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The centrosymmetric tetrameric title compound, bis­(methyl­imino­diethano­lato-κ5O:O,N,O′:O′)­tetra-μ-n-propanolato-κ8O:O-octa-n-propanolato-κO-tetrazirconium, [Zr4(C5H11NO2)2(C3H7O)12], contains eight μ2-O-atom Zr—O—Zr bridges. Each methyl­imino­diethano­late ligand is bound to one of the two central Zr atoms with a Zr—N distance of 2.412 (5) Å in a meridional configuration(s), with the ethano­late O atoms bridging both the central Zr atoms. Four n-propanolate ligands provide O atoms to bridge other pairs of Zr atoms. The remaining propanolate ligands bind terminally to one metal atom each, to make up 7- and 6-coordination for the the central and outer Zr atoms, respectively. The distorted ZrO6 octahedra each share a face with one of the central ZrO6N pentagonal bipyramids; these edge-share with each other across the centre of symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802017981/tk6081sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802017981/tk6081Isup2.hkl
Contains datablock I

CCDC reference: 200720

Key indicators

  • Single-crystal X-ray study
  • T = 170 K
  • Mean [sigma](C-C) = 0.014 Å
  • Some non-H atoms missing
  • R factor = 0.057
  • wR factor = 0.181
  • Data-to-parameter ratio = 21.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
ABSMU_01 Alert A The ratio of given/expected absorption coefficient lies outside the range 0.90 <> 1.10 Calculated value of mu = 0.353 Value of mu given = 0.705 CHEMW_01 Alert A The ratio of given/expected molecular weight as calculated from the _chemical_formula_sum lies outside the range 0.90 <> 1.10 Calculated formula weight = 654.1136 Formula weight given = 1308.2000
Yellow Alert Alert Level C:
CHEMW_01 Alert C The difference between the given and expected weight for compound is greater 1 mass unit. Check that all hydrogen atoms have been taken into account. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C23 H53 N1 O8 Zr2 Atom count from the _atom_site data: C46 H54 N2 O16 Zr4 CELLZ_01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C23 H53 N O8 Zr2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 92.00 184.00 -92.00 H 212.00 216.00 -4.00 N 4.00 8.00 -4.00 O 32.00 64.00 -32.00 Zr 8.00 16.00 -8.00 Difference between formula and atom_site contents detected. ALERT: Large difference may be due to a symmetry error - see SYMMG tests CHEMW_03 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 1308.20 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 46.00 552.51 H 1.01 54.00 54.43 N 14.01 2.00 28.01 O 16.00 16.00 255.98 Zr 91.22 4.00 364.90 Calculated formula weight 1255.83 The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.99 <> 1.01
2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996) and SADABS (Sheldrick, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 in WinGX (Farrugia, 1997, 1999); software used to prepare material for publication: SHELXL97.

bis(methyliminodiethanolato-κ5O:O,N,O':O')tetra-µ-n-propanolato-κ8O:O- octa-n-propanolato-κO-tetrazirconium top
Crystal data top
[Zr4(C5H11NO2)2(C3H7O)12]Dx = 1.388 Mg m3
Mr = 1308.2Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PbcaCell parameters from 8192 reflections
a = 18.271 (6) Åθ = 2.5–24.8°
b = 16.941 (5) ŵ = 0.71 mm1
c = 20.221 (6) ÅT = 170 K
V = 6259 (3) Å3Block, colourless
Z = 40.70 × 0.40 × 0.20 mm
F(000) = 2736
Data collection top
Siemens SMART CCD area-detector
diffractometer
6435 independent reflections
Radiation source: fine-focus sealed tube4298 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.095
Detector resolution: 8.192 pixels mm-1θmax = 26.5°, θmin = 2.2°
φ and ω scansh = 2222
Absorption correction: multi-scan
(Blessing, 1995)
k = 2118
Tmin = 0.555, Tmax = 0.868l = 2525
75801 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)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.181H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0932P)2 + 16.9738P]
where P = (Fo2 + 2Fc2)/3
6435 reflections(Δ/σ)max = 0.001
306 parametersΔρmax = 1.14 e Å3
2 restraintsΔρmin = 1.05 e Å3
Special details top

Experimental. Crystal decay was monitored by repeating the initial 10 frames at the end of the data collection and analyzing duplicate reflections. The standard 0.8 mm diameter collimator was used.

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. Conformational disorder in the methyliminodiethanolate (MDEA), bridging n-propanolate (O4) and in terminal n-propanolate ligands except those at O6 were modelled by two conformations (a/b) and a common isotropic thermal parameter. Specifically in the MDEA, C72a/C72b had final occupancies of 0.701 (13)/0.299 (13) and U of 0.054 (2) Å2; C21a,C22a,C23a/C21b,C22b,C23b 0.585 (11)/0.415 (11) and U of 0.099 (2) Å2; C31a,C32a,c33a/C31b,C32b,C33b 0.540 (11)/0.460 (11) and U of 0.103 (3) Å2 C41a,C43a/C42b,C43b 0.54 (2)/0.46 (2) and U of 0.076 (2) Å2. There was further disorder in the O6 n-propanolate which could only be modelled by constraining the sum occupancy of atoms C62a, C63a, C62b, C63b, C63c to be two carbon atoms (SHELXL SUMP function) with final common U of 0.103 (3) Å2; atoms 62a & 63a had the same occupancy at 0.390 (13); C63b is a common site for at least two of the conformations refining to an occupancy of 0.660 (14). The bondlength C41—C42a and C41—C42b were constrained to be the same length (SADI with e.s.d. 0.03).

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)
Zr10.22290 (3)0.62102 (3)0.45075 (3)0.04461 (18)
Zr20.07741 (3)0.51066 (3)0.44276 (2)0.03602 (16)
O10.3132 (2)0.5694 (3)0.4774 (3)0.0731 (14)
O20.2592 (2)0.6754 (3)0.3716 (2)0.0595 (11)
O30.2162 (3)0.7104 (3)0.5124 (2)0.0672 (13)
O40.15329 (19)0.5458 (2)0.51802 (18)0.0437 (8)
O50.10460 (19)0.6317 (2)0.42051 (19)0.0427 (8)
O60.0300 (2)0.4872 (3)0.3598 (2)0.0590 (11)
O70.1850 (2)0.5178 (2)0.3941 (2)0.0503 (10)
O80.02044 (19)0.4349 (2)0.51333 (18)0.0424 (8)
N10.1353 (3)0.3828 (3)0.4456 (3)0.0628 (15)
C110.3819 (5)0.5387 (7)0.4935 (7)0.136 (5)
H11A0.40410.51420.45390.163*
H11B0.37650.49750.52790.163*
C120.4349 (5)0.6094 (8)0.5208 (7)0.137 (5)
H12A0.48320.58710.53270.164*
H12B0.44240.64880.48530.164*
C130.4027 (8)0.6482 (9)0.5789 (8)0.159 (5)*
H13A0.35320.66640.56820.191*
H13B0.43300.69360.59150.191*
H13C0.40050.61070.61570.191*
C410.1458 (3)0.5526 (4)0.5871 (3)0.0589 (16)
H41A0.10640.51760.60360.071*
H41B0.13440.60770.59990.071*
C510.0886 (3)0.6703 (4)0.3589 (3)0.0556 (15)
H51A0.03820.65670.34500.067*
H51B0.12270.65090.32450.067*
C520.0953 (4)0.7578 (4)0.3642 (4)0.074 (2)
H52A0.14530.77180.37870.089*
H52B0.06030.77780.39760.089*
C530.0792 (6)0.7968 (6)0.2962 (5)0.124 (4)
H53A0.08420.85420.30010.186*
H53B0.02920.78380.28240.186*
H53C0.11400.77700.26330.186*
C610.0054 (8)0.4677 (8)0.2969 (5)0.143 (5)
C710.2267 (4)0.4495 (4)0.3801 (4)0.076 (2)
H71A0.27900.46370.37590.091*
H71B0.21040.42620.33770.091*
C21A0.2733 (10)0.6898 (11)0.3040 (10)0.099 (2)*0.596 (11)
C22A0.3471 (10)0.6611 (10)0.2866 (9)0.099 (2)*0.596 (11)
C23A0.3602 (10)0.6742 (11)0.2098 (9)0.099 (2)*0.596 (11)
C31A0.1610 (13)0.7661 (12)0.5369 (11)0.103 (3)*0.538 (12)
C32A0.1792 (11)0.7859 (12)0.6047 (11)0.103 (3)*0.538 (12)
C33A0.1246 (12)0.8457 (12)0.6358 (10)0.103 (3)*0.538 (12)
C42A0.2246 (8)0.5258 (12)0.6162 (9)0.077 (2)*0.547 (20)
C43A0.2230 (10)0.5369 (12)0.6918 (8)0.077 (2)*0.547 (20)
C62A0.0183 (16)0.5324 (16)0.2500 (15)0.103 (3)*0.374 (13)
C63A0.031 (2)0.5132 (17)0.1750 (15)0.103 (3)*0.374 (13)
C72A0.2171 (5)0.3918 (6)0.4338 (5)0.055 (2)*0.701 (13)
H72A0.24160.41070.47450.066*0.701 (13)
H72B0.23880.34040.42120.066*0.701 (13)
C730.0989 (6)0.3271 (5)0.4010 (5)0.105 (3)
H73A0.11810.27380.40870.126*
H73B0.10820.34250.35510.126*
H73C0.04610.32770.40950.126*
C740.1269 (4)0.3530 (4)0.5127 (4)0.076 (2)
H74A0.15800.38400.54330.092*
H74B0.14270.29720.51470.092*
C810.0474 (4)0.3598 (4)0.5332 (4)0.0672 (19)
H81A0.01840.31750.51190.081*
H82B0.04300.35400.58170.081*
C21B0.3011 (16)0.6567 (16)0.3159 (14)0.099 (2)*0.404 (11)
C22B0.2876 (13)0.7218 (15)0.2626 (14)0.099 (2)*0.404 (11)
C23B0.3481 (15)0.7236 (17)0.2049 (13)0.099 (2)*0.404 (11)
C31B0.1973 (15)0.7565 (15)0.5688 (14)0.103 (3)*0.462 (12)
C32B0.1141 (15)0.7752 (14)0.5568 (12)0.103 (3)*0.462 (12)
C33B0.0852 (14)0.8211 (14)0.6201 (12)0.103 (3)*0.462 (12)
C42B0.2163 (10)0.5566 (14)0.6246 (10)0.077 (2)*0.453 (20)
C43B0.2016 (12)0.5721 (14)0.6982 (10)0.077 (2)*0.453 (20)
C62B0.0419 (10)0.4968 (9)0.2456 (9)0.103 (3)*0.658 (14)
C63B0.012 (4)0.501 (3)0.177 (3)0.103 (3)*0.202 (22)
C63C0.1066 (16)0.4898 (15)0.2367 (14)0.103 (3)*0.392 (17)
C72B0.1955 (12)0.3817 (12)0.3963 (12)0.055 (2)*0.299 (13)
H72C0.23420.34630.41330.066*0.299 (13)
H72D0.17620.35760.35530.066*0.299 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.0334 (3)0.0465 (3)0.0540 (4)0.0050 (2)0.0023 (2)0.0042 (2)
Zr20.0311 (3)0.0354 (3)0.0415 (3)0.00093 (19)0.0041 (2)0.0025 (2)
O10.035 (2)0.098 (4)0.087 (3)0.006 (2)0.002 (2)0.021 (3)
O20.053 (2)0.067 (3)0.058 (3)0.014 (2)0.014 (2)0.003 (2)
O30.071 (3)0.063 (3)0.068 (3)0.019 (2)0.014 (2)0.013 (2)
O40.040 (2)0.049 (2)0.042 (2)0.0041 (17)0.0013 (16)0.0055 (17)
O50.0370 (19)0.045 (2)0.046 (2)0.0017 (16)0.0017 (16)0.0048 (16)
O60.046 (2)0.079 (3)0.052 (2)0.009 (2)0.0001 (19)0.016 (2)
O70.045 (2)0.045 (2)0.061 (3)0.0006 (17)0.0145 (19)0.0053 (18)
O80.0393 (19)0.0360 (18)0.052 (2)0.0024 (15)0.0088 (17)0.0028 (16)
N10.058 (3)0.041 (3)0.089 (4)0.002 (2)0.029 (3)0.006 (3)
C110.064 (6)0.133 (9)0.210 (14)0.025 (6)0.007 (7)0.068 (9)
C120.064 (6)0.177 (12)0.169 (12)0.017 (7)0.036 (7)0.028 (10)
C410.054 (4)0.086 (5)0.037 (3)0.020 (3)0.007 (3)0.005 (3)
C510.045 (3)0.063 (4)0.059 (4)0.002 (3)0.000 (3)0.016 (3)
C520.064 (4)0.065 (4)0.093 (6)0.014 (3)0.014 (4)0.032 (4)
C530.134 (9)0.105 (7)0.133 (9)0.026 (6)0.013 (7)0.081 (7)
C610.193 (13)0.179 (11)0.057 (6)0.038 (10)0.035 (7)0.022 (7)
C710.056 (4)0.064 (4)0.109 (6)0.006 (3)0.035 (4)0.013 (4)
C730.148 (9)0.062 (5)0.106 (7)0.002 (5)0.029 (7)0.017 (5)
C740.068 (5)0.057 (4)0.105 (6)0.016 (3)0.021 (4)0.015 (4)
C810.064 (4)0.048 (3)0.090 (5)0.014 (3)0.024 (4)0.018 (3)
Geometric parameters (Å, º) top
Zr1—O11.944 (4)C51—C521.490 (10)
Zr1—O21.962 (4)C51—H51A0.9900
Zr1—O31.965 (5)C51—H51B0.9900
Zr1—O72.202 (4)C52—C531.552 (11)
Zr1—O52.253 (4)C52—H52A0.9900
Zr1—O42.256 (4)C52—H52B0.9900
Zr2—O61.929 (4)C53—H53A0.9800
Zr2—O42.143 (4)C53—H53B0.9800
Zr2—O52.158 (4)C53—H53C0.9800
Zr2—O82.183 (3)C61—C62B1.33 (2)
Zr2—O8i2.199 (3)C61—C62A1.51 (3)
Zr2—O72.202 (4)C71—C72B1.32 (2)
Zr2—N12.412 (5)C71—C72A1.472 (12)
O1—C111.396 (9)C71—H71A0.9900
O2—C21B1.40 (3)C71—H71B0.9900
O2—C21A1.41 (2)C21A—C22A1.48 (3)
O3—C31B1.42 (3)C22A—C23A1.59 (2)
O3—C31A1.47 (2)C31A—C32A1.45 (3)
O4—C411.409 (7)C32A—C33A1.56 (3)
O5—C511.437 (7)C42A—C43A1.54 (2)
O6—C611.389 (10)C62A—C63A1.57 (4)
O7—C711.413 (7)C72A—H72A0.9900
O8—C811.422 (7)C72A—H72B0.9900
O8—Zr2i2.199 (3)C73—H73A0.9800
N1—C741.455 (10)C73—H73B0.9800
N1—C731.465 (11)C73—H73C0.9800
N1—C72B1.48 (2)C74—C811.515 (10)
N1—C72A1.521 (11)C74—H74A0.9900
C11—C121.635 (17)C74—H74B0.9900
C11—H11A0.9900C81—H81A0.9900
C11—H11B0.9900C81—H82B0.9900
C12—C131.469 (17)C21B—C22B1.56 (4)
C12—H12A0.9900C22B—C23B1.61 (4)
C12—H12B0.9900C31B—C32B1.57 (4)
C13—H13A0.9800C32B—C33B1.59 (3)
C13—H13B0.9800C42B—C43B1.53 (3)
C13—H13C0.9800C62B—C63C1.20 (3)
C41—C42B1.496 (17)C62B—C63B1.49 (6)
C41—C42A1.621 (15)C72B—H72C0.9900
C41—H41A0.9900C72B—H72D0.9900
C41—H41B0.9900
O1—Zr1—O298.7 (2)H13B—C13—H13C109.5
O1—Zr1—O3102.9 (2)O4—C41—C42B115.0 (10)
O2—Zr1—O3100.18 (19)O4—C41—C42A104.5 (8)
O1—Zr1—O793.1 (2)C42B—C41—C42A20.6 (9)
O2—Zr1—O793.15 (17)O4—C41—H41A110.9
O3—Zr1—O7157.25 (16)C42B—C41—H41A118.8
O1—Zr1—O5157.78 (18)C42A—C41—H41A110.9
O2—Zr1—O593.72 (16)O4—C41—H41B110.9
O3—Zr1—O592.87 (17)C42B—C41—H41B90.3
O7—Zr1—O567.75 (14)C42A—C41—H41B110.9
O1—Zr1—O493.29 (17)H41A—C41—H41B108.9
O2—Zr1—O4161.33 (16)O5—C51—C52112.0 (6)
O3—Zr1—O491.00 (17)O5—C51—H51A109.2
O7—Zr1—O471.82 (14)C52—C51—H51A109.2
O5—Zr1—O470.64 (13)O5—C51—H51B109.2
O6—Zr2—O4164.83 (16)C52—C51—H51B109.2
O6—Zr2—O596.78 (17)H51A—C51—H51B107.9
O4—Zr2—O574.63 (14)C51—C52—C53110.1 (7)
O6—Zr2—O8103.47 (16)C51—C52—H52A109.6
O4—Zr2—O890.44 (14)C53—C52—H52A109.6
O5—Zr2—O8143.59 (14)C51—C52—H52B109.6
O6—Zr2—O8i94.16 (16)C53—C52—H52B109.6
O4—Zr2—O8i97.05 (14)H52A—C52—H52B108.1
O5—Zr2—O8i82.69 (13)C52—C53—H53A109.5
O8—Zr2—O8i66.11 (15)C52—C53—H53B109.5
O6—Zr2—O791.37 (17)H53A—C53—H53B109.5
O4—Zr2—O773.99 (15)C52—C53—H53C109.5
O5—Zr2—O769.45 (14)H53A—C53—H53C109.5
O8—Zr2—O7138.59 (14)H53B—C53—H53C109.5
O8i—Zr2—O7152.05 (13)C62B—C61—O6117.7 (13)
O6—Zr2—N191.9 (2)C62B—C61—C62A52.0 (13)
O4—Zr2—N187.07 (18)O6—C61—C62A119.6 (15)
O5—Zr2—N1139.28 (16)C72B—C71—O7115.4 (10)
O8—Zr2—N170.45 (15)C72B—C71—C72A35.8 (10)
O8i—Zr2—N1136.36 (15)O7—C71—C72A109.4 (6)
O7—Zr2—N170.64 (16)C72B—C71—H71A130.4
C11—O1—Zr1174.2 (6)O7—C71—H71A109.8
C21B—O2—C21A32.8 (11)C72A—C71—H71A109.8
C21B—O2—Zr1137.4 (12)C72B—C71—H71B74.9
C21A—O2—Zr1158.8 (8)O7—C71—H71B109.8
C31B—O3—C31A37.8 (11)C72A—C71—H71B109.8
C31B—O3—Zr1161.0 (10)H71A—C71—H71B108.3
C31A—O3—Zr1138.8 (9)O2—C21A—C22A109.9 (15)
C41—O4—Zr2131.6 (3)C21A—C22A—C23A108.9 (15)
C41—O4—Zr1127.4 (3)C32A—C31A—O3108.1 (19)
Zr2—O4—Zr195.36 (14)C31A—C32A—C33A112.7 (19)
C51—O5—Zr2124.5 (3)C43A—C42A—C41108.0 (11)
C51—O5—Zr1117.8 (3)C61—C62A—C63A120 (2)
Zr2—O5—Zr195.03 (14)C71—C72A—N1107.4 (7)
C61—O6—Zr2172.1 (7)C71—C72A—H72A110.2
C71—O7—Zr2121.7 (4)N1—C72A—H72A110.2
C71—O7—Zr1125.8 (4)C71—C72A—H72B110.2
Zr2—O7—Zr195.28 (15)N1—C72A—H72B110.2
C81—O8—Zr2123.0 (3)H72A—C72A—H72B108.5
C81—O8—Zr2i122.9 (3)N1—C73—H73A109.5
Zr2—O8—Zr2i113.89 (15)N1—C73—H73B109.5
C74—N1—C73107.6 (6)N1—C73—H73C109.5
C74—N1—C72B134.4 (11)N1—C74—C81109.2 (6)
C73—N1—C72B85.1 (11)N1—C74—H74A109.8
C74—N1—C72A106.5 (6)C81—C74—H74A109.8
C73—N1—C72A114.5 (7)N1—C74—H74B109.8
C72B—N1—C72A33.7 (9)C81—C74—H74B109.8
C74—N1—Zr2106.7 (4)H74A—C74—H74B108.3
C73—N1—Zr2111.4 (5)O8—C81—C74108.8 (5)
C72B—N1—Zr2108.6 (8)O8—C81—H81A109.9
C72A—N1—Zr2109.7 (4)C74—C81—H81A109.9
O1—C11—C12109.8 (9)O8—C81—H82B109.9
O1—C11—H11A109.7C74—C81—H82B109.9
C12—C11—H11A109.7H81A—C81—H82B108.3
O1—C11—H11B109.7O2—C21B—C22B108 (2)
C12—C11—H11B109.7C21B—C22B—C23B114 (2)
H11A—C11—H11B108.2O3—C31B—C32B103 (2)
C13—C12—C11111.2 (11)C31B—C32B—C33B107 (2)
C13—C12—H12A109.4C41—C42B—C43B110.4 (14)
C11—C12—H12A109.4C63C—C62B—C61125 (2)
C13—C12—H12B109.4C63C—C62B—C63B103 (3)
C11—C12—H12B109.4C61—C62B—C63B124 (3)
H12A—C12—H12B108.0C71—C72B—N1118.4 (16)
C12—C13—H13A109.5C71—C72B—H72C107.7
C12—C13—H13B109.5N1—C72B—H72C107.7
H13A—C13—H13B109.5C71—C72B—H72D107.7
C12—C13—H13C109.5N1—C72B—H72D107.7
H13A—C13—H13C109.5H72C—C72B—H72D107.1
O1—Zr1—O2—C21B47.3 (17)O4—Zr1—O7—Zr235.00 (13)
O3—Zr1—O2—C21B152.2 (17)O6—Zr2—O8—C8196.3 (5)
O7—Zr1—O2—C21B46.3 (17)O4—Zr2—O8—C8177.6 (5)
O5—Zr1—O2—C21B114.2 (17)O5—Zr2—O8—C81141.8 (5)
O4—Zr1—O2—C21B81.9 (18)O8i—Zr2—O8—C81175.1 (6)
O1—Zr1—O3—C31A162.1 (14)O7—Zr2—O8—C8111.7 (6)
O2—Zr1—O3—C31A96.5 (14)N1—Zr2—O8—C819.1 (5)
O7—Zr1—O3—C31A28.4 (15)O6—Zr2—O8—Zr2i88.6 (2)
O5—Zr1—O3—C31A2.2 (14)O4—Zr2—O8—Zr2i97.52 (18)
O4—Zr1—O3—C31A68.5 (14)O5—Zr2—O8—Zr2i33.4 (3)
O6—Zr2—O4—C41174.0 (7)O7—Zr2—O8—Zr2i163.43 (17)
O5—Zr2—O4—C41117.0 (5)N1—Zr2—O8—Zr2i175.8 (2)
O8—Zr2—O4—C4129.3 (5)O6—Zr2—N1—C74135.5 (5)
O8i—Zr2—O4—C4136.7 (5)O4—Zr2—N1—C7459.7 (5)
O7—Zr2—O4—C41170.4 (5)O5—Zr2—N1—C74121.9 (4)
N1—Zr2—O4—C4199.7 (5)O8—Zr2—N1—C7431.8 (4)
O6—Zr2—O4—Zr120.0 (7)O8i—Zr2—N1—C7437.5 (6)
O5—Zr2—O4—Zr136.93 (13)O7—Zr2—N1—C74133.7 (5)
O8—Zr2—O4—Zr1176.71 (14)O6—Zr2—N1—C7318.3 (5)
O8i—Zr2—O4—Zr1117.31 (14)O4—Zr2—N1—C73176.9 (5)
O7—Zr2—O4—Zr135.62 (13)O5—Zr2—N1—C73120.9 (5)
N1—Zr2—O4—Zr1106.32 (17)O8—Zr2—N1—C7385.4 (5)
O1—Zr1—O4—C4176.1 (5)O8i—Zr2—N1—C7379.7 (6)
O2—Zr1—O4—C41154.0 (6)O7—Zr2—N1—C73109.1 (5)
O3—Zr1—O4—C4126.9 (5)O6—Zr2—N1—C72B73.8 (11)
O7—Zr1—O4—C41168.3 (5)O4—Zr2—N1—C72B91.1 (11)
O5—Zr1—O4—C41119.6 (5)O5—Zr2—N1—C72B28.8 (12)
O1—Zr1—O4—Zr2128.3 (2)O8—Zr2—N1—C72B177.4 (11)
O2—Zr1—O4—Zr21.6 (6)O8i—Zr2—N1—C72B171.8 (11)
O3—Zr1—O4—Zr2128.71 (19)O7—Zr2—N1—C72B17.0 (11)
O7—Zr1—O4—Zr236.11 (14)O6—Zr2—N1—C72A109.5 (6)
O5—Zr1—O4—Zr236.01 (13)O4—Zr2—N1—C72A55.3 (5)
O6—Zr2—O5—C511.3 (4)O5—Zr2—N1—C72A6.9 (7)
O4—Zr2—O5—C51166.0 (4)O8—Zr2—N1—C72A146.8 (6)
O8—Zr2—O5—C51125.1 (4)O8i—Zr2—N1—C72A152.5 (5)
O8i—Zr2—O5—C5194.6 (4)O7—Zr2—N1—C72A18.7 (5)
O7—Zr2—O5—C5187.6 (4)O1—C11—C12—C1358.2 (14)
N1—Zr2—O5—C5199.6 (5)Zr2—O4—C41—C42B163.2 (11)
O6—Zr2—O5—Zr1130.29 (16)Zr1—O4—C41—C42B50.1 (12)
O4—Zr2—O5—Zr136.96 (13)Zr2—O4—C41—C42A144.4 (8)
O8—Zr2—O5—Zr1105.9 (2)Zr1—O4—C41—C42A69.0 (9)
O8i—Zr2—O5—Zr1136.37 (16)Zr2—O5—C51—C52164.7 (4)
O7—Zr2—O5—Zr141.37 (15)Zr1—O5—C51—C5276.4 (6)
N1—Zr2—O5—Zr129.4 (3)O5—C51—C52—C53178.8 (6)
O1—Zr1—O5—C51123.7 (6)Zr2—O7—C71—C72B2.0 (16)
O2—Zr1—O5—C510.2 (4)Zr1—O7—C71—C72B127.4 (14)
O3—Zr1—O5—C51100.6 (4)Zr2—O7—C71—C72A36.3 (9)
O7—Zr1—O5—C5191.6 (4)Zr1—O7—C71—C72A89.0 (7)
O4—Zr1—O5—C51169.3 (4)O2—C21A—C22A—C23A177.3 (13)
O1—Zr1—O5—Zr29.9 (5)Zr1—O3—C31A—C32A147.9 (11)
O2—Zr1—O5—Zr2133.84 (17)O3—C31A—C32A—C33A179.3 (15)
O3—Zr1—O5—Zr2125.75 (18)O4—C41—C42A—C43A176.2 (10)
O7—Zr1—O5—Zr241.96 (14)C72B—C71—C72A—N156.7 (17)
O4—Zr1—O5—Zr235.70 (13)O7—C71—C72A—N150.1 (9)
O6—Zr2—O7—C7182.3 (5)C74—N1—C72A—C71157.5 (7)
O4—Zr2—O7—C71101.8 (5)C73—N1—C72A—C7183.6 (9)
O5—Zr2—O7—C71179.0 (6)C72B—N1—C72A—C7151.9 (16)
O8—Zr2—O7—C7130.0 (6)Zr2—N1—C72A—C7142.4 (8)
O8i—Zr2—O7—C71176.2 (5)C73—N1—C74—C8169.3 (8)
N1—Zr2—O7—C719.2 (5)C72B—N1—C74—C81170.1 (13)
O6—Zr2—O7—Zr1139.31 (18)C72A—N1—C74—C81167.5 (6)
O4—Zr2—O7—Zr136.64 (14)Zr2—N1—C74—C8150.4 (7)
O5—Zr2—O7—Zr142.59 (14)Zr2—O8—C81—C7414.8 (8)
O8—Zr2—O7—Zr1108.4 (2)Zr2i—O8—C81—C74159.9 (5)
O8i—Zr2—O7—Zr137.8 (4)N1—C74—C81—O844.0 (8)
N1—Zr2—O7—Zr1129.2 (2)C21A—O2—C21B—C22B13.5 (19)
O1—Zr1—O7—C718.4 (5)Zr1—O2—C21B—C22B162.3 (11)
O2—Zr1—O7—C7190.5 (5)O2—C21B—C22B—C23B163.1 (19)
O3—Zr1—O7—C71143.5 (6)C31A—O3—C31B—C32B18.6 (18)
O5—Zr1—O7—C71176.8 (5)Zr1—O3—C31B—C32B73 (4)
O4—Zr1—O7—C71100.8 (5)O3—C31B—C32B—C33B175.6 (16)
O1—Zr1—O7—Zr2127.45 (19)O4—C41—C42B—C43B174.4 (11)
O2—Zr1—O7—Zr2133.70 (18)C42A—C41—C42B—C43B123 (4)
O3—Zr1—O7—Zr27.6 (5)C74—N1—C72B—C71112.9 (17)
O5—Zr1—O7—Zr240.96 (14)
Symmetry code: (i) x, y+1, z+1.
 

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