The zirconium(IV) ion in the title compound, (C
5H
6N)
4[Zr(SO
4)
4]·H
2O, exists in a distorted dodecahedral geometry with four bidentate sulfate groups. The tetraanion, two of the pyridinium cations and water molecule all lie on special positions with
m site symmetry. A network of N—H
O and O—H
O hydrogen bonds helps to stabilize the structure.
Supporting information
CCDC reference: 282367
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.012 Å
- R factor = 0.055
- wR factor = 0.143
- Data-to-parameter ratio = 16.7
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D H1W .. H3N .. 2.09 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H1W .. H3N .. 2.09 Ang.
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.768 0.955
Tmin(prime) and Tmax expected: 0.888 0.953
RR(prime) = 0.863
Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.86
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C9
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C10
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12
PLAT731_ALERT_1_C Bond Calc 1.336(11), Rep 1.336(5) ...... 2.20 su-Rat
N2 -C8 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.362(13), Rep 1.362(5) ...... 2.60 su-Rat
N3 -C9 1.555 4.655
PLAT731_ALERT_1_C Bond Calc 1.362(13), Rep 1.362(5) ...... 2.60 su-Rat
N3 -C9 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.380(11), Rep 1.380(5) ...... 2.20 su-Rat
C4 -C5 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.389(12), Rep 1.388(5) ...... 2.40 su-Rat
C5 -C6 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.388(12), Rep 1.389(5) ...... 2.40 su-Rat
C6 -C7 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.382(12), Rep 1.381(5) ...... 2.40 su-Rat
C7 -C8 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.382(14), Rep 1.381(5) ...... 2.80 su-Rat
C9 -C10 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.380(16), Rep 1.380(5) ...... 3.20 su-Rat
C10 -C11 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 1.380(16), Rep 1.380(5) ...... 3.20 su-Rat
C11 -C10 1.555 4.655
PLAT733_ALERT_1_C Torsion Calc 178.6(3), Rep 178.57(12) ...... 2.50 su-Rat
O7 -ZR1 -O7 -S3 4.655 1.555 1.555 1.555
PLAT733_ALERT_1_C Torsion Calc 0.1(11), Rep 0.0(3) ...... 3.67 su-Rat
N1 -C1 -C2 -C3 1.555 1.555 1.555 1.555
PLAT733_ALERT_1_C Torsion Calc -0.2(14), Rep -0.1(6) ...... 2.33 su-Rat
C1 -C2 -C3 -C2 1.555 1.555 1.555 4.655
PLAT733_ALERT_1_C Torsion Calc 0.4(12), Rep 0.3(3) ...... 4.00 su-Rat
N2 -C4 -C5 -C6 1.555 1.555 1.555 1.555
PLAT733_ALERT_1_C Torsion Calc 0.6(19), Rep 0.5(6) ...... 3.17 su-Rat
C9 -C10 -C11 -C10 1.555 1.555 1.555 4.655
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C20 H26 N4 O17 S4 Zr1
Atom count from _chemical_formula_moiety:C20 H26 O17 S4 Zr1
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 27.50
From the CIF: _reflns_number_total 3766
Count of symmetry unique reflns 2009
Completeness (_total/calc) 187.46%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 1757
Fraction of Friedel pairs measured 0.875
Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
21 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
17 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Tetrapyridinium tetrasulfatozirconate(IV) monohydrate
top
Crystal data top
(C5H6N)4[Zr(SO4)4]·H2O | F(000) = 1656 |
Mr = 813.91 | Dx = 1.683 Mg m−3 |
Orthorhombic, Cmc21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C 2c -2 | Cell parameters from 1681 reflections |
a = 11.355 (1) Å | θ = 2.3–21.2° |
b = 17.568 (2) Å | µ = 0.68 mm−1 |
c = 16.102 (2) Å | T = 295 K |
V = 3212.2 (6) Å3 | Block, colorless |
Z = 4 | 0.17 × 0.12 × 0.07 mm |
Data collection top
Bruker APEX area-detector diffractometer | 3766 independent reflections |
Radiation source: fine-focus sealed tube | 2961 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
φ and ω scans | θmax = 27.5°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→12 |
Tmin = 0.768, Tmax = 0.955 | k = −22→21 |
9733 measured reflections | l = −20→20 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.055 | H-atom parameters constrained |
wR(F2) = 0.143 | w = 1/[σ2(Fo2) + (0.0816P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max = 0.001 |
3766 reflections | Δρmax = 0.80 e Å−3 |
226 parameters | Δρmin = −0.55 e Å−3 |
106 restraints | Absolute structure: Flack (1983) 1783 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.04 (8) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Zr1 | 0.5000 | 0.62620 (4) | 0.50000 (11) | 0.02980 (19) | |
S1 | 0.5000 | 0.57964 (13) | 0.33051 (17) | 0.0400 (5) | |
S2 | 0.5000 | 0.77279 (12) | 0.58032 (16) | 0.0368 (5) | |
S3 | 0.73205 (14) | 0.57931 (9) | 0.54217 (14) | 0.0424 (4) | |
O1 | 0.5000 | 0.6592 (4) | 0.3689 (4) | 0.0403 (15) | |
O2 | 0.5000 | 0.5331 (4) | 0.4102 (4) | 0.0424 (15) | |
O3 | 0.6066 (5) | 0.5673 (3) | 0.2842 (3) | 0.0595 (13) | |
O4 | 0.5000 | 0.7521 (3) | 0.4882 (4) | 0.0379 (14) | |
O5 | 0.5000 | 0.6933 (3) | 0.6162 (4) | 0.0419 (15) | |
O6 | 0.6049 (4) | 0.8126 (3) | 0.6007 (3) | 0.0520 (12) | |
O7 | 0.6143 (3) | 0.5510 (2) | 0.5726 (3) | 0.0421 (10) | |
O8 | 0.6894 (4) | 0.6411 (2) | 0.4850 (3) | 0.0448 (12) | |
O9 | 0.8023 (5) | 0.6094 (3) | 0.6078 (4) | 0.0629 (14) | |
O10 | 0.7911 (4) | 0.5201 (3) | 0.4961 (5) | 0.0732 (15) | |
O1w | 0.5000 | 0.9602 (10) | 0.5311 (10) | 0.195 (7) | |
H1w | 0.4413 | 0.9872 | 0.5159 | 0.234* | |
N1 | 0.5000 | 0.3999 (5) | 0.5881 (4) | 0.076 (3) | |
H1n | 0.5000 | 0.4488 | 0.5895 | 0.091* | |
N2 | 0.6824 (7) | 0.7910 (4) | 0.3790 (5) | 0.100 (3) | |
H2n | 0.6334 | 0.7663 | 0.4096 | 0.120* | |
N3 | 0.5000 | 0.9628 (7) | 0.6899 (10) | 0.160 (7) | |
H3n | 0.5000 | 0.9754 | 0.6383 | 0.192* | |
C1 | 0.3950 (6) | 0.3658 (4) | 0.5871 (3) | 0.078 (3) | |
H1 | 0.3252 | 0.3935 | 0.5879 | 0.094* | |
C2 | 0.3954 (6) | 0.2875 (4) | 0.5849 (5) | 0.082 (3) | |
H2 | 0.3244 | 0.2611 | 0.5841 | 0.098* | |
C3 | 0.5000 | 0.2478 (6) | 0.5839 (7) | 0.077 (3) | |
H3 | 0.5000 | 0.1949 | 0.5824 | 0.092* | |
C4 | 0.7117 (7) | 0.8614 (4) | 0.4006 (5) | 0.081 (3) | |
H4 | 0.6795 | 0.8830 | 0.4482 | 0.097* | |
C5 | 0.7898 (7) | 0.9028 (5) | 0.3529 (5) | 0.077 (3) | |
H5 | 0.8111 | 0.9521 | 0.3677 | 0.092* | |
C6 | 0.8355 (7) | 0.8687 (5) | 0.2821 (5) | 0.087 (3) | |
H6 | 0.8875 | 0.8957 | 0.2486 | 0.104* | |
C7 | 0.8046 (7) | 0.7948 (5) | 0.2607 (5) | 0.089 (3) | |
H7 | 0.8359 | 0.7715 | 0.2138 | 0.106* | |
C8 | 0.7259 (7) | 0.7569 (5) | 0.3115 (5) | 0.093 (3) | |
H8 | 0.7031 | 0.7075 | 0.2985 | 0.112* | |
C9 | 0.3961 (9) | 0.9529 (5) | 0.7307 (6) | 0.117 (4) | |
H9 | 0.3251 | 0.9598 | 0.7029 | 0.141* | |
C10 | 0.3963 (11) | 0.9325 (6) | 0.8136 (6) | 0.114 (4) | |
H10 | 0.3249 | 0.9260 | 0.8410 | 0.136* | |
C11 | 0.5000 | 0.9215 (9) | 0.8567 (13) | 0.176 (11) | |
H11 | 0.5000 | 0.9074 | 0.9123 | 0.211* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zr1 | 0.0294 (4) | 0.0285 (3) | 0.0315 (3) | 0.000 | 0.000 | 0.0045 (4) |
S1 | 0.0434 (13) | 0.0396 (12) | 0.0370 (11) | 0.000 | 0.000 | −0.0036 (9) |
S2 | 0.0382 (12) | 0.0345 (11) | 0.0377 (11) | 0.000 | 0.000 | −0.0025 (9) |
S3 | 0.0332 (8) | 0.0416 (8) | 0.0526 (9) | 0.0019 (7) | −0.0061 (7) | −0.0031 (7) |
O1 | 0.051 (4) | 0.033 (3) | 0.037 (3) | 0.000 | 0.000 | 0.003 (3) |
O2 | 0.050 (4) | 0.036 (3) | 0.042 (3) | 0.000 | 0.000 | −0.001 (3) |
O3 | 0.060 (3) | 0.070 (3) | 0.049 (3) | 0.007 (3) | 0.012 (2) | −0.001 (2) |
O4 | 0.045 (3) | 0.028 (3) | 0.041 (4) | 0.000 | 0.000 | 0.001 (3) |
O5 | 0.053 (4) | 0.038 (3) | 0.035 (3) | 0.000 | 0.000 | 0.004 (3) |
O6 | 0.044 (3) | 0.049 (3) | 0.063 (3) | −0.009 (2) | −0.007 (2) | −0.007 (2) |
O7 | 0.037 (2) | 0.038 (2) | 0.051 (3) | 0.0002 (19) | −0.007 (2) | 0.0129 (19) |
O8 | 0.037 (2) | 0.049 (2) | 0.048 (3) | −0.0043 (18) | 0.003 (2) | 0.012 (2) |
O9 | 0.055 (3) | 0.065 (3) | 0.068 (3) | −0.009 (3) | −0.021 (3) | −0.004 (3) |
O10 | 0.052 (3) | 0.066 (3) | 0.102 (4) | 0.016 (2) | −0.003 (3) | −0.027 (4) |
O1w | 0.27 (2) | 0.170 (15) | 0.141 (15) | 0.000 | 0.000 | 0.009 (12) |
N1 | 0.104 (7) | 0.044 (5) | 0.079 (6) | 0.000 | 0.000 | −0.001 (5) |
N2 | 0.123 (7) | 0.079 (5) | 0.098 (5) | −0.020 (5) | 0.033 (5) | 0.009 (5) |
N3 | 0.181 (11) | 0.165 (10) | 0.134 (10) | 0.000 | 0.000 | −0.020 (8) |
C1 | 0.076 (6) | 0.069 (5) | 0.090 (6) | 0.017 (4) | 0.008 (5) | −0.004 (4) |
C2 | 0.061 (5) | 0.066 (5) | 0.119 (6) | −0.006 (4) | −0.003 (5) | −0.010 (5) |
C3 | 0.073 (7) | 0.051 (6) | 0.107 (8) | 0.000 | 0.000 | −0.007 (6) |
C4 | 0.101 (6) | 0.077 (5) | 0.066 (5) | −0.006 (5) | 0.018 (5) | −0.011 (4) |
C5 | 0.082 (6) | 0.064 (5) | 0.084 (6) | −0.012 (5) | 0.001 (5) | −0.009 (4) |
C6 | 0.071 (5) | 0.106 (6) | 0.083 (6) | −0.021 (5) | 0.016 (5) | 0.030 (5) |
C7 | 0.087 (6) | 0.101 (6) | 0.078 (5) | 0.005 (5) | 0.020 (5) | −0.026 (5) |
C8 | 0.108 (7) | 0.065 (5) | 0.107 (7) | −0.020 (5) | 0.018 (6) | −0.019 (5) |
C9 | 0.101 (7) | 0.125 (7) | 0.126 (8) | −0.008 (6) | −0.026 (7) | −0.034 (7) |
C10 | 0.089 (7) | 0.138 (8) | 0.113 (7) | −0.015 (6) | −0.006 (6) | −0.019 (7) |
C11 | 0.171 (13) | 0.176 (13) | 0.181 (14) | 0.000 | 0.000 | −0.005 (9) |
Geometric parameters (Å, º) top
Zr1—O1 | 2.189 (6) | N2—H2n | 0.8600 |
Zr1—O2 | 2.183 (6) | N3—C9i | 1.362 (5) |
Zr1—O4 | 2.220 (5) | N3—C9 | 1.362 (5) |
Zr1—O5 | 2.211 (6) | N3—H3n | 0.8600 |
Zr1—O7 | 2.191 (4) | C1—C2 | 1.375 (5) |
Zr1—O7i | 2.191 (4) | C1—H1 | 0.9300 |
Zr1—O8 | 2.180 (4) | C2—C3 | 1.377 (5) |
Zr1—O8i | 2.180 (4) | C2—H2 | 0.9300 |
S1—O3i | 1.438 (5) | C3—C2i | 1.377 (5) |
S1—O3 | 1.438 (5) | C3—H3 | 0.9300 |
S1—O2 | 1.521 (7) | C4—C5 | 1.380 (5) |
S1—O1 | 1.528 (7) | C4—H4 | 0.9300 |
S2—O6i | 1.419 (4) | C5—C6 | 1.388 (5) |
S2—O6 | 1.419 (4) | C5—H5 | 0.9300 |
S2—O5 | 1.512 (6) | C6—C7 | 1.389 (5) |
S2—O4 | 1.528 (6) | C6—H6 | 0.9300 |
S3—O9 | 1.426 (5) | C7—C8 | 1.381 (5) |
S3—O10 | 1.443 (5) | C7—H7 | 0.9300 |
S3—O8 | 1.504 (4) | C8—H8 | 0.9300 |
S3—O7 | 1.509 (4) | C9—C10 | 1.381 (5) |
O1w—H1w | 0.85 | C9—H9 | 0.9300 |
N1—C1 | 1.335 (5) | C10—C11 | 1.380 (5) |
N1—C1i | 1.335 (5) | C10—H10 | 0.9300 |
N1—H1n | 0.8600 | C11—C10i | 1.380 (5) |
N2—C4 | 1.329 (5) | C11—H11 | 0.9300 |
N2—C8 | 1.336 (5) | | |
| | | |
O1—Zr1—O2 | 63.8 (2) | S1—O2—Zr1 | 99.0 (3) |
O1—Zr1—O4 | 69.7 (2) | S2—O4—Zr1 | 98.9 (3) |
O1—Zr1—O5 | 132.4 (2) | S2—O5—Zr1 | 99.7 (3) |
O1—Zr1—O7 | 132.4 (2) | S3—O7—Zr1 | 98.8 (2) |
O1—Zr1—O7i | 132.4 (2) | S3—O8—Zr1 | 99.4 (2) |
O1—Zr1—O8 | 82.0 (1) | C1—N1—C1i | 126.7 (10) |
O1—Zr1—O8i | 82.0 (1) | C1—N1—H1n | 116.7 |
O2—Zr1—O4 | 133.6 (2) | C1i—N1—H1n | 116.7 |
O2—Zr1—O5 | 163.7 (2) | C4—N2—C8 | 122.5 (8) |
O2—Zr1—O7 | 84.4 (2) | C4—N2—H2n | 118.7 |
O2—Zr1—O7i | 84.4 (2) | C8—N2—H2n | 118.7 |
O2—Zr1—O8 | 90.9 (1) | C9i—N3—C9 | 120.1 (17) |
O2—Zr1—O8i | 90.9 (1) | C9i—N3—H3n | 120.0 |
O4—Zr1—O5 | 62.7 (2) | C9—N3—H3n | 120.0 |
O4—Zr1—O7 | 130.3 (2) | N1—C1—C2 | 116.5 (8) |
O4—Zr1—O7i | 130.3 (2) | N1—C1—H1 | 121.8 |
O4—Zr1—O8 | 82.6 (1) | C2—C1—H1 | 121.8 |
O4—Zr1—O8i | 82.6 (1) | C1—C2—C3 | 120.6 (9) |
O5—Zr1—O7 | 82.5 (2) | C1—C2—H2 | 119.7 |
O5i—Zr1—O7 | 82.5 (2) | C3—C2—H2 | 119.7 |
O5—Zr1—O8 | 91.7 (1) | C2i—C3—C2 | 119.2 (11) |
O5—Zr1—O8i | 91.7 (1) | C2i—C3—H3 | 120.4 |
O7—Zr1—O7i | 72.6 (2) | C2—C3—H3 | 120.4 |
O7—Zr1—O8 | 63.1 (2) | N2—C4—C5 | 120.4 (8) |
O7—Zr1—O8i | 135.7 (2) | N2—C4—H4 | 119.8 |
O7i—Zr1—O8 | 135.7 (2) | C5—C4—H4 | 119.8 |
O7i—Zr1—O8i | 63.1 (2) | C4—C5—C6 | 118.0 (8) |
O8—Zr1—O8i | 161.2 (2) | C4—C5—H5 | 121.0 |
O3i—S1—O3 | 114.7 (5) | C6—C5—H5 | 121.0 |
O3i—S1—O2 | 110.9 (3) | C5—C6—C7 | 120.9 (8) |
O3—S1—O2 | 110.9 (3) | C5—C6—H6 | 119.6 |
O3i—S1—O1 | 110.3 (3) | C7—C6—H6 | 119.6 |
O3—S1—O1 | 110.3 (3) | C8—C7—C6 | 117.8 (8) |
O2—S1—O1 | 98.6 (3) | C8—C7—H7 | 121.1 |
O6i—S2—O6 | 114.0 (4) | C6—C7—H7 | 121.1 |
O6i—S2—O5 | 111.5 (2) | N2—C8—C7 | 120.4 (8) |
O6—S2—O5 | 111.5 (2) | N2—C8—H8 | 119.8 |
O6i—S2—O4 | 110.0 (3) | C7—C8—H8 | 119.8 |
O6—S2—O4 | 110.0 (3) | N3—C9—C10 | 119.9 (14) |
O5—S2—O4 | 98.7 (3) | N3—C9—H9 | 120.1 |
O9—S3—O10 | 112.9 (3) | C10—C9—H9 | 120.1 |
O9—S3—O8 | 111.5 (3) | C11—C10—C9 | 121.5 (16) |
O10—S3—O8 | 110.8 (4) | C11—C10—H10 | 119.2 |
O9—S3—O7 | 112.1 (3) | C9—C10—H10 | 119.2 |
O10—S3—O7 | 109.9 (3) | C10—C11—C10i | 117 (2) |
O8—S3—O7 | 98.7 (2) | C10—C11—H11 | 121.4 |
O8—S3—Zr1 | 49.16 (16) | C10i—C11—H11 | 121.4 |
S1—O1—Zr1 | 98.5 (3) | | |
| | | |
O3i—S1—O1—Zr1 | 116.1 (3) | O8—Zr1—O5—S2 | 80.75 (11) |
O3—S1—O1—Zr1 | −116.1 (3) | O2—Zr1—O5—S2 | 180.000 (3) |
O2—S1—O1—Zr1 | 0.0 | O1—Zr1—O5—S2 | 0.000 (1) |
O8i—Zr1—O1—S1 | −95.01 (12) | O7i—Zr1—O5—S2 | −143.32 (11) |
O8—Zr1—O1—S1 | 95.01 (12) | O7—Zr1—O5—S2 | 143.32 (11) |
O2—Zr1—O1—S1 | 0.0 | O4—Zr1—O5—S2 | 0.0 |
O7i—Zr1—O1—S1 | −53.4 (2) | O9—S3—O7—Zr1 | 119.2 (3) |
O7—Zr1—O1—S1 | 53.4 (2) | O10—S3—O7—Zr1 | −114.4 (3) |
O5—Zr1—O1—S1 | 180.0 | O8—S3—O7—Zr1 | 1.6 (3) |
O4—Zr1—O1—S1 | 180.0 | O8i—Zr1—O7—S3 | 178.3 (2) |
O3i—S1—O2—Zr1 | −115.7 (3) | O8—Zr1—O7—S3 | −1.2 (2) |
O3—S1—O2—Zr1 | 115.7 (3) | O2—Zr1—O7—S3 | 92.7 (2) |
O1—S1—O2—Zr1 | 0.0 | O1—Zr1—O7—S3 | 46.4 (3) |
O8i—Zr1—O2—S1 | 80.64 (11) | O7i—Zr1—O7—S3 | 178.57 (12) |
O8—Zr1—O2—S1 | −80.64 (11) | O5—Zr1—O7—S3 | −97.0 (2) |
O1—Zr1—O2—S1 | 0.0 | O4—Zr1—O7—S3 | −52.8 (3) |
O7i—Zr1—O2—S1 | 143.47 (11) | O9—S3—O8—Zr1 | −119.6 (3) |
O7—Zr1—O2—S1 | −143.47 (11) | O10—S3—O8—Zr1 | 113.7 (3) |
O5—Zr1—O2—S1 | 180.000 (3) | O7—S3—O8—Zr1 | −1.6 (3) |
O4—Zr1—O2—S1 | 0.0 | O8i—Zr1—O8—S3 | −177.7 (6) |
O6i—S2—O4—Zr1 | −116.8 (2) | O2—Zr1—O8—S3 | −82.0 (3) |
O6—S2—O4—Zr1 | 116.8 (2) | O1—Zr1—O8—S3 | −145.4 (3) |
O5—S2—O4—Zr1 | 0.0 | O7i—Zr1—O8—S3 | 0.9 (4) |
O8i—Zr1—O4—S2 | 95.80 (12) | O7—Zr1—O8—S3 | 1.2 (2) |
O8—Zr1—O4—S2 | −95.80 (12) | O5—Zr1—O8—S3 | 81.9 (3) |
O2—Zr1—O4—S2 | 180.000 (1) | O4—Zr1—O8—S3 | 144.1 (3) |
O1—Zr1—O4—S2 | 180.0 | N1—C1—C2—C3 | 0.0 (3) |
O7i—Zr1—O4—S2 | 50.97 (18) | C1—C2—C3—C2i | −0.1 (6) |
O7—Zr1—O4—S2 | −50.97 (18) | N2—C4—C5—C6 | 0.3 (3) |
O5—Zr1—O4—S2 | 0.0 | C4—C5—C6—C7 | −0.8 (6) |
O6i—S2—O5—Zr1 | 115.6 (3) | C5—C6—C7—C8 | 0.9 (8) |
O6—S2—O5—Zr1 | −115.6 (3) | C4—N2—C8—C7 | −0.1 (7) |
O4—S2—O5—Zr1 | 0.0 | C6—C7—C8—N2 | −0.4 (8) |
O8i—Zr1—O5—S2 | −80.75 (11) | C9—C10—C11—C10i | 0.5 (6) |
Symmetry code: (i) −x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w···O10ii | 0.85 | 1.83 | 2.656 (9) | 162 |
N1—H1n···O7 | 0.86 | 2.23 | 2.965 (9) | 143 |
N1—H1n···O7i | 0.86 | 2.23 | 2.965 (9) | 143 |
N2—H2n···O4 | 0.86 | 1.99 | 2.801 (9) | 157 |
N3—H3n···O1w | 0.86 | 1.75 | 2.56 (2) | 156 |
Symmetry codes: (i) −x+1, y, z; (ii) x−1/2, y+1/2, z. |