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The zirconium(IV) ion in the title compound, (C5H6N)4[Zr(SO4)4]·H2O, 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805021409/hb6238sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805021409/hb6238Isup2.hkl
Contains datablock I

CCDC reference: 282367

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](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

Computing details top

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]·H2OF(000) = 1656
Mr = 813.91Dx = 1.683 Mg m3
Orthorhombic, Cmc21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2Cell parameters from 1681 reflections
a = 11.355 (1) Åθ = 2.3–21.2°
b = 17.568 (2) ŵ = 0.68 mm1
c = 16.102 (2) ÅT = 295 K
V = 3212.2 (6) Å3Block, colorless
Z = 40.17 × 0.12 × 0.07 mm
Data collection top
Bruker APEX area-detector
diffractometer
3766 independent reflections
Radiation source: fine-focus sealed tube2961 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.053
φ and ω scansθmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1412
Tmin = 0.768, Tmax = 0.955k = 2221
9733 measured reflectionsl = 2020
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.055H-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 reflectionsΔρmax = 0.80 e Å3
226 parametersΔρmin = 0.55 e Å3
106 restraintsAbsolute structure: Flack (1983) 1783 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.04 (8)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Zr10.50000.62620 (4)0.50000 (11)0.02980 (19)
S10.50000.57964 (13)0.33051 (17)0.0400 (5)
S20.50000.77279 (12)0.58032 (16)0.0368 (5)
S30.73205 (14)0.57931 (9)0.54217 (14)0.0424 (4)
O10.50000.6592 (4)0.3689 (4)0.0403 (15)
O20.50000.5331 (4)0.4102 (4)0.0424 (15)
O30.6066 (5)0.5673 (3)0.2842 (3)0.0595 (13)
O40.50000.7521 (3)0.4882 (4)0.0379 (14)
O50.50000.6933 (3)0.6162 (4)0.0419 (15)
O60.6049 (4)0.8126 (3)0.6007 (3)0.0520 (12)
O70.6143 (3)0.5510 (2)0.5726 (3)0.0421 (10)
O80.6894 (4)0.6411 (2)0.4850 (3)0.0448 (12)
O90.8023 (5)0.6094 (3)0.6078 (4)0.0629 (14)
O100.7911 (4)0.5201 (3)0.4961 (5)0.0732 (15)
O1w0.50000.9602 (10)0.5311 (10)0.195 (7)
H1w0.44130.98720.51590.234*
N10.50000.3999 (5)0.5881 (4)0.076 (3)
H1n0.50000.44880.58950.091*
N20.6824 (7)0.7910 (4)0.3790 (5)0.100 (3)
H2n0.63340.76630.40960.120*
N30.50000.9628 (7)0.6899 (10)0.160 (7)
H3n0.50000.97540.63830.192*
C10.3950 (6)0.3658 (4)0.5871 (3)0.078 (3)
H10.32520.39350.58790.094*
C20.3954 (6)0.2875 (4)0.5849 (5)0.082 (3)
H20.32440.26110.58410.098*
C30.50000.2478 (6)0.5839 (7)0.077 (3)
H30.50000.19490.58240.092*
C40.7117 (7)0.8614 (4)0.4006 (5)0.081 (3)
H40.67950.88300.44820.097*
C50.7898 (7)0.9028 (5)0.3529 (5)0.077 (3)
H50.81110.95210.36770.092*
C60.8355 (7)0.8687 (5)0.2821 (5)0.087 (3)
H60.88750.89570.24860.104*
C70.8046 (7)0.7948 (5)0.2607 (5)0.089 (3)
H70.83590.77150.21380.106*
C80.7259 (7)0.7569 (5)0.3115 (5)0.093 (3)
H80.70310.70750.29850.112*
C90.3961 (9)0.9529 (5)0.7307 (6)0.117 (4)
H90.32510.95980.70290.141*
C100.3963 (11)0.9325 (6)0.8136 (6)0.114 (4)
H100.32490.92600.84100.136*
C110.50000.9215 (9)0.8567 (13)0.176 (11)
H110.50000.90740.91230.211*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.0294 (4)0.0285 (3)0.0315 (3)0.0000.0000.0045 (4)
S10.0434 (13)0.0396 (12)0.0370 (11)0.0000.0000.0036 (9)
S20.0382 (12)0.0345 (11)0.0377 (11)0.0000.0000.0025 (9)
S30.0332 (8)0.0416 (8)0.0526 (9)0.0019 (7)0.0061 (7)0.0031 (7)
O10.051 (4)0.033 (3)0.037 (3)0.0000.0000.003 (3)
O20.050 (4)0.036 (3)0.042 (3)0.0000.0000.001 (3)
O30.060 (3)0.070 (3)0.049 (3)0.007 (3)0.012 (2)0.001 (2)
O40.045 (3)0.028 (3)0.041 (4)0.0000.0000.001 (3)
O50.053 (4)0.038 (3)0.035 (3)0.0000.0000.004 (3)
O60.044 (3)0.049 (3)0.063 (3)0.009 (2)0.007 (2)0.007 (2)
O70.037 (2)0.038 (2)0.051 (3)0.0002 (19)0.007 (2)0.0129 (19)
O80.037 (2)0.049 (2)0.048 (3)0.0043 (18)0.003 (2)0.012 (2)
O90.055 (3)0.065 (3)0.068 (3)0.009 (3)0.021 (3)0.004 (3)
O100.052 (3)0.066 (3)0.102 (4)0.016 (2)0.003 (3)0.027 (4)
O1w0.27 (2)0.170 (15)0.141 (15)0.0000.0000.009 (12)
N10.104 (7)0.044 (5)0.079 (6)0.0000.0000.001 (5)
N20.123 (7)0.079 (5)0.098 (5)0.020 (5)0.033 (5)0.009 (5)
N30.181 (11)0.165 (10)0.134 (10)0.0000.0000.020 (8)
C10.076 (6)0.069 (5)0.090 (6)0.017 (4)0.008 (5)0.004 (4)
C20.061 (5)0.066 (5)0.119 (6)0.006 (4)0.003 (5)0.010 (5)
C30.073 (7)0.051 (6)0.107 (8)0.0000.0000.007 (6)
C40.101 (6)0.077 (5)0.066 (5)0.006 (5)0.018 (5)0.011 (4)
C50.082 (6)0.064 (5)0.084 (6)0.012 (5)0.001 (5)0.009 (4)
C60.071 (5)0.106 (6)0.083 (6)0.021 (5)0.016 (5)0.030 (5)
C70.087 (6)0.101 (6)0.078 (5)0.005 (5)0.020 (5)0.026 (5)
C80.108 (7)0.065 (5)0.107 (7)0.020 (5)0.018 (6)0.019 (5)
C90.101 (7)0.125 (7)0.126 (8)0.008 (6)0.026 (7)0.034 (7)
C100.089 (7)0.138 (8)0.113 (7)0.015 (6)0.006 (6)0.019 (7)
C110.171 (13)0.176 (13)0.181 (14)0.0000.0000.005 (9)
Geometric parameters (Å, º) top
Zr1—O12.189 (6)N2—H2n0.8600
Zr1—O22.183 (6)N3—C9i1.362 (5)
Zr1—O42.220 (5)N3—C91.362 (5)
Zr1—O52.211 (6)N3—H3n0.8600
Zr1—O72.191 (4)C1—C21.375 (5)
Zr1—O7i2.191 (4)C1—H10.9300
Zr1—O82.180 (4)C2—C31.377 (5)
Zr1—O8i2.180 (4)C2—H20.9300
S1—O3i1.438 (5)C3—C2i1.377 (5)
S1—O31.438 (5)C3—H30.9300
S1—O21.521 (7)C4—C51.380 (5)
S1—O11.528 (7)C4—H40.9300
S2—O6i1.419 (4)C5—C61.388 (5)
S2—O61.419 (4)C5—H50.9300
S2—O51.512 (6)C6—C71.389 (5)
S2—O41.528 (6)C6—H60.9300
S3—O91.426 (5)C7—C81.381 (5)
S3—O101.443 (5)C7—H70.9300
S3—O81.504 (4)C8—H80.9300
S3—O71.509 (4)C9—C101.381 (5)
O1w—H1w0.85C9—H90.9300
N1—C11.335 (5)C10—C111.380 (5)
N1—C1i1.335 (5)C10—H100.9300
N1—H1n0.8600C11—C10i1.380 (5)
N2—C41.329 (5)C11—H110.9300
N2—C81.336 (5)
O1—Zr1—O263.8 (2)S1—O2—Zr199.0 (3)
O1—Zr1—O469.7 (2)S2—O4—Zr198.9 (3)
O1—Zr1—O5132.4 (2)S2—O5—Zr199.7 (3)
O1—Zr1—O7132.4 (2)S3—O7—Zr198.8 (2)
O1—Zr1—O7i132.4 (2)S3—O8—Zr199.4 (2)
O1—Zr1—O882.0 (1)C1—N1—C1i126.7 (10)
O1—Zr1—O8i82.0 (1)C1—N1—H1n116.7
O2—Zr1—O4133.6 (2)C1i—N1—H1n116.7
O2—Zr1—O5163.7 (2)C4—N2—C8122.5 (8)
O2—Zr1—O784.4 (2)C4—N2—H2n118.7
O2—Zr1—O7i84.4 (2)C8—N2—H2n118.7
O2—Zr1—O890.9 (1)C9i—N3—C9120.1 (17)
O2—Zr1—O8i90.9 (1)C9i—N3—H3n120.0
O4—Zr1—O562.7 (2)C9—N3—H3n120.0
O4—Zr1—O7130.3 (2)N1—C1—C2116.5 (8)
O4—Zr1—O7i130.3 (2)N1—C1—H1121.8
O4—Zr1—O882.6 (1)C2—C1—H1121.8
O4—Zr1—O8i82.6 (1)C1—C2—C3120.6 (9)
O5—Zr1—O782.5 (2)C1—C2—H2119.7
O5i—Zr1—O782.5 (2)C3—C2—H2119.7
O5—Zr1—O891.7 (1)C2i—C3—C2119.2 (11)
O5—Zr1—O8i91.7 (1)C2i—C3—H3120.4
O7—Zr1—O7i72.6 (2)C2—C3—H3120.4
O7—Zr1—O863.1 (2)N2—C4—C5120.4 (8)
O7—Zr1—O8i135.7 (2)N2—C4—H4119.8
O7i—Zr1—O8135.7 (2)C5—C4—H4119.8
O7i—Zr1—O8i63.1 (2)C4—C5—C6118.0 (8)
O8—Zr1—O8i161.2 (2)C4—C5—H5121.0
O3i—S1—O3114.7 (5)C6—C5—H5121.0
O3i—S1—O2110.9 (3)C5—C6—C7120.9 (8)
O3—S1—O2110.9 (3)C5—C6—H6119.6
O3i—S1—O1110.3 (3)C7—C6—H6119.6
O3—S1—O1110.3 (3)C8—C7—C6117.8 (8)
O2—S1—O198.6 (3)C8—C7—H7121.1
O6i—S2—O6114.0 (4)C6—C7—H7121.1
O6i—S2—O5111.5 (2)N2—C8—C7120.4 (8)
O6—S2—O5111.5 (2)N2—C8—H8119.8
O6i—S2—O4110.0 (3)C7—C8—H8119.8
O6—S2—O4110.0 (3)N3—C9—C10119.9 (14)
O5—S2—O498.7 (3)N3—C9—H9120.1
O9—S3—O10112.9 (3)C10—C9—H9120.1
O9—S3—O8111.5 (3)C11—C10—C9121.5 (16)
O10—S3—O8110.8 (4)C11—C10—H10119.2
O9—S3—O7112.1 (3)C9—C10—H10119.2
O10—S3—O7109.9 (3)C10—C11—C10i117 (2)
O8—S3—O798.7 (2)C10—C11—H11121.4
O8—S3—Zr149.16 (16)C10i—C11—H11121.4
S1—O1—Zr198.5 (3)
O3i—S1—O1—Zr1116.1 (3)O8—Zr1—O5—S280.75 (11)
O3—S1—O1—Zr1116.1 (3)O2—Zr1—O5—S2180.000 (3)
O2—S1—O1—Zr10.0O1—Zr1—O5—S20.000 (1)
O8i—Zr1—O1—S195.01 (12)O7i—Zr1—O5—S2143.32 (11)
O8—Zr1—O1—S195.01 (12)O7—Zr1—O5—S2143.32 (11)
O2—Zr1—O1—S10.0O4—Zr1—O5—S20.0
O7i—Zr1—O1—S153.4 (2)O9—S3—O7—Zr1119.2 (3)
O7—Zr1—O1—S153.4 (2)O10—S3—O7—Zr1114.4 (3)
O5—Zr1—O1—S1180.0O8—S3—O7—Zr11.6 (3)
O4—Zr1—O1—S1180.0O8i—Zr1—O7—S3178.3 (2)
O3i—S1—O2—Zr1115.7 (3)O8—Zr1—O7—S31.2 (2)
O3—S1—O2—Zr1115.7 (3)O2—Zr1—O7—S392.7 (2)
O1—S1—O2—Zr10.0O1—Zr1—O7—S346.4 (3)
O8i—Zr1—O2—S180.64 (11)O7i—Zr1—O7—S3178.57 (12)
O8—Zr1—O2—S180.64 (11)O5—Zr1—O7—S397.0 (2)
O1—Zr1—O2—S10.0O4—Zr1—O7—S352.8 (3)
O7i—Zr1—O2—S1143.47 (11)O9—S3—O8—Zr1119.6 (3)
O7—Zr1—O2—S1143.47 (11)O10—S3—O8—Zr1113.7 (3)
O5—Zr1—O2—S1180.000 (3)O7—S3—O8—Zr11.6 (3)
O4—Zr1—O2—S10.0O8i—Zr1—O8—S3177.7 (6)
O6i—S2—O4—Zr1116.8 (2)O2—Zr1—O8—S382.0 (3)
O6—S2—O4—Zr1116.8 (2)O1—Zr1—O8—S3145.4 (3)
O5—S2—O4—Zr10.0O7i—Zr1—O8—S30.9 (4)
O8i—Zr1—O4—S295.80 (12)O7—Zr1—O8—S31.2 (2)
O8—Zr1—O4—S295.80 (12)O5—Zr1—O8—S381.9 (3)
O2—Zr1—O4—S2180.000 (1)O4—Zr1—O8—S3144.1 (3)
O1—Zr1—O4—S2180.0N1—C1—C2—C30.0 (3)
O7i—Zr1—O4—S250.97 (18)C1—C2—C3—C2i0.1 (6)
O7—Zr1—O4—S250.97 (18)N2—C4—C5—C60.3 (3)
O5—Zr1—O4—S20.0C4—C5—C6—C70.8 (6)
O6i—S2—O5—Zr1115.6 (3)C5—C6—C7—C80.9 (8)
O6—S2—O5—Zr1115.6 (3)C4—N2—C8—C70.1 (7)
O4—S2—O5—Zr10.0C6—C7—C8—N20.4 (8)
O8i—Zr1—O5—S280.75 (11)C9—C10—C11—C10i0.5 (6)
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w···O10ii0.851.832.656 (9)162
N1—H1n···O70.862.232.965 (9)143
N1—H1n···O7i0.862.232.965 (9)143
N2—H2n···O40.861.992.801 (9)157
N3—H3n···O1w0.861.752.56 (2)156
Symmetry codes: (i) x+1, y, z; (ii) x1/2, y+1/2, z.
 

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