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The two independent Zr atoms in the asymmetric unit of the title structure, (C2H10N2)5[Zr(SO4)5(H2O)][Zr(SO4)4(H2O)2], are both eight-coordinate. In the docedahedral aqua­penta­sulfatozirconate(IV) hexa­anion, three of the sulfate groups are monodentate, whereas the other two chelate to the metal atom. In the square-anti­prismatic diaqua­tetra­sulfato­zircon­ate(IV) tetra­anion, two of the sulfate groups are monodentate and two are bidentate. Two of the five 1,2-ethanediammonium cations lie about crystallographic centres of inversion. The cations and anions are linked into a three-dimensional network architecture by hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051750/lh2260sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051750/lh2260Isup2.hkl
Contains datablock I

CCDC reference: 633916

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.010 Å
  • Disorder in solvent or counterion
  • R factor = 0.066
  • wR factor = 0.177
  • Data-to-parameter ratio = 12.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT213_ALERT_2_B Atom O2 has ADP max/min Ratio ............. 5.00 oblat PLAT432_ALERT_2_B Short Inter X...Y Contact O24 .. C5' .. 2.79 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O28 .. C5 .. 2.87 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact O30 .. C6' .. 2.85 Ang.
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.119 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) . 100 Ang. PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.50 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S4 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C2 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C4 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 8.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6 PLAT731_ALERT_1_C Bond Calc 1.450(11), Rep 1.450(5) ...... 2.20 su-Ra N1 -C1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.459(12), Rep 1.458(5) ...... 2.40 su-Ra N2 -C2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.448(13), Rep 1.448(5) ...... 2.60 su-Ra N3 -C3 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.456(14), Rep 1.456(5) ...... 2.80 su-Ra N4 -C4 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.456(11), Rep 1.455(5) ...... 2.20 su-Ra N7 -C7 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.456(11), Rep 1.455(5) ...... 2.20 su-Ra N8 -C8 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.451(12), Rep 1.452(5) ...... 2.40 su-Ra N9 -C9 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.452(13), Rep 1.451(5) ...... 2.60 su-Ra N10 -C10 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.500(13), Rep 1.500(5) ...... 2.60 su-Ra C1 -C2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.489(14), Rep 1.489(5) ...... 2.80 su-Ra C3 -C4 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H4 O18 S4 Zr
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 25 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 16 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2006).

Pentakis(ethane-1,2-diammonium) aquapentasulfato-κ3O,κ4O,O')zirconate(IV) diaquatetrasulfato-κ2O,κ4O,O')zirconate(IV) top
Crystal data top
(C2H10N2)5[Zr(SO4)5(H2O)][Zr(SO4)4(H2O)2]F(000) = 2888
Mr = 1411.63Dx = 2.126 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 1024 reflections
a = 14.660 (1) Åθ = 2.7–19°
b = 16.845 (1) ŵ = 1.03 mm1
c = 17.887 (1) ÅT = 293 K
β = 93.298 (2)°Block, colourless
V = 4410.0 (6) Å30.09 × 0.07 × 0.05 mm
Z = 4
Data collection top
Bruker APEX area-detector
diffractometer
7733 independent reflections
Radiation source: fine-focus sealed tube4468 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.119
φ and w\ scansθmax = 25.0°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1217
Tmin = 0.913, Tmax = 0.950k = 1919
23065 measured reflectionsl = 2120
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)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.177H-atom parameters constrained
S = 0.99 w = 1/[σ2(Fo2) + (0.0719P)2]
where P = (Fo2 + 2Fc2)/3
7733 reflections(Δ/σ)max = 0.001
637 parametersΔρmax = 0.75 e Å3
385 restraintsΔρmin = 0.76 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr10.36847 (6)0.39772 (5)0.62589 (5)0.0132 (2)
Zr20.13910 (6)0.12896 (5)0.38775 (5)0.0158 (2)
S10.48846 (17)0.40929 (14)0.76150 (14)0.0211 (6)
S20.22301 (16)0.29022 (13)0.66352 (13)0.0176 (6)
S30.50564 (17)0.28391 (14)0.51044 (14)0.0201 (6)
S40.24721 (17)0.56678 (13)0.66613 (14)0.0182 (6)
S50.27267 (16)0.40024 (13)0.44235 (13)0.0176 (5)
S60.03106 (18)0.25372 (15)0.45633 (15)0.0265 (6)
S70.05892 (18)0.10762 (16)0.24578 (15)0.0278 (6)
S80.21505 (17)0.10618 (14)0.56743 (14)0.0201 (6)
S90.25644 (17)0.04497 (14)0.34651 (14)0.0207 (6)
O10.4984 (4)0.4460 (3)0.6866 (3)0.0196 (15)
O20.4054 (4)0.3592 (4)0.7441 (3)0.0207 (16)
O30.4712 (5)0.4670 (4)0.8183 (4)0.0318 (18)
O40.5675 (5)0.3611 (4)0.7844 (4)0.0337 (19)
O50.3157 (4)0.2702 (3)0.6372 (4)0.0200 (15)
O60.2307 (4)0.3788 (3)0.6715 (3)0.0143 (14)
O70.1527 (4)0.2700 (3)0.6060 (3)0.0211 (15)
O80.2090 (4)0.2549 (4)0.7346 (3)0.0250 (16)
O90.4628 (4)0.3253 (4)0.5745 (4)0.0252 (17)
O100.5710 (5)0.2264 (4)0.5419 (4)0.0317 (18)
O110.5527 (5)0.3434 (4)0.4680 (4)0.0346 (19)
O120.4351 (5)0.2431 (4)0.4652 (4)0.041 (2)
O130.3268 (4)0.5096 (4)0.6653 (4)0.0254 (16)
O140.1946 (6)0.5457 (5)0.7271 (4)0.050 (2)
O150.2878 (5)0.6454 (4)0.6787 (4)0.0304 (18)
O160.1952 (6)0.5631 (4)0.5943 (4)0.048 (2)
O170.2858 (4)0.3882 (4)0.5265 (3)0.0225 (16)
O180.2619 (5)0.3229 (3)0.4055 (3)0.0242 (16)
O190.1912 (4)0.4474 (4)0.4260 (4)0.0281 (17)
O200.3539 (4)0.4414 (4)0.4167 (4)0.0280 (17)
O210.1101 (5)0.2554 (4)0.3998 (4)0.0278 (17)
O220.0218 (4)0.1651 (4)0.4638 (4)0.0261 (17)
O230.0558 (5)0.2892 (4)0.5283 (4)0.040 (2)
O240.0486 (5)0.2891 (4)0.4268 (4)0.046 (2)
O250.1346 (5)0.1628 (4)0.2657 (4)0.0273 (17)
O260.0306 (5)0.0772 (4)0.3220 (4)0.0287 (17)
O270.0157 (5)0.1478 (5)0.2145 (4)0.046 (2)
O280.0966 (5)0.0447 (4)0.1999 (4)0.041 (2)
O290.2141 (4)0.1303 (4)0.4839 (3)0.0193 (15)
O300.1336 (5)0.0569 (4)0.5856 (4)0.0304 (18)
O310.2146 (5)0.1779 (4)0.6116 (4)0.0318 (18)
O320.2980 (4)0.0604 (4)0.5767 (4)0.0313 (18)
O330.2313 (4)0.0427 (3)0.3428 (4)0.0245 (16)
O340.1726 (5)0.0885 (4)0.3704 (4)0.0356 (19)
O350.2885 (5)0.0682 (4)0.2726 (4)0.0326 (19)
O360.3255 (5)0.0545 (4)0.4002 (4)0.039 (2)
O1W0.4309 (4)0.4849 (3)0.5498 (4)0.0245 (16)
H1W10.41250.53270.54480.029*
H1W20.42550.46450.50620.029*
O2W0.0819 (4)0.0228 (3)0.4463 (3)0.0202 (15)
H2W10.10210.01920.48920.024*
H2W20.09580.01870.42070.024*
O3W0.2698 (4)0.1980 (3)0.3548 (4)0.0246 (17)
H3W10.30760.16910.32830.030*
H3W20.25810.23900.32850.030*
N10.7057 (6)0.4308 (4)0.6768 (4)0.030 (2)
H1A0.67360.42540.71460.036*
H1B0.68680.47080.65130.036*
H1C0.76130.43780.69150.036*
N20.7422 (5)0.3127 (4)0.5056 (4)0.027 (2)
H2A0.77640.32370.47030.032*
H2B0.68670.31260.48900.032*
H2C0.75610.26710.52320.032*
N30.1794 (6)0.4204 (5)0.8225 (4)0.033 (2)
H3A0.20230.42970.78080.040*
H3B0.16740.46410.84360.040*
H3C0.13050.39370.81520.040*
N40.2553 (6)0.3131 (5)0.9994 (4)0.035 (2)
H4A0.22460.30851.03810.042*
H4B0.30510.33711.01100.042*
H4C0.26680.26730.98240.042*
N50.1063 (5)0.1276 (5)0.7935 (5)0.033 (2)
H5A0.12350.09610.82870.039*
H5B0.10650.17490.81010.039*
H5C0.14250.12410.75830.039*
N60.0054 (6)0.1831 (5)0.6496 (4)0.036 (2)
H6A0.04490.21070.62460.043*
H6B0.00240.13710.63040.043*
H6C0.04650.20560.64900.043*
N70.4048 (5)0.6300 (5)0.8085 (4)0.030 (2)
H7A0.39300.63730.85390.036*
H7B0.40940.58060.80000.036*
H7C0.36200.64940.78000.036*
N80.6020 (5)0.6920 (5)0.7006 (4)0.029 (2)
H8A0.61400.68480.65520.035*
H8B0.64290.67000.72920.035*
H8C0.60080.74150.70990.035*
N90.5672 (5)0.4186 (5)0.9603 (5)0.035 (2)
H9A0.55900.36860.95900.043*
H9B0.61780.42890.98390.043*
H9C0.56810.43640.91590.043*
N100.0753 (5)0.4307 (4)0.5589 (4)0.026 (2)
H10A0.06820.41050.60170.031*
H10B0.12450.45760.56040.031*
H10C0.07830.39390.52670.031*
C10.6977 (7)0.3601 (5)0.6307 (5)0.031 (3)
H1D0.63440.35140.61390.037*
H1E0.71900.31410.65930.037*
C20.7549 (7)0.3720 (6)0.5647 (5)0.044 (3)
H2D0.74110.42390.54340.053*
H2E0.81870.37210.58230.053*
C30.2441 (7)0.3759 (7)0.8702 (5)0.048 (3)
H3D0.29970.40640.87920.058*
H3E0.25950.32670.84570.058*
C40.2028 (8)0.3584 (8)0.9425 (6)0.070 (4)
H4D0.18700.40870.96470.084*
H4E0.14610.33010.93110.084*
C50.0142 (8)0.1065 (10)0.7654 (12)0.032 (4)0.50
H5D0.02130.08970.80670.038*0.50
H5E0.01700.06260.73050.038*0.50
C60.0316 (14)0.1763 (11)0.7267 (6)0.038 (4)0.50
H6D0.09730.17030.72710.045*0.50
H6E0.01470.22450.75370.045*0.50
C5'0.0100 (7)0.1479 (13)0.7842 (10)0.032 (4)0.50
H5F0.00240.20440.79250.038*0.50
H5G0.02350.11970.82110.038*0.50
C6'0.0280 (16)0.1269 (11)0.7073 (8)0.038 (4)0.50
H6F0.00530.07500.69420.045*0.50
H6G0.09400.12330.70810.045*0.50
C70.4905 (5)0.6691 (6)0.7938 (4)0.026 (2)
H7D0.53920.64760.82680.031*
H7E0.48560.72540.80410.031*
C80.5134 (5)0.6573 (6)0.7138 (4)0.025 (2)
H8D0.51450.60100.70250.030*
H8E0.46680.68190.68080.030*
C90.4934 (6)0.45598 (16)0.9980 (6)0.033 (3)
H9D0.49140.43471.04830.040*
H9E0.43560.44410.97120.040*
C100.0014 (7)0.4823 (7)0.5384 (3)0.055 (4)
H10D0.00300.52490.57470.066*
H10E0.05750.45210.54110.066*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.0136 (5)0.0139 (5)0.0122 (5)0.0007 (4)0.0013 (4)0.0009 (4)
Zr20.0145 (5)0.0169 (5)0.0160 (5)0.0000 (4)0.0008 (4)0.0017 (4)
S10.0216 (14)0.0203 (13)0.0208 (15)0.0024 (11)0.0028 (11)0.0010 (11)
S20.0153 (13)0.0176 (13)0.0199 (14)0.0019 (10)0.0011 (11)0.0006 (10)
S30.0201 (14)0.0237 (13)0.0168 (14)0.0001 (11)0.0028 (11)0.0025 (10)
S40.0179 (14)0.0136 (12)0.0235 (15)0.0015 (10)0.0031 (11)0.0011 (10)
S50.0180 (14)0.0199 (12)0.0146 (13)0.0011 (11)0.0011 (10)0.0002 (10)
S60.0221 (15)0.0239 (14)0.0330 (17)0.0049 (12)0.0030 (12)0.0021 (12)
S70.0254 (16)0.0400 (16)0.0182 (15)0.0019 (13)0.0041 (12)0.0003 (12)
S80.0190 (14)0.0199 (13)0.0218 (14)0.0022 (11)0.0034 (11)0.0023 (11)
S90.0229 (15)0.0172 (12)0.0220 (15)0.0025 (11)0.0017 (11)0.0007 (10)
O10.015 (3)0.023 (3)0.021 (4)0.003 (3)0.001 (3)0.006 (3)
O20.024 (4)0.030 (3)0.007 (3)0.000 (3)0.011 (3)0.003 (3)
O30.041 (4)0.035 (4)0.018 (4)0.002 (3)0.007 (3)0.005 (3)
O40.027 (4)0.036 (4)0.037 (4)0.005 (3)0.009 (3)0.008 (3)
O50.013 (3)0.014 (3)0.034 (4)0.001 (3)0.006 (3)0.001 (3)
O60.015 (3)0.014 (3)0.014 (3)0.003 (3)0.002 (3)0.003 (2)
O70.018 (4)0.021 (3)0.024 (4)0.003 (3)0.004 (3)0.004 (3)
O80.032 (4)0.030 (4)0.012 (4)0.003 (3)0.000 (3)0.014 (3)
O90.030 (4)0.026 (4)0.021 (4)0.004 (3)0.008 (3)0.004 (3)
O100.028 (4)0.029 (4)0.039 (4)0.005 (3)0.001 (3)0.000 (3)
O110.036 (4)0.039 (4)0.030 (4)0.005 (3)0.010 (3)0.007 (3)
O120.032 (4)0.052 (4)0.038 (5)0.005 (4)0.003 (4)0.014 (4)
O130.024 (4)0.023 (3)0.030 (4)0.001 (3)0.000 (3)0.001 (3)
O140.066 (5)0.048 (4)0.040 (5)0.014 (4)0.036 (4)0.014 (4)
O150.028 (4)0.020 (3)0.041 (4)0.001 (3)0.011 (3)0.001 (3)
O160.058 (5)0.038 (4)0.044 (5)0.006 (4)0.033 (4)0.000 (4)
O170.024 (4)0.030 (4)0.014 (3)0.001 (3)0.002 (3)0.006 (3)
O180.033 (4)0.024 (3)0.015 (4)0.004 (3)0.002 (3)0.003 (3)
O190.027 (4)0.030 (4)0.026 (4)0.003 (3)0.007 (3)0.004 (3)
O200.026 (4)0.026 (4)0.033 (4)0.007 (3)0.004 (3)0.003 (3)
O210.033 (4)0.022 (3)0.027 (4)0.005 (3)0.010 (3)0.002 (3)
O220.017 (4)0.021 (3)0.040 (4)0.002 (3)0.005 (3)0.002 (3)
O230.042 (5)0.032 (4)0.047 (5)0.001 (4)0.005 (4)0.011 (3)
O240.032 (4)0.050 (4)0.056 (5)0.023 (4)0.003 (4)0.013 (4)
O250.029 (4)0.034 (4)0.020 (4)0.007 (3)0.005 (3)0.007 (3)
O260.028 (4)0.038 (4)0.020 (4)0.005 (3)0.003 (3)0.001 (3)
O270.042 (5)0.061 (5)0.036 (5)0.013 (4)0.020 (4)0.002 (4)
O280.037 (4)0.045 (4)0.040 (5)0.002 (4)0.004 (4)0.009 (4)
O290.021 (4)0.029 (3)0.008 (3)0.003 (3)0.004 (3)0.005 (3)
O300.028 (4)0.035 (4)0.028 (4)0.009 (3)0.003 (3)0.008 (3)
O310.046 (4)0.029 (4)0.020 (4)0.003 (3)0.007 (3)0.009 (3)
O320.021 (4)0.034 (4)0.041 (4)0.007 (3)0.015 (3)0.004 (3)
O330.026 (4)0.016 (3)0.031 (4)0.003 (3)0.004 (3)0.001 (3)
O340.029 (4)0.021 (3)0.056 (5)0.006 (3)0.005 (4)0.007 (3)
O350.052 (5)0.032 (4)0.012 (4)0.002 (3)0.011 (3)0.000 (3)
O360.039 (4)0.037 (4)0.044 (5)0.002 (4)0.015 (4)0.002 (3)
O1W0.027 (4)0.023 (3)0.023 (4)0.005 (3)0.001 (3)0.002 (3)
O2W0.022 (4)0.024 (3)0.014 (3)0.003 (3)0.000 (3)0.004 (3)
O3W0.022 (4)0.014 (3)0.038 (4)0.000 (3)0.000 (3)0.003 (3)
N10.033 (5)0.039 (5)0.017 (4)0.005 (4)0.005 (4)0.001 (4)
N20.025 (5)0.027 (4)0.030 (5)0.000 (4)0.006 (4)0.008 (4)
N30.039 (5)0.031 (5)0.030 (5)0.002 (4)0.004 (4)0.002 (4)
N40.046 (5)0.034 (5)0.025 (5)0.007 (4)0.002 (4)0.006 (4)
N50.022 (5)0.043 (5)0.033 (5)0.001 (4)0.002 (4)0.009 (4)
N60.033 (5)0.038 (5)0.036 (5)0.005 (4)0.005 (4)0.013 (4)
N70.033 (5)0.036 (5)0.023 (5)0.005 (4)0.007 (4)0.007 (4)
N80.029 (5)0.031 (4)0.028 (5)0.005 (4)0.007 (4)0.003 (4)
N90.040 (5)0.033 (5)0.032 (5)0.001 (4)0.006 (4)0.002 (4)
N100.028 (5)0.031 (4)0.018 (4)0.000 (4)0.006 (4)0.007 (4)
C10.040 (6)0.037 (5)0.016 (5)0.008 (5)0.003 (5)0.009 (4)
C20.042 (6)0.036 (6)0.057 (7)0.009 (5)0.014 (5)0.015 (5)
C30.057 (7)0.057 (6)0.030 (6)0.017 (6)0.002 (5)0.005 (5)
C40.059 (7)0.073 (7)0.079 (8)0.018 (6)0.008 (7)0.024 (7)
C50.030 (6)0.038 (7)0.027 (6)0.002 (6)0.002 (5)0.002 (6)
C60.039 (6)0.042 (7)0.031 (7)0.008 (6)0.006 (5)0.004 (6)
C5'0.030 (6)0.038 (7)0.027 (6)0.002 (6)0.002 (5)0.002 (6)
C6'0.039 (6)0.042 (7)0.031 (7)0.008 (6)0.006 (5)0.004 (6)
C70.025 (5)0.032 (5)0.021 (5)0.014 (4)0.004 (4)0.008 (4)
C80.025 (5)0.031 (5)0.020 (5)0.006 (4)0.004 (4)0.002 (4)
C90.033 (6)0.038 (5)0.030 (6)0.007 (5)0.008 (5)0.007 (5)
C100.054 (7)0.062 (7)0.050 (7)0.023 (6)0.010 (6)0.017 (6)
Geometric parameters (Å, º) top
Zr1—O12.287 (6)N3—C31.448 (5)
Zr1—O22.248 (6)N3—H3A0.8500
Zr1—O52.296 (6)N3—H3B0.8500
Zr1—O62.245 (6)N3—H3C0.8500
Zr1—O92.096 (6)N4—C41.456 (5)
Zr1—O132.115 (6)N4—H4A0.8500
Zr1—O172.100 (6)N4—H4B0.8500
Zr1—O1W2.235 (6)N4—H4C0.8500
Zr2—O212.180 (6)N5—C5'1.453 (5)
Zr2—O222.216 (6)N5—C51.458 (5)
Zr2—O252.260 (7)N5—H5A0.8500
Zr2—O262.212 (7)N5—H5B0.8500
Zr2—O292.094 (6)N5—H5C0.8500
Zr2—O332.112 (6)N6—C6'1.452 (5)
Zr2—O2W2.213 (6)N6—C61.456 (5)
Zr2—O3W2.289 (6)N6—H6A0.8500
S1—O31.439 (7)N6—H6B0.8500
S1—O41.454 (7)N6—H6C0.8500
S1—O11.491 (6)N7—C71.455 (5)
S1—O21.500 (6)N7—H7A0.8500
S2—O81.429 (6)N7—H7B0.8500
S2—O71.455 (6)N7—H7C0.8500
S2—O51.503 (6)N8—C81.455 (5)
S2—O61.503 (6)N8—H8A0.8500
S3—O121.449 (7)N8—H8B0.8500
S3—O101.453 (7)N8—H8C0.8500
S3—O111.455 (7)N9—C91.452 (5)
S3—O91.509 (7)N9—H9A0.8500
S4—O141.416 (8)N9—H9B0.8500
S4—O161.458 (7)N9—H9C0.8500
S4—O151.465 (6)N10—C101.451 (5)
S4—O131.513 (7)N10—H10A0.8500
S5—O191.450 (6)N10—H10B0.8500
S5—O181.464 (6)N10—H10C0.8500
S5—O201.474 (7)C1—C21.500 (5)
S5—O171.520 (6)C1—H1D0.9700
S6—O241.439 (7)C1—H1E0.9700
S6—O231.483 (8)C2—H2D0.9700
S6—O211.493 (7)C2—H2E0.9700
S6—O221.504 (6)C3—C41.489 (5)
S7—O271.427 (8)C3—H3D0.9700
S7—O281.432 (7)C3—H3E0.9700
S7—O261.492 (7)C4—H4D0.9700
S7—O251.505 (7)C4—H4E0.9700
S8—O311.444 (6)C5—C61.503 (5)
S8—O321.458 (7)C5—H5D0.9700
S8—O301.475 (7)C5—H5E0.9700
S8—O291.549 (6)C6—H6D0.9700
S9—O351.431 (6)C6—H6E0.9700
S9—O361.444 (8)C5'—C6'1.497 (5)
S9—O341.474 (7)C5'—H5F0.9700
S9—O331.524 (6)C5'—H5G0.9700
O1W—H1W10.85C6'—H6F0.9700
O1W—H1W20.85C6'—H6G0.9700
O2W—H2W10.84C7—C81.502 (5)
O2W—H2W20.85C7—H7D0.9700
O3W—H3W10.86C7—H7E0.9700
O3W—H3W20.86C8—H8D0.9700
N1—C11.450 (5)C8—H8E0.9700
N1—H1A0.8500C9—C9i1.497 (5)
N1—H1B0.8500C9—H9D0.9700
N1—H1C0.8500C9—H9E0.9700
N2—C21.458 (5)C10—C10ii1.501 (5)
N2—H2A0.8500C10—H10D0.9700
N2—H2B0.8500C10—H10E0.9700
N2—H2C0.8500
O1—Zr1—O260.5 (2)C1—N1—H1A109.5
O1—Zr1—O5124.5 (2)C1—N1—H1B109.5
O1—Zr1—O6128.3 (2)H1A—N1—H1B109.5
O1—Zr1—O982.1 (2)C1—N1—H1C109.5
O1—Zr1—O1376.9 (2)H1A—N1—H1C109.5
O1—Zr1—O17148.6 (2)H1B—N1—H1C109.5
O1—Zr1—O1W72.3 (2)C2—N2—H2A109.5
O2—Zr1—O573.2 (2)C2—N2—H2B109.5
O2—Zr1—O677.9 (2)H2A—N2—H2B109.5
O2—Zr1—O996.6 (2)C2—N2—H2C109.5
O2—Zr1—O1390.1 (2)H2A—N2—H2C109.5
O2—Zr1—O17150.5 (2)H2B—N2—H2C109.5
O2—Zr1—O1W132.7 (2)C3—N3—H3A109.5
O5—Zr1—O661.4 (2)C3—N3—H3B109.5
O5—Zr1—O974.2 (2)H3A—N3—H3B109.5
O5—Zr1—O13134.4 (2)C3—N3—H3C109.5
O5—Zr1—O1779.8 (2)H3A—N3—H3C109.5
O5—Zr1—O1W145.2 (2)H3B—N3—H3C109.5
O6—Zr1—O9135.0 (2)C4—N4—H4A109.5
O6—Zr1—O1373.8 (2)C4—N4—H4B109.5
O6—Zr1—O1779.0 (2)H4A—N4—H4B109.5
O6—Zr1—O1W136.4 (2)C4—N4—H4C109.5
O9—Zr1—O13151.1 (3)H4A—N4—H4C109.5
O9—Zr1—O1W79.2 (2)H4B—N4—H4C109.5
O9—Zr1—O1787.0 (2)C5—N5—H5A109.5
O13—Zr1—O17100.8 (2)C5—N5—H5B109.5
O13—Zr1—O1W75.8 (2)H5A—N5—H5B109.5
O17—Zr1—O1W76.8 (2)C5—N5—H5C109.5
O21—Zr2—O2262.0 (2)H5A—N5—H5C109.5
O21—Zr2—O2580.4 (2)H5B—N5—H5C109.5
O21—Zr2—O26107.2 (3)C6—N6—H6A109.5
O21—Zr2—O2991.0 (3)C6—N6—H6B109.5
O21—Zr2—O33145.8 (2)H6A—N6—H6B109.5
O21—Zr2—O2W132.5 (2)C6—N6—H6C109.5
O21—Zr2—O3W71.7 (2)H6A—N6—H6C109.5
O22—Zr2—O25117.3 (2)H6B—N6—H6C109.5
O22—Zr2—O2683.0 (2)C7—N7—H7A109.5
O22—Zr2—O2985.3 (2)C7—N7—H7B109.5
O22—Zr2—O33151.6 (2)H7A—N7—H7B109.5
O22—Zr2—O2W70.9 (2)C7—N7—H7C109.5
O22—Zr2—O3W128.8 (2)H7A—N7—H7C109.5
O25—Zr2—O2661.5 (2)H7B—N7—H7C109.5
O25—Zr2—O29146.8 (2)C8—N8—H8A109.5
O25—Zr2—O3381.9 (2)C8—N8—H8B109.5
O25—Zr2—O2W129.0 (2)H8A—N8—H8B109.5
O25—Zr2—O3W72.2 (2)C8—N8—H8C109.5
O26—Zr2—O29150.3 (2)H8A—N8—H8C109.5
O26—Zr2—O3389.4 (3)H8B—N8—H8C109.5
O26—Zr2—O2W70.6 (2)C9—N9—H9A109.5
O26—Zr2—O3W132.9 (2)C9—N9—H9B109.5
O29—Zr2—O3388.0 (3)H9A—N9—H9B109.5
O29—Zr2—O2W79.8 (2)C9—N9—H9C109.5
O29—Zr2—O3W74.6 (2)H9A—N9—H9C109.5
O33—Zr2—O2W80.8 (2)H9B—N9—H9C109.5
O33—Zr2—O3W75.1 (2)C10—N10—H10A109.5
O2W—Zr2—O3W145.2 (2)C10—N10—H10B109.5
O3—S1—O4110.4 (4)H10A—N10—H10B109.5
O3—S1—O1112.6 (4)C10—N10—H10C109.5
O4—S1—O1111.5 (4)H10A—N10—H10C109.5
O3—S1—O2110.7 (4)H10B—N10—H10C109.5
O4—S1—O2111.6 (4)N1—C1—C2107.9 (7)
O1—S1—O299.6 (3)N1—C1—H1D110.1
O8—S2—O7113.5 (4)C2—C1—H1D110.1
O8—S2—O5111.3 (4)N1—C1—H1E110.1
O7—S2—O5110.1 (4)C2—C1—H1E110.1
O8—S2—O6110.1 (4)H1D—C1—H1E108.4
O7—S2—O6110.3 (3)N2—C2—C1115.1 (7)
O5—S2—O6100.9 (4)N2—C2—H2D108.5
O12—S3—O10109.5 (4)C1—C2—H2D108.5
O12—S3—O11112.3 (4)N2—C2—H2E108.5
O10—S3—O11109.8 (4)C1—C2—H2E108.5
O12—S3—O9109.2 (4)H2D—C2—H2E107.5
O10—S3—O9107.9 (4)N3—C3—C4109.2 (7)
O11—S3—O9108.0 (4)N3—C3—H3D109.8
O14—S4—O16112.8 (5)C4—C3—H3D109.8
O14—S4—O15110.0 (5)N3—C3—H3E109.8
O16—S4—O15111.2 (4)C4—C3—H3E109.8
O14—S4—O13107.5 (4)H3D—C3—H3E108.3
O16—S4—O13109.2 (4)N4—C4—C3119.1 (8)
O15—S4—O13105.7 (4)N4—C4—H4D107.5
O19—S5—O18109.3 (4)C3—C4—H4D107.5
O19—S5—O20110.5 (4)N4—C4—H4E107.5
O18—S5—O20110.3 (4)C3—C4—H4E107.5
O19—S5—O17109.2 (4)H4D—C4—H4E107.0
O18—S5—O17109.3 (4)N5—C5—C6110.4 (14)
O20—S5—O17108.2 (4)N5—C5—H5D109.6
O24—S6—O23113.3 (5)C6—C5—H5D109.6
O24—S6—O21111.0 (4)N5—C5—H5E109.6
O23—S6—O21111.2 (4)C6—C5—H5E109.6
O24—S6—O22111.9 (5)H5D—C5—H5E108.1
O23—S6—O22110.4 (4)N6—C6—C5111.3 (14)
O21—S6—O2298.1 (4)N6—C6—H6D109.4
O27—S7—O28113.9 (5)C5—C6—H6D109.4
O27—S7—O26109.9 (4)N6—C6—H6E109.4
O28—S7—O26110.3 (4)C5—C6—H6E109.4
O27—S7—O25113.1 (4)H6D—C6—H6E108.0
O28—S7—O25109.1 (4)N5—C5'—C6'111.0 (14)
O26—S7—O2599.5 (4)N5—C5'—H5F109.4
O31—S8—O32111.0 (4)C6'—C5'—H5F109.4
O31—S8—O30111.8 (4)N5—C5'—H5G109.4
O32—S8—O30110.3 (4)C6'—C5'—H5G109.4
O31—S8—O29108.0 (4)H5F—C5'—H5G108.0
O32—S8—O29107.6 (4)N6—C6'—C5'114.2 (14)
O30—S8—O29107.9 (4)N6—C6'—H6F108.7
O35—S9—O36112.3 (5)C5'—C6'—H6F108.7
O35—S9—O34110.8 (4)N6—C6'—H6G108.7
O36—S9—O34110.9 (4)C5'—C6'—H6G108.7
O35—S9—O33106.9 (4)H6F—C6'—H6G107.6
O36—S9—O33108.5 (4)N7—C7—C8110.8 (6)
O34—S9—O33107.2 (4)N7—C7—H7D109.5
S1—O1—Zr199.1 (3)C8—C7—H7D109.5
S1—O2—Zr1100.4 (3)N7—C7—H7E109.5
S2—O5—Zr197.6 (3)C8—C7—H7E109.5
S2—O6—Zr199.8 (3)H7D—C7—H7E108.1
S3—O9—Zr1156.3 (4)N8—C8—C7110.6 (6)
S4—O13—Zr1143.9 (4)N8—C8—H8D109.5
S5—O17—Zr1149.6 (4)C7—C8—H8D109.5
S6—O21—Zr2100.9 (3)N8—C8—H8E109.5
S6—O22—Zr298.9 (3)C7—C8—H8E109.5
S7—O25—Zr297.8 (3)H8D—C8—H8E108.1
S7—O26—Zr2100.3 (3)N9—C9—C9i110.7 (8)
S8—O29—Zr2145.5 (4)N9—C9—H9D109.5
S9—O33—Zr2143.2 (4)C9i—C9—H9D109.5
Zr1—O1W—H1W1123.1N9—C9—H9E109.5
Zr1—O1W—H1W2105.8C9i—C9—H9E109.5
H1W1—O1W—H1W2106.0H9D—C9—H9E108.1
Zr2—O2W—H2W1110.3N10—C10—C10ii114.1 (8)
Zr2—O2W—H2W2109.7N10—C10—H10D108.7
H2W1—O2W—H2W2110.1C10ii—C10—H10D108.7
Zr2—O3W—H3W1111.1N10—C10—H10E108.7
Zr2—O3W—H3W2111.1C10ii—C10—H10E108.7
H3W1—O3W—H3W2107.2H10D—C10—H10E107.6
O3—S1—O1—Zr1111.9 (4)O24—S6—O21—Zr2120.0 (4)
O4—S1—O1—Zr1123.4 (3)O23—S6—O21—Zr2112.9 (4)
O2—S1—O1—Zr15.4 (4)O22—S6—O21—Zr22.8 (4)
O9—Zr1—O1—S1106.3 (3)O29—Zr2—O21—S682.1 (4)
O17—Zr1—O1—S1177.1 (4)O33—Zr2—O21—S6170.0 (4)
O13—Zr1—O1—S193.6 (3)O26—Zr2—O21—S674.1 (4)
O1W—Zr1—O1—S1172.6 (4)O2W—Zr2—O21—S65.1 (6)
O6—Zr1—O1—S136.9 (4)O22—Zr2—O21—S62.1 (3)
O2—Zr1—O1—S14.1 (3)O25—Zr2—O21—S6130.2 (4)
O5—Zr1—O1—S141.7 (4)O3W—Zr2—O21—S6155.5 (4)
O3—S1—O2—Zr1113.2 (4)O24—S6—O22—Zr2119.3 (4)
O4—S1—O2—Zr1123.5 (4)O23—S6—O22—Zr2113.5 (4)
O1—S1—O2—Zr15.5 (4)O21—S6—O22—Zr22.7 (4)
O9—Zr1—O2—S181.1 (3)O29—Zr2—O22—S691.5 (4)
O17—Zr1—O2—S1176.7 (4)O33—Zr2—O22—S6168.5 (4)
O13—Zr1—O2—S170.7 (3)O21—Zr2—O22—S62.1 (3)
O1W—Zr1—O2—S10.2 (5)O26—Zr2—O22—S6115.8 (4)
O6—Zr1—O2—S1144.2 (3)O2W—Zr2—O22—S6172.3 (4)
O1—Zr1—O2—S14.1 (3)O25—Zr2—O22—S662.9 (4)
O5—Zr1—O2—S1152.4 (4)O3W—Zr2—O22—S625.6 (5)
O8—S2—O5—Zr1121.8 (3)O27—S7—O25—Zr2124.0 (4)
O7—S2—O5—Zr1111.4 (3)O28—S7—O25—Zr2108.1 (4)
O6—S2—O5—Zr15.0 (3)O26—S7—O25—Zr27.4 (4)
O9—Zr1—O5—S2169.0 (4)O29—Zr2—O25—S7161.9 (3)
O17—Zr1—O5—S279.2 (3)O33—Zr2—O25—S788.2 (3)
O13—Zr1—O5—S215.9 (5)O21—Zr2—O25—S7121.2 (4)
O1W—Zr1—O5—S2127.4 (4)O26—Zr2—O25—S75.6 (3)
O6—Zr1—O5—S23.8 (3)O2W—Zr2—O25—S717.0 (5)
O2—Zr1—O5—S288.9 (3)O22—Zr2—O25—S769.8 (4)
O1—Zr1—O5—S2122.6 (3)O3W—Zr2—O25—S7165.1 (4)
O8—S2—O6—Zr1122.9 (3)O27—S7—O26—Zr2126.6 (4)
O7—S2—O6—Zr1111.1 (4)O28—S7—O26—Zr2106.9 (4)
O5—S2—O6—Zr15.2 (4)O25—S7—O26—Zr27.6 (4)
O9—Zr1—O6—S26.1 (5)O29—Zr2—O26—S7160.4 (4)
O17—Zr1—O6—S280.5 (3)O33—Zr2—O26—S775.4 (3)
O13—Zr1—O6—S2174.8 (3)O21—Zr2—O26—S774.2 (4)
O1W—Zr1—O6—S2137.7 (3)O2W—Zr2—O26—S7155.9 (4)
O2—Zr1—O6—S281.1 (3)O22—Zr2—O26—S7132.0 (4)
O1—Zr1—O6—S2116.8 (3)O25—Zr2—O26—S75.7 (3)
O5—Zr1—O6—S23.8 (3)O3W—Zr2—O26—S76.4 (5)
O12—S3—O9—Zr149.2 (11)O31—S8—O29—Zr2113.9 (7)
O10—S3—O9—Zr1168.1 (10)O32—S8—O29—Zr2126.2 (7)
O11—S3—O9—Zr173.2 (11)O30—S8—O29—Zr27.2 (8)
O17—Zr1—O9—S315.9 (10)O33—Zr2—O29—S8107.9 (7)
O13—Zr1—O9—S391.1 (11)O21—Zr2—O29—S8106.3 (7)
O1W—Zr1—O9—S361.2 (10)O26—Zr2—O29—S822.5 (10)
O6—Zr1—O9—S387.0 (11)O2W—Zr2—O29—S826.9 (7)
O2—Zr1—O9—S3166.5 (10)O22—Zr2—O29—S844.5 (7)
O1—Zr1—O9—S3134.6 (11)O25—Zr2—O29—S8179.9 (5)
O5—Zr1—O9—S396.1 (10)O3W—Zr2—O29—S8177.0 (7)
O14—S4—O13—Zr187.0 (8)O35—S9—O33—Zr2146.0 (7)
O16—S4—O13—Zr135.7 (8)O36—S9—O33—Zr292.7 (8)
O15—S4—O13—Zr1155.5 (6)O34—S9—O33—Zr227.2 (8)
O9—Zr1—O13—S4133.4 (6)O29—Zr2—O33—S976.7 (7)
O17—Zr1—O13—S429.8 (7)O21—Zr2—O33—S9165.5 (6)
O1W—Zr1—O13—S4103.1 (7)O26—Zr2—O33—S973.8 (7)
O6—Zr1—O13—S445.3 (7)O2W—Zr2—O33—S93.3 (7)
O2—Zr1—O13—S4122.6 (7)O22—Zr2—O33—S90.3 (11)
O1—Zr1—O13—S4177.8 (7)O25—Zr2—O33—S9135.1 (7)
O5—Zr1—O13—S456.3 (8)O3W—Zr2—O33—S9151.3 (8)
O19—S5—O17—Zr1125.0 (8)N1—C1—C2—N2169.6 (9)
O18—S5—O17—Zr1115.5 (8)N3—C3—C4—N4179.4 (10)
O20—S5—O17—Zr14.7 (9)C5'—N5—C5—C644.6 (17)
O9—Zr1—O17—S558.8 (8)C6'—N6—C6—C538.6 (15)
O13—Zr1—O17—S593.2 (8)N5—C5—C6—N683 (2)
O1W—Zr1—O17—S520.8 (8)C5—N5—C5'—C6'42.2 (17)
O6—Zr1—O17—S5164.2 (8)C6—N6—C6'—C5'39.5 (15)
O2—Zr1—O17—S5156.9 (6)N5—C5'—C6'—N678 (2)
O1—Zr1—O17—S510.7 (11)N7—C7—C8—N8176.3 (8)
O5—Zr1—O17—S5133.3 (8)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O11iii0.852.162.921 (9)148
O1W—H1W2···O200.851.902.678 (9)150
O2W—H2W1···O300.841.922.708 (9)156
O2W—H2W2···O340.851.832.630 (9)156
O3W—H3W1···O4iv0.862.022.814 (9)154
O3W—H3W2···O15ii0.862.002.715 (8)140
N1—H1A···O40.852.323.10 (1)154
N1—H1B···O20iii0.851.982.83 (1)175
N1—H1C···O28v0.852.102.93 (1)166
N2—H2A···O16iii0.852.282.93 (1)134
N2—H2B···O110.852.052.87 (1)163
N2—H2C···O31vi0.852.203.00 (1)156
N3—H3A···O140.852.182.73 (1)123
N3—H3B···O30vii0.852.092.93 (1)168
N3—H3C···O26viii0.852.423.08 (1)135
N3—H3C···O27viii0.852.493.21 (1)142
N4—H4A···O7viii0.852.122.86 (1)146
N4—H4B···O36vii0.852.433.01 (1)126
N4—H4C···O18viii0.852.052.85 (1)156
N5—H5A···O19viii0.852.092.90 (1)161
N5—H5B···O24viii0.852.382.93 (1)123
N5—H5C···O80.852.452.86 (1)110
N5—H5C···O35ix0.852.433.15 (1)142
N5—H5C···O34ix0.852.443.21 (1)151
N5—H5C···O80.852.452.86 (1)110
N6—H6A···O230.852.172.88 (1)140
N6—H6B···O300.852.453.02 (1)125
N6—H6C···O70.852.082.89 (1)158
N7—H7A···O32vii0.852.312.90 (1)127
N7—H7A···O10x0.852.433.13 (1)141
N7—H7B···O30.852.132.92 (1)153
N7—H7C···O150.852.062.82 (1)148
N8—H8A···O18iii0.852.182.84 (1)135
N8—H8B···O35v0.852.112.89 (1)152
N8—H8C···O2x0.852.152.99 (1)169
N9—H9A···O10viii0.852.182.84 (1)135
N9—H9B···O32v0.852.022.81 (1)154
N9—H9C···O30.852.252.95 (1)140
N10—H10A···O27viii0.852.413.25 (1)168
N10—H10B···O160.852.132.89 (1)148
N10—H10C···O240.852.533.37 (1)167
Symmetry codes: (ii) x, y+1, z+1; (iii) x+1, y+1, z+1; (iv) x1, y+1/2, z1/2; (v) x+1, y+1/2, z+1/2; (vi) x+1, y, z; (vii) x, y+1/2, z+3/2; (viii) x, y+1/2, z+1/2; (ix) x, y, z+1; (x) x+1, y+1/2, z+3/2.
 

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