712480 (15)0.01377 (8)
O1W0.24256 (14)0.23269 (12)0.03362 (9)0.0364 (5)
H1Y0.19050.23530.04040.055*
H1Z0.25060.19260.0380.055*
O2W0.16924 (15)0.26920 (11)0.84058 (9)0.0344 (5)
H2Y0.12880.29550.8440.052*
H2Z0.20140.2770.86750.052*
O3W0.77424 (14)0.20544 (11)0.07112 (9)0.0323 (5)
H3Y0.82150.22420.07330.048*
H3Z0.7650.22360.04050.048*
O4W0.02890 (15)0.97971 (11)0.83342 (10)0.0361 (6)
H4Y0.0090.95170.83860.054*
H4Z0.02031.0150.85020.054*
O5W0.56885 (15)0.37872 (12)0.90100 (11)0.0425 (7)
H5Y0.610.3950.88380.064*
H5Z0.57190.3410.91420.064*
O6W0.16377 (18)0.99142 (14)0.90416 (11)0.0514 (7)
H6Y0.12210.98760.88270.077*
H6Z0.20831.00190.88730.077*
O7W0.39819 (17)0.06258 (15)0.50689 (13)0.0541 (7)
H7Y0.38030.0470.47690.081*
H7Z0.35990.05460.53020.081*
O8W0.52174 (18)0.15943 (14)0.53674 (13)0.0531 (7)
H8Y0.55560.12810.54020.08*
H8Z0.48560.13120.52790.08*
O9W0.23533 (19)0.20076 (17)0.59497 (11)0.0653 (9)
H9Y0.19430.22540.58780.098*
H9Z0.23770.17710.62330.098*
O10W0.7312 (2)0.53583 (19)0.91553 (14)0.0788 (10)
H10Y0.72250.50460.89380.118*
H10Z0.76470.52920.9420.118*
O11W0.9076 (3)0.78596 (18)0.92935 (15)0.0816 (11)
O12A0.2820 (3)0.0854 (2)0.0213 (2)0.0374 (11)0.6
O12B0.2685 (5)0.1070 (4)0.0465 (3)0.0409 (17)0.4
H12W0.22970.10490.02270.061*0.4
H12X0.25010.09590.07780.061*0.4
C64A0.7987 (5)0.2060 (8)0.6069 (3)0.034 (2)0.615 (4)
H64A0.85440.18540.60330.041*0.615 (4)
H64B0.80520.24320.63180.041*0.615 (4)
C65A0.7728 (4)0.2315 (3)0.5502 (2)0.0380 (16)0.615 (4)
H65A0.75370.19490.52670.046*0.615 (4)
C66A0.7015 (4)0.2816 (4)0.5555 (3)0.060 (2)0.615 (4)
H66A0.6540.26240.5750.072*0.615 (4)
H66B0.68350.29530.51890.072*0.615 (4)
H66C0.72190.3190.5760.072*0.615 (4)
C67A0.8515 (5)0.2633 (4)0.5243 (4)0.0610 (18)0.615 (4)
H67A0.84070.27260.48560.073*0.615 (4)
H67B0.89930.2340.52740.073*0.615 (4)
H67C0.86410.30350.54370.073*0.615 (4)
C64B0.7931 (9)0.2160 (13)0.6118 (4)0.034 (2)0.385 (4)
H64C0.84620.2180.63260.041*0.385 (4)
H64D0.76190.25630.61920.041*0.385 (4)
C65B0.8137 (6)0.2132 (5)0.5503 (4)0.0371 (16)0.385 (4)
H65B0.85460.17770.54310.045*0.385 (4)
C66B0.7332 (5)0.2021 (4)0.5160 (3)0.029 (2)0.385 (4)
H66D0.69330.2370.52320.043*0.385 (4)
H66E0.70790.16090.52630.043*0.385 (4)
H66F0.74750.20160.4770.043*0.385 (4)
C67B0.8537 (7)0.2788 (6)0.5346 (6)0.0609 (18)0.385 (4)
H67D0.81710.31390.54660.073*0.385 (4)
H67E0.86090.2810.49470.073*0.385 (4)
H67F0.90850.28290.55240.073*0.385 (4)
O150.6320 (5)0.3506 (5)0.6113 (3)0.066 (3)0.385 (4)
C700.5537 (7)0.3265 (5)0.5318 (4)0.044 (3)0.385 (4)
H70A0.52980.29250.55480.067*0.385 (4)
H70B0.58180.30710.50010.067*0.385 (4)
H70C0.50880.35490.51910.067*0.385 (4)
C690.6160 (6)0.3646 (6)0.5646 (4)0.051 (3)0.385 (4)
C680.6580 (14)0.4192 (11)0.5326 (8)0.150 (11)0.385 (4)
H68A0.69780.44160.55650.224*0.385 (4)
H68B0.61520.44950.51990.224*0.385 (4)
H68C0.68790.40130.5010.224*0.385 (4)
O13W0.6540 (8)0.4881 (5)0.5058 (6)0.102 (4)0.35
O14W0.7010 (16)0.4291 (12)0.5930 (11)0.177 (9)*0.3
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0142 (14)0.0120 (13)0.0183 (13)0.0016 (10)0.0008 (11)0.0009 (11)
C20.0124 (13)0.0164 (14)0.0177 (14)0.0010 (11)0.0007 (11)0.0009 (11)
C30.0136 (13)0.0178 (14)0.0182 (14)0.0009 (11)0.0003 (11)0.0028 (11)
C40.0128 (13)0.0174 (14)0.0139 (13)0.0011 (10)0.0012 (10)0.0039 (10)
C50.0155 (14)0.0168 (14)0.0164 (13)0.0039 (11)0.0007 (10)0.0018 (11)
C60.0168 (14)0.0142 (13)0.0149 (13)0.0047 (11)0.0004 (11)0.0013 (11)
C70.0182 (15)0.0155 (14)0.0185 (14)0.0018 (11)0.0002 (11)0.0032 (11)
C80.0152 (14)0.0136 (13)0.0241 (14)0.0003 (11)0.0019 (11)0.0056 (10)
C90.0186 (14)0.0142 (14)0.0156 (14)0.0005 (11)0.0003 (11)0.0037 (11)
C100.0170 (14)0.0179 (14)0.0215 (15)0.0003 (11)0.0008 (11)0.0049 (12)
C110.0147 (14)0.0165 (14)0.0152 (13)0.0019 (11)0.0001 (11)0.0006 (11)
C120.0132 (14)0.0174 (14)0.0216 (14)0.0006 (11)0.0011 (11)0.0014 (11)
C130.0118 (12)0.0152 (13)0.0238 (15)0.0013 (10)0.0014 (10)0.0002 (11)
C140.0156 (13)0.0202 (14)0.0146 (13)0.0012 (11)0.0040 (11)0.0022 (11)
C150.0167 (13)0.0153 (13)0.0171 (14)0.0026 (11)0.0005 (10)0.0003 (11)
C160.0187 (14)0.0128 (13)0.0106 (12)0.0010 (11)0.0018 (10)0.0010 (10)
C170.0124 (13)0.0160 (14)0.0187 (14)0.0007 (11)0.0001 (11)0.0020 (11)
C180.0132 (14)0.0139 (13)0.0202 (14)0.0018 (11)0.0004 (11)0.0011 (10)
C190.0112 (13)0.0145 (13)0.0187 (13)0.0025 (10)0.0008 (10)0.0000 (11)
C200.0154 (14)0.0136 (13)0.0170 (14)0.0004 (11)0.0005 (11)0.0006 (11)
C210.0156 (13)0.0153 (13)0.0252 (15)0.0004 (11)0.0022 (11)0.0007 (12)
C220.0124 (13)0.0217 (15)0.0235 (15)0.0014 (11)0.0005 (11)0.0026 (12)
C230.0140 (14)0.0247 (16)0.0284 (16)0.0005 (12)0.0010 (12)0.0102 (13)
C240.0133 (13)0.0184 (14)0.0218 (15)0.0007 (10)0.0002 (11)0.0011 (11)
C250.0167 (14)0.0223 (15)0.0241 (15)0.0004 (12)0.0018 (11)0.0013 (12)
C260.0165 (15)0.0329 (18)0.0260 (16)0.0076 (13)0.0005 (12)0.0014 (13)
C270.0155 (14)0.0287 (17)0.0331 (18)0.0016 (13)0.0001 (13)0.0110 (14)
C280.0218 (15)0.0201 (15)0.0250 (15)0.0050 (12)0.0015 (12)0.0028 (12)
C290.0209 (15)0.0204 (15)0.0189 (14)0.0008 (12)0.0006 (11)0.0067 (12)
C300.0262 (16)0.0235 (16)0.0162 (14)0.0010 (13)0.0001 (12)0.0049 (12)
C310.0199 (16)0.0171 (13)0.0243 (15)0.0010 (12)0.0010 (12)0.0022 (11)
C320.0175 (15)0.0235 (15)0.0260 (15)0.0009 (12)0.0012 (12)0.0014 (12)
C330.0220 (16)0.0202 (15)0.0266 (16)0.0050 (12)0.0009 (12)0.0090 (12)
C340.0237 (17)0.0283 (17)0.0225 (16)0.0012 (13)0.0059 (12)0.0039 (13)
C350.0165 (14)0.0186 (15)0.0359 (18)0.0013 (12)0.0007 (13)0.0067 (13)
C360.0171 (14)0.0194 (14)0.0195 (14)0.0021 (12)0.0013 (11)0.0013 (12)
C370.0177 (15)0.0222 (15)0.0219 (14)0.0018 (12)0.0047 (11)0.0019 (12)
C380.0120 (13)0.0213 (15)0.0302 (16)0.0021 (11)0.0038 (11)0.0010 (12)
C390.0139 (14)0.0210 (15)0.0317 (17)0.0006 (12)0.0019 (12)0.0008 (12)
C400.0193 (13)0.0179 (14)0.0205 (14)0.0034 (12)0.0005 (11)0.0044 (12)
C410.0156 (14)0.0181 (15)0.0304 (16)0.0002 (11)0.0011 (12)0.0014 (12)
C420.0118 (14)0.0201 (15)0.0307 (17)0.0022 (11)0.0052 (12)0.0002 (13)
C430.0146 (12)0.0145 (12)0.0206 (13)0.0015 (11)0.0012 (11)0.0002 (12)
C440.0268 (16)0.0219 (16)0.0193 (15)0.0055 (13)0.0030 (12)0.0025 (12)
C450.0220 (15)0.0195 (15)0.0258 (16)0.0022 (12)0.0041 (12)0.0070 (13)
C460.0299 (17)0.0195 (15)0.0244 (16)0.0051 (13)0.0086 (13)0.0000 (12)
C470.0206 (14)0.0213 (15)0.0203 (14)0.0051 (13)0.0023 (11)0.0009 (12)
C480.0278 (18)0.0345 (19)0.0301 (18)0.0091 (14)0.0082 (14)0.0022 (15)
C490.0174 (14)0.0186 (14)0.0186 (14)0.0012 (11)0.0036 (11)0.0008 (11)
C500.0206 (14)0.0182 (15)0.0170 (14)0.0010 (11)0.0006 (11)0.0004 (11)
C510.0232 (15)0.0150 (14)0.0162 (14)0.0000 (11)0.0024 (11)0.0005 (11)
C520.0225 (15)0.0257 (16)0.0187 (15)0.0026 (13)0.0003 (12)0.0045 (12)
C530.0223 (16)0.039 (2)0.0257 (17)0.0032 (14)0.0010 (13)0.0070 (14)
C540.0175 (14)0.0149 (13)0.0206 (14)0.0012 (11)0.0002 (11)0.0026 (11)
C550.0192 (15)0.0159 (14)0.0258 (15)0.0015 (12)0.0001 (12)0.0042 (12)
C560.0238 (16)0.0171 (15)0.0306 (17)0.0011 (12)0.0047 (13)0.0018 (13)
C570.0315 (18)0.0165 (15)0.0270 (16)0.0021 (13)0.0045 (14)0.0026 (12)
C580.0292 (16)0.0218 (15)0.0202 (14)0.0034 (13)0.0007 (13)0.0009 (11)
C590.0193 (14)0.0148 (14)0.0210 (15)0.0016 (11)0.0004 (11)0.0063 (11)
C600.0191 (15)0.0128 (12)0.0183 (13)0.0037 (11)0.0030 (11)0.0033 (10)
C610.0292 (18)0.0330 (19)0.043 (2)0.0080 (15)0.0029 (15)0.0029 (16)
C620.049 (2)0.034 (2)0.0348 (19)0.0156 (17)0.0043 (17)0.0065 (16)
C630.0218 (15)0.0239 (14)0.0144 (13)0.0075 (12)0.0015 (12)0.0016 (11)
N10.0139 (11)0.0127 (11)0.0137 (11)0.0012 (9)0.0027 (9)0.0021 (9)
N20.0149 (11)0.0138 (11)0.0173 (11)0.0029 (10)0.0013 (9)0.0029 (9)
N30.0114 (11)0.0155 (12)0.0187 (12)0.0018 (9)0.0014 (8)0.0006 (9)
N40.0134 (12)0.0164 (11)0.0130 (10)0.0011 (9)0.0002 (8)0.0002 (9)
N50.0180 (13)0.0449 (18)0.0306 (15)0.0007 (12)0.0074 (11)0.0008 (13)
N60.0362 (17)0.0500 (19)0.0250 (15)0.0201 (14)0.0053 (12)0.0057 (13)
N70.0272 (14)0.0337 (15)0.0259 (14)0.0009 (12)0.0063 (11)0.0019 (12)
N80.0286 (15)0.0269 (14)0.0251 (13)0.0012 (11)0.0049 (11)0.0025 (11)
N90.0205 (13)0.0201 (12)0.0348 (15)0.0015 (10)0.0019 (11)0.0000 (11)
N100.0240 (13)0.0151 (12)0.0268 (13)0.0003 (10)0.0006 (10)0.0021 (10)
N110.0246 (14)0.0265 (14)0.0198 (13)0.0019 (11)0.0042 (10)0.0029 (11)
N120.0207 (13)0.0170 (12)0.0172 (12)0.0017 (10)0.0036 (10)0.0026 (10)
N130.0149 (11)0.0151 (11)0.0205 (12)0.0003 (9)0.0019 (9)0.0015 (9)
O10.0165 (11)0.0345 (13)0.0363 (13)0.0052 (9)0.0013 (9)0.0051 (10)
O20.0498 (15)0.0315 (13)0.0306 (13)0.0160 (12)0.0073 (11)0.0032 (10)
O30.0330 (13)0.0299 (13)0.0344 (13)0.0002 (10)0.0034 (10)0.0044 (10)
O40.0225 (12)0.0338 (13)0.0289 (12)0.0011 (9)0.0049 (9)0.0049 (10)
O50.0234 (11)0.0228 (11)0.0303 (11)0.0003 (9)0.0050 (9)0.0013 (9)
O60.0313 (12)0.0245 (11)0.0269 (12)0.0017 (9)0.0069 (9)0.0012 (9)
O70.0244 (11)0.0305 (12)0.0284 (11)0.0021 (10)0.0043 (9)0.0018 (10)
O80.0241 (11)0.0216 (11)0.0252 (11)0.0002 (9)0.0035 (9)0.0006 (9)
O90.0253 (11)0.0300 (12)0.0208 (10)0.0029 (9)0.0029 (9)0.0013 (9)
O100.0295 (12)0.0164 (10)0.0197 (10)0.0006 (9)0.0058 (8)0.0021 (8)
O110.0239 (11)0.0211 (11)0.0189 (10)0.0020 (9)0.0000 (8)0.0028 (8)
O120.0185 (11)0.0293 (11)0.0222 (11)0.0017 (9)0.0001 (8)0.0100 (9)
O130.0215 (11)0.0210 (11)0.0209 (10)0.0063 (9)0.0022 (8)0.0038 (8)
O140.0280 (12)0.0352 (13)0.0298 (12)0.0086 (10)0.0059 (10)0.0085 (10)
P0.0196 (4)0.0181 (4)0.0158 (3)0.0013 (3)0.0017 (3)0.0020 (3)
Co0.01113 (16)0.01275 (16)0.01742 (17)0.00076 (14)0.00072 (14)0.00235 (14)
O1W0.0202 (12)0.0531 (15)0.0358 (12)0.0117 (11)0.0001 (10)0.0047 (11)
O2W0.0327 (13)0.0348 (13)0.0356 (13)0.0054 (11)0.0046 (10)0.0068 (11)
O3W0.0263 (12)0.0349 (13)0.0358 (13)0.0041 (10)0.0022 (10)0.0003 (10)
O4W0.0342 (13)0.0290 (13)0.0451 (15)0.0030 (10)0.0039 (11)0.0073 (11)
O5W0.0273 (13)0.0349 (14)0.0654 (17)0.0090 (11)0.0143 (12)0.0230 (13)
O6W0.0495 (17)0.0555 (18)0.0492 (16)0.0003 (14)0.0062 (14)0.0182 (14)
O7W0.0375 (15)0.0628 (19)0.0620 (19)0.0057 (14)0.0038 (14)0.0118 (15)
O8W0.0428 (16)0.0432 (16)0.073 (2)0.0146 (13)0.0018 (14)0.0012 (15)
O9W0.0463 (17)0.115 (3)0.0347 (15)0.0134 (19)0.0037 (14)0.0125 (16)
O10W0.073 (2)0.099 (3)0.064 (2)0.006 (2)0.0026 (19)0.0061 (19)
O11W0.096 (3)0.075 (2)0.074 (2)0.018 (2)0.034 (2)0.0183 (19)
O12A0.031 (3)0.050 (3)0.031 (3)0.003 (2)0.008 (2)0.002 (2)
O12B0.040 (4)0.043 (4)0.040 (4)0.012 (3)0.005 (4)0.004 (3)
C64A0.036 (2)0.037 (5)0.028 (2)0.014 (2)0.0057 (18)0.008 (3)
C65A0.037 (4)0.052 (4)0.025 (2)0.021 (3)0.000 (3)0.005 (2)
C66A0.061 (2)0.060 (2)0.059 (2)0.0009 (10)0.0007 (10)0.0005 (10)
C67A0.0619 (19)0.061 (2)0.0599 (19)0.0024 (8)0.0007 (8)0.0015 (8)
C64B0.036 (2)0.037 (5)0.028 (2)0.014 (2)0.0055 (18)0.008 (3)
C65B0.036 (4)0.051 (4)0.024 (2)0.021 (3)0.000 (3)0.004 (3)
C66B0.039 (5)0.036 (5)0.011 (4)0.002 (4)0.003 (3)0.002 (3)
C67B0.0618 (19)0.061 (2)0.060 (2)0.0020 (8)0.0007 (8)0.0010 (8)
O150.054 (5)0.086 (7)0.058 (5)0.005 (5)0.011 (4)0.007 (5)
C700.048 (6)0.038 (6)0.048 (6)0.007 (5)0.008 (5)0.002 (5)
C690.047 (6)0.072 (8)0.035 (6)0.004 (6)0.013 (5)0.020 (6)
C680.16 (2)0.18 (2)0.106 (14)0.127 (18)0.076 (14)0.070 (14)
O13W0.076 (8)0.065 (7)0.165 (13)0.001 (6)0.010 (8)0.001 (8)
Geometric parameters (Å, º) top
C1—N11.504 (3)C48—H48A0.98
C1—C201.535 (4)C48—H48B0.98
C1—C191.558 (4)C48—H48C0.98
C1—C21.582 (4)C49—O121.430 (4)
C2—C211.528 (4)C49—N121.447 (3)
C2—C221.560 (4)C49—C501.529 (4)
C2—C31.561 (4)C49—H491
C3—C41.523 (4)C50—O131.407 (3)
C3—C241.559 (4)C50—C511.515 (4)
C3—H31C50—H501
C4—N11.291 (3)C51—O101.429 (3)
C4—C51.453 (4)C51—C521.528 (4)
C5—C61.359 (4)C51—H511
C5—C271.525 (4)C52—O121.453 (4)
C6—N21.405 (4)C52—C531.512 (4)
C6—C71.552 (4)C52—H521
C7—C281.534 (4)C53—O141.405 (4)
C7—C81.559 (4)C53—H53A0.99
C7—C291.564 (4)C53—H53B0.99
C8—C91.501 (4)C54—N131.313 (4)
C8—C311.562 (4)C54—N121.358 (4)
C8—H81C54—H540.95
C9—N21.338 (3)C55—C561.394 (4)
C9—C101.383 (4)C55—C601.397 (4)
C10—C111.383 (4)C55—H550.95
C10—H100.95C56—C571.426 (5)
C11—N31.346 (3)C56—C611.503 (4)
C11—C121.522 (4)C57—C581.388 (5)
C12—C351.531 (4)C57—C621.512 (4)
C12—C341.534 (4)C58—C591.407 (4)
C12—C131.554 (4)C58—H580.95
C13—C141.534 (4)C59—C601.387 (4)
C13—C361.549 (4)C59—N121.395 (4)
C13—H131C60—N131.414 (4)
C14—C151.371 (4)C61—H61A0.98
C14—N31.386 (3)C61—H61B0.98
C15—C161.446 (4)C61—H61C0.98
C15—C391.518 (4)C62—H62A0.98
C16—N41.303 (4)C62—H62B0.98
C16—C171.543 (4)C62—H62C0.98
C17—C431.542 (4)C63—C64A1.454 (10)
C17—C401.544 (4)C63—C64B1.506 (18)
C17—C181.560 (4)C63—Co2.044 (3)
C18—C191.536 (4)C63—H63A0.99
C18—C411.543 (4)C63—H63B0.99
C18—H181N1—Co1.869 (2)
C19—N41.490 (3)N2—Co1.914 (2)
C19—H191N3—Co1.915 (2)
C20—H20A0.98N4—Co1.889 (2)
C20—H20B0.98N5—H5A0.88
C20—H20C0.98N5—H5B0.88
C21—H21A0.98N6—H6A0.88
C21—H21B0.98N6—H6B0.88
C21—H21C0.98N7—H7A0.88
C22—C231.526 (4)N7—H7B0.88
C22—H22A0.99N8—H8A0.88
C22—H22B0.99N8—H8B0.88
C23—O11.235 (4)N9—H9A0.88
C23—N51.334 (4)N9—H9B0.88
C24—C251.537 (4)N10—H10A0.88
C24—H24A0.99N10—H10B0.88
C24—H24B0.99N11—H110.88
C25—C261.513 (4)N13—Co2.277 (2)
C25—H25A0.99O8—P1.496 (2)
C25—H25B0.99O9—P1.486 (2)
C26—O21.248 (4)O10—P1.606 (2)
C26—N61.320 (4)O11—P1.583 (2)
C27—H27A0.98O13—H13A0.84
C27—H27B0.98O14—H140.84
C27—H27C0.98O1W—H1Y0.8492
C28—H28A0.98O1W—H1Z0.8508
C28—H28B0.98O2W—H2Y0.8503
C28—H28C0.98O2W—H2Z0.8498
C29—C301.520 (4)O3W—H3Y0.8504
C29—H29A0.99O3W—H3Z0.8507
C29—H29B0.99O4W—H4Y0.8489
C30—O31.240 (4)O4W—H4Z0.8503
C30—N71.339 (4)O5W—H5Y0.8505
C31—C321.532 (4)O5W—H5Z0.849
C31—H31A0.99O6W—H6Y0.851
C31—H31B0.99O6W—H6Z0.8501
C32—C331.498 (4)O7W—H7Y0.8491
C32—H32A0.99O7W—H7Z0.8509
C32—H32B0.99O8W—H8Y0.8499
C33—O41.247 (4)O8W—H8Z0.8506
C33—N81.333 (4)O9W—H9Y0.8495
C34—H34A0.98O9W—H9Z0.8506
C34—H34B0.98O10W—H10Y0.85
C34—H34C0.98O10W—H10Z0.8505
C35—H35A0.98O12A—H12W0.9298
C35—H35B0.98O12B—H12W0.8509
C35—H35C0.98O12B—H12X0.8504
C36—C371.542 (4)C64A—C65A1.538 (7)
C36—H36A0.99C64A—H64A0.99
C36—H36B0.99C64A—H64B0.99
C37—C381.505 (4)C65A—C66A1.549 (9)
C37—H37A0.99C65A—C67A1.555 (7)
C37—H37B0.99C65A—H65A1
C38—O51.249 (4)C66A—H66A0.98
C38—N91.327 (4)C66A—H66B0.98
C39—H39A0.98C66A—H66C0.98
C39—H39B0.98C67A—H67A0.98
C39—H39C0.98C67A—H67B0.98
C40—H40A0.98C67A—H67C0.98
C40—H40B0.98C64B—C65B1.538 (7)
C40—H40C0.98C64B—H64C0.99
C41—C421.514 (4)C64B—H64D0.99
C41—H41A0.99C65B—C66B1.549 (9)
C41—H41B0.99C65B—C67B1.555 (7)
C42—O61.245 (4)C65B—H65B1
C42—N101.321 (4)C66B—H66D0.98
C43—C441.537 (4)C66B—H66E0.98
C43—H43A0.99C66B—H66F0.98
C43—H43B0.99C67B—H67D0.98
C44—C451.524 (4)C67B—H67E0.98
C44—H44A0.99C67B—H67F0.98
C44—H44B0.99O15—C691.205 (10)
C45—O71.236 (4)C70—C691.503 (12)
C45—N111.347 (4)C70—H70A0.98
C46—N111.452 (4)C70—H70B0.98
C46—C471.527 (4)C70—H70C0.98
C46—H46A0.99C69—C681.531 (14)
C46—H46B0.99C68—H68A0.98
C47—O111.453 (3)C68—H68B0.98
C47—C481.515 (4)C68—H68C0.98
C47—H471
N1—C1—C20109.7 (2)O7—C45—C44121.2 (3)
N1—C1—C19102.4 (2)N11—C45—C44117.5 (3)
C20—C1—C19108.5 (2)N11—C46—C47111.8 (2)
N1—C1—C2101.9 (2)N11—C46—H46A109.3
C20—C1—C2113.6 (2)C47—C46—H46A109.3
C19—C1—C2119.5 (2)N11—C46—H46B109.3
C21—C2—C22110.3 (2)C47—C46—H46B109.3
C21—C2—C3114.3 (2)H46A—C46—H46B107.9
C22—C2—C3107.2 (2)O11—C47—C48109.1 (2)
C21—C2—C1113.1 (2)O11—C47—C46104.9 (2)
C22—C2—C1110.1 (2)C48—C47—C46112.2 (3)
C3—C2—C1101.4 (2)O11—C47—H47110.1
C4—C3—C24110.8 (2)C48—C47—H47110.1
C4—C3—C2101.4 (2)C46—C47—H47110.1
C24—C3—C2118.5 (2)C47—C48—H48A109.5
C4—C3—H3108.5C47—C48—H48B109.5
C24—C3—H3108.5H48A—C48—H48B109.5
C2—C3—H3108.5C47—C48—H48C109.5
N1—C4—C5124.6 (2)H48A—C48—H48C109.5
N1—C4—C3112.2 (2)H48B—C48—H48C109.5
C5—C4—C3123.2 (2)O12—C49—N12106.9 (2)
C6—C5—C4120.9 (2)O12—C49—C50106.4 (2)
C6—C5—C27123.8 (2)N12—C49—C50113.4 (2)
C4—C5—C27115.3 (2)O12—C49—H49110
C5—C6—N2124.1 (2)N12—C49—H49110
C5—C6—C7128.5 (2)C50—C49—H49110
N2—C6—C7107.5 (2)O13—C50—C51111.6 (2)
C28—C7—C6117.6 (2)O13—C50—C49108.0 (2)
C28—C7—C8111.0 (2)C51—C50—C49100.5 (2)
C6—C7—C8100.4 (2)O13—C50—H50112.1
C28—C7—C29110.8 (2)C51—C50—H50112.1
C6—C7—C29110.9 (2)C49—C50—H50112.1
C8—C7—C29105.0 (2)O10—C51—C50111.8 (2)
C9—C8—C7100.7 (2)O10—C51—C52110.3 (2)
C9—C8—C31110.1 (2)C50—C51—C52103.3 (2)
C7—C8—C31113.7 (2)O10—C51—H51110.4
C9—C8—H8110.7C50—C51—H51110.4
C7—C8—H8110.7C52—C51—H51110.4
C31—C8—H8110.7O12—C52—C53108.4 (3)
N2—C9—C10126.3 (3)O12—C52—C51104.3 (2)
N2—C9—C8110.7 (2)C53—C52—C51115.4 (3)
C10—C9—C8123.0 (2)O12—C52—H52109.5
C11—C10—C9125.1 (3)C53—C52—H52109.5
C11—C10—H10117.4C51—C52—H52109.5
C9—C10—H10117.4O14—C53—C52112.8 (3)
N3—C11—C10124.8 (3)O14—C53—H53A109
N3—C11—C12111.9 (2)C52—C53—H53A109
C10—C11—C12123.3 (2)O14—C53—H53B109
C11—C12—C35113.0 (2)C52—C53—H53B109
C11—C12—C34108.4 (2)H53A—C53—H53B107.8
C35—C12—C34109.3 (2)N13—C54—N12114.3 (3)
C11—C12—C13100.5 (2)N13—C54—H54122.8
C35—C12—C13116.6 (2)N12—C54—H54122.8
C34—C12—C13108.5 (2)C56—C55—C60119.2 (3)
C14—C13—C36106.6 (2)C56—C55—H55120.4
C14—C13—C12101.9 (2)C60—C55—H55120.4
C36—C13—C12116.9 (2)C55—C56—C57120.2 (3)
C14—C13—H13110.3C55—C56—C61119.6 (3)
C36—C13—H13110.3C57—C56—C61120.3 (3)
C12—C13—H13110.3C58—C57—C56121.1 (3)
C15—C14—N3127.1 (2)C58—C57—C62118.6 (3)
C15—C14—C13123.5 (2)C56—C57—C62120.3 (3)
N3—C14—C13109.2 (2)C57—C58—C59117.0 (3)
C14—C15—C16121.0 (2)C57—C58—H58121.5
C14—C15—C39118.6 (2)C59—C58—H58121.5
C16—C15—C39120.4 (2)C60—C59—N12105.9 (2)
N4—C16—C15122.3 (2)C60—C59—C58123.0 (3)
N4—C16—C17111.7 (2)N12—C59—C58131.2 (3)
C15—C16—C17125.8 (2)C59—C60—C55119.6 (3)
C43—C17—C16116.1 (2)C59—C60—N13109.6 (2)
C43—C17—C40108.5 (2)C55—C60—N13130.7 (3)
C16—C17—C40107.6 (2)C56—C61—H61A109.5
C43—C17—C18112.2 (2)C56—C61—H61B109.5
C16—C17—C18100.7 (2)H61A—C61—H61B109.5
C40—C17—C18111.6 (2)C56—C61—H61C109.5
C19—C18—C41114.0 (2)H61A—C61—H61C109.5
C19—C18—C17102.9 (2)H61B—C61—H61C109.5
C41—C18—C17115.6 (2)C57—C62—H62A109.5
C19—C18—H18108C57—C62—H62B109.5
C41—C18—H18108H62A—C62—H62B109.5
C17—C18—H18108C57—C62—H62C109.5
N4—C19—C18102.9 (2)H62A—C62—H62C109.5
N4—C19—C1105.4 (2)H62B—C62—H62C109.5
C18—C19—C1121.8 (2)C64A—C63—Co119.0 (3)
N4—C19—H19108.7C64B—C63—Co116.0 (4)
C18—C19—H19108.7C64A—C63—H63A107.6
C1—C19—H19108.7C64B—C63—H63A116.9
C1—C20—H20A109.5Co—C63—H63A107.6
C1—C20—H20B109.5C64A—C63—H63B107.6
H20A—C20—H20B109.5C64B—C63—H63B100.9
C1—C20—H20C109.5Co—C63—H63B107.6
H20A—C20—H20C109.5H63A—C63—H63B107
H20B—C20—H20C109.5C4—N1—C1112.1 (2)
C2—C21—H21A109.5C4—N1—Co130.71 (19)
C2—C21—H21B109.5C1—N1—Co117.19 (16)
H21A—C21—H21B109.5C9—N2—C6110.5 (2)
C2—C21—H21C109.5C9—N2—Co122.65 (19)
H21A—C21—H21C109.5C6—N2—Co126.73 (18)
H21B—C21—H21C109.5C11—N3—C14110.0 (2)
C23—C22—C2114.4 (2)C11—N3—Co124.03 (18)
C23—C22—H22A108.6C14—N3—Co125.97 (18)
C2—C22—H22A108.6C16—N4—C19111.5 (2)
C23—C22—H22B108.6C16—N4—Co133.07 (19)
C2—C22—H22B108.6C19—N4—Co114.79 (16)
H22A—C22—H22B107.6C23—N5—H5A120
O1—C23—N5121.9 (3)C23—N5—H5B120
O1—C23—C22121.7 (3)H5A—N5—H5B120
N5—C23—C22116.4 (3)C26—N6—H6A120
C25—C24—C3112.8 (2)C26—N6—H6B120
C25—C24—H24A109H6A—N6—H6B120
C3—C24—H24A109C30—N7—H7A120
C25—C24—H24B109C30—N7—H7B120
C3—C24—H24B109H7A—N7—H7B120
H24A—C24—H24B107.8C33—N8—H8A120
C26—C25—C24111.9 (2)C33—N8—H8B120
C26—C25—H25A109.2H8A—N8—H8B120
C24—C25—H25A109.2C38—N9—H9A120
C26—C25—H25B109.2C38—N9—H9B120
C24—C25—H25B109.2H9A—N9—H9B120
H25A—C25—H25B107.9C42—N10—H10A120
O2—C26—N6122.5 (3)C42—N10—H10B120
O2—C26—C25121.3 (3)H10A—N10—H10B120
N6—C26—C25116.2 (3)C45—N11—C46120.9 (3)
C5—C27—H27A109.5C45—N11—H11119.6
C5—C27—H27B109.5C46—N11—H11119.6
H27A—C27—H27B109.5C54—N12—C59106.1 (2)
C5—C27—H27C109.5C54—N12—C49125.4 (2)
H27A—C27—H27C109.5C59—N12—C49124.6 (2)
H27B—C27—H27C109.5C54—N13—C60104.0 (2)
C7—C28—H28A109.5C54—N13—Co121.55 (19)
C7—C28—H28B109.5C60—N13—Co134.32 (18)
H28A—C28—H28B109.5C51—O10—P120.87 (17)
C7—C28—H28C109.5C47—O11—P121.13 (18)
H28A—C28—H28C109.5C49—O12—C52110.0 (2)
H28B—C28—H28C109.5C50—O13—H13A109.5
C30—C29—C7117.5 (2)C53—O14—H14109.5
C30—C29—H29A107.9O9—P—O8117.72 (12)
C7—C29—H29A107.9O9—P—O11105.40 (12)
C30—C29—H29B107.9O8—P—O11112.29 (12)
C7—C29—H29B107.9O9—P—O10111.33 (12)
H29A—C29—H29B107.2O8—P—O10108.81 (12)
O3—C30—N7122.4 (3)O11—P—O1099.82 (11)
O3—C30—C29119.2 (3)N1—Co—N483.33 (9)
N7—C30—C29118.4 (3)N1—Co—N290.39 (10)
C32—C31—C8113.3 (2)N4—Co—N2173.40 (10)
C32—C31—H31A108.9N1—Co—N3172.56 (10)
C8—C31—H31A108.9N4—Co—N390.44 (9)
C32—C31—H31B108.9N2—Co—N395.97 (10)
C8—C31—H31B108.9N1—Co—C6392.63 (11)
H31A—C31—H31B107.7N4—Co—C6390.60 (10)
C33—C32—C31117.2 (3)N2—Co—C6387.66 (10)
C33—C32—H32A108N3—Co—C6391.49 (11)
C31—C32—H32A108N1—Co—N1389.77 (9)
C33—C32—H32B108N4—Co—N1396.46 (9)
C31—C32—H32B108N2—Co—N1385.49 (9)
H32A—C32—H32B107.2N3—Co—N1386.89 (9)
O4—C33—N8120.8 (3)C63—Co—N13172.76 (10)
O4—C33—C32119.9 (3)H1Y—O1W—H1Z100.6
N8—C33—C32119.2 (3)H2Y—O2W—H2Z105
C12—C34—H34A109.5H3Y—O3W—H3Z90.3
C12—C34—H34B109.5H4Y—O4W—H4Z114
H34A—C34—H34B109.5H5Y—O5W—H5Z120.8
C12—C34—H34C109.5H6Y—O6W—H6Z112.2
H34A—C34—H34C109.5H7Y—O7W—H7Z105.2
H34B—C34—H34C109.5H8Y—O8W—H8Z85.9
C12—C35—H35A109.5H9Y—O9W—H9Z123.3
C12—C35—H35B109.5H10Y—O10W—H10Z116.8
H35A—C35—H35B109.5H12W—O12B—H12X110.3
C12—C35—H35C109.5C63—C64A—C65A116.6 (5)
H35A—C35—H35C109.5C63—C64A—H64A108.1
H35B—C35—H35C109.5C65A—C64A—H64A108.1
C37—C36—C13117.3 (2)C63—C64A—H64B108.1
C37—C36—H36A108C65A—C64A—H64B108.1
C13—C36—H36A108H64A—C64A—H64B107.3
C37—C36—H36B108C64A—C65A—C66A110.8 (6)
C13—C36—H36B108C64A—C65A—C67A107.2 (5)
H36A—C36—H36B107.2C66A—C65A—C67A109.9 (5)
C38—C37—C36112.9 (2)C64A—C65A—H65A109.7
C38—C37—H37A109C66A—C65A—H65A109.7
C36—C37—H37A109C67A—C65A—H65A109.7
C38—C37—H37B109C63—C64B—C65B114.6 (14)
C36—C37—H37B109C63—C64B—H64C108.6
H37A—C37—H37B107.8C65B—C64B—H64C108.6
O5—C38—N9122.5 (3)C63—C64B—H64D108.6
O5—C38—C37120.7 (3)C65B—C64B—H64D108.6
N9—C38—C37116.8 (3)H64C—C64B—H64D107.6
C15—C39—H39A109.5C64B—C65B—C66B110.7 (6)
C15—C39—H39B109.5C64B—C65B—C67B107.1 (5)
H39A—C39—H39B109.5C66B—C65B—C67B109.7 (5)
C15—C39—H39C109.5C64B—C65B—H65B109.7
H39A—C39—H39C109.5C66B—C65B—H65B109.7
H39B—C39—H39C109.5C67B—C65B—H65B109.7
C17—C40—H40A109.5C65B—C66B—H66D109.5
C17—C40—H40B109.5C65B—C66B—H66E109.5
H40A—C40—H40B109.5H66D—C66B—H66E109.5
C17—C40—H40C109.5C65B—C66B—H66F109.5
H40A—C40—H40C109.5H66D—C66B—H66F109.5
H40B—C40—H40C109.5H66E—C66B—H66F109.5
C42—C41—C18113.4 (2)C65B—C67B—H67D109.5
C42—C41—H41A108.9C65B—C67B—H67E109.5
C18—C41—H41A108.9H67D—C67B—H67E109.5
C42—C41—H41B108.9C65B—C67B—H67F109.5
C18—C41—H41B108.9H67D—C67B—H67F109.5
H41A—C41—H41B107.7H67E—C67B—H67F109.5
O6—C42—N10122.1 (3)C69—C70—H70A109.5
O6—C42—C41120.3 (3)C69—C70—H70B109.5
N10—C42—C41117.6 (3)H70A—C70—H70B109.5
C44—C43—C17115.8 (2)C69—C70—H70C109.5
C44—C43—H43A108.3H70A—C70—H70C109.5
C17—C43—H43A108.3H70B—C70—H70C109.5
C44—C43—H43B108.3O15—C69—C70121.1 (10)
C17—C43—H43B108.3O15—C69—C68124.6 (11)
H43A—C43—H43B107.4C70—C69—C68114.2 (9)
C45—C44—C43109.2 (2)C69—C68—H68A109.5
C45—C44—H44A109.8C69—C68—H68B109.5
C43—C44—H44A109.8H68A—C68—H68B109.5
C45—C44—H44B109.8C69—C68—H68C109.5
C43—C44—H44B109.8H68A—C68—H68C109.5
H44A—C44—H44B108.3H68B—C68—H68C109.5
O7—C45—N11121.3 (3)
N1—C1—C2—C21153.5 (2)O12—C52—C53—O1457.6 (3)
C20—C1—C2—C2135.5 (3)C51—C52—C53—O1458.9 (4)
C19—C1—C2—C2194.8 (3)C60—C55—C56—C570.2 (4)
N1—C1—C2—C2282.6 (2)C60—C55—C56—C61179.9 (3)
C20—C1—C2—C22159.5 (2)C55—C56—C57—C580.1 (5)
C19—C1—C2—C2229.2 (3)C61—C56—C57—C58179.8 (3)
N1—C1—C2—C330.6 (2)C55—C56—C57—C62178.4 (3)
C20—C1—C2—C387.3 (3)C61—C56—C57—C621.7 (5)
C19—C1—C2—C3142.4 (2)C56—C57—C58—C590.9 (4)
C21—C2—C3—C4153.0 (2)C62—C57—C58—C59177.7 (3)
C22—C2—C3—C484.4 (2)C57—C58—C59—C601.3 (4)
C1—C2—C3—C431.0 (2)C57—C58—C59—N12178.6 (3)
C21—C2—C3—C2431.5 (3)N12—C59—C60—C55178.9 (2)
C22—C2—C3—C24154.1 (2)C58—C59—C60—C551.0 (4)
C1—C2—C3—C2490.5 (3)N12—C59—C60—N130.1 (3)
C24—C3—C4—N1105.1 (3)C58—C59—C60—N13179.9 (2)
C2—C3—C4—N121.6 (3)C56—C55—C60—C590.2 (4)
C24—C3—C4—C572.5 (3)C56—C55—C60—N13179.1 (3)
C2—C3—C4—C5160.8 (2)C5—C4—N1—C1178.8 (2)
N1—C4—C5—C69.4 (4)C3—C4—N1—C11.3 (3)
C3—C4—C5—C6167.9 (3)C5—C4—N1—Co3.5 (4)
N1—C4—C5—C27170.1 (3)C3—C4—N1—Co178.98 (18)
C3—C4—C5—C2712.6 (4)C20—C1—N1—C4101.3 (3)
C4—C5—C6—N25.7 (4)C19—C1—N1—C4143.6 (2)
C27—C5—C6—N2173.7 (3)C2—C1—N1—C419.4 (3)
C4—C5—C6—C7174.6 (3)C20—C1—N1—Co80.6 (2)
C27—C5—C6—C76.0 (5)C19—C1—N1—Co34.5 (2)
C5—C6—C7—C2836.1 (4)C2—C1—N1—Co158.65 (16)
N2—C6—C7—C28144.2 (2)C10—C9—N2—C6164.4 (3)
C5—C6—C7—C8156.6 (3)C8—C9—N2—C614.8 (3)
N2—C6—C7—C823.7 (3)C10—C9—N2—Co12.6 (4)
C5—C6—C7—C2992.9 (3)C8—C9—N2—Co168.27 (18)
N2—C6—C7—C2986.8 (3)C5—C6—N2—C9173.5 (3)
C28—C7—C8—C9155.0 (2)C7—C6—N2—C96.7 (3)
C6—C7—C8—C929.9 (2)C5—C6—N2—Co9.7 (4)
C29—C7—C8—C985.3 (2)C7—C6—N2—Co170.07 (17)
C28—C7—C8—C3137.3 (3)C10—C11—N3—C14172.2 (3)
C6—C7—C8—C3187.8 (2)C12—C11—N3—C148.9 (3)
C29—C7—C8—C31157.1 (2)C10—C11—N3—Co6.5 (4)
C7—C8—C9—N229.2 (3)C12—C11—N3—Co172.32 (18)
C31—C8—C9—N291.2 (3)C15—C14—N3—C11176.7 (3)
C7—C8—C9—C10150.0 (3)C13—C14—N3—C118.5 (3)
C31—C8—C9—C1089.6 (3)C15—C14—N3—Co4.5 (4)
N2—C9—C10—C115.6 (5)C13—C14—N3—Co170.26 (18)
C8—C9—C10—C11175.3 (3)C15—C16—N4—C19171.4 (2)
C9—C10—C11—N35.0 (5)C17—C16—N4—C193.5 (3)
C9—C10—C11—C12173.7 (3)C15—C16—N4—Co1.0 (4)
N3—C11—C12—C35146.5 (2)C17—C16—N4—Co173.90 (18)
C10—C11—C12—C3534.6 (4)C18—C19—N4—C1622.5 (3)
N3—C11—C12—C3492.1 (3)C1—C19—N4—C16151.2 (2)
C10—C11—C12—C3486.7 (3)C18—C19—N4—Co165.15 (16)
N3—C11—C12—C1321.6 (3)C1—C19—N4—Co36.5 (2)
C10—C11—C12—C13159.6 (3)O7—C45—N11—C462.8 (4)
C11—C12—C13—C1424.0 (3)C44—C45—N11—C46179.1 (3)
C35—C12—C13—C14146.4 (2)C47—C46—N11—C4582.5 (3)
C34—C12—C13—C1489.7 (3)N13—C54—N12—C593.7 (3)
C11—C12—C13—C3691.8 (3)N13—C54—N12—C49162.1 (3)
C35—C12—C13—C3630.7 (3)C60—C59—N12—C542.0 (3)
C34—C12—C13—C36154.6 (2)C58—C59—N12—C54178.0 (3)
C36—C13—C14—C1573.3 (3)C60—C59—N12—C49160.6 (3)
C12—C13—C14—C15163.7 (3)C58—C59—N12—C4919.3 (5)
C36—C13—C14—N3101.8 (3)O12—C49—N12—C5447.0 (3)
C12—C13—C14—N321.3 (3)C50—C49—N12—C5469.9 (3)
N3—C14—C15—C162.2 (4)O12—C49—N12—C59158.4 (2)
C13—C14—C15—C16171.9 (2)C50—C49—N12—C5984.7 (3)
N3—C14—C15—C39176.9 (3)N12—C54—N13—C603.7 (3)
C13—C14—C15—C399.0 (4)N12—C54—N13—Co172.91 (17)
C14—C15—C16—N40.7 (4)C59—C60—N13—C542.2 (3)
C39—C15—C16—N4179.8 (2)C55—C60—N13—C54176.7 (3)
C14—C15—C16—C17173.5 (3)C59—C60—N13—Co173.70 (18)
C39—C15—C16—C175.6 (4)C55—C60—N13—Co7.4 (4)
N4—C16—C17—C43137.9 (2)C50—C51—O10—P123.0 (2)
C15—C16—C17—C4347.3 (4)C52—C51—O10—P122.6 (2)
N4—C16—C17—C40100.3 (3)C48—C47—O11—P102.8 (3)
C15—C16—C17—C4074.4 (3)C46—C47—O11—P136.8 (2)
N4—C16—C17—C1816.6 (3)N12—C49—O12—C52135.3 (2)
C15—C16—C17—C18168.7 (2)C50—C49—O12—C5213.9 (3)
C43—C17—C18—C19152.7 (2)C53—C52—O12—C49134.5 (2)
C16—C17—C18—C1928.7 (2)C51—C52—O12—C4911.1 (3)
C40—C17—C18—C1985.2 (3)C47—O11—P—O9177.44 (19)
C43—C17—C18—C4182.4 (3)C47—O11—P—O853.2 (2)
C16—C17—C18—C41153.6 (2)C47—O11—P—O1061.9 (2)
C40—C17—C18—C4139.7 (3)C51—O10—P—O984.4 (2)
C41—C18—C19—N4157.1 (2)C51—O10—P—O847.0 (2)
C17—C18—C19—N431.2 (2)C51—O10—P—O11164.7 (2)
C41—C18—C19—C185.4 (3)C4—N1—Co—N4164.6 (3)
C17—C18—C19—C1148.8 (2)C1—N1—Co—N413.05 (18)
N1—C1—C19—N441.6 (2)C4—N1—Co—N213.4 (2)
C20—C1—C19—N474.3 (3)C1—N1—Co—N2168.98 (18)
C2—C1—C19—N4153.2 (2)C4—N1—Co—C6374.3 (3)
N1—C1—C19—C18157.9 (2)C1—N1—Co—C63103.34 (19)
C20—C1—C19—C1842.0 (3)C4—N1—Co—N1398.9 (2)
C2—C1—C19—C1890.5 (3)C1—N1—Co—N1383.49 (18)
C21—C2—C22—C2366.8 (3)C16—N4—Co—N1175.2 (3)
C3—C2—C22—C2358.2 (3)C19—N4—Co—N114.61 (18)
C1—C2—C22—C23167.7 (2)C16—N4—Co—N30.7 (3)
C2—C22—C23—O161.8 (4)C19—N4—Co—N3169.47 (18)
C2—C22—C23—N5118.8 (3)C16—N4—Co—C6392.2 (3)
C4—C3—C24—C25155.5 (2)C19—N4—Co—C6377.98 (19)
C2—C3—C24—C2587.9 (3)C16—N4—Co—N1386.2 (3)
C3—C24—C25—C26171.0 (2)C19—N4—Co—N13103.61 (18)
C24—C25—C26—O290.6 (4)C9—N2—Co—N1167.5 (2)
C24—C25—C26—N690.8 (3)C6—N2—Co—N116.0 (2)
C28—C7—C29—C3084.6 (3)C9—N2—Co—N38.6 (2)
C6—C7—C29—C3047.9 (3)C6—N2—Co—N3167.8 (2)
C8—C7—C29—C30155.5 (2)C9—N2—Co—C6399.9 (2)
C7—C29—C30—O399.7 (3)C6—N2—Co—C6376.6 (2)
C7—C29—C30—N782.8 (3)C9—N2—Co—N1377.8 (2)
C9—C8—C31—C3249.9 (3)C6—N2—Co—N13105.8 (2)
C7—C8—C31—C32162.0 (2)C11—N3—Co—N4178.2 (2)
C8—C31—C32—C33178.0 (2)C14—N3—Co—N43.2 (2)
C31—C32—C33—O4168.6 (3)C11—N3—Co—N20.2 (2)
C31—C32—C33—N812.2 (4)C14—N3—Co—N2178.3 (2)
C14—C13—C36—C37170.6 (2)C11—N3—Co—C6387.6 (2)
C12—C13—C36—C3776.2 (3)C14—N3—Co—C6393.9 (2)
C13—C36—C37—C3841.4 (4)C11—N3—Co—N1385.3 (2)
C36—C37—C38—O5106.7 (3)C14—N3—Co—N1393.2 (2)
C36—C37—C38—N972.7 (3)C64A—C63—Co—N1129.8 (7)
C19—C18—C41—C42175.2 (2)C64B—C63—Co—N1119.3 (10)
C17—C18—C41—C4265.9 (3)C64A—C63—Co—N446.4 (7)
C18—C41—C42—O653.4 (4)C64B—C63—Co—N436.0 (10)
C18—C41—C42—N10127.1 (3)C64A—C63—Co—N2139.9 (7)
C16—C17—C43—C4449.2 (3)C64B—C63—Co—N2150.4 (10)
C40—C17—C43—C44170.5 (2)C64A—C63—Co—N344.0 (7)
C18—C17—C43—C4465.7 (3)C64B—C63—Co—N354.5 (10)
C17—C43—C44—C45161.5 (2)C54—N13—Co—N1137.1 (2)
C43—C44—C45—O763.8 (4)C60—N13—Co—N147.6 (2)
C43—C44—C45—N11114.3 (3)C54—N13—Co—N453.8 (2)
N11—C46—C47—O1163.3 (3)C60—N13—Co—N4130.8 (2)
N11—C46—C47—C48178.3 (3)C54—N13—Co—N2132.5 (2)
O12—C49—C50—O1384.2 (3)C60—N13—Co—N242.8 (2)
N12—C49—C50—O1333.0 (3)C54—N13—Co—N336.3 (2)
O12—C49—C50—C5132.8 (3)C60—N13—Co—N3139.1 (2)
N12—C49—C50—C51150.0 (2)C64B—C63—C64A—C65A96 (3)
O13—C50—C51—O1043.1 (3)Co—C63—C64A—C65A170.6 (7)
C49—C50—C51—O10157.3 (2)C63—C64A—C65A—C66A75.6 (11)
O13—C50—C51—C5275.5 (3)C63—C64A—C65A—C67A164.6 (10)
C49—C50—C51—C5238.7 (3)C64A—C63—C64B—C65B39 (2)
O10—C51—C52—O12151.3 (2)Co—C63—C64B—C65B149.5 (6)
C50—C51—C52—O1231.7 (3)C63—C64B—C65B—C66B51.8 (12)
O10—C51—C52—C5390.0 (3)C63—C64B—C65B—C67B171.5 (12)
C50—C51—C52—C53150.5 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N5—H5A···O9W0.882.233.085 (4)165
N5—H5B···O8W0.882.213.025 (4)153
N6—H6A···O12Ai0.882.333.101 (6)147
N6—H6B···O9ii0.882.052.931 (4)179
N7—H7A···O7W0.882.173.020 (4)163
N7—H7B···O5Wiii0.882.122.891 (4)146
N8—H8B···O1iii0.882.162.948 (3)148
N9—H9A···O1iv0.882.23.020 (3)154
N9—H9B···O2Wiv0.881.972.843 (4)170
N10—H10A···O5v0.882.163.021 (3)165
N10—H10B···O2vi0.882.012.862 (4)162
N11—H11···O12Bvii0.882.153.025 (8)171
N11—H11···O12Avii0.882.233.097 (5)167
O13—H13A···O1Wvii0.841.872.705 (3)178
O14—H14···O6Wviii0.841.932.759 (3)168
O1W—H1Y···O8ix0.851.842.687 (3)180
O1W—H1Z···O12B0.851.812.664 (8)179
O2W—H2Y···O7x0.851.962.810 (3)180
O2W—H2Z···O3Wxi0.851.932.780 (3)180
O3W—H3Y···O9xii0.851.862.715 (3)180
O3W—H3Z···O1Wxiii0.852.062.906 (3)180
O4W—H4Y···O4xiv0.851.932.777 (3)180
O4W—H4Z···O12xiv0.852.193.036 (3)180
O5W—H5Y···O60.851.932.780 (3)179
O5W—H5Z···O8ii0.851.852.699 (3)178
O6W—H6Y···O4W0.851.922.770 (4)179
O6W—H6Z···O2xv0.852.142.987 (4)180
O7W—H7Y···O6Wxvi0.852.072.919 (4)180
O7W—H7Z···O10Wiii0.8522.856 (5)179
O8W—H8Y···O30.851.942.788 (4)180
O8W—H8Z···O7W0.852.062.911 (4)180
O9W—H9Y···O11Wiii0.852.12.948 (5)180
O9W—H9Z···O5x0.851.992.836 (4)180
O10W—H10Y···O60.851.972.823 (4)179
O10W—H10Z···O13Wxvii0.852.062.908 (15)179
O12B—H12W···O14ix0.852.042.886 (8)180
O12B—H12X···O6xi0.852.132.981 (8)180
Symmetry codes: (i) x, y, z+1; (ii) x1/2, y+1/2, z+2; (iii) x+1, y1/2, z+3/2; (iv) x+1, y, z; (v) x+2, y+1/2, z+3/2; (vi) x+1, y+1/2, z+3/2; (vii) x+1/2, y+1/2, z+1; (viii) x+1, y1, z; (ix) x1, y, z1; (x) x1, y, z; (xi) x1/2, y+1/2, z+1; (xii) x, y, z1; (xiii) x+1/2, y+1/2, z; (xiv) x1, y+1, z; (xv) x, y+1, z; (xvi) x+1/2, y+1, z1/2; (xvii) x+3/2, y+1, z+1/2.

Experimental details

Crystal data
Chemical formula[Co(C5H11)(C62H88N13O14P)]·0.385C3H6O·12.650H2O
Mr1650.69
Crystal system, space groupOrthorhombic, P212121
Temperature (K)123
a, b, c (Å)15.959 (3), 20.793 (4), 24.403 (5)
V3)8098 (3)
Z4
Radiation typeMo Kα
µ (mm1)0.32
Crystal size (mm)0.48 × 0.26 × 0.26
Data collection
DiffractometerBruker SMART CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.863, 0.922
No. of measured, independent and
observed [I > 2σ(I)] reflections
45443, 16502, 14388
Rint0.031
(sin θ/λ)max1)0.628
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.043, 0.107, 1.05
No. of reflections16502
No. of parameters1085
No. of restraints45
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.59, 0.44
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881, 7369 Friedel pairs.
Absolute structure parameter0.010 (10)

Computer programs: SMART (Bruker,1998), SMART, SAINT (Bruker,1999), SHELXTL (Bruker,1999), SHELXTL, ORTEP-3 (Farrugia,1997).

Selected geometric parameters (Å, º) top
C63—C64A1.454 (10)N2—Co1.914 (2)
C63—C64B1.506 (18)N3—Co1.915 (2)
C63—Co2.044 (3)N4—Co1.889 (2)
N1—Co1.869 (2)N13—Co2.277 (2)
C64A—C63—Co119.0 (3)C64B—C63—Co116.0 (4)
 

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