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The crystal structure of the title compound, [Zn(C62H66N4O10Si2)(H2O)], has been determined at 160 (2) K by utilization of a synchrotron X-ray source. The molecular units dimerize via hydrogen bonds involving the water mol­ecules, and these dimers form π-stacks via interactions between the hydro­phobic porphyrin faces.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801014854/wn6049sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801014854/wn6049Isup2.hkl
Contains datablock I

CCDC reference: 175333

Key indicators

  • Single-crystal synchrotron study
  • T = 160 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in main residue
  • R factor = 0.054
  • wR factor = 0.135
  • Data-to-parameter ratio = 16.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.13 From the CIF: _reflns_number_total 12222 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 14289 Completeness (_total/calc) 85.53% Alert B: < 90% complete (theta max?)
Yellow Alert Alert Level C:
PLAT_301 Alert C Main Residue Disorder ........................ 1.00 Perc. PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C(28) - C(31) = 1.45 Ang. PLAT_371 Alert C Long C(sp2)-C(sp1) Bond C(39) - C(42) = 1.46 Ang. General Notes
ABSMU_01 Radiation type not identified. Calculation of _exptl_absorpt_correction_mu not performed.
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
3 Alert Level C = Please check

Comment top

The bright-orange monomeric dioxoporphyrin unit aqua{5,15-bis[4-(2-trimethylsilylacetylene)phenyl]-2,8,12,18-tetrakis(2- methoxycarbonylethyl)-3,7,13,17-tetramethyl-10,20-dioxoporphyrinato}zinc(II), (I), is prepared by thallium trifluoroacetate oxidation (McCallien & Sanders, 1995) of the purple porphyrinic zinc precursor (Bampos et al., 1998). The presence of electron-withdrawing cross-conjugated carbonyl groups on the macrocyclic periphery gives (I) two characteristic properties in solution: lack of a diagnostic NMR diamagnetic ring current and an increased Lewis acidity of the central metal ion, leading to stronger binding of N– and O-ligands. Both these properties make (I) attractive as a building block in the templated construction of supramolecular architectures (Clyde-Watson et al., 1998).

(I) crystallizes with a saddle conformation (Scheidt & Lee, 1987) characterized by alternate pyrrole-ring displacements above and below the least-squares plane through the 24 atoms of the porphyrin unit (Fig. 1). Molecules of (I) are linked into centrosymmetric dimers via hydrogen bonds formed by the zinc-bound water molecule with one oxo group in the 10-position of an adjacent porphyrin and one carbonyl oxygen of a 2-methoxycarbonylethyl side chain [H11A···O3i = 2.13 (3) Å, O11—H11A···O3i = 144 (4)°; H11B···O2i = 1.92 (2) Å, O11—H11B···O2i = 168 (4)°; symmetry code: (i) -1 - x, -y, -z] (Fig. 2). The hydrogen-bond arrangement is reminiscent of that observed in the dihydrates of ethyl chlorophyllide a and b, in which magnesium-bound water molecules hydrogen bond to oxo groups of neighbouring chlorophyllide units and also via a second water molecule to the carbonyl oxygen of a methyl ester side chain, forming one-dimensional polymers (Chow et al., 1975; Serlin et al., 1975). The omission of the second water molecule in (I) allows both interactions to form between the same molecular units, giving rise to the observed dimers.

Dimers are π-stacked via interactions between hydrophobic porphyrin faces, with the stacking direction approximately perpendicular to (110). Least-squares planes through adjacent porphyrin units in the stacks are coplanar with a separation of ca 3.8 Å, and a Zn1···Zn1ii distance of 5.719 (1) Å [symmetry code: (ii) -2 - x, -y, -z] (Fig. 3). In adjacent molecules, phenyl groups of the 4-(2-trimethylsilylacetylene)phenyl substituents are twisted with respect to each other by an angle of ca 33°, adopting a geometry indicative of an edge-to-face C—H···π interaction [H30···(centroid C36—C41)ii = 3.45 Å, C30—H30···centroid = 163°] (Desiraju & Steiner, 1999). This interaction may contribute towards the stability of the π-stacks. The 4-(2-trimethylsilylacetylene)phenyl substituents in adjacent stacks are interdigitated, maximizing dispersion interactions between stacks (Fig. 4).

Experimental top

Crystals of (I) were grown from a solution in dichloromethane, layered with methanol.

Refinement top

H atoms attached to C atoms were placed geometrically and refined using a riding model with an isotropic displacement parameter fixed at 1.2Ueq for the carbon to which they are attached (1.5Ueq for methyl groups). H11A and H11B, associated with the water molecule, were located in a difference Fourier map and refined with an isotropic displacement parameter and the O11—H distance restrained to be 0.84 (1) Å. The terminal methyl group of one 2-methoxycarbonylethyl side chain was found to be disordered and was modelled as two equally occupied sites (C62 and C62'), each refined with an isotropic displacement parameter. The O10—C62 and O10—C62' bond distances were restrained to be identical, with an s.u. of 0.02 Å.

Computing details top

Data collection: SMART (Siemens, 1994); cell refinement: LSCELL (Clegg, 1995); data reduction: SAINT (Siemens, 1994); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Sheldrick, 1993); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular unit in (I) showing displacement ellipsoids at the 50% probability level (XP; Sheldrick, 1993).
[Figure 2] Fig. 2. The molecules of (I) linked into dimers via hydrogen bonds. All H atoms not involved in hydrogen bonding have been omitted for clarity (CAMERON; Watkin, 1996).
[Figure 3] Fig. 3. View along the stacking direction (approximately along [110]) showing adjacent π-stacked molecules of (I). The C—H···π interaction is indicated by a dotted line. All other H atoms have been omitted for clarity (CAMERON; Watkin, 1996).
[Figure 4] Fig. 4. Projection onto the (100) plane showing interdigitation of adjacent stacks. H atoms are omitted for clarity (CAMERON; Watkin, 1996).
Aqua{5,15-bis[4-(2-trimethylsilylacetylene)phenyl]-2,8,12,18-tetrakis(2- methoxycarbonylethyl)-3,7,13,17-tetramethyl-10,20-dioxoporphyrinato}zinc(II) top
Crystal data top
[Zn(C62H66N4O10Si2)(H2O)]Z = 2
Mr = 1166.75F(000) = 1228
Triclinic, P1Dx = 1.324 Mg m3
a = 12.570 (2) ÅSynchrotron radiation, λ = 0.6879 Å
b = 14.285 (3) ÅCell parameters from 17561 reflections
c = 17.502 (4) Åθ = 3.4–27.1°
α = 85.082 (10)°µ = 0.52 mm1
β = 69.225 (12)°T = 160 K
γ = 87.07 (2)°Plate, red
V = 2926.9 (11) Å30.07 × 0.06 × 0.02 mm
Data collection top
Bruker SMART CCD
diffractometer
12222 independent reflections
Radiation source: Daresbury SRS, Station 9.88256 reflections with I > 2σ(I)
Silicon 111 monochromatorRint = 0.066
Detector resolution: 8.192 pixels mm-1θmax = 27.1°, θmin = 3.4°
Thin–slice ω scansh = 1516
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997b)
k = 1817
Tmin = 0.964, Tmax = 0.990l = 1822
17561 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)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.135H atoms treated by a mixture of independent and constrained refinement
S = 0.92 w = 1/[σ2(Fo2) + (0.0676P)2]
where P = (Fo2 + 2Fc2)/3
12222 reflections(Δ/σ)max = 0.023
743 parametersΔρmax = 1.19 e Å3
4 restraintsΔρmin = 1.10 e Å3
Crystal data top
[Zn(C62H66N4O10Si2)(H2O)]γ = 87.07 (2)°
Mr = 1166.75V = 2926.9 (11) Å3
Triclinic, P1Z = 2
a = 12.570 (2) ÅSynchrotron radiation, λ = 0.6879 Å
b = 14.285 (3) ŵ = 0.52 mm1
c = 17.502 (4) ÅT = 160 K
α = 85.082 (10)°0.07 × 0.06 × 0.02 mm
β = 69.225 (12)°
Data collection top
Bruker SMART CCD
diffractometer
12222 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1997b)
8256 reflections with I > 2σ(I)
Tmin = 0.964, Tmax = 0.990Rint = 0.066
17561 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0544 restraints
wR(F2) = 0.135H atoms treated by a mixture of independent and constrained refinement
S = 0.92Δρmax = 1.19 e Å3
12222 reflectionsΔρmin = 1.10 e Å3
743 parameters
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.

Least-squares plane (x,y,z in crystal coordinates) through the porphyrin unit (C1 - C20, N1 - N4) and deviations from it (* indicates atom used to define plane)

-7.1883 (0.0040) x + 10.7118 (0.0051) y + 1.5154 (0.0044) z = 5.2523 (0.0031)

* 0.0897 (0.0027) C1 * 0.3722 (0.0026) C2 * 0.4631 (0.0026) C3 * 0.1661 (0.0027) C4 * -0.0258 (0.0027) C5 * -0.1854 (0.0028) C6 * -0.5396 (0.0027) C7 * -0.4606 (0.0027) C8 * -0.0656 (0.0027) C9 * 0.2611 (0.0029) C10 * 0.2402 (0.0027) C11 * 0.4150 (0.0026) C12 * 0.2771 (0.0026) C13 * 0.0278 (0.0027) C14 * -0.1558 (0.0027) C15 * -0.2134 (0.0027) C16 * -0.3064 (0.0027) C17 * -0.1742 (0.0026) C18 * -0.0901 (0.0027) C19 * -0.0930 (0.0026) C20 * -0.0120 (0.0023) N1 * 0.0773 (0.0024) N2 * 0.0223 (0.0024) N3 * -0.0901 (0.0023) N4

Rms deviation of fitted atoms = 0.2527

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zn10.75965 (3)0.03363 (2)0.06889 (2)0.01340 (10)
Si10.22319 (9)0.39349 (6)0.71803 (6)0.0279 (2)
Si21.23771 (9)0.50192 (7)0.57031 (6)0.0303 (2)
O11.0236 (2)0.12280 (18)0.18284 (14)0.0355 (6)
O20.53290 (18)0.10361 (15)0.05309 (12)0.0212 (5)
O30.3745 (2)0.33046 (16)0.04603 (15)0.0334 (6)
O40.5287 (2)0.42532 (16)0.08533 (14)0.0332 (6)
O50.9140 (3)0.0986 (2)0.50853 (17)0.0615 (9)
O61.0661 (2)0.1460 (2)0.40254 (16)0.0470 (7)
O71.2229 (2)0.40948 (16)0.03632 (15)0.0361 (6)
O81.0887 (2)0.47144 (16)0.07073 (15)0.0333 (6)
O90.5939 (3)0.2617 (2)0.2393 (2)0.0642 (10)
O100.5951 (3)0.13257 (19)0.31931 (17)0.0459 (7)
O110.63680 (19)0.14123 (15)0.11010 (14)0.0210 (5)
H11A0.664 (3)0.1942 (14)0.090 (2)0.046 (9)*
H11B0.579 (2)0.135 (3)0.097 (2)0.046 (9)*
N10.6404 (2)0.07446 (16)0.10596 (14)0.0131 (5)
N20.7850 (2)0.00377 (16)0.18002 (14)0.0140 (5)
N30.9068 (2)0.11268 (16)0.02437 (14)0.0155 (5)
N40.7602 (2)0.03532 (16)0.04996 (14)0.0138 (5)
C10.5894 (2)0.11158 (19)0.05962 (17)0.0140 (6)
C20.5207 (2)0.1901 (2)0.10161 (18)0.0162 (6)
C30.5313 (2)0.20206 (19)0.17711 (17)0.0156 (6)
C40.6026 (2)0.12709 (19)0.18121 (17)0.0147 (6)
C50.6259 (2)0.1033 (2)0.25000 (17)0.0149 (6)
C60.7036 (2)0.0365 (2)0.25159 (17)0.0156 (6)
C70.7190 (3)0.0031 (2)0.32272 (18)0.0171 (6)
C80.8108 (3)0.0553 (2)0.29349 (18)0.0175 (6)
C90.8492 (2)0.05648 (19)0.20619 (17)0.0144 (6)
C100.9538 (3)0.1038 (2)0.15226 (18)0.0188 (6)
C110.9757 (2)0.13275 (19)0.06533 (18)0.0157 (6)
C121.0711 (2)0.18767 (19)0.01454 (17)0.0151 (6)
C131.0592 (2)0.2031 (2)0.06061 (17)0.0146 (6)
C140.9559 (2)0.15625 (19)0.05430 (17)0.0147 (6)
C150.9097 (3)0.15124 (19)0.11698 (17)0.0160 (6)
C160.8198 (2)0.0962 (2)0.11630 (17)0.0157 (6)
C170.7802 (3)0.0879 (2)0.18404 (18)0.0175 (6)
C180.7006 (3)0.0185 (2)0.15846 (18)0.0165 (6)
C190.6877 (2)0.0098 (2)0.07523 (17)0.0141 (6)
C200.6007 (2)0.07527 (19)0.02337 (18)0.0148 (6)
C210.4837 (3)0.2838 (2)0.23826 (19)0.0250 (7)
H21A0.45930.33190.21160.038*
H21B0.54240.31060.25900.038*
H21C0.41830.26210.28390.038*
C220.6499 (3)0.0224 (2)0.41234 (18)0.0286 (8)
H22A0.66800.02350.44410.043*
H22B0.56870.01740.42030.043*
H22C0.66820.08590.43080.043*
C231.1440 (3)0.2554 (2)0.13378 (18)0.0201 (7)
H23A1.20690.27550.11880.030*
H23B1.17350.21390.17880.030*
H23C1.10640.31060.15120.030*
C240.8071 (3)0.1428 (2)0.26567 (19)0.0272 (8)
H24A0.74640.13480.28730.041*
H24B0.81290.20950.25890.041*
H24C0.87950.11980.30390.041*
C250.5603 (3)0.1549 (2)0.32990 (17)0.0167 (6)
C260.4480 (3)0.1306 (2)0.37082 (18)0.0202 (7)
H26A0.41330.08000.34860.024*
C270.3849 (3)0.1788 (2)0.44388 (18)0.0204 (7)
H27A0.30740.16180.47120.025*
C280.4367 (3)0.2528 (2)0.47704 (18)0.0200 (7)
C290.5506 (3)0.2772 (2)0.43475 (19)0.0227 (7)
H29A0.58620.32750.45650.027*
C300.6118 (3)0.2287 (2)0.36158 (18)0.0207 (7)
H30A0.68890.24590.33310.025*
C310.3718 (3)0.3018 (2)0.55412 (19)0.0237 (7)
C320.3174 (3)0.3406 (2)0.6182 (2)0.0270 (8)
C330.0783 (3)0.3943 (3)0.7123 (2)0.0398 (9)
H33A0.05140.32960.70570.060*
H33B0.08100.42830.66530.060*
H33C0.02620.42550.76270.060*
C340.2768 (4)0.5149 (3)0.7336 (3)0.0493 (11)
H34A0.35700.51310.72800.074*
H34B0.23230.54160.78850.074*
H34C0.26920.55390.69250.074*
C350.2282 (4)0.3181 (3)0.7983 (2)0.0417 (10)
H35A0.21670.25210.78190.063*
H35B0.16810.33620.85040.063*
H35C0.30250.32630.80480.063*
C360.9652 (2)0.2105 (2)0.19475 (17)0.0155 (6)
C370.9314 (3)0.3045 (2)0.20132 (19)0.0218 (7)
H37A0.87380.33100.15650.026*
C380.9825 (3)0.3594 (2)0.27410 (19)0.0244 (7)
H38A0.96010.42360.27850.029*
C391.0660 (3)0.3207 (2)0.34003 (18)0.0221 (7)
C401.0980 (3)0.2261 (2)0.33287 (18)0.0206 (7)
H40A1.15480.19910.37780.025*
C411.0476 (3)0.1718 (2)0.26076 (18)0.0194 (7)
H41A1.06960.10750.25650.023*
C421.1222 (3)0.3779 (2)0.4154 (2)0.0275 (8)
C431.1686 (3)0.4253 (2)0.4766 (2)0.0298 (8)
C441.2121 (4)0.4546 (3)0.6576 (2)0.0531 (12)
H44A1.25340.39440.66980.080*
H44B1.13050.44510.64320.080*
H44C1.23910.49920.70580.080*
C451.3928 (3)0.5024 (3)0.5888 (3)0.0485 (11)
H45A1.42540.43910.60010.073*
H45B1.43010.54640.63580.073*
H45C1.40450.52200.54010.073*
C461.1728 (3)0.6214 (3)0.5531 (2)0.0419 (10)
H46A1.09120.61900.54350.063*
H46B1.18350.64450.50530.063*
H46C1.20920.66390.60150.063*
C470.4532 (3)0.2499 (2)0.06896 (19)0.0209 (7)
H47A0.40300.29080.11470.025*
H47B0.40420.20850.04640.025*
C480.5285 (3)0.3109 (2)0.0025 (2)0.0240 (7)
H48A0.56510.36090.02810.029*
H48B0.58970.27180.03680.029*
C490.4673 (3)0.3561 (2)0.0439 (2)0.0246 (7)
C500.4839 (4)0.4645 (3)0.1414 (2)0.0438 (10)
H50A0.53260.51750.16660.066*
H50B0.40650.48640.11120.066*
H50C0.48220.41610.18420.066*
C510.8578 (3)0.1081 (2)0.34478 (19)0.0210 (7)
H51A0.89670.16450.31200.025*
H51B0.79400.12950.39270.025*
C520.9419 (3)0.0483 (2)0.3751 (2)0.0310 (8)
H52A1.01200.03560.32800.037*
H52B0.90760.01280.40050.037*
C530.9715 (3)0.0984 (3)0.4364 (2)0.0320 (8)
C541.1006 (4)0.1982 (4)0.4566 (3)0.0669 (15)
H54A1.17440.22670.42600.100*
H54B1.04370.24770.47870.100*
H54C1.10730.15570.50170.100*
C551.1650 (2)0.2219 (2)0.03925 (18)0.0170 (6)
H55A1.18660.17110.07340.020*
H55B1.23240.23480.01080.020*
C561.1339 (3)0.3107 (2)0.08685 (19)0.0214 (7)
H56A1.17940.31070.12290.026*
H56B1.05260.30860.12230.026*
C571.1539 (3)0.4007 (2)0.0327 (2)0.0241 (7)
C581.1065 (4)0.5610 (2)0.0221 (3)0.0424 (10)
H58A1.04980.60730.05140.064*
H58B1.18300.58280.01270.064*
H58C1.09860.55300.03070.064*
C590.6465 (3)0.0250 (2)0.21044 (18)0.0198 (7)
H59A0.56280.02440.18260.024*
H59B0.66410.01260.26350.024*
C600.6900 (3)0.1272 (2)0.2261 (2)0.0246 (7)
H60A0.68920.16010.17370.030*
H60B0.76990.12610.26430.030*
C610.6215 (3)0.1817 (2)0.2609 (2)0.0302 (8)
C620.5097 (8)0.1822 (7)0.3416 (6)0.043 (2)*0.50
H62A0.44010.19070.29350.065*0.50
H62B0.49200.14480.38540.065*0.50
H62C0.54090.24380.36060.065*0.50
C62'0.5431 (9)0.1785 (7)0.3677 (6)0.048 (3)*0.50
H62D0.55950.14330.42110.072*0.50
H62E0.57400.24270.37570.072*0.50
H62F0.46050.18030.33890.072*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.01236 (18)0.01553 (17)0.01190 (17)0.00457 (13)0.00401 (13)0.00260 (13)
Si10.0326 (5)0.0224 (5)0.0187 (5)0.0059 (4)0.0021 (4)0.0059 (4)
Si20.0286 (5)0.0321 (5)0.0243 (5)0.0078 (4)0.0047 (4)0.0140 (4)
O10.0274 (14)0.0593 (17)0.0240 (13)0.0231 (13)0.0142 (11)0.0112 (12)
O20.0197 (12)0.0270 (12)0.0201 (11)0.0088 (9)0.0104 (10)0.0017 (9)
O30.0372 (15)0.0275 (13)0.0439 (15)0.0053 (11)0.0232 (13)0.0065 (11)
O40.0466 (16)0.0234 (12)0.0326 (14)0.0006 (11)0.0162 (12)0.0087 (10)
O50.058 (2)0.096 (3)0.0323 (16)0.0207 (19)0.0134 (15)0.0133 (16)
O60.0521 (18)0.0595 (18)0.0317 (15)0.0256 (15)0.0124 (13)0.0120 (13)
O70.0419 (16)0.0250 (13)0.0315 (14)0.0053 (11)0.0006 (12)0.0001 (11)
O80.0343 (15)0.0263 (13)0.0348 (14)0.0026 (11)0.0062 (12)0.0059 (11)
O90.082 (3)0.0319 (16)0.095 (3)0.0181 (16)0.051 (2)0.0040 (16)
O100.063 (2)0.0447 (16)0.0455 (17)0.0187 (15)0.0368 (16)0.0024 (13)
O110.0184 (12)0.0198 (11)0.0267 (12)0.0030 (9)0.0102 (10)0.0008 (10)
N10.0136 (12)0.0158 (12)0.0087 (11)0.0021 (10)0.0025 (10)0.0011 (9)
N20.0121 (12)0.0171 (12)0.0115 (12)0.0055 (10)0.0026 (10)0.0025 (10)
N30.0153 (13)0.0174 (12)0.0145 (12)0.0051 (10)0.0066 (10)0.0033 (10)
N40.0108 (12)0.0158 (12)0.0147 (12)0.0036 (10)0.0046 (10)0.0009 (10)
C10.0124 (14)0.0134 (14)0.0172 (15)0.0024 (11)0.0066 (12)0.0002 (11)
C20.0114 (15)0.0171 (14)0.0184 (15)0.0038 (12)0.0029 (12)0.0005 (12)
C30.0151 (15)0.0148 (14)0.0153 (15)0.0023 (12)0.0035 (12)0.0007 (12)
C40.0124 (14)0.0146 (14)0.0146 (14)0.0027 (11)0.0022 (12)0.0017 (11)
C50.0132 (15)0.0172 (14)0.0115 (14)0.0026 (12)0.0018 (12)0.0051 (11)
C60.0140 (15)0.0183 (15)0.0120 (14)0.0032 (12)0.0018 (12)0.0016 (12)
C70.0173 (16)0.0201 (15)0.0136 (15)0.0022 (12)0.0046 (12)0.0025 (12)
C80.0201 (16)0.0158 (14)0.0169 (15)0.0018 (12)0.0066 (13)0.0008 (12)
C90.0147 (15)0.0140 (14)0.0137 (14)0.0031 (12)0.0046 (12)0.0042 (11)
C100.0153 (16)0.0244 (16)0.0186 (16)0.0074 (13)0.0083 (13)0.0031 (13)
C110.0140 (15)0.0157 (14)0.0177 (15)0.0040 (12)0.0060 (12)0.0005 (12)
C120.0112 (14)0.0150 (14)0.0176 (15)0.0027 (11)0.0034 (12)0.0012 (12)
C130.0098 (14)0.0163 (14)0.0142 (14)0.0031 (11)0.0000 (12)0.0010 (11)
C140.0139 (15)0.0131 (14)0.0153 (15)0.0028 (11)0.0031 (12)0.0008 (11)
C150.0176 (16)0.0140 (14)0.0154 (15)0.0006 (12)0.0054 (13)0.0027 (11)
C160.0133 (15)0.0197 (15)0.0120 (14)0.0027 (12)0.0024 (12)0.0026 (12)
C170.0158 (15)0.0207 (15)0.0170 (15)0.0011 (12)0.0074 (13)0.0015 (12)
C180.0147 (15)0.0186 (15)0.0172 (15)0.0005 (12)0.0069 (12)0.0019 (12)
C190.0123 (14)0.0177 (14)0.0133 (14)0.0020 (12)0.0057 (12)0.0006 (11)
C200.0114 (14)0.0140 (14)0.0189 (15)0.0001 (11)0.0048 (12)0.0033 (12)
C210.0323 (19)0.0197 (16)0.0242 (17)0.0138 (14)0.0110 (15)0.0045 (13)
C220.031 (2)0.0364 (19)0.0154 (16)0.0146 (16)0.0024 (15)0.0032 (14)
C230.0115 (15)0.0288 (17)0.0160 (15)0.0087 (13)0.0006 (12)0.0009 (13)
C240.0301 (19)0.0317 (18)0.0245 (18)0.0130 (15)0.0168 (15)0.0122 (14)
C250.0177 (16)0.0194 (15)0.0135 (15)0.0089 (12)0.0056 (13)0.0026 (12)
C260.0203 (17)0.0205 (15)0.0192 (16)0.0019 (13)0.0072 (13)0.0039 (13)
C270.0169 (16)0.0268 (17)0.0151 (15)0.0050 (13)0.0024 (13)0.0009 (13)
C280.0246 (17)0.0218 (16)0.0139 (15)0.0112 (13)0.0074 (13)0.0049 (12)
C290.0199 (17)0.0265 (17)0.0210 (16)0.0059 (14)0.0072 (14)0.0050 (13)
C300.0147 (16)0.0260 (16)0.0200 (16)0.0035 (13)0.0055 (13)0.0044 (13)
C310.0256 (18)0.0263 (17)0.0182 (16)0.0069 (14)0.0060 (14)0.0002 (14)
C320.0276 (19)0.0278 (18)0.0229 (18)0.0074 (15)0.0054 (15)0.0022 (14)
C330.032 (2)0.034 (2)0.042 (2)0.0134 (17)0.0023 (18)0.0014 (17)
C340.060 (3)0.027 (2)0.048 (3)0.003 (2)0.006 (2)0.0122 (18)
C350.052 (3)0.042 (2)0.029 (2)0.004 (2)0.0121 (19)0.0034 (17)
C360.0148 (15)0.0175 (14)0.0145 (15)0.0055 (12)0.0057 (12)0.0028 (12)
C370.0251 (18)0.0205 (16)0.0162 (16)0.0016 (13)0.0032 (14)0.0006 (13)
C380.0304 (19)0.0176 (15)0.0248 (17)0.0073 (14)0.0101 (15)0.0065 (13)
C390.0243 (18)0.0281 (17)0.0168 (16)0.0124 (14)0.0117 (14)0.0090 (13)
C400.0173 (16)0.0303 (17)0.0143 (15)0.0048 (13)0.0054 (13)0.0001 (13)
C410.0202 (17)0.0186 (15)0.0195 (16)0.0033 (13)0.0072 (13)0.0009 (12)
C420.0288 (19)0.0297 (18)0.0257 (18)0.0110 (15)0.0122 (15)0.0062 (15)
C430.034 (2)0.0317 (19)0.0244 (18)0.0149 (16)0.0119 (16)0.0124 (15)
C440.068 (3)0.058 (3)0.034 (2)0.004 (2)0.021 (2)0.003 (2)
C450.031 (2)0.044 (2)0.058 (3)0.0070 (19)0.004 (2)0.020 (2)
C460.031 (2)0.043 (2)0.047 (2)0.0058 (18)0.0113 (19)0.0125 (19)
C470.0191 (16)0.0222 (16)0.0224 (16)0.0099 (13)0.0083 (14)0.0028 (13)
C480.0246 (18)0.0215 (16)0.0305 (18)0.0023 (14)0.0147 (15)0.0033 (14)
C490.031 (2)0.0176 (16)0.0260 (18)0.0069 (14)0.0112 (15)0.0023 (13)
C500.067 (3)0.030 (2)0.040 (2)0.008 (2)0.023 (2)0.0104 (17)
C510.0271 (18)0.0194 (15)0.0187 (16)0.0068 (13)0.0103 (14)0.0004 (13)
C520.041 (2)0.0268 (18)0.035 (2)0.0013 (16)0.0247 (18)0.0055 (15)
C530.036 (2)0.040 (2)0.027 (2)0.0004 (17)0.0200 (17)0.0036 (16)
C540.071 (4)0.079 (3)0.063 (3)0.032 (3)0.030 (3)0.026 (3)
C550.0125 (15)0.0208 (15)0.0173 (15)0.0023 (12)0.0051 (12)0.0008 (12)
C560.0182 (16)0.0249 (16)0.0205 (16)0.0044 (13)0.0053 (13)0.0029 (13)
C570.0209 (17)0.0258 (17)0.0273 (18)0.0041 (14)0.0092 (15)0.0064 (14)
C580.052 (3)0.0218 (18)0.052 (3)0.0019 (18)0.017 (2)0.0038 (17)
C590.0210 (17)0.0258 (16)0.0137 (15)0.0060 (13)0.0072 (13)0.0017 (13)
C600.0221 (18)0.0304 (18)0.0199 (17)0.0009 (14)0.0044 (14)0.0075 (14)
C610.030 (2)0.0292 (19)0.0290 (19)0.0035 (15)0.0055 (16)0.0079 (15)
Geometric parameters (Å, º) top
Zn1—N42.076 (2)C25—C301.386 (4)
Zn1—N32.085 (2)C26—C271.387 (4)
Zn1—N22.086 (2)C26—H26A0.9500
Zn1—O112.103 (2)C27—C281.405 (4)
Zn1—N12.104 (2)C27—H27A0.9500
Si1—C321.851 (3)C28—C291.400 (5)
Si1—C331.860 (4)C28—C311.446 (4)
Si1—C341.862 (4)C29—C301.384 (4)
Si1—C351.862 (4)C29—H29A0.9500
Si2—C431.850 (3)C30—H30A0.9500
Si2—C441.855 (4)C31—C321.191 (4)
Si2—C461.855 (4)C33—H33A0.9800
Si2—C451.860 (4)C33—H33B0.9800
O1—C101.229 (3)C33—H33C0.9800
O2—C201.243 (3)C34—H34A0.9800
O3—C491.216 (4)C34—H34B0.9800
O4—C491.322 (4)C34—H34C0.9800
O4—C501.454 (4)C35—H35A0.9800
O5—C531.213 (4)C35—H35B0.9800
O6—C531.319 (4)C35—H35C0.9800
O6—C541.444 (4)C36—C411.384 (4)
O7—C571.212 (4)C36—C371.395 (4)
O8—C571.333 (4)C37—C381.397 (4)
O8—C581.455 (4)C37—H37A0.9500
O9—C611.202 (4)C38—C391.389 (5)
O10—C611.320 (4)C38—H38A0.9500
O10—C62'1.452 (9)C39—C401.398 (4)
O10—C621.493 (9)C39—C421.456 (4)
O11—H11A0.84 (2)C40—C411.383 (4)
O11—H11B0.84 (2)C40—H40A0.9500
N1—C11.351 (3)C41—H41A0.9500
N1—C41.396 (3)C42—C431.191 (4)
N2—C91.346 (4)C44—H44A0.9800
N2—C61.405 (3)C44—H44B0.9800
N3—C111.359 (4)C44—H44C0.9800
N3—C141.398 (4)C45—H45A0.9800
N4—C191.356 (3)C45—H45B0.9800
N4—C161.393 (4)C45—H45C0.9800
C1—C21.432 (4)C46—H46A0.9800
C1—C201.460 (4)C46—H46B0.9800
C2—C31.370 (4)C46—H46C0.9800
C2—C471.509 (4)C47—C481.522 (4)
C3—C41.453 (4)C47—H47A0.9900
C3—C211.507 (4)C47—H47B0.9900
C4—C51.407 (4)C48—C491.501 (4)
C5—C61.409 (4)C48—H48A0.9900
C5—C251.499 (4)C48—H48B0.9900
C6—C71.448 (4)C50—H50A0.9800
C7—C81.377 (4)C50—H50B0.9800
C7—C221.508 (4)C50—H50C0.9800
C8—C91.429 (4)C51—C521.536 (4)
C8—C511.503 (4)C51—H51A0.9900
C9—C101.476 (4)C51—H51B0.9900
C10—C111.472 (4)C52—C531.498 (4)
C11—C121.437 (4)C52—H52A0.9900
C12—C131.374 (4)C52—H52B0.9900
C12—C551.508 (4)C54—H54A0.9800
C13—C141.456 (4)C54—H54B0.9800
C13—C231.511 (4)C54—H54C0.9800
C14—C151.420 (4)C55—C561.534 (4)
C15—C161.406 (4)C55—H55A0.9900
C15—C361.498 (4)C55—H55B0.9900
C16—C171.454 (4)C56—C571.507 (4)
C17—C181.376 (4)C56—H56A0.9900
C17—C241.504 (4)C56—H56B0.9900
C18—C191.432 (4)C58—H58A0.9800
C18—C591.502 (4)C58—H58B0.9800
C19—C201.466 (4)C58—H58C0.9800
C21—H21A0.9800C59—C601.544 (4)
C21—H21B0.9800C59—H59A0.9900
C21—H21C0.9800C59—H59B0.9900
C22—H22A0.9800C60—C611.496 (4)
C22—H22B0.9800C60—H60A0.9900
C22—H22C0.9800C60—H60B0.9900
C23—H23A0.9800C62—H62A0.9800
C23—H23B0.9800C62—H62B0.9800
C23—H23C0.9800C62—H62C0.9800
C24—H24A0.9800C62'—H62D0.9800
C24—H24B0.9800C62'—H62E0.9800
C24—H24C0.9800C62'—H62F0.9800
C25—C261.379 (4)
N4—Zn1—N388.75 (9)C32—C31—C28178.7 (4)
N4—Zn1—N2166.17 (9)C31—C32—Si1175.2 (3)
N3—Zn1—N290.33 (9)Si1—C33—H33A109.5
N4—Zn1—O1197.99 (9)Si1—C33—H33B109.5
N3—Zn1—O1199.99 (9)H33A—C33—H33B109.5
N2—Zn1—O1195.76 (9)Si1—C33—H33C109.5
N4—Zn1—N190.20 (9)H33A—C33—H33C109.5
N3—Zn1—N1165.65 (9)H33B—C33—H33C109.5
N2—Zn1—N187.28 (9)Si1—C34—H34A109.5
O11—Zn1—N194.34 (9)Si1—C34—H34B109.5
C32—Si1—C33106.54 (17)H34A—C34—H34B109.5
C32—Si1—C34108.52 (18)Si1—C34—H34C109.5
C33—Si1—C34111.30 (19)H34A—C34—H34C109.5
C32—Si1—C35107.17 (16)H34B—C34—H34C109.5
C33—Si1—C35111.88 (19)Si1—C35—H35A109.5
C34—Si1—C35111.19 (19)Si1—C35—H35B109.5
C43—Si2—C44108.79 (18)H35A—C35—H35B109.5
C43—Si2—C46107.85 (17)Si1—C35—H35C109.5
C44—Si2—C46110.1 (2)H35A—C35—H35C109.5
C43—Si2—C45108.22 (17)H35B—C35—H35C109.5
C44—Si2—C45110.5 (2)C41—C36—C37119.9 (3)
C46—Si2—C45111.28 (19)C41—C36—C15120.3 (3)
C49—O4—C50115.7 (3)C37—C36—C15119.7 (3)
C53—O6—C54116.5 (3)C36—C37—C38119.7 (3)
C57—O8—C58114.3 (3)C36—C37—H37A120.1
C61—O10—C62'119.9 (5)C38—C37—H37A120.1
C61—O10—C62111.0 (5)C39—C38—C37120.3 (3)
C62'—O10—C6219.5 (6)C39—C38—H38A119.8
Zn1—O11—H11A111 (3)C37—C38—H38A119.8
Zn1—O11—H11B113 (3)C38—C39—C40119.3 (3)
H11A—O11—H11B108 (4)C38—C39—C42120.8 (3)
C1—N1—C4105.3 (2)C40—C39—C42119.8 (3)
C1—N1—Zn1126.86 (18)C41—C40—C39120.4 (3)
C4—N1—Zn1127.70 (18)C41—C40—H40A119.8
C9—N2—C6105.3 (2)C39—C40—H40A119.8
C9—N2—Zn1123.24 (18)C40—C41—C36120.4 (3)
C6—N2—Zn1124.55 (18)C40—C41—H41A119.8
C11—N3—C14105.2 (2)C36—C41—H41A119.8
C11—N3—Zn1127.52 (19)C43—C42—C39179.3 (4)
C14—N3—Zn1127.24 (19)C42—C43—Si2178.2 (4)
C19—N4—C16105.5 (2)Si2—C44—H44A109.5
C19—N4—Zn1126.71 (19)Si2—C44—H44B109.5
C16—N4—Zn1126.74 (19)H44A—C44—H44B109.5
N1—C1—C2112.4 (2)Si2—C44—H44C109.5
N1—C1—C20124.3 (2)H44A—C44—H44C109.5
C2—C1—C20123.3 (2)H44B—C44—H44C109.5
C3—C2—C1105.9 (2)Si2—C45—H45A109.5
C3—C2—C47126.6 (3)Si2—C45—H45B109.5
C1—C2—C47127.4 (3)H45A—C45—H45B109.5
C2—C3—C4106.8 (2)Si2—C45—H45C109.5
C2—C3—C21124.0 (3)H45A—C45—H45C109.5
C4—C3—C21129.1 (3)H45B—C45—H45C109.5
N1—C4—C5122.9 (2)Si2—C46—H46A109.5
N1—C4—C3109.4 (2)Si2—C46—H46B109.5
C5—C4—C3127.6 (2)H46A—C46—H46B109.5
C4—C5—C6127.0 (2)Si2—C46—H46C109.5
C4—C5—C25116.0 (2)H46A—C46—H46C109.5
C6—C5—C25117.0 (2)H46B—C46—H46C109.5
N2—C6—C5122.6 (3)C2—C47—C48112.8 (3)
N2—C6—C7109.5 (2)C2—C47—H47A109.0
C5—C6—C7127.7 (3)C48—C47—H47A109.0
C8—C7—C6106.4 (2)C2—C47—H47B109.0
C8—C7—C22124.1 (3)C48—C47—H47B109.0
C6—C7—C22129.5 (3)H47A—C47—H47B107.8
C7—C8—C9106.3 (3)C49—C48—C47114.6 (3)
C7—C8—C51125.8 (3)C49—C48—H48A108.6
C9—C8—C51127.9 (3)C47—C48—H48A108.6
N2—C9—C8112.5 (3)C49—C48—H48B108.6
N2—C9—C10124.5 (3)C47—C48—H48B108.6
C8—C9—C10122.8 (3)H48A—C48—H48B107.6
O1—C10—C11119.0 (3)O3—C49—O4123.6 (3)
O1—C10—C9117.8 (3)O3—C49—C48124.7 (3)
C11—C10—C9123.2 (3)O4—C49—C48111.6 (3)
N3—C11—C12112.2 (2)O4—C50—H50A109.5
N3—C11—C10124.1 (3)O4—C50—H50B109.5
C12—C11—C10123.7 (3)H50A—C50—H50B109.5
C13—C12—C11106.2 (2)O4—C50—H50C109.5
C13—C12—C55127.1 (3)H50A—C50—H50C109.5
C11—C12—C55126.7 (3)H50B—C50—H50C109.5
C12—C13—C14106.5 (2)C8—C51—C52112.6 (3)
C12—C13—C23123.9 (3)C8—C51—H51A109.1
C14—C13—C23129.5 (3)C52—C51—H51A109.1
N3—C14—C15123.0 (2)C8—C51—H51B109.1
N3—C14—C13109.8 (2)C52—C51—H51B109.1
C15—C14—C13127.2 (3)H51A—C51—H51B107.8
C16—C15—C14128.4 (3)C53—C52—C51110.3 (3)
C16—C15—C36115.5 (2)C53—C52—H52A109.6
C14—C15—C36116.1 (2)C51—C52—H52A109.6
N4—C16—C15123.3 (3)C53—C52—H52B109.6
N4—C16—C17109.9 (2)C51—C52—H52B109.6
C15—C16—C17126.7 (3)H52A—C52—H52B108.1
C18—C17—C16106.1 (2)O5—C53—O6123.1 (3)
C18—C17—C24122.1 (3)O5—C53—C52124.6 (4)
C16—C17—C24131.7 (3)O6—C53—C52112.3 (3)
C17—C18—C19106.6 (2)O6—C54—H54A109.5
C17—C18—C59126.4 (3)O6—C54—H54B109.5
C19—C18—C59126.8 (3)H54A—C54—H54B109.5
N4—C19—C18111.8 (3)O6—C54—H54C109.5
N4—C19—C20125.1 (3)H54A—C54—H54C109.5
C18—C19—C20123.0 (3)H54B—C54—H54C109.5
O2—C20—C1117.6 (3)C12—C55—C56114.4 (2)
O2—C20—C19117.4 (3)C12—C55—H55A108.6
C1—C20—C19125.0 (2)C56—C55—H55A108.6
C3—C21—H21A109.5C12—C55—H55B108.6
C3—C21—H21B109.5C56—C55—H55B108.6
H21A—C21—H21B109.5H55A—C55—H55B107.6
C3—C21—H21C109.5C57—C56—C55113.7 (3)
H21A—C21—H21C109.5C57—C56—H56A108.8
H21B—C21—H21C109.5C55—C56—H56A108.8
C7—C22—H22A109.5C57—C56—H56B108.8
C7—C22—H22B109.5C55—C56—H56B108.8
H22A—C22—H22B109.5H56A—C56—H56B107.7
C7—C22—H22C109.5O7—C57—O8123.4 (3)
H22A—C22—H22C109.5O7—C57—C56124.7 (3)
H22B—C22—H22C109.5O8—C57—C56111.9 (3)
C13—C23—H23A109.5O8—C58—H58A109.5
C13—C23—H23B109.5O8—C58—H58B109.5
H23A—C23—H23B109.5H58A—C58—H58B109.5
C13—C23—H23C109.5O8—C58—H58C109.5
H23A—C23—H23C109.5H58A—C58—H58C109.5
H23B—C23—H23C109.5H58B—C58—H58C109.5
C17—C24—H24A109.5C18—C59—C60111.1 (2)
C17—C24—H24B109.5C18—C59—H59A109.4
H24A—C24—H24B109.5C60—C59—H59A109.4
C17—C24—H24C109.5C18—C59—H59B109.4
H24A—C24—H24C109.5C60—C59—H59B109.4
H24B—C24—H24C109.5H59A—C59—H59B108.0
C26—C25—C30120.0 (3)C61—C60—C59113.9 (3)
C26—C25—C5120.0 (3)C61—C60—H60A108.8
C30—C25—C5119.9 (3)C59—C60—H60A108.8
C25—C26—C27121.0 (3)C61—C60—H60B108.8
C25—C26—H26A119.5C59—C60—H60B108.8
C27—C26—H26A119.5H60A—C60—H60B107.7
C26—C27—C28119.4 (3)O9—C61—O10122.9 (3)
C26—C27—H27A120.3O9—C61—C60124.5 (3)
C28—C27—H27A120.3O10—C61—C60112.6 (3)
C29—C28—C27119.1 (3)O10—C62—H62A109.5
C29—C28—C31121.5 (3)O10—C62—H62B109.5
C27—C28—C31119.5 (3)O10—C62—H62C109.5
C30—C29—C28120.6 (3)O10—C62'—H62D109.5
C30—C29—H29A119.7O10—C62'—H62E109.5
C28—C29—H29A119.7H62D—C62'—H62E109.5
C29—C30—C25119.9 (3)O10—C62'—H62F109.5
C29—C30—H30A120.1H62D—C62'—H62F109.5
C25—C30—H30A120.1H62E—C62'—H62F109.5
N4—Zn1—N1—C14.2 (2)Zn1—N3—C14—C150.5 (4)
N3—Zn1—N1—C190.0 (4)C11—N3—C14—C130.8 (3)
N2—Zn1—N1—C1170.6 (2)Zn1—N3—C14—C13179.09 (18)
O11—Zn1—N1—C193.8 (2)C12—C13—C14—N30.2 (3)
N4—Zn1—N1—C4171.2 (2)C23—C13—C14—N3176.8 (3)
N3—Zn1—N1—C485.5 (4)C12—C13—C14—C15178.8 (3)
N2—Zn1—N1—C44.8 (2)C23—C13—C14—C151.7 (5)
O11—Zn1—N1—C490.8 (2)N3—C14—C15—C168.0 (5)
N4—Zn1—N2—C9107.5 (4)C13—C14—C15—C16170.3 (3)
N3—Zn1—N2—C921.4 (2)N3—C14—C15—C36173.5 (3)
O11—Zn1—N2—C978.6 (2)C13—C14—C15—C368.1 (4)
N1—Zn1—N2—C9172.7 (2)C19—N4—C16—C15175.2 (3)
N4—Zn1—N2—C6106.1 (4)Zn1—N4—C16—C1515.8 (4)
N3—Zn1—N2—C6167.9 (2)C19—N4—C16—C170.7 (3)
O11—Zn1—N2—C667.8 (2)Zn1—N4—C16—C17168.33 (19)
N1—Zn1—N2—C626.3 (2)C14—C15—C16—N40.0 (5)
N4—Zn1—N3—C11169.8 (2)C36—C15—C16—N4178.5 (3)
N2—Zn1—N3—C113.6 (2)C14—C15—C16—C17175.2 (3)
O11—Zn1—N3—C1192.3 (2)C36—C15—C16—C173.3 (4)
N1—Zn1—N3—C1183.9 (4)N4—C16—C17—C182.7 (3)
N4—Zn1—N3—C1410.1 (2)C15—C16—C17—C18173.0 (3)
N2—Zn1—N3—C14176.3 (2)N4—C16—C17—C24173.4 (3)
O11—Zn1—N3—C1487.8 (2)C15—C16—C17—C2410.8 (5)
N1—Zn1—N3—C1496.0 (4)C16—C17—C18—C193.5 (3)
N3—Zn1—N4—C19175.8 (2)C24—C17—C18—C19173.1 (3)
N2—Zn1—N4—C1989.6 (4)C16—C17—C18—C59171.2 (3)
O11—Zn1—N4—C1984.3 (2)C24—C17—C18—C5912.2 (5)
N1—Zn1—N4—C1910.1 (2)C16—N4—C19—C181.6 (3)
N3—Zn1—N4—C1617.4 (2)Zn1—N4—C19—C18170.64 (19)
N2—Zn1—N4—C16103.7 (4)C16—N4—C19—C20174.6 (3)
O11—Zn1—N4—C1682.5 (2)Zn1—N4—C19—C205.6 (4)
N1—Zn1—N4—C16176.9 (2)C17—C18—C19—N43.4 (3)
C4—N1—C1—C21.7 (3)C59—C18—C19—N4171.3 (3)
Zn1—N1—C1—C2174.57 (19)C17—C18—C19—C20172.9 (3)
C4—N1—C1—C20177.1 (3)C59—C18—C19—C2012.4 (5)
Zn1—N1—C1—C206.6 (4)N1—C1—C20—O2166.3 (3)
N1—C1—C2—C30.7 (3)C2—C1—C20—O212.4 (4)
C20—C1—C2—C3179.6 (3)N1—C1—C20—C1915.4 (4)
N1—C1—C2—C47178.8 (3)C2—C1—C20—C19165.9 (3)
C20—C1—C2—C472.4 (5)N4—C19—C20—O2172.8 (3)
C1—C2—C3—C42.8 (3)C18—C19—C20—O23.1 (4)
C47—C2—C3—C4179.1 (3)N4—C19—C20—C18.9 (5)
C1—C2—C3—C21172.8 (3)C18—C19—C20—C1175.2 (3)
C47—C2—C3—C215.3 (5)C4—C5—C25—C2676.7 (4)
C1—N1—C4—C5172.3 (3)C6—C5—C25—C26103.2 (3)
Zn1—N1—C4—C511.5 (4)C4—C5—C25—C30101.7 (3)
C1—N1—C4—C33.4 (3)C6—C5—C25—C3078.4 (4)
Zn1—N1—C4—C3172.81 (19)C30—C25—C26—C270.1 (5)
C2—C3—C4—N14.0 (3)C5—C25—C26—C27178.5 (3)
C21—C3—C4—N1171.3 (3)C25—C26—C27—C280.7 (5)
C2—C3—C4—C5171.5 (3)C26—C27—C28—C291.0 (4)
C21—C3—C4—C513.3 (5)C26—C27—C28—C31178.7 (3)
N1—C4—C5—C611.8 (5)C27—C28—C29—C300.5 (5)
C3—C4—C5—C6173.4 (3)C31—C28—C29—C30179.2 (3)
N1—C4—C5—C25168.1 (3)C28—C29—C30—C250.4 (5)
C3—C4—C5—C256.7 (4)C26—C25—C30—C290.7 (5)
C9—N2—C6—C5174.4 (3)C5—C25—C30—C29179.1 (3)
Zn1—N2—C6—C534.2 (4)C16—C15—C36—C4182.1 (4)
C9—N2—C6—C71.9 (3)C14—C15—C36—C4196.6 (3)
Zn1—N2—C6—C7149.5 (2)C16—C15—C36—C3796.2 (3)
C4—C5—C6—N212.3 (5)C14—C15—C36—C3785.1 (4)
C25—C5—C6—N2167.8 (3)C41—C36—C37—C381.2 (5)
C4—C5—C6—C7172.0 (3)C15—C36—C37—C38179.5 (3)
C25—C5—C6—C77.8 (5)C36—C37—C38—C390.5 (5)
N2—C6—C7—C81.2 (3)C37—C38—C39—C400.2 (5)
C5—C6—C7—C8174.9 (3)C37—C38—C39—C42178.3 (3)
N2—C6—C7—C22176.9 (3)C38—C39—C40—C410.3 (5)
C5—C6—C7—C227.0 (5)C42—C39—C40—C41178.2 (3)
C6—C7—C8—C90.0 (3)C39—C40—C41—C360.3 (5)
C22—C7—C8—C9178.2 (3)C37—C36—C41—C401.1 (4)
C6—C7—C8—C51178.8 (3)C15—C36—C41—C40179.3 (3)
C22—C7—C8—C510.6 (5)C3—C2—C47—C48108.3 (3)
C6—N2—C9—C81.9 (3)C1—C2—C47—C4869.3 (4)
Zn1—N2—C9—C8149.9 (2)C2—C47—C48—C49167.8 (3)
C6—N2—C9—C10172.9 (3)C50—O4—C49—O35.9 (5)
Zn1—N2—C9—C1035.3 (4)C50—O4—C49—C48171.5 (3)
C7—C8—C9—N21.2 (3)C47—C48—C49—O318.5 (5)
C51—C8—C9—N2177.5 (3)C47—C48—C49—O4164.2 (3)
C7—C8—C9—C10173.7 (3)C7—C8—C51—C5284.8 (4)
C51—C8—C9—C107.6 (5)C9—C8—C51—C5296.7 (4)
N2—C9—C10—O1156.5 (3)C8—C51—C52—C53170.9 (3)
C8—C9—C10—O117.8 (4)C54—O6—C53—O51.2 (6)
N2—C9—C10—C1126.3 (5)C54—O6—C53—C52178.9 (4)
C8—C9—C10—C11159.4 (3)C51—C52—C53—O582.5 (5)
C14—N3—C11—C121.1 (3)C51—C52—C53—O695.1 (4)
Zn1—N3—C11—C12178.81 (19)C13—C12—C55—C5698.8 (3)
C14—N3—C11—C10177.5 (3)C11—C12—C55—C5680.7 (4)
Zn1—N3—C11—C102.7 (4)C12—C55—C56—C5786.1 (3)
O1—C10—C11—N3177.5 (3)C58—O8—C57—O70.5 (5)
C9—C10—C11—N35.3 (5)C58—O8—C57—C56178.5 (3)
O1—C10—C11—C124.1 (5)C55—C56—C57—O726.2 (5)
C9—C10—C11—C12173.1 (3)C55—C56—C57—O8155.8 (3)
N3—C11—C12—C131.0 (3)C17—C18—C59—C60109.1 (3)
C10—C11—C12—C13177.6 (3)C19—C18—C59—C6064.7 (4)
N3—C11—C12—C55179.5 (3)C18—C59—C60—C61167.0 (3)
C10—C11—C12—C552.0 (5)C62'—O10—C61—O98.0 (7)
C11—C12—C13—C140.4 (3)C62—O10—C61—O911.2 (7)
C55—C12—C13—C14180.0 (3)C62'—O10—C61—C60171.3 (6)
C11—C12—C13—C23177.7 (3)C62—O10—C61—C60169.5 (5)
C55—C12—C13—C232.8 (5)C59—C60—C61—O9137.5 (4)
C11—N3—C14—C15179.4 (3)C59—C60—C61—O1043.2 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O11—H11B···O2i0.84 (2)1.92 (2)2.748 (3)168 (4)
O11—H11A···O3i0.84 (2)2.13 (3)2.853 (3)144 (4)
Symmetry code: (i) x1, y, z.

Experimental details

Crystal data
Chemical formula[Zn(C62H66N4O10Si2)(H2O)]
Mr1166.75
Crystal system, space groupTriclinic, P1
Temperature (K)160
a, b, c (Å)12.570 (2), 14.285 (3), 17.502 (4)
α, β, γ (°)85.082 (10), 69.225 (12), 87.07 (2)
V3)2926.9 (11)
Z2
Radiation typeSynchrotron, λ = 0.6879 Å
µ (mm1)0.52
Crystal size (mm)0.07 × 0.06 × 0.02
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1997b)
Tmin, Tmax0.964, 0.990
No. of measured, independent and
observed [I > 2σ(I)] reflections
17561, 12222, 8256
Rint0.066
(sin θ/λ)max1)0.663
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.054, 0.135, 0.92
No. of reflections12222
No. of parameters743
No. of restraints4
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.19, 1.10

Computer programs: SMART (Siemens, 1994), LSCELL (Clegg, 1995), SAINT (Siemens, 1994), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP (Sheldrick, 1993), SHELXL97.

 

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